Cold-rolled complex-phase (CP) steel grades with optimised bendability, stretch-flangeability and anisotropy (CP-Steels)

Interested in European research?

RTD info is our quarterly magazine keeping you in touch with main developments (results, programmes, events, etc.). It is available in English, French and German. A free sample copy or free subscription can be obtained from: Directorate-General for Research and Innovation Information and Communication Unit European Commission 1049 Bruxelles/Brussel BELGIQUE/BELGI Fax +32 229-58220 E-mail: research@ec.europa.eu Internet: http://ec.europa.eu/research/rtdinfo.html

EUROPEAN COMMISSION Directorate-General for Research and Innovation Research Fund for Coal and Steel Unit Contact: RFCS publications Address: European Commission, CDMA 0/178, 1049 Bruxelles/Brussel, BELGIQUE/BELGI Fax +32 229-65987; e-mail: rtd-steel-coal@ec.europa.eu

European Commission

Research Fund for Coal and Steel

Cold-rolled complex-phase (CP) steel grades with optimised bendability, stretch-flangeability and anisotropy (CP-Steels)
L. Ryde
Swerea KIMAB Box 55970, SE-10216 Stockholm, SWEDEN

O. Lyytinen, P. Peura
Ruukki Metals Oy Harvialantie 420, 13300 Hmeenlinna, FINLAND

M. Titova
RWTH Department of Ferrous Metallurgy, Inzestrae 1, 52072 Aachen, GERMANY

Y. Vilander Granbom
SSAB EMEA SE-781 84 Borlnge, SWEDEN

T. Hebesberger
voestalpine Stahl Research & Development B3E, Materials Development, Voest-Alpine-Strae 3, Postfach 3, 4031 Linz, AUSTRIA

Contract No RFSR-CT-2006-00021 1 July 2006 to 30 June 2010

Final report

Directorate-General for Research and innovation

2012

EUR 25041 EN

LEGALNOTICE Neither the European Commission nor any person acting on behalf of the Commission is responsible for the use which might be made of the following information. .

Europe Direct is a service to help you find answers to your questions about the European Union Freephone number (*):

00 800 6 7 8 9 10 11
(*) Certain mobile telephone operators do not allow access to 00 800 numbers or these calls may be billed.

A great deal of additional information on the European Union is available on the Internet. It can be accessed through the Europa server (http://europa.eu). Cataloguing data can be found at the end of this publication. Luxembourg: Publications Office of the European Union, 2012 ISBN 978-92-79-22146-0 doi:10.2777/97678 ISSN 1831-9424 European Union, 2012 Reproduction is authorised provided the source is acknowledged. Printed in Luxembourg
Printed on white chlorine-free paper

Table of contents
1. FINAL SUMMARY ................................................................................................. 7
1.1 Main objectives............................................................................................................................................7

1.2 The work programme .................................................................................................................................7 1.2.1 CP-steels and selection of alloys ..............................................................................................................7 1.2.2 WP1 delivery of material ..........................................................................................................................7 1.2.3 WP2 transformation behaviour .................................................................................................................7 1.2.4 WP3 Laboratory annealing simulations to produce different microstructures ..........................................8 1.2.5 WP4 analysing properties and structures ..................................................................................................8 1.2.6 WP5 Industrial processing of optimised material and characterisation of the properties for the end user .....................................................................................................................................................9 1.2.7 WP6 Coordination and reports .................................................................................................................9 1.3 1.4 Conclusions ................................................................................................................................................10 Implementation of the research and transferability of results ..............................................................10

2. SCIENTIFIC AND TECHNICAL DESCRIPTION OF THE RESULTS ................. 11

2.1 2.2 Objectives of the project ...........................................................................................................................11 Comparison of initially planned activities and work accomplished .....................................................11

2.3 WP1 Processing / delivery of different steel grades ...............................................................................13 2.3.1 Objectives and tasks of WP1 ..................................................................................................................13 2.3.2 Description of activities and discussion of WP1 ....................................................................................13 2.3.2.1 Task 1.1 Delivery of fully industrially produced material from three processing routes ...............13 2.3.2.2 Task 1.2 Industrially as cold-rolled material ..................................................................................14 2.3.2.3 Task 1.3 Processing of material with different texture ..................................................................14 2.3.2.3.1 Industrially produced material with varying texture .................................................................17 2.3.2.3.2 Conclusions regarding texture and hole expansion from task 1.3 .............................................22 2.3.2.4 Task 1.4 Lab processed material ....................................................................................................22 2.3.2.5 Task 1.5 Characterisation of all the delivered materials. ...............................................................23 2.3.3 Conclusions from WP1, delivery of material .........................................................................................23 2.4 WP2 Transformation behaviour during annealing ...............................................................................25 2.4.1 Objectives and tasks of WP2 ..................................................................................................................25 2.4.2 Description of activities and discussion of WP2 ....................................................................................25 2.4.2.1 Task 2.1 Kinetics of the cementite dissolution and austenite formation in the two phase region and austenite range .........................................................................................................................25 2.4.2.1.1 Carbide dissolution and microstructure change during annealing ............................................26 2.4.2.1.2 Transformation of ferrite to austenite during heating and soaking. ..........................................27 2.4.2.2 Task 2.2 Transformation kinetics during cooling ..........................................................................30 2.4.2.2.1 CCT-diagrams for transformation kinetics during cooling .......................................................30 2.4.2.3 Task 2.4 Conclusions from transformation behaviour during annealing and cooling ....................34 2.5 WP3 - different microstructures ..............................................................................................................35 2.5.1 Objectives and tasks of WP3 ..................................................................................................................35 2.5.2 Description of activities and discussion of results in WP3 .....................................................................35 2.5.2.1 Task 3.1: Processing of different microstructures based on industrial as cold-rolled material ......35 2.5.2.2 Task 3.2: Processing of a wide range of special microstructures based on suggestions from WP 4 ..............................................................................................................................................37 2.5.2.3 Task 3.3 Processing of special microstructures based on suggestions from WP 4 ........................40 2.5.2.3.1 Annealing trials for a continuous annealing line with gas cooling, CAL-GQ ..........................40 2.5.2.3.2 Annealing trials for a continuous annealing with water quenching, CAL-WQ: .......................42 2.5.2.3.3 Annealing trials for a hot dip galvanizing line, HDG ...............................................................43

2.6 WP4 - the relation between microstructure and formability ................................................................45 2.6.1 Objectives and tasks of WP4 ..................................................................................................................45 2.6.2 Task 4.1 Formability and Task 4.2 - Microstructures ..........................................................................45 2.6.2.1 Formability and tensile testing .......................................................................................................45 2.6.2.2 Characterisation of microstructure and texture ..............................................................................46 2.6.2.3 Properties and microstructures of the industrial material, Task 1.1 ...............................................46 2.6.2.4 Properties and microstructures of samples from task 1.4 - Laboratory produced material ............47 2.6.2.5 Properties and microstructures of samples from task 3.1 - Initial laboratory annealing simulations .....................................................................................................................................48 2.6.2.6 Properties and microstructures of samples from task 3.2 a wide range of microstructures.........51 2.6.2.7 Properties and microstructures of samples from task 3.3 special microstructures from dedicated lab annealing ..................................................................................................................56 2.6.2.8 Properties of the samples from task 5.1 - industrial trials ..............................................................59 2.6.3 Task 4.3 Characterisation of the failure mechanism on pre-strained industrially produced materials....61 2.6.3.1.1 Fracture analyses on the fractured hole expansion specimens ..................................................61 2.6.3.1.2 Analysis of the microstructure beneath the punched edge surface after HE testing .................62 2.6.4 Task 4.4 Critical evaluation and correlation of the formability, microstructure including texture and the detected failure mechanism, conclusions of WP4 ......................................................................63 2.7 WP 5: Semi-industrial/industrial processing of optimised material .....................................................69 2.7.1 Objectives and tasks of WP5, industrial processing of optimised material ............................................69 2.7.2 Task 5.1 Processing of material with optimised microstructure on industrial scale ...............................69 2.7.2.1 Initial trials of HDG at Ruukki.......................................................................................................69 2.7.2.2 Final on line trials of HDG at Ruukki ............................................................................................70 2.7.2.3 Previous trials of CAL-WQ at SSAB.............................................................................................73 2.7.2.3.1 Annealing simulation using dilatometry at KIMAB .................................................................73 2.7.2.3.2 Annealing simulation at voestalpine .........................................................................................74 2.7.2.4 On line trials for CAL-WQ at SSAB .............................................................................................74 2.7.2.4.1 Summary of on line trials of CAL-WQ at SSAB ......................................................................75 2.7.2.5 Final on line trials of CAL-GQ at voestalpine ...............................................................................75 2.7.3 Task 5.2 Critical evaluation of the results from WP4 .............................................................................77 2.7.4 Task 5.3 Critical comparison of the objectives of the project and the results obtained in the project ....79 2.7.5 Task 5.4 Basic characterisation of the formability based on forming limit diagrams .............................81 2.7.6 Task 5.5 impact of the strain rate and temperature on the mechanical properties samples from industrial trials ........................................................................................................................................85 2.7.6.1 Tensile testing, room temperature and at -40C and 100C ...........................................................85 2.7.6.2 Dynamic tensile tests .....................................................................................................................86 2.7.7 Task 5.6 impact of the strain state on mechanical properties .................................................................86 2.7.8 Task 5.8 constitutive modelling and determination of the parameters relevant for the selected CP grades ................................................................................................................................................88 2.8 2.9 Conclusions ................................................................................................................................................91 Exploitation and impact of the research results .....................................................................................93

3. LIST OF FIGURES, TABLES, ACRONYMS AND ABBREVIATIONS ................ 94

3.1 3.2 3.3 List of Figures ............................................................................................................................................94 List of tables...............................................................................................................................................97 List of acronyms and abbreviations ........................................................................................................98

4. LIST OF REFERENCES ...................................................................................... 99 5. APPENDICES.................................................................................................... 100

5.1 5.2 Appendix 1 All included steels per task and annealing simulation schedules ...................................100 Appendix 2 Results from Industrially produced material with varying texture, task 1.3. ...............103

5.3 5.4 5.5 5.6 5.7

Appendix 3 Results from initial laboratory simulations, task 3.1 .......................................................103 Appendix 4 Results from laboratory simulations of a wide range of microstructures, task 3.2 ......104 Appendix 5 Results from laboratory simulations of dedicated microstructures, task 3.3 ................105 Appendix 6 Results from final on line trials, task 5.1 ..........................................................................106 Appendix 7 Results from final on line trials; Effect of strain rate and temperature, task 5.5 .........106

1. 1.1

FINAL SUMMARY MAIN OBJECTIVES

The over all goal of this project was to identify microstructures with optimised balance between strength, bendability and stretch-flangeability and to develop guidelines of how to produce this cold rolled sheet steel through three processing routes, i.e. continuous annealing with gas cooling, continuous annealing with quenching and the third route is hot dip galvanizing. The objectives were to produce material via the three routes with the following properties; A tensile strength of more than 800MPa, a hole expansion ratio (HE) of more than 35%, a bending angle, Ri/t<1. The final objective was to characterise the produced materials for the end user with e.g. forming limit diagrams and flow curves. All the main objectives have been fulfilled. 1.2 1.2.1 THE WORK PROGRAMME CP-steels and selection of alloys

From a scientific and technical point of view, advanced high strength steel grades and especially CP grades are very interesting and challenging. By adjusting the chemical composition, the hot- and coldrolling parameters and particularly the annealing parameters, a remarkable variation of microstructures and textures can be produced. The selected chemical composition range for this project is presented in Table 1. Table 1. %C 0.05-0.20 1.2.2 Selected range for alloy composition %Si %Mn %Cr+%Mo <0.5 1.2-2.5 <1

%Ti+%Nb <0.15

%Fe Bal

WP1 delivery of material

Work package 1 (WP1) dealt with processing and delivery of different steel grades. Some laboratory materials were also included to be able to vary parameters, e.g. chemical composition and texture, more widely than was possible from current industrial production. Industrially produced materials were delivered as a start, 10 different grades after annealing a reference point and 3 grades in a cold rolled state for further laboratory annealing simulations. During the course of the project more steels have been added and in total have 18 different alloy compositions been used in this project, see also appendix 1 in chapter 5.1. Laboratory heats and additional full scale coils were also produced for the final trials in line. 1.2.3 WP2 transformation behaviour Transformation behaviour during annealing were analysed in WP2. This WP was used to find processing windows (chemical composition, time and temperature) to produce the desired balance between selected phases in the microstructure. The main work was performed using dilatometry and a Gleeble and analysing the microstructures in SEM and TEM. Calculations of the transformation behaviour during heating, soaking and cooling based on thermodynamic (ThermoCalc) and kinetic (Dictra) modelling has been made, but the outcome of the kinetic calculations have not shown very useful and are extracted from this final report. The reason for this is that the necessary assumptions of the allowed diffusion distances influence the result to such a dramatic extent that the predictions were of no practical use; a small change in diffusion distances, based on microstructural observations, would change the predicted dissolutions time from too short to too long, compared to those used in the annealing lines. The calculations were able to predict that the more alloyed steels were likely to need longer soaking times for dissolution compared to the leaner, but this was also found in the laboratory studies. Therefore, it was better to rely on the laboratory simulations and limit further use of Dictra calculations. The results showed that carbide dissolution kinetics will control the rate of the phase transformation if the annealing temperature is low or the soaking time is short. The kinetics varies with the chemical composition of the steel and it was shown that a Cr-addition will slow down the dissolution rate. A phase transformation close to equilibrium was usually achieved at a soaking time of 80s or more, although much of the phase transformation is done during the heating, before the actual annealing temperature is reached. 7

The CCT diagrams determined show very different behaviour for the investigated steels. It seems that the additions of slowly diffusing elements (Mn, Mo and Cr) have a stronger impact on the transformation kinetics than C. The maximum continuous cooling rate used in the dilatometry investigations was 285C/s. This was enough to describe the transformation behaviour in a CAL (continuous annealing line) and HDG (hot dip galvanizing) line, with gas quenching, but too low of a cooling rate for a CAL with water quenching. 1.2.4 WP3 Laboratory annealing simulations to produce different microstructures WP3 of this project was concerned with producing different microstructures based on WP 1, 2 and 4. The objectives of this work package has been to narrow the processing parameters in three steps to optimise the required properties. This meant producing sheet material in industrial production and laboratory in quantities large enough to be able to analyse the forming properties in WP4. For all simulations the same cold rolled material was used, see Table 2. Table 2.
Material V1-CR R4-CR S7-CR

Chemical analysis, laboratory annealing

Grade Supplier Voest Ruukki SSAB Gauge [mm] 1.50 1.2 1.23 C 0.11 0.14 0.135 Mn 2.1 1.7 1.5 Si 0.15 0.18 0.5 Cr 0 0.3 Mo 0.2 0.15 Nb 0.02 0.015

[wt%] [wt%] [wt%] [wt%] [wt%] [wt%]

VA CP800-Mo CP800-1 TS 800

1.2.5

WP4 analysing properties and structures

In work package 4 (WP4) the relation between microstructure and formability was studied which included analysis of tensile behaviour, hole expansion and bendability. The main delivery from this WP was basic know-how of the impact of the microstructure on the formability and fracture behaviour. This work has also been performed stepwise when new material has been delivered from WP3. The first demand on the material was to obtain enough strength, i.e. Rm>800MPa and when this was achieved the next property to optimise was the hole expansion or the bending behaviour, depending on which was the poorest. The experimental findings for the investigated materials allow the following hypothesis to be established regarding stretch-flangeability: Cleanliness of the steels is an important factor and was not intended to vary within the frame of this project and thus will not be considered here. The strength/hardness difference between the matrix phases in the microstructure must not be high. This mechanical homogeneity prevents local hot-spots of stress and/or strain in the microstructure especially at phase boundaries which act as nucleation sites for voids. Several possibilities have been tried to reach this goal for CP-grades: Reducing the grain size of the hard martensite Replacing hard martensite by softer tempered martensite or bainite. Increasing the strength of the matrix by grain size reduction, other strengthening mechanisms (solution or precipitation hardening) and /or the introduction of more bainite. Reducing the amount of soft ferrite The experimental findings for the investigated materials regarding bending is not as obvious as for hole expansion but the best results were achieved with the following principles: Reducing the grain size of all constituents in the microstructure. Reduce the hardness difference between different phases Replacing hard martensite and/or soft ferrite by bainite or tempered martensite. Ferrite is not poor for bending but the required strength level will not be reached if too much ferrite is present at the same time as martensite is avoided. The experimental finding for nearly fully martensitic DP-grades TS1200M with 96.5% of tempered martensite have also established that the homogeneous microstructure of this material provides high strength and good hole expansion level, although the tensile elongation is low, and that this steel shows better HE than a dual phase microstructure with ferrite and martensite. 8

Our results indicate that optimum crystallographic texture also can provide additional improvements in the forming properties, but this was considered more difficult than manipulating the phase constituents and was not considered in the final trials. It was shown that the best texture was achieved annealing in the austenite-ferrite region, a processing condition that will be difficult to use in HDG or CAL-GQ. These processes normally use full austenitisation to achieve a bainitic transformation during the isothermal holding section. Without complete transformation during annealing it is likely that the yield strength level will be too low without more additions of alloying elements. Another possibility to improve the texture is to increase the cold rolling reduction, and this was shown in laboratory trials but could not be tested in full scale. The obtained variations in crystallographic texture have been very small in all experiments except for the specific tests performed under task 1.3. Our findings have resulted in selected processing conditions for the industrial trials presented inWP5. 1.2.6 WP5 Industrial processing of optimised material and characterisation of the properties for the end user

Semi-industrial / industrial processing of optimised material and characterisation of the material for the end user was the task for work package 5 (WP5). This included, besides the production of the material, characterisation of the formability, mechanical properties as a function of strain rate and temperature and constitutive equations and flow curves. The required properties from the initial project objectives; Rm>800MPa, Ri/t<1 and HE>35% have all been met for all three production lines although the microstructures are different. Complex phase microstructures with bainite, martensite, ferrite and retained austenite were produced in the CAL-GQ and HDG but it was particularly difficult to produce a bainitic microstructure in the continuously annealing line with water quenching. This microstructure was more of a dual phase type. By comparing the forming limit diagrams of the initially delivered industrially produced steels and the steels from the final industrial trials based on the results of this project, it is possible to draw some conclusions of other forming properties: Improved biaxial balanced stretch forming, plane strain and stretch-flangeability has been achieved for the steels produced through a hot dip galvanizing line and continuous annealing with gas section (steels R and V). This improvement is a result of a reduction of the size of the martensite grains, elimination of the soft ferrite phase and by replacing of hard martensite by tempered martensite or bainite. The continuously annealed and water quenched industrially produced materials have (steels S), however, better biaxial balanced stretch forming, plane strain, stretch-flangeability and uniaxial tensile properties in comparison with the results from the final industrial trails, due to a more homogeneous microstructure and smaller martensite grain size. The project has resulted in a new product for SSAB, a LCE1000, which has a leaner chemical composition compared to DP1000, improved hole expansion due to less difference between the phase constituents and better weldability due to lower carbon equivalent. 1.2.7 WP6 Coordination and reports Co-ordination and reports (WP6) was taken care of by the co-ordinator KIMAB. The project was delayed and granted an extension with one extra year. The reason for this was twofold: The tasks of WP3 and WP4 could not run in parallel with WP2, as was intended in the initial plan, since the transformation kinetics were needed to set up the laboratory trials The financial crisis during 2008-2009 made all on line trials impossible at that time. All reports were delivered on time

1.3

CONCLUSIONS

The following conclusions can be drawn from the work performed in this project: General conclusions: The project objectives have been met; improving the properties of steel products from three different annealing lines to obtain a tensile strength of >800MPa, bending radii <1 and hole expansion ratio>35% A new steel, SSABs LCE1000, has been the outcome of this project together with adjustments of the existing process parameters and compositions for the CP-steels with Rm 800MPa at Rautaruukki and voestalpine The properties and microstructures are not identical between the three products so there is still room for improvement It is very difficult to obtain a bainitic structure in the CAL-WQ process due to the lack of intermediate temperature holding zones. About microstructure, texture and hole expansion (stretch-flangeability) or bending: The strength/hardness difference between the matrix phases in the microstructure must not be high. This mechanical homogeneity prevents local hot-spots of stress and/or strain in the microstructure especially at phase boundaries which act as nucleation sites for voids. Several possibilities have been tried to reach this goal for CP-grades: Reducing the grain size of the hard martensite Replacing hard martensite by softer tempered martensite or bainite. Increasing the strength of the matrix by grain size reduction, other strengthening mechanisms (solution or precipitation hardening) and /or the introduction of more bainite. Reducing the amount of soft ferrite The experimental findings regarding bending is not as obvious as for hole expansion but the best results were achieved with the following principles: Reducing the grain size of all constituents in the microstructure. Reduce the hardness difference between different phases Replacing hard martensite and/or soft ferrite by bainite or tempered martensite. Ferrite is not poor for bending but the required strength level will not be reached if too much ferrite is present at the same time as martensite is avoided. The texture investigation implies that a strong {111}-texture should be beneficial for the hole expansion properties. IMPLEMENTATION OF THE RESEARCH AND TRANSFERABILITY OF RESULTS

1.4

One of the major goals of this project has been to develop guidelines of how to produce the material, by an appropriate alloy design, and well-adjusted processing parameters through several processing routes, i.e. continuous annealing and hot dip galvanizing, which should make the results transferable throughout Europe. This has been successful in the lines available in this project and since the main three commercial annealing processes are covered, the results of this project will be able to benefit not only the three industrial partners of this consortium, but many other steel producers in Europe. Only minor adjustments are intended in each type of facility to produce advanced high-strength CP material. Another objective was to characterise the material for the end user, which will aid the user to use the full potential of the high strength material. This has been made through FLDs and flow curves of all the new steels and are presented in the chapter on WP5 and in the appendices.

10

2. 2.1

SCIENTIFIC AND TECHNICAL DESCRIPTION OF THE RESULTS OBJECTIVES OF THE PROJECT

This project has dealt with the relationship between microstructure and formability of cold-rolled complex-phase steels. The over all goal of this project was to identify microstructures with optimised balance between strength, bendability and stretch-flangeability and to develop guidelines of how to produce these cold rolled sheet steel through three processing routes, i.e. continuous annealing with gas cooling, continuous annealing with quenching and the third route was hot dip galvanizing. The objectives were: To achieve an improved strength-formability balance with particular focus on bendability, stretch-flangeability and deep-drawing capacity. A tensile strength of more than 800MPa, a hole expansion ratio (HE) of more than 35%, a bending angle, Ri/t<1 were the targets. To develop guidelines of how to produce the material, by an appropriate alloy design, and well-adjusted processing parameters. To produce these steels, with the above mentioned properties, through different available processing routes, i.e. continuous annealing lines with either water or gas quenching facilities, or hot dip galvanizing lines. To characterise the material for the end user including constitutive equations for the performance of the material. 2.2 COMPARISON OF INITIALLY PLANNED ACTIVITIES AND WORK ACCOMPLISHED

The principle of this project has been to produce a wide variety of microstructures to shed light on the impact of the CP steel microstructure on formability and the project plan of this project has included six work packages with the following sequence: 1. Work package 1 (WP1) dealt with processing and delivery of different steel grades. Some laboratory materials were also included to be able to vary parameters, e.g. chemical composition and texture, more widely than is possible from current industrial production. 2. Transformation behaviour during annealing were analysed in WP2. This WP was very important to find processing windows (chemical composition, time and temperature) to produce the desired balance between selected phases in the microstructure. The main work was performed using dilatometry and analysing the microstructures in SEM and TEM, but an effort was also made to use ThermoCalc and Dictra. 3. Work package 3 (WP3): Material with different microstructures was produced, i.e. sheet material in industrial production and laboratory in quantities and sizes large enough to be able to analyse the forming properties in WP4. 4. In work package 4 (WP4) the relation between microstructure, including texture, and formability was studied which included analysis of mechanical properties, bendability and stretch-flangeability. 5. Semi-industrial / industrial processing of optimised material and characterisation of the material for the end user was the task for work package 5 (WP5). This included, besides the production of the material, characterisation of the formability, mechanical properties as a function of strain rate and temperature and constitutive equations and material parameters. 6. Evaluation, co-ordination and reports were the tasks for (WP6). WP3 and WP4 were looped three times to narrow the processing parameters before the final annealing trials on industrial scale in WP5. The project has encountered a few problems during the course of the project: It has not been possible to find a laboratory cold rolling mill that was strong enough to deform sheets with a width of more than 100mm to more than 70% reduction. The size needed for annealing in voestalpines annealing simulator is 450x250mm and the reduced width created problems for their staff during annealing and at RWTH for tensile testing and hole expansion tests. Consequently, the task 1.3 (processing of materials with different texture) in WP1 was delayed and it was decided to exclude cold rolling reductions above 70% for the mechanical and forming tests. This made the number of samples

11

with a large variation in texture too small to make any texture modelling; however, there are some indications of the effect on the properties from our laboratory trials. The delay in WP1 caused another delay in WP3, which in turn resulted in a delay in the tasks of WP4 (microstructure vs. properties) and WP5 (industrial processing) since these were depending on results from WP3 (laboratory simulations) and WP4 (microstructure vs. properties). It was impossible to define a project plan before these WPs were finished in order to perform the relevant final annealing trials and produce the materials on an industrial scale. The project also encountered problems to run industrial trials due to the financial crisis during 2009 but was gratefully granted an extension with one year which enabled the project to be successfully finished. Apart from these problems, the project has been running smoothly and all the project objectives have been met in the final industrial annealing trials.

12

2.3 2.3.1

WP1 PROCESSING / DELIVERY OF DIFFERENT STEEL GRADES Objectives and tasks of WP1

WP1 deals with processing and delivery of different steel grades. Some laboratory materials are also included to be able to vary parameters, e.g. processing parameters and texture, more widely than is possible from current industrial production. The objectives were the same as the tasks of this work package and were divided into 5 tasks listed in Table 3 below. Table 3. Tasks of WP1 Task 1.1 Delivery of fully industrially produced material from three processing routes Task 1.2 Industrially as cold-rolled material Task 1.3 Task 1.4 Task 1.5 2.3.2 2.3.2.1 Processing of material with different texture Lab processed material Characterisation of all the delivered materials.

voestalpine, SSAB, Ruukki Ruukki, SSAB, voestalpine KIMAB, SSAB voestalpine Ruukki, SSAB, voestalpine

Description of activities and discussion of WP1 Task 1.1 Delivery of fully industrially produced material from three processing routes

The following materials has been selected from the shelf, see Table 4. All have a tensile strength of more than 800MPa. Table 4.
Material R1 R2 R3 V1 V2 S1 S2 S3 S4 S5

Selected materials, (wt%)

Supplier Gauge Ruukki Ruukki Ruukki voest voest SSAB SSAB SSAB SSAB SSAB 1.20 2.50 1.20 1.50 1.50 1.50 1.80 1.00 1.60 1.65 C 0.17 0.17 0.17 0.11 0.14 Mn Si Cr Mo Nb Rp0.2 Rm A80 [MPa] [MPa] [%] 626 574 568 0.02 0.02 0.018 720 620 640 855 846 836 920 790 840 1140 1030 1220 1200 16 14 14 11 16 15 6 8 4 5 Rp0.2/ Rm 0.73 0.68 0.68 0.78 0.78 0.76 0.93 0.91 0.98 0.81

1.7 0.18 0.3 0.15 1.7 0.18 0.3 0.15 1.7 0.18 0.3 0.16 2.1 0.15 2.1 0 0.2 0 0.2 0.3

0.144 1.52 0.48 0.172 1.59 0.51 0.170 1.63 0.47 0.178 1.41 0.44 0.135 1.53 0.18

0.017 1060 0.017 940

0.016 1190 0.015 970

A description and motivation for the selected steels are given below: Rautaruukki has chosen one steel grade for the starting point of complex phase (CP) -steel development, a hot dip galvanized LITEC 800DPF. The steel grade represents the complex phase steels of Rautaruukki at the time for the start of the project. Rautaruukki has processed and delivered two gauges of this CP800-steel grade: thicknesses 1.20 and 2.50 mm, R1 and R2. The material was analysed and tested at Ruukki, KIMAB and RWTH. The two gauges of CP800 are produced via different galvanizing lines i.e. they have the same alloy design, but have different annealing cycle. The composition is shown in Table 4. The same material and thickness has also been processed and delivered in a cold-rolled state (task 1.2). This has been used for laboratory annealing and dilatometry simulations at the University of Oulu (subcontractor of Ruukki) and at voestalpine (only 1.20 mm thickness). These materials were used for adjusting different microstructures in laboratory annealing simulators in order to obtain optimal properties for CP-steels. Based on the

13

transformation characteristics found in WP2, Rautaruukki developed a new coil that was included as industrial material for further tests, the R3. This development will be described later in the report. voestalpine has selected two CP-grades with a minimum tensile strength of 800MPa. The chemical compositions of these two grades are given in Table 4. Generally, CP-grades have a complex microstructure consisting of bainite, martensite, tempered martensite, and minor polygonal ferrite. In comparison to DP-grades, such a microstructure is characterised by a high yield ratio and a lower uniform and total elongation in the tensile test. However, CP-grades show excellent bendability and stretch-flangeability. One main task for producing such microstructures is to suppress or at least minimise the formation of polygonal ferrite. Molybdenum is very effective in avoiding the formation of polygonal ferrite and therefore it is often found in CP-grades (V1, VA_CP800_Mo). However, molybdenum has also its disadvantages as it increases the hot rolling forces significantly and it is also quite expensive. The second steel grade (V2, VA_CP800) is a try to compensate molybdenum with chromium and higher carbon content. Four different steel grades of a DP-type have been chosen for the project by SSAB, see Table 4. These grades have a tensile strength between 800 and 1200 MPa after continuous annealing. For a tensile strength of 1000 MPa, two coils with different thickness have been processed. For a tensile strength of 1200 MPa, two coils with different properties have been processed. One is a fully martensitic steel and the other has 10 to 15 % second phase. Below, in Table 5, you find the annealing temperatures for the chosen steel grades. Table 5. Annealing temperatures Material Grade Thickness [mm] S1 TS 800 1.50 S2 S3 S4 S5 TS 1000-1 TS 1000-2 TS 1200 (M) TS 1200 (DP) 1.80 1.00 1.60 1.65

Annealing temperature [C] 760 810 790 850 850

Overageing temperature [C] 400 400 400 400 200

2.3.2.2

Task 1.2 Industrially as cold-rolled material

The industrially as cold rolled materials selected are all aiming for the same strength level, with a tensile strength of more than 800 MPa. These were the steels used in most laboratory simulations, see Table 6. The only exception is the final task 3.3 where new steels were added. Those steels are described in the chapter 2.5.2.3. Table 6. Chemical composition of the industrially cold rolled materials (wt%) Material Grade Supplier Gauge C Mn Si Cr Mo [mm] V1-CR VA CP800-Mo voest 1.50 0.11 2.1 0.15 0 0.2 R4-CR CP800-1 Ruukki 1.2 0.14 1.7 0.18 0.3 0.15 S7-CR TS 800 SSAB 1.23 0.135 1.5 0.5

Nb 0.02 0.015

2.3.2.3

Task 1.3 Processing of material with different texture

Task 1.3 includes the processing of material with different texture both in laboratory and in the continuous annealing line by KIMAB and SSAB. voestalpine has assisted with annealing larger pieces for mechanical properties and RWTH did hole expansion testing on those. The variations in texture were obtained through variations in the rolling schedule and coiling temperature, see Table 7. 14

Table 7. Task 1.3 Texture programme, chemical composition, coiling and cold reduction Grade Material Supplier Gauge C Mn Si Nb Condition (mm) (%) (%) (%) (%) S6 TS 800 SSAB 1.5 0.13 1.51 0.21 0.015 Contin. An. S1-HR TS 800 LAB SSAB 3.47 0.144 1.52 0.48 0.018 Hot rolled Grade S6-A S6-B1, S6-B2 S6-C S1-Tex1 S1-Tex2 S1-Tex3 S1-Tex4 S1-Tex5 Material TS 800-CT1 TS 800-CT2 TS 800-CT3 TS 800 LAB Coiling temperature [C] 515 600 660 600 Cold rolling [%] 56% 56%, 69% 56% 50%, 60%, 70%, (77%, 84%)

The first three grades are industrially processed by SSAB and their properties and structures will be discussed in the following chapter. The laboratory material was delivered after hot rolling and coiling and was cold rolled to different reductions in the laboratory. The highest cold rolling reductions, i.e. more than 70%, was not possible to achieve in the available semi sized laboratory cold rolling mill for the widths necessary for forming tests and further attempts to find an alternative mill was not successful in the available time frame. The highest reductions, 77% and 84%, were only achieved on samples too narrow to be tested for hole expansion or tensile testing. Initial annealing simulations of small pieces for texture analysis and microstructure characterisation have been performed on samples between 50% reduction and 84% in a quenching dilatometer. Based on the results from these tests, larger samples were then annealed in voestalpines annealing simulator with principally the same annealing schedules. The purpose of the laboratory tests was to find heating routes to vary the strength of the crystallographic textures while maintaining the martensite content at approximately 20-25% and thereby the required strength level. The performed annealing schedules are shown in Figure 1. The annealing simulation was made in a Bhr 805 Dilatometer to ensure that the time-temperature schedule was controlled with high accuracy. The dilatometry tests results in rather small samples, fit only for texture and microstructure analysis.
1000 900 800 700 quenching austenitised

Temperature, C

600 500 400 300 200 100 0 0 100 200 300 400 500 600

Time, s

Figure 1.

Two temperature schedules were selected; one with annealing in the two phase region and one in the austenite region

15

The annealing schedules were selected to simulate continuous annealing to produce a dual phase steel with a strength level of approximately 800 MPa through: 1. 2. annealing in the ferrite-austenite region and natural cooling in the gasjet section before quenching at a relatively high temperature, above AC1 completely austenitise the material and then cool down with gas to a low temperature to allow for ferrite to transform and then quench to maintain approximately 25% martensite.

The overageing temperature was selected deliberately high, 350C, to be able to analyse the martensite texture with EBSD. A change in the overageing temperature is not expected to alter the texture or martensite content unless much higher temperatures are applied than are used here. In the larger samples, annealed by voestalpine, this is corrected for to achieve a correct strength. For the intercritical anneal, called quenching the overageing temperature was set to 200C and for the austenitising schedule the top temperature was increased to 900C to ensure complete phase transformation. For the latter an overageing temperature of 400C was selected. The textures of the investigated samples shown as ODF sections with 2=45 are found in Figure 2. The texture is weaker if the material is annealed above AR3 (labelled austenitised) compared to in the two phase region (AR1). The texture is also weaker at lower cold rolling reductions, as expected. Another notable feature in the crystallographic textures of the samples annealed in the two phase region (labelled quench) is the strong -fibre, particularly in the 50% cold rolled material. This indicates that there may be unrecrystallised regions in the material. For deep drawing, a strong -fibre is beneficial and a strong -fibre is detrimental, but it is not certain how the texture will affect other forming properties. The relationship between deep drawing and texture is well established for single phase material but it is likely that multi phase material will behave somewhat different and these results show a promising range of textures to test this.

Austenitised 50%CR

Austenitised 60%CR

Austenitised 70%CR

Austenitised 77%CR

Austenitised 84%CR

Quench 50%CR Figure 2.

Quench 60%CR

Quench 70%CR

Quench 77%CR

Quench 84%CR

The texture is weaker if the material is annealed in the austenite region or if the cold rolling reduction is reduced. ODF sections with 2=45

The microstructure of four samples (50% and 70% cold rolling and austenitised and quenched respectively) has been studied with EBSD to analyse the approximate amount of martensite and the results are shown in Figure 3. The level of martensite after annealing in the austenite region is measured to minimum 22% and maximum 28%, which is promising in order to achieve the correct strength level. However, the investigate area is rather small, so the results may be somewhat uncertain. The suspicion of partly recrystallised structured as indicated previously from the crystallographic texture showed to be correct; the EBSD mapping of the 50% cold rolled sample annealed in the two phase region showed 30% unrecrystallised grains. There was no evidence of unrecrystallised areas in the 70% cold rolled sample.

16

Austenitised 50%CR, 22% martensite

Austenitised 70%CR, 27% martensite

Quench 50%CR, 25% martensite (black), Quench 70%CR, 25% unrecrystallised structure(red) 28% martensite Figure 3. The microstructure is showing approximately the same level of martensite (here in dark grey or black) and there are unrecrystallised structures in the sample with 50% cold rolling and annealed in the two phase region

Figure 4.

Hole expansion ratio of annealed SSAB-materials with different textures

The results of the hole expansion tests, see Figure 4, show that with an increase in the cold rolling reduction the hole expansion value increases. The hole expansion values of SSAB-grades, which have been annealed in the two phase region, are a little higher than the hole expansion of the samples which have been annealed in the austenitic range. This is an indication that the same textures that are favourable for deep drawing may also be beneficial for a high hole expansion value, i.e. a strong {111}ND texture is preferable. It is however, necessary to point out that the samples have different thickness due to the different cold rolling levels and that this also has an influence on the forming properties. In comparison with the industrially produced TS800, the hole expansion values are substantially better for the laboratory samples, 48% as minimum for the 50% cold rolled material annealed in the two phase region, whereas the industrially produced had a hole expansion ratio of 35%. 2.3.2.3.1 Industrially produced material with varying texture SSAB provided material with different textures through variation of coiling temperature after hot rolling and cold rolling reduction as described in Table 7.

17

The mechanical behaviour of the different TS800 texture materials were investigated both in the as hot rolled condition and after cold rolling and annealing, i.e. the finished DP-product. For the as hot rolled materials, the true stress-true strain curves are presented in Figure 5 and the values of the yield and tensile strength and elongation in Table 8 and micrographs of the structures (optical micrographs) are shown in Figure 6. As can be seen from graphs and tables, an additional coiling temperature of 470C is included. This material was only added for comparison here and is not tested for hole expansion.
800

700 Stress [MPa]

600

500 C.T. 470 C C.T. 515 C C.T. 600 C C.T. 660 C 0.02 0.04 0.06 0.08 0.10 Strain [mm] 0.12 0.14 0.16

400

300 0.00

Figure 5.

True stress-true strain of the as hot rolled materials.

From the curves above we see that the lower the coiling temperature the higher the yield strength. We also achieve a pronounced Lders strain for the higher coiling temperature as well as a larger fracture elongation. The differences are pronounced. Table 8. C.T. [C] 660 600 515 470 As hot rolled condition: YS [MPa] 444/442 513/520 574/572 585/590

TS [MPa] 551/550 615/616 667/665 680/679

A80 [%] 24/23 16/14 14/8* 11/11

*) Fracture outside the gauge length

The microstructures of the texture materials in the as hot rolled condition are presented in Figure 6. A more homogenous microstructure is achieved when the material is coiled at lower temperatures. Higher coiling temperatures (660C and 600C) result in a banded structure where the dark bands consist of pearlite. The structure of the lower coiling temperatures is best described as bainitic.

C.T. 660 C

C.T. 600C

C.T. 515C

C.T. 470 C

Figure 6.

Microstructure of the as hot rolled materials.

18

After cold rolling and annealing, the difference in mechanical properties is smaller; see Figure 7 and Table 9. The sheet with the lowest coiling temperatures (470C and 515C) exhibit higher yield and tensile properties than the ones with the higher (660C and 600C) coiling temperatures.
1000 900 800 700 600 500 400 0 0.02 0.04 0.06 Strain [mm/mm] 0.08 0.1 0.12

Stress [MPa]

C.T. 660 C C.T. 600 C C.T. 515 C C.T. 470 C

Figure 7. Table 9. C.T. [C] 660 600 515 470

True stress-true strain of the cold rolled and annealed samples. Mechanical properties of the finished products (DP-steels) YS [MPa] TS [MPa] 552/553 854/857 553/549 839/839 578/571 882/877 566/567 873/874

A80 [%] 16/14 13/14 15/13 13/14

The microstructure after cold rolling and annealing seem to be reversed in fineness and banding compared to the hot rolled structures; Coiling at temperatures above 600C seems to result in the smallest and the most homogenous ferrite grain size, as well as the most finely dispersed martensite particles, see the micrographs in Figure 8.

C.T 660 C

C.T 600 C

C.T 515 C

C.T 470 C

Figure 8.

Microstructure of the DP texture materials after cold rolling and annealing.

An explanation to this behaviour may be found in the effect of Nb. The precipitation of Nb-carbides is known to be most efficient around 600C, and may be incomplete at lower. It is likely that higher coiling temperatures will allow the particles to grow somewhat. Besides varying the coiling temperature, the cold rolling reduction was also varied; a TS800 strip was subjected to two cold rolling reductions; one at low reduction (L.R. 56%) and one with high reduction (H.R. 69%). Looking at the true stress-true strain curves presented in Figure 9, there does not seem to be a significant difference in mechanical properties after annealing as a result of the different rolling reductions.

19

900 800

Engineering stress [MPa]

700 600 500 400 300 0.0% H.R. L.R.

5.0%

10.0% Engineering strain

15.0%

20.0%

Figure 9.

True stress strain curves for the high and low cold rolling reduction

However, high cold rolling reduction does seem to give the highest uniform elongation and fracture elongation and a slightly higher deformation hardening rate (n-value).

CRR H.R. L.R.

Table 10. Comparison of tensile data for high and low cold rolling reduction YS [MPa] TS [MPa] A80 [%] n (4-8%) 489/490 780/782 17/17 0.15/0.15 534/534 822/822 15/13 0.11/0.11

High cold rolling reduction yields a higher driving force for recrystallisation and more nucleation sites for austenite formation upon phase transformation during annealing. A high cold rolling reduction should thus result in a smaller ferrite grain size and and smaller and more homogenously distributed martensite phase, which also is confirmed in the micrographs in Figure 10. Since the finer structure is not reflected in the yield strength, and the strength is actually slightly lower, it has to be explained by either; a smaller volume of martensite, softer martensite or harder ferrite, but this cannot be confirmed from the observed microstructures.

Figure 10.

Microstructure of TS800 with low (LR) and high (HR) cold rolling reduction.

The textures of the industrially produced materials are shown in Figure 11. The -fibre of the crystallographic texture varies only slightly with the coiling temperature except that the highest coiling temperature shows a very weak -fibre and strong -fibre. This result is somewhat uncertain since it is measured on the head of a tensile test sample. The effect of higher cold rolling reduction, increased from 56% to 69%, results in a switch from {111}<1-10>towards {111}<11-2> which was also found in the laboratory tests, see Figure 2. The increase in texture strength with higher reduction is, however, not found here and the -fiber, particularly the {001}<110> is much stronger compared to the lower deformation. This indicates that the material is is not completely recrystallised and that, although the two coils were subjected to the same annealing code, it is possible that the temperature was somewhat lower

20

for the coil with the higher cold rolling reduction. A higher reduction should increase the driving force for recrystallisation, which is why only a shorter annealing or a lower temperature could explain the results.

CR CR 56%, CT 515C 56%, CT 600C CR 56%, CT 660C

Figure 11.

CR 69%, CT 600C The crystallographic texture of the industrially produced coils with varying texture. ODF sections with 2=45

EBSD confirmed that there were deformed areas in the microstructure of the 69% cold rolled material and only recrystallised grains with the typical -fibre orientation in the material that was cold rolled 56% prior to annealing, see Figure 12. The orientations are coloured relative to the end orientation of the -fibre, {001}<110> and allowing 7 spread. Grains with an orientation that deviates more than 7 are grey.

a) Deviation from {001}<110> Figure 12.

b) EBSD maps of the a) 56% cold rolled and b) 69% cold rolled steel. Coiling temperature after hot rolling of 600C. The orientations are coloured relative to the end orientation of the -fibre, {001}<110>.

Tensile data and hole expansion results are also shown in appendix 2, chapter 5.1.The results from the hole expansion tests of the industrially produced textured material are shown in Figure 13. The best hole expansion value was found for material coiled at 600C and cold rolled to 56%. This material showed a hole expansion value of 51% and this result is much better than the industrially produced TS800, that only had 35%. The main difference between these two materials seems to be a 100MPa lower yield stress for the new coil (CT600C-CR56%), which may explain the better hole expansion. The explanation for the poor result of the higher cold rolling (69%) is probably that the unrecrystallised

21

regions, which were found with EBSD, will reduce the forming properties. The poor result for the material with the high coiling temperature, CT 660C, is probably also caused by unrecrystallised remaining areas, as indicated by the strong -fibre in the texture. The pronounced banding may also decrease the HE results.

Figure 13.

Hole expansion tests of the various cold rolling reductions and coiling temperatures

2.3.2.3.2 Conclusions regarding texture and hole expansion from task 1.3 The conclusions from the textured materials are that: A strong {111}-ND texture seems to be beneficial to obtain a high hole expansion ratio. This texture is also known to result in high r-values. The best production route to achieve a strong {111}-ND texture and is to use a coiling temperature around 600C, as high cold rolling reduction as possible, anneal the material in the two phase region BUT ensure that the material is completely recrystallised. 2.3.2.4 Task 1.4 Lab processed material

For the processing of different microstructures based on lab processed material, Rautaruukki studied the effect of microalloying on the structure and mechanical properties of CP-steel. At the same time the possibility of reducing the amount of Mo was studied. Two laboratory heats, Ru-4 and Ru-5, were prepared with 0,015 wt% Nb additions without or with Mo (Table 11). Table 11. Chemical compositions of the investigated steels in wt%. Material C Si Mn Cr Mo Nb Ru-1 (normal CP800) 0.17 0.18 1.7 0.3 0.15 Ru-4 Ru-5 0.17 0.17 0.18 0.18 1.7 1.7 0.3 0.3 0.15 0.015 0.015

The heats were cast by using a vacuum induction furnace. After cooling, the ingots were wrapped in stainless steel foil heated to 1200C and held for 24 hours for homogenizing. After removing the scale and cutting the ingots to suitable sizes the pieces were reheated in Argon shielding gas to 1240C for one hour and hot rolled. The finish rolling temperature was 750 - 800C and samples were cooled down (at 1-2C/s) to a temperature of 500 - 600C, where they were held to simulate coiling. After this, the samples were cold rolled with 50 % reduction. The cold rolled samples were heat treated according to various temperature schedules in a Gleeble 1500 simulator to simulate the galvanizing line. The annealing and holding zone temperatures were varied. Two tests were carried out for each simulation cycle. One was used for testing the RT-tensile properties and the other specimen for microstructure analysis employing the LePera's etchant, see chapter 2.6.2.4 in WP4.

22

2.3.2.5

Task 1.5 Characterisation of all the delivered materials.

The microstructure analysis resulted in the following phases in the respective material, see Table 12. An additional coil was also included from Ruukki; this coil was produced based on the phase transformation results under WP2 and should belong to the tasks under WP3 (Processing of material with different microstructure and texture) but is included here since both the microstructure and properties of the industrial materials are compared here. Table 12. Phase\Material Thickness, mm Ferrite(F) Martensite(M) Tempered Martensite(TM) Carbide free Bainite(CfB) Bainite (B) Rm, [MPa] Ri/t HE [%] 2.3.3 Summary of the phase constituents (%) and properties of the different industrially produced steels R1 R2 R3 S1 S2 S3 S4 S5 V1 V2 1.2 2.5 1.25 1.5 1.8 1 1.6 1.65 1.5 1.5 37.0 37.0 15 76 20 30 3.5 14 42 36 13.0 13.0 12.0 4 7 2.6 42.0 5.4 855 1.2 19 2.6 42.0 5.4 846 3 17 29 44 820 1.2 56 840 0.7 35 1140 3.5 30 1030 1 71 1220 3.5 44 1200 1 40 24 80 70 96.5 86 15 27 12 920 3 47 790 1.7 58 57

Conclusions from WP1, delivery of material

All included industrial materials have tensile strengths above 800 MPa which is the target of this project. It is clear that this strength level can be obtained through a large variation in phase constituents which allows for freedom to design a suitable microstructure for the required properties It seems that the bending properties need to be improved to meet the required level, except for a few of these steels. The best bending properties are found for the continuously annealed and quenched steels, whereas the bending properties of the CP-structures after hot dip galvanizing or continuously annealed with gas cooling, needs to be better. The claimed good hole expansion for a complex phase structure is found for the steels of voestalpine, however the first steels delivered by Ruukki, with a CP-structure, showed poor HE. The explanation for this lies in the high amount of soft ferrite in combination with a large fraction of untempered martensite. Since the hot dip galvanizing line does not allow any overageing, tempering of the martensite is not realistic and the hardness difference between the phases must be reduced by removing the soft ferrite. In the third material that Ruukki included, much of the soft ferrite is replaced by bainite, and the HE-value is dramatically enhanced. The improved forming properties are likely to be related to the more homogeneous structure, and the reduced difference in hardness between the phases. The hole expansion values of the steels with very high levels of martensite also strengthens this theory. These HE values are around 40%, which implies that strength alone does not deteriorate the hole expansion, but rather the difference in hardness between soft and hard phases, and good HE can be achieved when the fraction of the hard phase is large enough to make it continuous. Furthermore, the hole expansion value does not only depend on the phase fraction of material, but also on the thickness of the sheets. The thicker TS1000-1 shows a much poorer HE than TS1000-2, even though the phase constituents are nearly the same. The steels from Ruukki are also delivered in two gauges, 1.25mm and 2.5mm respectively, but the thickness effect is not obvious here, since the HE values are very poor for both steels for other reasons discussed earlier. The texture investigation implies that a strong {111}-texture should be beneficial for the hole expansion properties. Very promising results were obtained in the laboratory tests by modifying the chemical composition using Nb microalloying. Some additional study is still needed, in order to reduce the amount of Mo.

23

2.4 2.4.1

WP2 TRANSFORMATION BEHAVIOUR DURING ANNEALING Objectives and tasks of WP2

Transformation behaviour during annealing was analysed in order to find processing windows, i.e. chemical composition, time and temperatures, to produce the desired balance between selected phases in the microstructure. The main work was performed using interrupted annealing trials, dilatometry and ThermoCalc calculations and by analysing the microstructures in SEM and TEM. Dictra calculations were also used but with limited usefulness. The objectives were the same as the tasks and the work was divided into four tasks, see Table 13: Table 13. Tasks of WP2 Task 2.1 Kinetics of the cementite dissolution and austenite formation in the two phase region and austenite range Task 2.2 Transformation kinetics during cooling Task 2.3 Task 2.4 Calculation of the transformation behaviour during heating, soaking and cooling Delivery of know-how

KIMAB, voestalpine, Ruukki Ruukki, voestalpine KIMAB, voestalpine KIMAB, voestalpine, Ruukki

Task 2.1: Kinetics of the cementite dissolution and austenite formation in the two phase region and austenite range has been investigated for three steels by interrupted annealing trials and dilatometric investigations and microstructure investigations. Task 2.2: Transformation kinetics during cooling has been studied for the same three steels with a Gleeble and CCT diagrams for these are presented in the report. The microstructures of the samples were also compared with the Gleeble results. Task 2.3: Calculation of the transformation behaviour during heating, soaking and cooling based on thermodynamic (ThermoCalc) and kinetic (Dictra) modelling has been made, but the outcome of the kinetic calculations have not shown very useful and are extracted from this final report. The reason for this is that the necessary assumptions of the allowed diffusion distances influence the result to such a dramatic extent that the predictions were of no practical use; a small change in diffusion distances, based on microstructural observations, would change the predicted dissolutions time from too short to too long, compared to those used in the annealing lines. The calculations were able to predict that the more alloyed steels were likely to need longer soaking times for dissolution compared to the leaner, but this was also found in the laboratory studies. Therefore, it was better to rely on the laboratory simulations and limit further use of Dictra calculations. The results from Tasks 1 and 2 are more valuable in determining new processing parameters for modifying the microstructure. Equilibrium calculations by ThermoCalc are helpful in identifying differences in transformation temperatures, but since only a few of the studied annealing processes reach equilibrium and have high heating and cooling rates, this can only be used as a rough estimate. The used calculations are indicated in the graphs of task 2.1. Task 2.4: delivery of know-how is the summary of all results in WP1.

2.4.2 2.4.2.1

Description of activities and discussion of WP2 Task 2.1 Kinetics of the cementite dissolution and austenite formation in the two phase region and austenite range

The formation of austenite is of fundamental interest for CP grades, as bainite, martensite, and tempered martensite typical constituents of a CP microstructure are products of the transformation from austenite during cooling. Therefore, experiments on the annealing simulator and in the dilatometer were done by voestalpine. Three industrially produced grades were investigated. The basic difference between the three compositions is the alloying levels of C, Mn and Mo, even though small fractions of Cr (Ruukki) and Nb are also present in (SSAB and voestalpine) the steels. The chemical compositions of the grades are given in Table 14.

25

Table 14. Chemical composition of the industrially produced CP-grades (wt%) Material Supplier C Mn Cr Mo Si V1 S7 R4 voestalpine SSAB Ruukki 0.11 0.14 0.16 2.1 1.5 1.75 0 0 0.3 0.2 0 0.15 0.15 0.2 0.18

Nb 0.02 0.015 0

The materials were heat treated with different parameters for time and temperature. The annealing temperature (Tan) varied from 760C to 840C, the heating rate (HR) varied from 1/s to 80/s, and the holding time at (tan) was changed from 0 seconds to 80 seconds. After simulating the different time temperature cycles, the microstructure and the mechanical properties of the samples were investigated with optical microscopy and tensile testing. Carbide dissolution with FEG SEM was also studied after either etching with Picral (picric acid in ethanol) or in light electrolytic etch (3 V-10 s) in Chromium-acid (water solution of CrO3 ). 2.4.2.1.1 Carbide dissolution and microstructure change during annealing The basic raw material was available as cold rolled (V1, S7, R4) and as hot rolled (V1, R4 only) In the Ruukki and SSAB materials the carbide phase appeared in the cold rolled condition in long pearlitic areas that were 100m long or more, but only one m or a few m wide. The distance between these areas were somewhere between a few m and over 10m. Within these areas the carbide particles occurred as plates with thickness around 0.1m or rounded with diameters from 0.1- 0.25m. The voestalpine cold rolled material differed somewhat from the previous two. The pearlite area length was from 50- 100m and the width from few m to 10m. There were also more rounded carbides, with diameters from 0.25m to 1 m. An example of the microstructure of the studied materials as cold rolled and as heat treated is shown in Figure 14. The two etching techniques used are also illustrated.

a) Figure 14.

b) In a) an example of cold rolled Ruukki material and in b) after annealing, HR=20/s, Tan=760C, tan=0s. In a) Picral was used as etchant and the carbides appear white. In b) Cr-acid was used as etchant and carbides appear black.

Complete carbide dissolution is a prerequisite for the full utilization of the alloying elements strengthening potential. This is not only since carbon is the most important alloying element but also because other important elements may be locked in the carbides; e.g. it is found that carbides are enriched with Mn, the second most important alloying element. The rate of carbide dissolution varies between the three steels, where the fastest to dissolve its carbides is the steel from voestalpine. The slowest dissolution is shown in the steel from Ruukki, probably due to the Cr-content of this material. The results show that carbide dissolution rate may be the factor that controls the amount of austenite during the annealing if the soaking time is short or if the temperature is not high enough.

26

A summary of the results from the carbide dissolution analysis is shown in Figure 15 for the heating rate of 20C/s, which is selected since this is the most relevant heating rate for the industrial annealing schedules involved. Complete dissolution of carbides is achieved at the indicated dotted lines.

Figure 15.

Dissolution time of carbides at different temperatures for the three steels, V1, R4 and S7 (voestalpine, Ruukki and SSAB).

2.4.2.1.2 Transformation of ferrite to austenite during heating and soaking. Austenite formation was studied using dilatometry and microstructure studies. Dilatometry produced the phase transformation curves and microstructure studies of the annealing simulator samples revealed the amount of martensite in the steel, see Figure 16. The data presented here were collected from 0s and 80s of annealing at various temperatures, i.e. quenched immediately after reaching the desired temperature or after a hold that corresponds to a normal annealing time in an industrial line. The heating rate up to the selected temperatures was 20 C/s. The austenite fractions from dilatometry data, the martensite fractions from the annealing simulations and phase equilibrium calculated with ThermoCalc for various annealing temperatures at annealing times of 0s and 80s respectively for the three steels are compared in Figure 17. A large fraction of austenite is already present immediately after heating up to the soaking temperature and thus transform during heating. The results also shows that 80s of annealing is usually very close to equilibrium for all the investigated steels. There is a slight discrepancy between the results from the carbide dissolution studies and these data since both the steel from Ruukki and SSAB seem to be closer to equilibrium than the steel from voestalpine, whereas the carbide dissolution study showed the Ruukki steel to be the slowest to dissolve. It is however, possible that shorter annealing times would have given a different result. In some of the graphs it seems that the volume fraction of austenite (or martensite) is higher than equilibrium, which of course is impossible, but this is due to the precision when evaluating dilatometry curves or optical micrographs of these fine structures. An example of the changes in microstructure is shown in Figure 16, along with the tensile strength as a function of the annealing temperature and time.

27

HR_20K/s; t an _ 0s

T an= 760 C

T an = 780 C

Tan= 800 C

Tan= 820 C

T an= 840 C

1015 MPa

1092 MPa

1106 MPa
Rolling Direction

1178 MPa

1293 MPa

HR_20K/s; t an _ 80s

T an= 760 C

T an= 780 C

Tan= 800 C

Tan= 820 C

Tan= 840 C

1162 MPa

1214 MPa

1293 MPa

1343 MPa

1340 MPa

Figure 16.

An example of the microstructure and tensile strength of the voestalpine grade as a function of the annealing time (0s and 80s) and annealing temperature (760C 840C)

28

Figure 17.

A Comparison between ThermoCalc calculations and results from dilatometry and microstructures after annealing simulations show that 80s of annealing is usually very close to equilibrium for all the investigated steel.

29

2.4.2.2

Task 2.2 Transformation kinetics during cooling

For the investigation of transformation kinetics during cooling the same three steel grades were selected as in the previous tasks. The chemical composition of the three steels is given in Table 14. In the tests the effect of process temperatures on the mechanical properties and microstructure was studied and CCT-diagrams were produced from the dilatometry data. 2.4.2.2.1 CCT-diagrams for transformation kinetics during cooling CCT diagrams were determined using the data acquired from the dilatation measurements using a Gleeble 1500 simulator at University of Oulu. The specimens were heated at 20C/s to 860C (austenitic range), held for 40s prior to cooling at different rates. The target range for the cooling rates was from 1C/s to 300-400C/s. For cooling rates of 100C/s, specimens were thinned to achieve the desired cooling rates. The cooling rates of greatest interest from the point of view of development of CP steels were quite different depending on the steel composition in question. The variety of different cooling rates was included in order to achieve more complete CCT diagrams. Higher cooling rates beyond about 250C/s were not easily accessible on the Gleeble simulator, even for the thinned specimens. Samples can be thinned only to a certain level, until thinning will lead to a disturbingly large slipping and/or tilting of the C-strain gauge. Austenite decomposition into ferrite, bainite, martensite or a mixture of these phases can be ascertained by the inflexion point in the shape of the dilatation curves. The effect of cooling rate and the reheating (annealing) temperature on the phase transformation characteristics is clearly revealed in the dilatation curves. 2.4.2.2.1.1 CCT diagram for the SSAB steel, S7 The CCT diagram of SSAB steel is presented in Figure 18, which shows a large ferrite phase field (As/Af) extending over at least until 200C/s, beyond which it is possible to achieve bainite and/or martensite by continuous cooling at 285C/s. It is possible that a very small fraction of high C martensite (M2) forms at lower temperatures, owing to C-enrichment of remaining austenite following nearly complete ferrite transformation at higher temperatures. Even though C content is about 0.14% in this steel, but in the absence of B and any strong austenite stabilizer except 1.5%Mn, the steel has shown poor hardenability until at least a cooling rate of 100C/s. Reheating at a different annealing temperature at 780C and cooling at 20C/s (broken cooling curve in Figure 18) did not show any significant effect on the phase transformation temperatures.
1000 900 800 700 600 500 400 300 M2 200 100 0 1 10 Time, s 100 1000 F+B F

1C/s 5C/s 20C/s 50C/s 75C/s 100C/s 200C/s 285C/s As Af/Bf M2 20C/s_RH780C As_RH780C Af_RH780C

Temperature, C

Figure 18.

CCT diagram for the SSAB steel, S7

30

2.4.2.2.1.2 CCT diagram for the voestalpine steel, V1 The CCT diagram for the voestalpine steel is shown in Figure 19. It also revealed a large ferrite field, but a bainite nose appeared beyond about 50C/s cooling rate suggesting the possibility of achieving bainite and/or martensite beyond this cooling rate and nearly complete martensite beyond about 100C/s by continuous cooling. This steel showed relatively higher hardenability obviously due to the presence of Mo (0.2%) and higher Mn content (2.17%), despite the fact that C content was lowest (about 0.11%), if compared with that of other steels (Table 14). Mo is known to delay ferrite formation, though it is a strong carbide and/or ferrite former. As a result, the ferrite nose appears at about 50C/s cooling rate, even though higher Mn too has a strong effect. Both Mn and Mo are known to delay bainite formation as well [6] and hence, move the bainite nose to right, so that it is possible to get completely displacive transformation of austenite to martensite by continuous cooling at rates over 100C/s. Both the start (Ms) and end (Mf) of martensite temperatures could be easily identified from the dilatation curves and the Ms temperature is quite close to that predicted by equations given by Stuhlmann [7]. At lower cooling rates, it is possible to achieve a very small fraction of high Cmartensite (M2) as revealed by the inflexion in the dilatation curves and shown in the CCT diagram. Changing the annealing temperature from 860C to 780C prior to continuous cooling at 20C/s did not, however, show any marked difference, even though the austenite fractions and their C contents can be slightly different at the two reheating (annealing) temperatures. It is noteworthy that both the steels from SSAB and VA have a small fraction of Nb, which is also expected to increase the hardness and improve the hardenability, provided the cooling rate and composition are such that polygonal ferrite is not formed during cooling [8]. However, the data here is not adequate to explain the effect of Nb in these CCT diagrams and also, the boron-alloyed steels used by Somani et al. [8] were somewhat different, essentially meant for direct quenching.

1000 900 800 700 600 B 500 400 300 200 100 0 1 10 Time, s 100 1000 M M2 F

1C/s 5C/s 20C/s 50C/s 75C/s 100C/s 200C/s 285C/s As Af Bs Bf Ms Mf M2 20C/s_RH780C As_RH780C M2_RH780C

Temperature, C

Figure 19.

CCT diagram for the voestalpine steel, V1

2.4.2.2.1.3 CCT diagram for the Ruukki steel, R4 The CCT diagram for the Ruukki Steel is shown in Figure 20. The phase transformation behaviour in this steel was somewhat between the two steels from SSAB and voestalpine. Even though the ferrite phase field is large and nearly similar as seen in the CCT diagram of voestalpine steel (Figure 19), the bainite nose has extended beyond about 285C/s, thus depicting the fact that bainite will be obtained in addition to martensite (fractions depending on cooling rate) by continuous cooling at all cooling rates between 50-285C/s. It is expected that nearly complete martensite can be achieved by fast cooling

31

beyond about 300C/s, even though there are no data to show that. The Ms and Mf temperatures can be conveniently computed from the inflexion in the dilatation curves and the prediction from Stuhlmanns equation [7] for Ms temperature is also close to those achieved here at different cooling rates, although the C content can significantly vary owing to the formation of different fractions of bainite prior to the formation of martensite. There appears to be a bay between ferrite and bainite phase fields extending between 1-20C/s cooling rates. Inflexion in the curves at very low temperatures at 1-5C/s cooling rates suggest formation of a very small fraction of M2 martensite, but needs to be checked by microscopy more closely. There seems to be some effect of reheating temperature at 780C, instead of 860C normally used for all the experiments here. The ferrite transformation temperature is not very different (720C), but bainite start (Bs) temperature is relatively lower by about 50 and no martensite could be achieved. Presence of a very small fraction of M2 martensite cannot be ruled out, as marked in the CCT diagram. Even though the steel from Ruukki has relatively higher C (0.16%C), it showed relatively lower hardenability compared to that of voestalpine steel (0.11%C) with the bainite nose extending to very high cooling rates up to at least 285C/s, possibly due to somewhat lower Mn and Mo contents and absence of Nb, although there is a small fraction of Cr (0.3%) in Ruukkis steel. C, Mn, Nb, Cr and Mo are all known to retard the bainite formation [6], but their individual effects are not easy to ascertain or compute and also, the prior thermal history including the cooling rate can strongly influence the transformation characteristics.
1000 900 800 700 600 B 500 400 300 200 100 0 1 10 Time, s 100 1000 M M2 F 1C/s 5C/s 20C/s 50C/s 75C/s 100C/s 200C/s 285C/s As Af Bs Bf Ms Mf M2 20C/s_RH780C As_RH780C Bs_RH780C Bf_RH780C M2_RH780C

Temperature, C

Figure 20.

CCT diagrams for the Ruukki Steel, R4.

2.4.2.2.1.4 Correlation between microstructure and CCT-diagrams for all steels Selected specimens from the dilatation curves were examined for microstructures by optical microscopy to correlate to the CCT diagrams (Figure 21-Figure 24). The specimens were etched with LePera to reveal the distinction between martensite, bainite and ferrite phases. Microstructures of samples annealed in the austenitic region (860C) with different cooling rates (1, 20, 100 and 200C/s) are shown in Figure 21 for the SSAB steel grade, in Figure 22 for the steel grade of voestalpine and in Figure 23 for the steel grade of Ruukki. Microstructures of all the three steel grades annealed in the intercritical temperature (780C) for 40 seconds and cooled 20C/s are shown in Figure 24.

32

a) Figure 21.

b) c) d) Microstructures of the SSAB steel S7, temperature 860C, cooling rate a) 1C/s b) 20C/s c) 100C/s d) 200C/s, holding time 40s, heating rate 20C/s, etched with LePera.

The microstructure of the steel grade from SSAB was quite coarse and banded with lower cooling rates and a fine microstructure was only achieved with the highest cooling rates. The coarse grain structure was probably due to the lack of Mo in alloying combined with relatively high C content. The microstructure of CP-steel of voestalpine was the finest of all the three CP-steels for all the cooling rates. The microstructure refinement was most likely due to alloying elements Mo and Nb [9].

a) Figure 22.

d) b) c) Microstructures of the voestalpine steel V1, temperature 860C, cooling rate a) 1C/s b) 20C/s c) 100C/s d) 200C/s s, holding time 40s, heating rate 20C/s, etched with LePera

The microstructure of the steel of Ruukki was somewhere in the middle of the two other steels grades: banded with the low cooling rate (1 C/s) and finer with the higher cooling rates which is probably due to the effect of Mo on the microstructure refinement.

a) Figure 23.

b) c) d) Microstructures of the Ruukki steel R4, temperature 860C, cooling rate a) 1C/s b) 20C/s c) 100C/s d) 200C/s s, holding time 40s, heating rate 20C/s, etched with LePera

The microstructures resulting from the intercritical annealing differed somewhat from the other results, see Figure 24. The steel grade of Ruukki seemed most banded, but the difference between the steel grades was quite small. The steel grade of Ruukki has the highest C content and quite high Mn content, so the banded structure could be a result of segregation of these elements. All the microstructures from the intercritical annealing seemed to be only partly recrystallised.

33

a) Figure 24.

b) c) Microstructures of CP800 of a) SSAB b) voestalpine and c) Ruukki, temperature 780C, cooling rate 20C/s, holding time 40s, heating rate 20C/s, etched with LePera

2.4.2.3

Task 2.4 Conclusions from transformation behaviour during annealing and cooling

The carbide dissolution kinetics will control the rate of the phase transformation if the annealing temperature is low or the soaking time is short. The kinetics varies with the chemical composition of the steel and it was shown that a Cr-addition will slow down the dissolution rate. A phase transformation close to equilibrium was usually achieved at a soaking time of 80 s or more, although much of the phase transformation is done during the heating, before the actual annealing temperature is reached. The CCT diagrams, determined in the dilatometry investigations, show very different transformation behaviour for the investigated steels. It seems that the additions of slowly diffusing elements (Mn, Mo and Cr) have a stronger impact on the transformation kinetics than C. The maximum continuous cooling rate used in the dilatometry investigations was 285C/s. This was enough to describe the transformation behaviour in a CAL (continuous annealing line) and HDG (hot dip galvanizing) line, with gas quenching, but too low of a cooling rate for a CAL with water quenching. According to the dilatometry investigations, the steel from SSAB has the poorest hardenability, due to its lean alloy composition. It requires cooling rates of more than 285C/s to transform to martensite and/or bainite. The steel from voestalpine has the highest hardenability of the three investigated steels. This is due to the high Mn-content and the Mo-addition. Bainite can be achieved at cooling rates between 50C/s and 100C/s and the material will transform to martensite at rates over 100C/s. The steel from Ruukki has an intermediate hardenability. Full martensite transformation will only be achieved at rates above 285C/s, but bainite is formed between 50C/s and 285C/s. The hardenability can be explained by the chemical composition of the Ruukki steel, which is leaner, compared to the steel from voestalpine, although the Cr-content may be responsible for the extended bainite field.

34

2.5 2.5.1

WP3 - DIFFERENT MICROSTRUCTURES Objectives and tasks of WP3

WP3 of this project was concerned with producing different microstructures based on WP 1, 2 and 4. WP3 consists of task 3.1, 3.2, and 3.3 (Table 15). The objectives of this work package has been to narrow the processing parameters in three steps to optimise the required properties. Details on the annealing simulations are found in appendix 1. Table 15. Tasks of WP3 Task 3.1 Processing of different microstructures and textures based on industrial as cold-rolled material or lab processed material Task 3.2 Processing of a wide range of special microstructures and textures based on suggestions from WP 4 Task 3.3 Based on the work in WP 4 and WP2 microstructures and textures resulting in particular excellent formability will be produced 2.5.2 Description of activities and discussion of results in WP3

Ruukki and voestalpine

Ruukki and voestalpine Ruukki and voestalpine

As described previously, WP 3 consisted of three loops of annealing simulations in order to narrow the processing parameters stepwise. For all simulations the same cold rolled material was used, see Table 16. Table 16. Chemical analysis, laboratory annealing Material Grade Supplier Gauge C Mn [mm] V1-CR VA CP800-Mo voest 1.50 0.11 2.1 R4-CR CP800-1 Ruukki 1.2 0.14 1.7 S7-CR TS 800 SSAB 1.23 0.135 1.5 2.5.2.1

Si 0.15 0.18 0.5

Cr 0 0.3

Mo 0.2 0.15

Nb 0.02 0.015

Task 3.1: Processing of different microstructures based on industrial as coldrolled material

The first laboratory annealing performed in the annealing simulator were the following for the different annealing cycles and steels, see Figure 25 to Figure 27. These were selected in order to investigate the effect of varying processing parameters for each individual line. It was made using the steel of each individual partner; i.e. the V1 steel was used for the CAL with gas quenching, the R4 steel was used for the hot dip galvanizing simulation and the S7 was used for the CAL process with water quenching. The schedule for a continuous annealing line with gas quenching is shown in Figure 25. The parameters that can be adjusted in this process are the temperature of annealing (Tan), the quenching temperature (TQ) and temperature of overageing (TOA). It is also possible to adjust the times during the process but this is done by changing the line speed and will affect all other parameters, which is true for all three investigated processes. In this project we were interested in producing a product with a complex phase microstructure which includes different variants of bainite. The selected parameters were therefore: annealing in the fully austenitic range, gas quenching from one selected temperature, and finally overageing at different temperatures. The main part of the phase transformation from austenite to bainite is supposed to happen during the overageing stage, if ferrite formation during cooling can be avoided. The CCT diagram of the V1 steel, see Figure 19, indicates that the cooling rate must be more than 50C/s and that the martensite start temperature is approximately 420C. The overageing temperatures selected lies between 300C and 500C, see Figure 25, to produce various bainites with different amounts of martensite. Some ferrite is normally formed during the cooling stages, which enriches the austenite in carbon, which in turn decrease the Ms temperature. It is therefore not expected that any of the selected schedules would produce a fully martensitic microstructure. The schedule for the annealing stage of a continuous annealing line with water quenching is shown in Figure 26. There is also a section with overageing in the line but that was not considered in this initial experiment. The parameters that were adjusted in this experiment are the temperature of annealing (Tan)

35

and the quenching temperature (TQ). The CCT diagram of this steel, see Figure 18, indicate that bainite formation is very difficult to achieve. A wide range of annealing temperatures, both in the intercritical range and fully austenitic, followed by very different quenching temperatures were selected to evaluate the possibilities. The selected schedules for the hot dip galvanizing process, see Figure 27, were focused annealing temperature, since the CCT diagram, see Figure 20, indicated that annealing in the intercritical range would change the transformation kinetics, and on the overageing time, i.e. the time that is needed for the bainitic transformation.

Cycle 1 2 3 4 5

Tan [C] 830 830 830 830 830

TQ [C] 700 700 700 700 700

TOA [C] 500 450 400 350 300

Figure 25.

Schematic time-temperature cycle of the lab anneals simulating a continuous annealing line with gas quenching for steel V1. T2 T3 CR1 T4 [C] [C] [C/s] [C] 6 760 780 -2.5 730 7 740 760 -2.5 710 8 780 800 -20 400 9 820 840 -8 680 10 820 840 -22 400 Schematic time-temperature cycle of the lab anneals simulating a continuous annealing line with water quenching for steel S7. Cycle

Figure 26.

Cycle 11 12 13 14 15

Tan [C] 830 830 780 780 805

TQ [C] 720 720 700 700 710

toa [s] 48 95 48 95 95

Figure 27. Schematic time-temperature cycle of the hot dip galvanizing laboratory cycles for steel R4

The mechanical properties and the hole expansion (HE) values achieved in the first laboratory annealed samples are presented in Table 17.

36

Table 17. Properties of the first laboratory annealed samples Material Cycle Gauge Rp0.2 Rm Ag [mm] [MPa] [MPa] [%] V1 1 1.52 509 898 8.3 V1 2 1.52 411 766 12.7 V1 3 1.51 437 597 13.0 V1 4 1.52 466 806 10.2 V1 5 1.53 478 851 9.1 S7 S7 S7 S7 S7 R4 R4 R4 R4 R4 6 7 8 9 10 11 12 13 14 15 1.24 1.23 1.23 1.23 1.23 1.19 1.18 1.18 1.18 1.18 576 541 463 685 388 530 529 438 422 498 1143 1116 959 1078 790 812 801 821 807 801 4.9 7.5 12.0 2.3 16.2 9.3 8.3 8.1 7.1 7.3

A80 [%] 11.7 18.0 18.3 14.5 12.2 5.6 8.7 14.5 3.5 21.8 13.3 11.2 11.6 10.3 11.1

HE [%] 49 64 73 71 55 16 14 18 10 29 59 60 36 32 64

2.5.2.2

Task 3.2: Processing of a wide range of special microstructures based on suggestions from WP 4

In Task 3.2 ten different time-temperature schedules were tested by voestalpine in the annealing simulator, with the aim to produce various combinations of different phases in the microstructure. The same three materials, which were used in previous annealing simulations, were selected (Table 16). These ten annealing cycles are presented in Figure 28-Figure 30. The performed simulations of a continuous annealing line with water quenching and separate overageing is shown in Figure 28 . Annealing both in the austenite region as well as in the intercritical range was performed and various overageing temperatures were investigated. Figure 29 shows how the simulations of a continuous annealing line with water quenching, soft cooling in the gas jet section and overageing was made. Annealing was performed only in the austenite region and the overageing temperatures were set to 200C. Figure 30 illustrates the simulations of a continuous annealing line with gas quenching or hot dip galvanizing line. Annealing was performed in the austenite region and various overageing temperatures were tested. The detailed analysis of the annealed samples can be found in WP4. A short summery of the results of this analysis is depicted in Table 18. The best combination of HE values and bending properties were found for cycle 9; which consists of annealing in the fully austenitic region at 880C, gas cooling to 450C and overageing at this temperature for 40s before cooling to room temperature.

37

100 0 90 0 80 0 70 0 60 0

cycles 1, 2, 3

cycles 4, 5, 6

T [C]

50 0

cycles 1, 4
40 0

cycles 2, 5
30 0 20 0

cycles 3, 6
10 0 0 0 50 10 0 1 50 20 0 25 0

t [s]

Figure 28. Simulations of a continuous annealing line with water quenching and separate overageing. Annealing both in the austenite region as well as in the intercritical range was performed and various overageing temperatures were tested.
1000

cycle 7
900 800 700 600

T [C]

500 400 300 200 100 0 0 50 100 150 200 250

t [s]

Figure 29. Simulations of a continuous annealing line with water quenching, soft cooling in the gas jet section and overageing. Annealing was performed in the austenite region and the overageing temperatures were set to 200C.
1000

cycles 8, 9, 10
900 800 700 600

T [C]

cycle 8
500

cycle 9
400

cycle 10
300 200 100 0 0 50 100 150 200 250

t [s]

Figure 30. Simulations of a continuous annealing line with gas quenching or hot dip galvanizing line. Annealing was performed in the austenite region and various overageing temperatures were tested.

38

Table 18. Cycle 1 V1-C1 S7-C1 R4-C1 Cycle 2 V1-C2 S7-C2 R4-C2 Cycle 3 V1-C3 S7-C3 R4-C3 Cycle 4 V1-C4 S7-C4 R4-C4 Cycle 5 V1-C5 S7-C5 R4-C5 Cycle 6 V1-C6 S7-C6 R4-C6 Cycle 7 V1-C7 S7-C7 R4-C7 Cycle 8 V1-C8 S7-C8 R4-C8 Cycle 9 V1-C9 S7-C9 R4-C9 Cycle 10 V1-C10 S7-C10 R4-C10

Properties and microstructures obtained in task 3.2 Rp 0,2 Rm Ag A25 Ri/t HE Phase constituents
[MPa] 1169 938 1216 859 908 1230 1141 1181 1211 910 699 [MPa] 1172 973 1245 898 848 1373 1145 1383 1450 947 833 882 950 1137 1376 1145 962 1488 948 779 1122 985 603 1046 788 664 841 856 665 920 [%] 0,2 3,6 2,2 1,4 5,2 3,2 0,9 1,4 2,3 1,6 5,8 5,2 0,2 6,1 2,5 4,8 9,5 2,6 3,3 14,6 7,1 9,2 11,3 10 11,8 5,5 8,3 8,3 5,1 5,7 [%] 2,4 8,7 5 3,5 7,3 7,4 4,3 1,5 5,8 4,1 11,1 6,5 0,2 10,7 2,9 9,4 10,8 3,2 5,6 19,2 8,5 12,1 13 16,1 18,5 6,2 13,4 12,8 5,1 10,5 6,7 5,3 6,7 4,7 4 5 2,7 3 4,2 5 1,1 6,7 4 1,3 5 3 1,7 4,2 0,8 0,7 1,7 1,3 0,5 1,7 0,8 0,5 1,25 0,8 0,7 1 [%] [%] 52 100%M 67 80%M 20%F 88 100%M 73 51 87 72 33 69 42 33 83 33 26 73 29 23 44 38 24 22 24 84 16 71 48 59 46 28 49 100%M 94%M 6%F 100%M 100%M 95%M 5%F 100%M 70%M 30%F 60%M 40%F 82%M 18%F 67%M 33%F 61%M 39%F 86%M 14%F 83%M 17%F 66%M 34%F 94%M 6%F 33%M 60%F 7%CFB 19%M 79%F 2%CFB 47%M 37%F 16%CFB 36%M 62%F 2%UB 86%F 14%P 41%M 54%F 5%UB 10%M 40%F 20%UB 30%CFB 1%M 84%F 15%P 10%M 90%UB 7%M 30%F 33%LB 30%CFB 10%M 80%F 10%P 5%M 5%UB 80%LB 10%CFB

900 872 1285 907 551 1241 676 446 705 602 499 608 597 484 658 605 391 690

M=Martensite, F=Ferrite, UB=Upper bainite, LB=Lower bainite, CFB= Carbide free bainite, P=Pearlite

39

2.5.2.3

Task 3.3 Processing of special microstructures based on suggestions from WP 4

In task 3.3, the main task was to perform laboratory annealing trials in order to find optimal processing parameters for the industrial trials. Each industrial partner has suggested five time temperature cycles corresponding to their production facilities; SSAB: continuous annealing line with water quench; voestalpine: continuous annealing line with gas jet cooling; Ruukki: hot dip galvanizing line. The selected time-temperature schedules are based on the previous results from phase transformation data from WP2, task 3.1, task 3.2 and on other knowledge about the specific production route. In order to get enough material for a systematic investigation, each time temperature cycle was performed for four samples with a size of 450x250mm. After annealing, the samples were pickled and the edges were cut off since these were not annealed. Then three samples were sent to RWTH Aachen for mechanical testing and one sample was sent to KIMAB for microstructural investigation. The results of these investigations (see WP4) were the basis for selecting the proper time temperature cycles for the industrial trials. 2.5.2.3.1 Annealing trials for a continuous annealing line with gas cooling, CAL-GQ

2.5.2.3.1.1 Material: The chemical composition of the material selected for these annealing trials is given in Table 19. The CP800 grade without molybdenum was chosen as the results of this annealing simulation should be the basis for industrial trials. Molybdenum, despite being a very interesting alloying element, has to be avoided in the industrial production as much as possible due to economic reasons because of its very high price. Table 19. Chemical composition of the lab annealed samples (wt%) Material Grade C Mn Cr Mo
V2-CR VA_CP800 0.14 2.1 0.3 0

Si 0.2

Nb 0.02

2.5.2.3.1.2 Time temperature cycles: The annealing parameters (Tan: annealing temperature, TQ: quenching temperature; Toa: overageing temperature) for the five time temperature cycles can be found in Table 20. Additionally, cycle 1 to 3 and cycle 4 & 5 are depicted in Figure 31 and Figure 32, respectively. For all time temperature cycles an annealing temperature of 840C was applied. The quenching temperature was varied between 680C and 750C and the overageing temperature was varied in the range of 350C to 400C. Table 20. Annealing parameters for the five time temperature cycles Tan TQ Toa Cycle [C] [C] [C] 1 840 680 350 2 840 680 375 3 840 680 400 4 840 750 350 5 840 750 400

40

Cycle 1, 2, 3
900 800 700 600 500 400 300 200 100 0 0 200 400 600 800 1000

T [ C]

t [s]

Figure 31. Time-temperature cycle 1, 2 and 3 for the continuous annealing line CALVAS

Cycle 4, 5
900 800 700 600 500 400 300 200 100 0 0 200 400 600 800 1000

T [ C]

t [s]

Figure 32. Time-temperature cycle 4 and 5 for the continuous annealing line CALVAS 2.5.2.3.1.3 Results: The results obtained by RWTH Aachen reveal, that for all five annealing cycles excellent hole expansion ratios (>70%!) and bending results could be obtained. The results will be shown in detail in WP4. Also the total elongation is very high (clearly above 10%) for all cycles. The results of cycle 1 to 3 show that with increasing overageing temperature the yield strength increases and the tensile stress decreases. This is a very typical behaviour as with an increasing overageing temperature a bainite is formed during overageing that is softer but has a higher yield ratio. A comparison of the results of cycle 1 and 3 with cycle 4 and 5 indicates that by decreasing the quenching temperature also slightly higher yield strength can be obtained. Due to a higher quenching temperature less ferrite is formed during soft cooling, whereas more bainite can be formed during overageing, leading to higher yield strength.

41

2.5.2.3.1.4 Industrial trials: Based on these results, two industrial trials were planned. As for all cycles in the laboratory experiment excellent hole expansion ratios and bending results have been obtained, the main goal for the industrial trials is to produce two CP800 grades with different yield strength levels. That can be achieved by applying different quenching temperatures (680C and 750C). In order to get a tensile strength clearly above 800MPa, an overageing temperature of 350C has to be chosen. Therefore, cycle 1 and cycle 4 have been selected for the industrial trials.
2.5.2.3.2 Annealing trials for a continuous annealing with water quenching, CAL-WQ:

2.5.2.3.2.1 Material: The chemical composition of the material selected for annealing trials for the continuous annealing line with water quenching is given in Table 21. Two different alloys were selected, S8 and S9, based on previous industrial results at SSAB, where the strength became a little too low, see WP 5. Carbon and Manganese has been adjusted to higher levels compared to the previous steel. Table 21. Chemical composition of the lab annealed samples (wt%) Material Coil C Mn Si 0.10 0.8 0.2 Previous on line trial S8 756598 0.14 1.5 0.2 S9 720009 0.13 1.0 0.2

Nb 0.015 0.015 0.015

2.5.2.3.2.2 Time temperature cycles: The selected parameters for the annealing simulation can be found in Table 22 (Tan: annealing temperature, Tq: quenching temperature; Toa: overageing temperature). A graph showing one of the time temperature schedules can be found in Figure 33. Table 22. Annealing parameters for the five time temperature Tan Tq Toa Cycle Steel [C] [C] [C] 1 S8 880 650 200 2 S8 850 700 200 3 S8 850 650 200 4 S9 845 830 200 5 S9 845 795 200

Figure 33. Time-temperature cycle for the continuous annealing line with water quenching.

42

2.5.2.3.2.3 Results: The results obtained by RWTH Aachen reveal, that only the leaner of the two alloys (S9) managed to receive acceptable hole expansion ratios (>35%) and the same result was found for the bending results by SSAB; S9 showed an Ri/t<1 whereas S8 had an Ri/t>1. The tensile strength found by RWTH is very high for all cycles. The results will be shown in detail in the chapter on WP4. The low overageing temperature may be the cause of the high strength and poor ductility. 2.5.2.3.2.4 Industrial trials: Based on these results, two industrial trials were planned for the leaner alloy S9, repeating the annealing cycles performed in the annealing simulator, i.e. cycle 4 and 5.
2.5.2.3.3 Annealing trials for a hot dip galvanizing line, HDG

2.5.2.3.3.1 Material: The chemical composition of the material selected for the annealing trials for the hot dip galvanizing line is given in Table 23. Table 23. Chemical composition of the lab annealed samples (wt%) Designation Mtrl C Mn Si Cr Mo R6 Ru-5 0.15 1.7 0.2 0.3 0.15

Nb 0.015

2.5.2.3.3.2 Time temperature cycles: The parameters selected for the annealing simulation can be found in Table 24 (Tan: annealing temperature, Tq: quenching after soft cooling; toa: time at overageing temperature). A graph showing one of those time temperature schedules can be found in Figure 34. Table 24. Annealing parameters for the five time temperature cycles Tan TQ toa Cycle [C] [C] [s] 830 740 95 1 860 740 95 2 900 780 95 3 860 740 15 4 830 800 95 5

Figure 34. Time-temperature cycle for the hot dip galvanizing lab anneals.

43

2.5.2.3.3.3 Results: The results obtained by RWTH Aachen reveal, that all except the first samples (cycle 1) had acceptable hole expansion ratios (>35%). All samples showed good bendability in SSABs tests with Ri/t<1. The tensile strength found by RWTH is close to or above 800MPa which was the goal for the project. The results will be shown in detail in WP4. 2.5.2.3.3.4 Industrial trials: The annealing cycles for the industrial trials were chosen according to the results from previous industrial trials and the results from the laboratory anneals. Compared to previous results, the aim was now to get a finer, more homogeneous microstructure with a lower fraction of ferrite. It was tried to achieved this with a lower annealing temperature (<860C) and various different soft cooling temperatures.

44

2.6 2.6.1

WP4 - THE RELATION BETWEEN MICROSTRUCTURE AND FORMABILITY Objectives and tasks of WP4

In work package 4 (WP4) the relation between microstructure and formability is studied which includes analysis of bendability and stretch-flangeability.

Table 25. Task 4.1

Task 4.2 Task 4.3 Task 4.4 Task 4.5-4.7 Task 4.8

Tasks of WP4 Characterisation of the formability and mechanical properties Characterisation of the microstructure and texture
Failure mechanism on prestrained material Correlation of the formability, microstructure Repetition and critical check Suggestions on further improvement

RWTH, SSAB, Ruukki, voestalpine KIMAB RWTH RWTH, KIMAB RWTH, KIMAB All

The objectives of work package 4 were to Evaluate mechanical properties through mechanical testing; tensile properties, bending and hole expansion. Investigate the fracture path to obtain information of the processes responsible for the fracture. Study void nucleation and growth for knowledge of the nucleation sites and the grow path of voids. Correlate microstructure and properties Based on these results the most promising microstructure and texture will be identified and this material will be processed in WP5 and tested in WP4.

2.6.2 2.6.2.1

Task 4.1 Formability and Task 4.2 - Microstructures Formability and tensile testing

The tensile tests were done according to the standard EN 10 002. The hole expansion tests of investigated CP-grades have been carried out at the Department of Ferrous Metallurgy, of RWTH Aachen University according to the standard ISO/TS 16630 (Figure 35).

Figure 35.

Experimental setup of the hole expansion test a) before the test; b) after the test

The limiting hole expansion ratio for each of the three test pieces was calculate as ratio of the increase in the hole diameter to the original hole size as defined by the following equation: = (Dh-D0)/D0100 where:
-the limiting hole expansion ratio in percent D0-the original hole diameter (D0=10 mm) Dh-the hole diameter after rupture, in millimetres

45

Tensile tests were carried out at room temperature according to the standard DIN EN 10002 to determine mechanical properties of investigated materials. The samples for the tensile tests were taken at angles of 0 and 90 and sometime 45 to the rolling direction. To perform the mechanical testing a computer controlled universal testing machine with a maximum force of 100 kN was used. As crosshead speed 7 mm/ min was chosen, 3 tests were performed. All bending tests have been performed by SSAB and the bend is in the rolling direction (the sample is taken in the transverse direction). The aim of the project is to produce material with bending radii better than Ri/t<1.0.

2.6.2.2

Characterisation of microstructure and texture

The microstructures of the steels in this project have been analysed both with optical microscopy and SEM, using EBSD, EDS and various detectors. The SEM investigations have been performed in a LEO 1530 Gemini FEG SEM with EBSD. The sample preparation consisted of normal grinding and polishing followed by Le Peras etching for optical microscopy. This was finished by 20 minutes silica polishing before the EBSD measurements. The samples for conventional SEM micrographs were electropolished in 10% perchloric acid in acetic acid at 18V for 30s followed by etching in Nital for 4s. The EBSD analysis was made using a Nordlys II digital EBSD camera and the HKL fast acquisition software and the mappings are recorded with a speed of minimum 300 Hz. Texture was analysed from EBSD data on ODF sections 2=45 using the Channel5 software.

2.6.2.3

Properties and microstructures of the industrial material, Task 1.1

The properties of the as received industrial steels are found in Table 26. This was the starting point of the project and the current status of the product at this strength level from the three steel producers involved in the project. The microstructure of these steels are summarised in Table 27. The steels from CAL with gas quenching and hot dip galvanizing shows a complex microstructure (CP), whereas the CAL water quenched steels are of dual phase type (ferrite and martensite) or almost fully martensitic.

Table 26.
ID R1 R2 R3 dir 0 90 0 90 0 90 0 90 0 90 0 90 0 90 0 90 0 90 0 90 supplier Ruukki Ruukki Ruukki Ruukki Ruukki Ruukki voest voest voest voest SSAB SSAB SSAB SSAB SSAB SSAB SSAB SSAB SSAB SSAB

Mechanical Properties of the industrial samples

ReH MPa ReL MPa Rp0.2 MPa 585 608 555 555 587 596 769 712 625 626 607 616 949 1008 883 936 1202 994 982 Rm MPa 863 870 826 829 818 825 951 960 794 804 809 822 1137 1142 933 970 1235 1242 1214 1211 Ag % 11.4 10.8 11.0 10.2 8.1 9.0 7.4 6.6 9.9 9.6 9.8 9.5 2.7 3.4 5.1 4.5 2.7 2.7 4.1 3.6 A80 % 15 14 16 13 13 14 12 11 15 15 16 15 6 5 8 6 5 5 6 5 remark r8, n5-10 r8, n5-10 r8, n5-10 r8, n5-10 r6, n4-8 r6, n4-8 r6, n2-6 r6, n4-6 r8, n5-10 r8, n2-6 r8, n4-6 r8, n4-6 r2, n2-3 r2, n2-3 r2, n2-4 r2, n2-4 r2, n2-3 r2, n2-3 r2, n2-4 r2, n2-4 r 0.85 1.02 0.76 0.95 0.97 0.99 0.76 0.97 0.75 0.98 0.86 1.02 1.08 1.10 1.07 1.44 0.90 1.30 0.96 1.25 n 0.14 0.14 0.12 0.12 0.13 0.12 0.08 0.07 0.11 0.10 0.12 0.13 0.05 0.04 0.06 0.05 0.04 0.03 0.06 0.05 Ri/t 1.2 3 1.2 3 1.7 0.7 1 3.5 1 3.5 58 35 30 71 44 40 HE % 19 17 56

V2 S1 S2 S3 S4 S5

614 617

615 619

888 936 1194 1208

908 947 1209

46

Table 27. Microstructures of the industrial samples Ferrite Martensite Tempered Carbide Free Steel [%] [%] Martensite [%] Bainite [%] R1 37 13 2.6 42 R2 37 13 2.6 42 R3 12 15 29
S1 S2 S3 S4 S5 V1 V2 76 20 30 3.5 14 42 36 24 80 70 96.5 86 15

Bainite [%] 5.4 5.4 44

4 7

27 57

12

2.6.2.4

Properties and microstructures of samples from task 1.4 - Laboratory produced material

The mechanical properties of the laboratory processed steel obtained with Nb microalloying are shown in Figure 36 as a function of annealing temperature. Increase in annealing temperature results in decrease in tensile strength and increase in uniform elongation. Mo increases tensile strength and reduces uniform elongation, as expected. The effect of Mo on the yield strength is in line with the previous results. Mechanical properties, especially the yield strength, of the CP steel grade alloyed with both Mo and Nb seem to be less sensitive to changes in the annealing temperature. Without Mo some additional strengthening is still needed. The microstructures achieved with different annealing temperatures are shown in Figure 37. The microstructure with both Mo and Nb seems to be fine and homogenous. The combination of Mo alloying and Nb microalloying facilitates the best response for the development of a CP-steel, i.e. homogenous and fine microstructure with significant amount of bainite. However, the microstructure of R5, without Mo, was coarser and less homogenous. Additions of Nb are known to affect a finer microstructure and improve stretch-flangeability in steels, with a higher strength level [12]. Mo decreases critical cooling rates for bainite formation and the bainite start temperature and increases the strength due to solid solution hardening [3-4]. Thus Mo decreases the hardness difference between ferrite and the hard phases and thereby improves stretch-flangeability and bendability [5].
950 900 850 Rm (Nb) 800 Stength [MPa] 750
Agt (Nb)

30 Rm (Mo+Nb) 25

20 Elongation [%]

700
Agt (Mo+Nb)

15

650 600 550 Rp0.2 (Mo+Nb) 500 450 770 0 840 10 Rp0.2 (Nb) 5

780

790

800

810

820

830

Annealing temperature [C]

Figure 36. Mechanical properties of laboratory produced material as a function of annealing temperature
47

a)

b)

c)

d)

f) e) Figure 37. Microstructures of CP-steel R5 (Nb)(a, c, e), and R6 (Mo+Nb) (b, d, f) annealing temperature (a+b) 780 C(c+d) 805 C and (e+f) 830 C, etched with LePera. The bar is 20 m.
Very promising results were obtained in the laboratory tests by modifying the chemical composition using Nb microalloying. Some additional study is still needed, in order to reduce the amount of Mo. The development work will continue in the industrial scale based on these results.

2.6.2.5

Properties and microstructures of samples from task 3.1 - Initial laboratory annealing simulations

Properties of the first laboratory annealed materials (task 3.1) are shown in the appendices, chapter 5.3. The microstructure from the initial laboratory simulations are shown in Figure 39.

48

The CAL with gas quenching tests (cycles 1-5) all shows a mixed microstructure with ferrite, bainite and martensite with various amounts. It is clear that the quenching temperature of 700C was too low to avoid ferrite formation and this temperature should be increased. The tensile properties show that overageing temperatures over 400C gives too low strength. The microstructures from the simulations of CAL with water quench shows a typical dual phase structure for the cycles 6, 7 and 9 reaching a tensile strength of about ~1100MPa. Among these three samples the tensile strength is rising with increasing starting temperature of water quenching. The samples 8 and 10 are exhibiting too low tensile strengths (below 800MPa) due to the low starting temperature of water quenching (400C). The microstructures of these samples show high fractions of ferrite and also some pearlite. The laboratory simulations of the hot dip galvanized material (cycles 11-15) was focused on the maximum annealing temperature (780C - 830C) and the length of the intermediate zone at 480C, 48s and 95s. The microstructures shows ferrite and bainite in the matrix with martensite islands and all samples have a similar tensile strength of about 800MPa. The yield strength is clearly reduced for lower annealing temperatures. For shorter holding periods at 460C the tensile strength is a little bit increased. It was shown that the target for Rm was achieved for all samples but the best elongation and HE was obtained with the highest annealing temperatures. The effect of the length of the intermediate zone seems weak. Conclusions from the initial laboratory simulations: The CAL with gas quenching need a quenching temperature above 700C was too low to avoid ferrite formation and an overageing temperature below 400C to achieve enough strength. The the CAL with water quenching needs a quenching temperature well above 400C to reach the desired strength level and avoid pearlite formation. The process parameters for hot dip galvanizing should be; annealing temperature above 805C and 48s in the intermediate zone is enough for the transformation to occur.
1200 Tensile strength, [MPa] 1100 1000 900 800 700 600 500 300 400 500 600 Overageing Temperature, TOA, [C] Tensile strength, [MPa] 1200 1100 1000 900 800 700 600 300 500 700 900 Qenching Temperature, TQ, [C]

a)
70 Hole expansion, [%] 60 50 40 30 20 750 800 Annealing Temperature, Tan, [C] 850

b) Figure 38. Results from the initial laboratory annealing simulations showing a) tensile strength vs. overageing temperature for CAL GQ, b) tensile strength vs. quenching temperature for CAL WQ and c) hole expansion vs. annealing temperature for the hot dip galvanizing cycle.

c)

49

CAL GQ

CAL WQ

HDG

11

12

13

14

5 10 15 Figure 39. Microstructures after the laboratory simulations of task 3.1. The numbers indicate the cycle tested.

50

2.6.2.6

Properties and microstructures of samples from task 3.2 a wide range of microstructures

The mechanical properties from the laboratory simulations producing a wide range of microstructures are presented in appendix 4 , see chapter 5.4. A summary is found in Table 28. In this task the three steel compositions are tested with all cycles, where cycle 1-7 can be described as CAL with water quench and 8-10 for CAL with gas quenching or hot dip galvanizing.

Table 28.

Microstructures and properties of the samples in task 3.2 A wide range of microstructures Rp 0,2 Rm Ag A25 Ri/t HE Phase constituents

Steel

[MPa] [MPa] [%] [%] [%] [%] Cycle 1 1169 1172 0,2 2,4 6,7 52 100%M V1-C1 S7-C1 938 973 3,6 8,7 5,3 67 80%M 20%F R4-C1 1216 1245 2,2 5 6,7 88 100%M Cycle 2 V1-C2 859 898 1,4 3,5 4,7 73 100%M 908 848 5,2 7,3 4 51 94%M 6%F S7-C2 R4-C2 1230 1373 3,2 7,4 5 87 100%M Cycle 3 1141 1145 0,9 4,3 2,7 72 100%M V1-C3 S7-C3 1181 1383 1,4 1,5 3 33 95%M 5%F 1211 1450 2,3 5,8 4,2 69 100%M R4-C3 Cycle 4 910 947 1,6 4,1 5 42 70%M 30%F V1-C4 S7-C4 699 833 5,8 11,1 1,1 33 60%M 40%F R4-C4 882 5,2 6,5 6,7 83 82%M 18%F Cycle 5 V1-C5 900 950 0,2 0,2 4 33 67%M 33%F 872 1137 6,1 10,7 1,3 26 61%M 39%F S7-C5 R4-C5 1285 1376 2,5 2,9 5 73 86%M 14%F Cycle 6 907 1145 4,8 9,4 3 29 83%M 17%F V1-C6 S7-C6 551 962 9,5 10,8 1,7 23 66%M 34%F 1241 1488 2,6 3,2 4,2 44 94%M 6%F R4-C6 Cycle 7 676 948 3,3 5,6 0,8 38 33%M 60%F 7%CFB V1-C7 S7-C7 446 779 14,6 19,2 0,7 24 19%M 79%F 2%CFB R4-C7 705 1122 7,1 8,5 1,7 22 47%M 37%F 16%CFB Cycle 8 V1-C8 602 985 9,2 12,1 1,3 24 36%M 62%F 2%UB 499 603 11,3 13 0,5 84 86%F 14%P S7-C8 R4-C8 608 1046 10 16,1 1,7 16 41%M 54%F 5%UB Cycle 9 597 788 11,8 18,5 0,8 71 10%M 40%F 20%UB 30%CFB V1-C9 S7-C9 484 664 5,5 6,2 0,5 48 1%M 84%F 15%P 658 841 8,3 13,4 1,25 59 10%M 90%UB R4-C9 Cycle 10 605 856 8,3 12,8 0,8 46 7%M 30%F 33%LB 30%CFB V1-C10 S7-C10 391 665 5,1 5,1 0,7 28 10%M 80%F 10%P R4-C10 690 920 5,7 10,5 1 49 5%M 5%UB 80%LB 10%CFB M=Martensite, F=Ferrite, UB=Upper bainite, LB=Lower bainite, CFB= Carbide free bainite, P=Pearlite 51

The requirement for the tensile properties (>800MPa) are met for most cycles except for the leanest steel composition S7 for the cycles without water quenching (8-10), see Figure 40. These are marked by lighter colours in the graph. The requirement for bending (Ri/t<1) are more difficult to achieve for laboratory annealed samples, it is known to be better after industrial production, probably due to better surfaces. Good bending is achieved for cycles with gas cooling in the soft cooling section, cycles 7-10, but may also be acceptable for the leanest steel, S7, annealed in the two phase region, cycle 4-6, see Figure 41. The requirement for hole expansion (HE>35) are not difficult to achieve except for the intermediately annealed DP-steels of cycle 4-6, see Figure 42.

Tensile Strength, [MPa]

1400 900 400
1 2 3 4 V1 5 S7 6 R4 7 8 9 10

Figure 40. Tensile strength for all steels and cycles in task 3.2 wide range of microstructures. The lighter colours indicate too low tensile strength. Bending, Ri/t
8 6 4 2 0 1 2 3 4
V1

5
S7

6
R4

10

Figure 41. Bending properties for all steels and cycles in task 3.2 wide range of microstructures. The lighter colours indicate too poor bending.

Hole Expansion, [%]

100

50

0
1 2 3 4 5 6 7 8 9 10

V1

S7

R4

Figure 42. Hole expansion for all steels and cycles in task 3.2 wide range of microstructures. The lighter colours indicate too poor HE value.

52

The microstructures of the different cycles 1-10 are shown in Figure 43 - Figure 46. The microstructure of the first three cycles (no 1-3) are supposed to be fully martensitic with various degree of overageing, since the temperature of annealing was 880C and the overageing temperatures were 400C, 300C and 200C respectively, see Figure 43, but the amount of ferrite in the S7 material for cycles 1-3 vary between 5-20%. The steels V1 and R4 are both fully martensitic.

S7 1 - 880C/400C

V1

R4

3 - 880C/200C Figure 43. Cycle 1-3. Simulations of continuous annealing in the austenite region (880C), water quenching and various overageing temperatures were tested (1=400C, 2=300C, 3=200C). The bar shows 1-3 m and all images have the same magnification.
Examples of the microstructures of the following 3 cycles, no 4-6, are shown in Figure 44. These cycles represents a simulation of a continuous annealing in the two phase region (780C) followed by water quenching and various overageing temperatures (4=400C, 5=300C, 6=200C). This annealing schedule produces dual phase steels, and as can be seen from Figure 44, ferrite and martensite are the constituents of all three materials. The S7 samples have the highest amount of ferrite and steel R4 have the smallest quantity, which is expected from to the composition. The ferrite of the V1 and the S7 material is not fully recrystallised, which is probably due to the small Nb-content of these steels and is likely to have negative influence on the properties. Cycle 7 was designed to simulate continuous annealing with soft cooling in a gas jet section before quenching. In this way it is possible to alter the crystallographic texture by annealing in the austenite region (Normalising) compared to intercritical annealing and the soft cooling is to re-transform a suitable amount of ferrite to reach a tensile strength in the range 800-1000MPa. The overageing was performed at 200C. If the soft cooling is fast enough, and the quenching temperature is below pearlite transformation but over the martensite start temperature, it is also possible to have bainitic phases in the microstructure, depending on the alloy composition. It was found that all samples had a mixture of ferrite, martensite and carbide free bainite after annealing with cycle 7. The steel with the leanest composition (S7) had 79% ferrite, 19% martensite and 2% carbide free bainite. The intermediate composition (V1) had 60% ferrite, 33% martensite and 7% carbide free bainite. The strongest composition (R4) showed 37% ferrite, 47% martensite and 16% carbide free bainite. 53

2- 880C/300C

S7 4 - 780C/400C

V1

R4

6 - 780C/200C Figure 44. Cycle 4-6. Simulations of continuous annealing in the two phase region (780C), water quenching and various overageing temperatures were tested (4=400C, 5=300C, 6=200C). The bar shows 2-3 m and all images have the same magnification. S7 V1 R4 7 Figure 45. Cycle 7 - annealing in the austenite region at 880C followed by soft cooling in the gas jet section to 450C. Quenching in water and overageing at 200C The bar shows 1-2 m and all images have the same magnification.
The last three annealing cycles (no 8-10) were designed to simulate continuous annealing with gas cooling or a hot dip galvanizing line. The parameter varied was the overageing temperature (550C, 450C or 350C). The S7 material, with the least amount of alloying additions, had too poor hardenability for these heating schedules. The phases found after cycles 8-10 were ferrite, pearlite and martensite. The fraction of martensite in this steel increased with decreasing overageing temperature and increasing cooling rate in the gas jet section. At the overageing temperature of 350C the amount of martensite was 10% for this steel. The V1 steel showed much better hardenability and had a CP microstructure with 36% martensite, 62% ferrite and a small fraction (2%) of upper bainite after overageing at 550C. The microstructure was completely altered after using the annealing cycle 9 (overageing at 450C) with a much higher content of bainite, 20% upper bainite and 30% carbide free bainite. The rest of the microstructure consisted of 40% ferrite and 10% martensite. The main difference between cycle 9 and 10 was the exchange of upper bainite with lower bainite at the lower temperature, and a decrease in the ferrite fraction. 54

5- 780C/300C

The R4 steel, with the strongest composition did also have a very good hardenability. The austenite grain size during annealing of this steel seems to have been larger than for the S7 and the V1 steel and this could be explained by the Nb-content of the two latter and a lower A3-temperature for the R4 composition. The austenite grain size is affecting the hardenability of the structure during cooling. The microstructure after cycle 8 (550C) consisted of 54% ferrite, 41% martensite and 5% upper bainite. After cycle 9 (450C) there was no ferrite but 10% martensite and 90% upper bainite. Overageing at 350C (cycle 10) gave 5% martensite, 5% upper bainite, 80% lower bainite and 10% carbide free bainite. S7 V1 R4

10 Figure 46. Cycle 8, 9 and10 - annealing in the austenite region at 880C gas quenching to various overageing temperatures 550C, 450C and 350C gas quenching to room temperature. The bar shows 1-2 m and all images have the same magnification.
Conclusions from task 3.2- laboratory simulations of a wide range of microstructures: There are several alternative processing parameters for CAL with gas quenching and hot dip galvanizing that can be selected to achieve the required properties, but the most promising seem to be close to cycle 9 and to use the steels V1 and R4. For a CAL with water quenching is the cycle 4 or 7 the best alternative and there seems to be no reason to use an alloy with stronger alloying composition than S7.

55

2.6.2.7

Properties and microstructures of samples from task 3.3 special microstructures from dedicated lab annealing

The results from the tensile and forming tests and the phase constituents of the dedicated laboratory simulations are shown in Table 29 and in appendix 5 in chapter 5.5. These simulations were designed to achieve the required properties, and as the bending properties was difficult to obtain in task 3.2, this has been particularly considered for task 3.3, which has turned out very good; only the S8 steel shows too poor bending. It is clear from the results that it is possible to achieve the required properties but the processing parameters need to be slightly adjusted for the R4 steel for hot dip galvanizing to ensure that a strength level of more than 800MPa is obtained.

Table 29.
Samples-ID CAL-WQ S8-D1_TD S8-D2_TD S8-D3_TD S9-D1_TD S9-D2_TD Samples-ID CAL-GQ V2-D1_TD V2-D2_TD V2-D3_TD V2-D4_TD V2-D5_TD Samples-ID HDG R6-D1_TD R6-D2_TD R6-D3_TD R6-D4_TD

Microstructures and properties of the samples in task 3.3 special microstructures

Rm MPa 1020 1273 960 950 921 Rm MPa 885 804 803 877 866 Rm MPa 789 777 790 825 Ag % 5,6 2,1 10,7 2,3 2,2 Ag % 9,3 9,7 10,5 9,8 10,2 Ag % 12,1 10,5 10,3 11,6 A80 % 6,8 2,2 12,9 2,4 2,3 A80 % 11 14,3 14,8 14,2 12,1 A80 % 15,9 14,5 15 16 Ri/t 1,7 1,7 1,7 1 0,5-1,0 Ri/t <0,5 <0,5 0,5-1,0 <0,5 <0,5 Ri/t 0,3-1,3 0,3-0,7 0,3-0,7 0,3-0,7 HE % 25 34 23 44 48 HE % 75 84 83 76 79 HE % 32 40 44 40 Phase constituents [%] 28%TM, 72%F 54%TM, 46%F 16%TM, 84%F 40%TM, 45%F 15%B 10%TM, 49%F 41%B Phase constituents [%] 2%M, 20,6%TM 49,8%F 27,4%LB 0,2%RA 1%M, 19,4%TM 44%F 34,6%LB 1%RA 1,5%M, 20,8%TM 45%F 32%LB 0,7%RA 1%M, 24,1%TM 36,6%F 37,9%LB 0,4%RA 2%M, 23,6%TM 38%F 35,9%LB 0,5%RA Phase constituents [%] 2,5%M 36%F 59%B 2,5%RA 4,5%M 22%F 70%B 3,5%RA 4,2%M 10%F 84%B 1,8%RA 3,3%M 13%F 80,8%B 2,9%RA 1,9%M 20%F 74,9%B 3,2%RA

Rp 0.2 MPa 685 1061 521 654 521 Rp 0.2 MPa 608 616 490 576 535 Rp 0.2 MPa 538 526 580 541

R6-D5_TD 505 798 12,2 16,2 0,3-0,7 39 TD= transverse direction, RD= rolling direction, D=45 direction

M=Martensite, TM=Tempered martensite, F=Ferrite, B=Bainite, LB=Lower bainite bainite, RA=Retained austenite

The microstructures of the samples subjected to the continuous annealing cycle with water quenching are found in Figure 47. The annealing parameters and chemical composition of the used alloy are also presented in the same figure. This consists of annealing close to or in the austenite region, soft cooling to a selected temperature, water quenching down to room temperature. The main parameters that varied were; annealing temperature and quenching temperature (at the end of soft cooling). The challenge with this process is to find an alloy and process parameters that allow bainite formation since there is no isothermal hold. The transformation has to be obtained during cooling to the quenching temperature or to use an alloy with a low hardenability. For the laboratory trials SSAB has chosen to try both; a lean alloy in combination with rather high quenching temperatures (S9) or a normal alloy with a low quenching temperature (S8) The results show that it is very difficult to get any bainite with the latter principle without an isothermal hold; the samples S8 sample 1-3 contains only ferrite and martensite with varying amounts. The S9 samples show some interesting structures and it was found in the microstructure analysis that 15-40% of the structure could be described as bainitic. 56

a) S9 cycle 1

a) S9 cycle 2

a) S8 cycle 1

a) S8 cycle 2
S9 - %C 0.13, %Mn 1, %Si 0.2, %Nb 0.015, S8 - %C 0.125, %Mn 1.52, %Si 0.2, %Nb 0.017

Cycle 1 2 3 1 2

Steel S8 S8 S8 S9 S9

Tan (C) 880 850 850 845 845

Tq (C) 650 700 650 830 795

Toa (C) 200 200 200 200 200

a) S8 cycle 3 Figure 47. In lens micrographs of the 5 samples subjected to the continuous annealing cycle with water quenching.

The microstructures of the samples subjected to the continuous annealing cycle with gas cooling are found in Figure 48. The annealing parameters and chemical composition of the used alloy are also presented in the same figure. This consists of annealing in the austenite region, region, soft cooling to a selected temperature, gas quenching down to an overageing temperature which can be more freely defined compared to the galvanizing cycle since the melting temperature of zinc is not involved here. The tempering (overageing) section is followed by gas cooling to room temperature. The main parameters that were varied were; gas quenching temperature (at the end of soft cooling) and the overageing temperature. Most of the structure seems to be ferrite and lower bainite but there are also also tempered martensite and carbide free bainite.

57

a) cycle 1

b) cycle 2

c) cycle 3

d) cycle 4
%C 0.136, %Mn 2.17, %Si 0.19, %Cr 0,28, %Nb 0.023

Cycle 1 2 3 4 5

Tan 840 840 840 840 840

Tq 680 680 680 750 750

Toa 350 375 400 350 400

e) cycle 5 Figure 48. In lens micrographs of the 5 samples subjected to the continuous annealing cycle with gas cooling.

The microstructures of the samples subjected to the galvanizing cycle are found in Figure 49 The annealing parameters and chemical composition of the used alloy are also presented in the same figure. This consists of annealing in the austenite region, soft cooling to a selected temperature, gas quenching down to a temperature close to the temperature temperature of the zinc pot and a holding time in this section before the material enters the pot, which is followed by gas cooling to room temperature. Most of the structure seems to be upper bainite but there are also untempered martensite and carbide free bainite and ferrite. One goal for the laboratory simulations was to achieve as fine grain size as possible. From the results here it can be concluded that it is necessary to use as low annealing temperature as possible. With a low annealing temperature the amount of untempered martensite is reduced but the fraction of retained austenite is larger. It seems that the amount of retained austenite + untempered martensite is almost constant in these samples.

58

a) cycle 1

b) cycle 2

c) cycle 3

d) cycle 4
%C 0.16, %Mn 1.75, %Nb 0.01, %Mo 0.15 %Si 0.2, %Cr 0,3,

Tan Cycle (C) 1 830 2 860 3 900 4 860 5 830

Tsc (C) 740 740 780 740 800

tpot Tpot (C) (s) 480-465 95 480-465 95 480-465 95 480-465 15 480-465 95

e) cycle 5 Figure 49. In lens micrographs of the 5 samples subjected to the galvanizing cycle.

2.6.2.8

Properties of the samples from task 5.1 - industrial trials

Microstructures of the steels after final on line trials are not presented here but in the chapter on the on line trials in WP5. The obtained tensile strength is shown in Figure 50. All steels except one of the coils from the hot dip galvanizing line reached the minimum target strength of 800MPa. The two coils from the continuous annealing with water quenching have a much higher tensile strength, minimum 1000MPa. All steels were tested for hole expansion and the results are shown in Figure 51. All steels have a HE value above 35%, which was the target of this project.

59

It was decided to chose the steels with the best hole expansion and tensile strength for the further analysis of properties and bending properties were evaluated on the steels R7-F2, V2-F1, V2-F2 and S9-F2. The results show that all steels meet the required aim of Ri/t<1, see Figure 52. It can therefore be concluded that the objectives for the properties of this project has been fulfilled

Tensile strength, [MPa]

1200 1000 800 600 400 200 0 R7-F2 R7-F5 V2-F1 V2-F2 S9-F1 S9-F2
TD RD

Figure 50. Tensile strength of the steels from the on line trials Hole expansion, [%]
60 50 40 30 20 10 0 R7-F2 R7-F5 V2-F1 V2-F2 S9-F1 S9-F2

Figure 51. Hole expansion of the steels from the on line trials Bending, Ri/t
1.2 1 0.8 0.6 0.4 0.2 0
R7-F2 V2-F1 V2-F2 S9-F2 TD

RD

Figure 52. Bending results of the steels from the on line trials
The more extensive evaluation of the properties temperature and strain rate sensitivity and complete FLDs are presented in the following chapters.

60

2.6.3

Task 4.3 Characterisation of the failure mechanism on pre-strained industrially produced materials

Micro-void formation and micro-crack development has been investigated on the cross-section of tensile specimen (longitudinal direction) after 2%- and 5% pre-straining. These were all produced industrially and have approximately the same strength level. Special attention was also paid to the role of cavities and distribution around inclusions on crack propagation. Nucleation Nucleation sites of micro-voids as well as micro-voids density, distribution and mode of individual micro-void growth have been highlighted.
S6-B2 V1

S4

Figure 53.

Micro void development at 5% prestraining in DP-Grade S6-B2 and CP-Grade V1; and at 2% pre-straining in fully martensitic grade S4

Examples are given for micro void development for three types of steel in Figure 53. It can be concluded that micro voids are located predominantly between martensite grains in martensite bands, but they can also be generated either by the martensite cracking or/and by decohesion decohesion of the interfaces of the second phases (intergranular fracture) in DP-grades. In fully martensitic grades the micro-void nucleation is generated by cracking of martensite grains or can be initiated by non-metallic inclusions.

In CP-grades micro-voids are nucleated predominantly by cracking of large martensite grains or by decohesion of adjacent martensite grains in banded martensite areas. Plastic rupture of the ferrite matrix can be observed only by decohesion of the matrix from non-metallic inclusions. Micro-void formation on ferrite/martensite interfaces can only seldom be observed in these materials after 5% pre-straining.

2.6.3.1.1 Fracture analyses on the fractured hole expansion specimens Fractured hole expansion specimens have been used for investigations of both the fracture surface and on the bulk material close to fracture on cross-section parallel planes. Observation of characteristics fracture surface features provides information on fracture mode (macro scale behaviour). To identify the mechanism (or mechanisms) by which the fracture develops (micro scale behaviour) the microscopic investigations of the cross-section is useful in relation to microstructure components responsible for micro-void formation and crack development.

61

Figure 54 shows some representative micrographs, taken with SEM, for DP- (S1), CP- (V1) and martensitic steel (S4) grades. The images contain highlighted areas that are marked by the same numbers as is in the text to allow the reader to follow the explanations more easily.

S4 1, 3 1, 3

S1

V1 2

Figure 54. Fracture surface of steel samples with different microstructures

In all investigated materials a similar character of the fracture appearances has been noted and specified in four groups: Micro voids nucleation at ferrite/martensite, cracking of martensite and adjacent martensite islands (1) parts of low ductility martensite islands (2) decohesion of ductile matrix from the brittle islands, propagation of ductile cracks by joining up of voids (3) inclusions induced dimples (4) 2.6.3.1.2 Analysis of the microstructure beneath the punched edge surface after HE testing

Figure 55 illustrates the microstructure of representative micrographs taken with SEM for CP- grades (V2-F1), DP-grades (S1) and martensitic grades (S5). In the CP-steel (grade V2-F1) micro voids were nucleated predominately between adjacent martensite grains and in martensite/ferrite interfaces. Micro void nucleation by martensite cracking has been observed in large martensite grains. Micro void coalescence and propagation of ductile cracks by joining up of voids have also been observed.

62

V2_F1

S5

S1

Figure 55. Microstructure of investigated steel samples from the industrial trials beneath the punched edge surface after HE testing at 3000x-magnification
In the DP-grade (S1) the micro voids were mainly located in the cracked martensite grains, between the adjacent grains of the brittle second phase and at the ferrite/martensite interfaces. The growth of voids by further separation of the cracked martensite areas has been observed. The plastic ruptures of ferrite grains by decohesion of matrix from the non-metallic inclusions and inhomogenities have also been observed. Micro void coalescence and propagation of ductile cracks by joining up of voids have been noted. In the martensitic steel sample S5 the micro voids were found propagating both transgranular as well as in the boundaries of the martensite grains.

2.6.4

Task 4.4 Critical evaluation and correlation of the formability, microstructure including texture and the detected failure mechanism, conclusions of WP4

The results for bending and hole expansion for the laboratory annealed samples and the final industrial samples are plotted in Figure 56. The goals of the project was for bending a Ri/t<1 and for hole expansion, HE>35%. These are both achieved in the lower right corner of the graph and the steels from final industrial trials have managed to obtain these values. It is clear from the graph that particularly the bending property has been rather difficult to achieve with the required strength maintained in the tests of this project. In order to understand the effect of different constituents and processing parameters, it has been necessary to concentrate on one factor at the time. The first parameter shown here is tempering of the martensite. This has been studied on the martensitic and dual phase (martensite-ferrite) samples and is shown in Figure 57. It is clear that the hole expansion value is improved when the tempering temperature is increased and this is true both for 95% martensite and for 65% martensite. The DP-steels shows a poorer hole expansion due to the difference in hardness between the two phases and the tempering effect is clear but not as effective as for the almost single phase material.

63

7
Task 3.2

6 5 4 Ri/t

Task 3.3 - CAL-WQ Task 3.3 - CAL-GQ Task 3.3 - HDG On line trials

3 2 1 0 0 20 40 HE, [%] 60 80 100

Figure 56. Hole expansion versus bending for laboratory samples and the final industrial trials. The project goals are in the lower right corner of the graph; Ri/t<1, HE>35%.
80 70 60 HE, [%] 50 40 30 20 10 0 100 200 300 400 Overageing temperature, [C] 1 0 100 200 300 400 Overageing temperature, [C] Ri/t 4 3 2 95% Martensite 65% Martensite 6 5 95% Martensite 65% Martensite

Figure 57. Hole expansion and bending versus tempering temperature for steels with high martensite content.
For bending it is not as obvious if tempering is beneficial, see Figure 57. The bending property is deteriorated for the almost fully martensitic steel with increasing tempering temperature, whereas it is improved when 35% ferrite is present. This may be explained by the different effects that tempering is expected to have in ferrite and martensite. Tempering will reduce the difference in hardness between the two phases although both martensite and ferrite will be softer. Carbon will precipitate as carbides in both martensite and ferrite and these will be larger the higher the overageing temperature is. Finally; carbon diffusion to dislocations may result in aging of both phases. Both the size of the carbides as well as the ageing effect may be the reason for the reduction in bending properties. The conclusions from these results are that tempering at high temperatures is beneficial for both hole expansion and bending if the martensite content is less than ~65%. This is normally the case for the strength levels that this project is aiming for. The effect on hole expansion ratio, HE, and bending, Ri/t, as a function of the martensite content is shown in Figure 58 and Figure 59. Material with either very low levels of martensite or very high fractions show very good hole expansion and the martensite content should be below 20% or above 80% to achieve the project goals, but as has been pointed out previously, tempering may allow the martensite content to be increased above 20%. 64

Figure 58. Hole expansion ratio versus martensite content.

For good bending, martensite should be avoided. The relationship is in principal linear with the best bending with no martensite, see Figure 59. It seems to be possible to reach the target for bending if the amount of martensite is below 25%.
4,5
y = 0,0001x + 0,0176x + 0,4998
2

4 3,5 3 2,5 2 1,5 1 0,5 0 0 10 20 30 40 50 60 70 80 90 100

Ri/t

Martensite, [%]

Figure 59. Bending versus martensite content.

The effect of ferrite content in the CP-structured samples is shown in Figure 60. It is obvious that the soft ferritic phase should be avoided and for enough strength; replaced by bainite.

65

Figure 60. Effect of ferrite on the hole expansion ratio in the alloy from Ruukki. The structures are of CP-type.
The microstructure analysis of the fractured surfaces and the cross sections next to the fracture performed to identify the damage mechanisms operating in industrial or laboratory samples show the following common features, irrespective of the type of test considered: Failure is initiated frequently by decohesion of the matrix from inclusions at their common phase boundary. When the second phase appears in bands, voids formed by separation (cracking) of adjacent second phase grains can frequently be observed. The relative hardness of the constituting phases has a marked influence on the density of voids. In microstructures with moderate hardness ratio such voids appear at higher plastic strain. Plastic failure of the ductile ferritic matrix is observed only seldom and then it is correlated with the presence of non-metallic inclusions and decohesion of the matrix from these inclusions or hard second phase. The experimental findings for the investigated materials allow the following hypothesis to be established with respect to stretch-flangeability: Cleanliness of the steels is an important factor but not possible to vary within the frame of this project and this will not be discussed further. The strength/hardness difference between the matrix phases in the microstructure must not be high. This mechanical homogeneity prevents local hot-spots of stress and/or strain in the microstructure especially at phase boundaries which act as nucleation sites for voids. Several possibilities have been tried to reach this goal for CP-grades: Reducing the grain size of the hard martensite Replacing hard martensite by softer tempered martensite or bainite. Increasing the strength of the matrix by grain size reduction, other strengthening mechanisms (solution or precipitation hardening) and /or the introduction of more bainite. Reducing the amount of soft ferrite The experimental findings for the investigated materials regarding bending is not as obvious as for hole expansion but the best results were achieved with the following principles: Reducing the grain size of all constituents in the microstructure. Reduce the hardness difference between different phases Replacing hard martensite and/or soft ferrite by bainite or tempered martensite. Ferrite is not poor for bending but the required strength level will not be reached if too much ferrite is present at the same time as martensite is avoided. 66

The experimental finding for nearly fully martensitic DP-grades TS1200M with 96.5% of tempered martensite have also established that the homogeneous microstructure of this material provides high strength and good hole expansion level although the tensile elongation is low, and that this steel shows better HE than a dual phase microstructure with ferrite and martensite. Our results indicate that optimum crystallographic texture also can provide additional improvements in the forming properties, but this was considered more difficult than manipulating the phase constituents and was not considered in the final trials. It was shown that the best texture was achieved annealing in the austenite-ferrite region, a processing condition that will be difficult to use in HDG or CAL-GQ. These processes normally use full austenitisation to achieve a bainitic transformation during the isothermal holding section. Without complete transformation during annealing it is likely that the yield strength level will be too low without more additions of alloying elements. Another possibility to improve the texture is to increase the cold rolling reduction, and this was shown in laboratory trials but could not be tested in full scale. The obtained variations in crystallographic texture have been very small in all experiments except for the specific tests performed under task 1.3. Our findings have resulted in selected processing conditions for the industrial trials presented in the following chapter.

67

2.7 2.7.1

WP 5: SEMI-INDUSTRIAL/INDUSTRIAL PROCESSING OF OPTIMISED MATERIAL Objectives and tasks of WP5, industrial processing of optimised material

The most important task of WP5 is the on line trials based on the laboratory results in the earlier part of the project. For a successful implementation of new steel grades a basic characterisation of the properties of the material for the end user is essential. Therefore the following tasks are included in the work package, see Table 30.

Table 30. Task 5.1

Task 5.2 Task 5.3 Task 5.4 Task 5.5 Task 5.6 Task 5.7 Task 5.8

Tasks of WP5 Processing of material with optimised microstructure on industrial scale Critical evaluation of the results from WP 4 Critical comparison of the objectives of the project and the results obtained in the project Basic characterisation of the formability based on forming limit diagrams impact of the strain rate and temperature on the mechanical properties
impact of the strain state on the formability modelling of anisotropy constitutive modelling and determination of the parameters relevant for the selected CP grades

SSAB, Ruukki, voestalpine SSAB, Ruukki, voestalpine, RWTH SSAB, Ruukki, voestalpine, RWTH RWTH RWTH RWTH Swerea KIMAB RWTH and Swerea KIMAB

2.7.2 2.7.2.1

Task 5.1 Processing of material with optimised microstructure on industrial scale Initial trials of HDG at Ruukki

Ruukki studied the effect of microalloying and a higher annealing temperature on the structure and mechanical properties of CP-steel and these trials were based on the laboratory trials performed at Oulu University, see chapter 2.3.2.4. Two different compositions, alloyed with either Nb or Mo (Table 31), were processed in a hot dip galvanizing line with a high annealing temperature of 860C

Table 31. Material TS800 CP Mo TS800 CP Nb

Chemical compositions of the investigated steels in wt%. C Si Mn Cr Mo Nb 0.17 0.18 1.76 0.3 0.15 0.14 0.31 1.77 0.5 0.015

The mechanical properties for both compositions are shown in Table 32. The Mo-version experiences a significantly higher yield strength and a bit lower tensile strength than the Nb-version. Both the elongation to fracture and the uniform elongation are higher in the Nb-version, but the post-uniform elongation is virtually the same for both steels.

Table 32.
Material TS800 CP Mo

TS800 CP Nb

Mechanical properties of the investigated steels. Rp0.2 Rm A80 Direction Rp0.2/Rm [MPa] [MPa] [%] 90 681 817 0.83 12 0 667 812 0.82 12 45 671 794 0.85 14 90 617 834 0.74 16 0 589 828 0.71 17 45 594 821 0.72 17
69

Ag [%] 7.0 7.6 7.3 10.8 11.5 11.6

r-value 0.99 0.88 1.0 0.88 0.82 0.95

Results from the formability tests, for the investigated steels, are shown in Table 33. The Nb-version had a moderate hole expansion value, but the hole expansion value of 48 % for the Mo-version was excellent. The bending test results were good especially for the Mo-version. The results for the Erichsen and LDR (limit drawing ratio) -tests were good and practically the same for both steels. The LDR-test result of 2.0 is a typical value for this strength category. The results of the high temperature experiments are promising, but it seems that Mo-alloying is still needed to get a homogeneous microstructure with a good hole expansion value

Table 33.
Material TS800 CP Mo TS800 CP Nb

Results from the formability tests for the investigated steels. Bending test 180 (Ri/t) Hole expansion Erichsen LDR [%] TD RD 48 0 1.0 13.4 2.0 27 1.0 1.3 14 2.0

2.7.2.2

Final on line trials of HDG at Ruukki

During the previous seasons the composition of TS800 CP was optimised in order to fulfil the mechanical property targets. The optimised composition is shown in the Table 34. Compared to previous trials, the aim was now to get a finer, more homogeneous, microstructure with a lower fraction of ferrite. The optimised composition was also chosen for the last laboratory annealing trials (Task 3.3). Line trials were performed using five different annealing cycles (Table 35). Cycles 1 to 3 were performed in order to optimise the HE ratio. The Cycles 4 and 5 were performed in order to find if the target properties (HE > 35 % and Ri/t<1) can be reached in commercial production.

Table 34. Chemical composition used in the industrial trials [wt%]. Material C Si Mn Cr Mo TS800 CP Mo+Nb 0.15 0.2 1.7 0.3 0.15 Annealing cycles used in line trials. Cycle 1 Cycle 2 Annealing temperature (C) 860 860 Soft cooling temperature (C) 800 780 Rapid cooling end temperature (C) 465 465 Table 35.

Nb 0.01

Cycle 3 860 750 465

Cycle 4 830 720 465

Cycle 5 830 760 465

The investigated steel was hot rolled to 3.0mm thickness with a finish rolling temperature 910C and coiling temperature of 600C. The hot rolled material was cold rolled with 50% reduction and annealed in a hot dip galvanizing line. After cold rolling appropriate samples for the laboratory trials were cut out from the full hard material. Table 36. Mechanical properties of the modified composition Rp0.2 Rm A80 Ag Material Cycle Direction Rp0.2/Rm r-value [Mpa] [Mpa] [%] [%] 90 676 817 0.83 14 8.2 1.09 1 0 650 826 0.79 15 9.1 0.82 45 658 800 0.82 14 8.7 1.03 90 670 814 0.82 17 9.1 0.93 2 0 643 823 0.78 15 9.3 0.82 45 651 788 0.83 14 8.3 1.05 90 641 793 0.83 16 9.1 0.91 TS800 CP 3 0 615 802 0.82 15 9.6 0.76 45 636 781 0.85 16 9.4 1.08 90 557 794 0.70 17 10.9 0.88 4 0 560 797 0.70 16 11.1 0.75 45 558 787 0.71 18 12.0 1.00 90 575 805 0.71 17 11.4 0.86 5 0 560 799 0.70 17 11.6 0.76 45 555 794 0.70 19 12.3 1.11 70

The results of tensile tests are summarised in Table 36. All cycles resulted in a typical CP-like behaviour, with a high yield-ratio. It is clear that higher annealing temperature resulted in a higher yield strength (Figure 61a). An increase in the soft cooling temperature also results in higher yield strength (Figure 61b) due to a reduction in the ferrite content. In the formability tests (Table 37) the hole expansion rate has the same trend (Figure 62). There are indications (Table 36), that a lower annealing temperature has no effect on the minimum bending radius but will results in a slightly reduced LDR.

Table 37. Material

Forming tests. Cycle Hole Erichsen expansion [%]

1 2 3 4 5 40.2 43.8 37.5 22.4 38.3 10.8 10.7 10.9 10.6 11.6

TS800 CP

Bending test 180, Ri//t TD RD. 0.7 0.3 0.3 0.3 0 0.5 1 1 0.3 0

LDR

>2.0 >2.0 2.02 1.80 >2.0

a) b) Figure 61. Yield strength as a function of a) annealing and b) soft cooling temperatures.

a) b) Figure 62. Hole expansion rate as a function of a) annealing and b) soft cooling temperature.
Optical metallography carried out after line trials revealed apparent differences in the microstructure between different cycles. Typical micrographs after each of the annealing cycles are shown in Figure 63. As previously reported, the cycles 1 and 2 resulted in very fine microstructure with a high fraction of bainite. Similar microstructure is observed when the samples were annealed using cycle 5. These cycles resulted in target properties both in mechanical and forming tests.

71

It seems that the annealing temperature is having less effect than the soft cooling temperature. In order to get reasonable CP type structures and satisfactory mechanical properties it is essential to have a high soft cooling together with a high annealing temperature. When the soft cooling temperature is reduced, the amount of bainite decreases and ferrite increases (Figure 63). This results in a reduced HE ratio (Table 37).

Figure 63. Optical micrographs showing the general microstructure of microalloyed composition after each annealing cycle.

72

2.7.2.3

Previous trials of CAL-WQ at SSAB

The first attempt to produce a CP800 in a continuous annealing line (CAL) with water quenching (WQ), with improved formability which was the aim of the project included a lean chemical composition, annealed in the austenitic range. Chemical composition and annealing temperatures are presented in Table 38.

Table 38. Table 1: Chemical composition and annealing temperatures C Si Mn TSoaking T Quench TTemper Nb 0.10 0.20 0.80 0.015 870C 820C 200C

A SEM-picture of the microstructure is presented in Figure 64. The picture shows a complex structure with phases of ferrite, martensite and features of what is likely to be bainite.

Figure 64. Complex phase microstructure

Tensile testing was performed, and results are presented in Table 39.

Table 39. Results from tensile testing Rp0.2 [MPa] Rm [MPa] A80 [%] 460 720 19
Since the tensile strength is below 800MPa, the material is too soft. A somewhat more stable analysis is required to achieve the desired properties, using the above annealing conditions. 2.7.2.3.1 Annealing simulation using dilatometry at KIMAB Using a dilatometer to perform annealing annealing simulation, a screening was done on a large number of annealing temperature combinations, using two different chemical compositions; see Table 40, both with higher levels of C and Mn.

Table 40. Grade A B

Table 3: Chemical composition for dilatometer trials, [wt%] C Mn Si Nb 0.13 1.0 0.2 0.015 0.13 1.5 0.2 0.017

The dilatometer trials were evaluated by studying the microstructures and measuring the hardness of the material. Since the hardness very well reflects the tensile strength, the samples for further annealing simulation on a larger scale at voestalpine, were chosen with respect to the proper hardness level as well as to adequate microstructures.

73

2.7.2.3.2 Annealing simulation at voestalpine Annealing conditions in the annealing simulator are presented in Table 41, as well as the results of the measured phase fractions for the samples.

Grade A-1 A-2 B-1 B-2 B-3

Table 41. Annealing conditions Tannealing T(OA) Tquench 845 200 830 845 200 795 880 200 650 850 200 700 850 200 650

Martensite % 40 2 28 54 16

Ferrite % 45 49 72 46 84

Bainite % 15 49 -

The sample A-2 seems to give the desired microstructure. Results from mechanical testing are presented in Table 42. The values of the yield strength are remarkably low and the fracture elongations are intentionally excluded due to unreasonable low values, probably due to problems with the used equipment. However, the subsequent in-line trials, described below, are based on the outcome of these tests. Table 42. Results from mechanical testing Grade YS [MPa] TS [MPa] HE [%] A-1 654 950 44 A-2 521 921 48 B-1 685 1020 25 B-2 1061 1273 34 B-3 521 960 23

2.7.2.4

On line trials for CAL-WQ at SSAB

SSAB has performed an industrial trial using the chemical composition and annealing conditions according to Table 43.

Table 43. Chemical composition and annealing parameters, parameters, on line trials CAL-WQ Trial C Mn Si Nb Tannealing T(OA) Tquench 1 0.13 1.0 0.2 0.015 850 200 795 2 0.13 1.0 0.2 0.015 850 200 780
Mechanical testing of the strips above is presented in Table 44 and microstructures in Figure 65.

Table 44. Sample SSAB-795 SSAB-780

Mechanical properties, on line trials CAL-WQ Th mm YS [MPa] TS [MPa] 1.0 758 1074 1.0 625 988

A80 7.5 9.5

HET % 46 38

Figure 65. Microstructures of industrial trials of CAL-WQ at SSAB

74

The microstructure of the SSAB-780 sample points to a DP-structure with features of bainite. Some features of bainite are also visible in the 795-sample, but not as frequently as in the 780-sample. According to the mechanical properties, the amount of ferrite is most likely larger in the 780-sample. 2.7.2.4.1 Summary of on line trials of CAL-WQ at SSAB The chemical composition 0.13C, 1.0Mn, 0.2Si, 0.015Nb, annealed in the austenitic range (A3=835C) and cooled to 795C or 780C prior to water quenching, seems to give a high strength steel with good formability.

2.7.2.5

Final on line trials of CAL-GQ at voestalpine

Two industrial trials on the continuous annealing line was performed, in order to produce two CP800 grades with good formability properties (bending, hole expansion, and tensile test). The processing parameters for these industrial trials have been selected on the basis of the results of laboratory annealing simulations that have been done previously during this project. The goal for these two industrial trials was to produce two CP800 grades with different yield strength levels but both with tensile strengths of more than 800MPa. One CP800 grade should have a yield strength higher than 600MPa, whereas the other CP800 grade should exhibit a yield strength higher than 680MPa. A yield strength level higher than 600MPa is very important for voestalpine, as the conditions of delivery contain minimum yield strength of 600MPa for a CP800. On the other hand, some customers demand a CP800 grade with minimum yield strength of 680MPa in order to save more weight. The chemical composition of the material, selected for the industrial trials (Table 45), is the same that has been used for the final laboratory annealing simulations.

Table 45.

Chemical composition of the industrially produced CP800 grades [wt%]

C Mn 2.1 Cr 0.3 Mo 0 Si 0.2 Nb 0.02

VA_CP800

0.14

The annealing parameters (Tan: annealing temperature, Tq: quenching temperature; Toa: overageing temperature) have been selected on the basis of the results of laboratory annealing simulations. In order to achieve a CP800 grade with a minimum yield strength of 600MPa, an annealing temperature of 840C, a quenching temperature of 680C, and an overageing temperature of 350C have been applied. An increase of the yield strength can be managed, by increasing the quenching temperature. Hence, for the CP800 grade with minimum yield strength of 680MPa a quenching temperature of 750C was determined. The annealing parameters for both industrial trials are given in Table 46. Both industrial trials on the continuous annealing line were conducted with material of 1.2mm thickness. During the industrial trials, no problems occurred and the planned time temperature cycles could be met quite well. After the production, samples have been taken from both strips. A first basic investigation, including mechanical testing, hole expansion testing, and optical metallography, has been carried out by voestalpine. Additionally, samples have been sent to RWTH, KIMAB and SSAB for further investigations.

75

Table 46.

Annealing parameters for the industrial trials

Tan 840 840 Tq 680 750 Toa 350 350

Cycle CP800_Tq680 CP800_Tq750

The mechanical properties of the industrial trials are displayed in Table 47. Both grades show a tensile strength higher than 800MPa and elongation values clearly higher than 10%. For a quenching temperature of 680C, a yield strength of about 640MPa is obtained. In the case of a quenching temperature of 750C, a yield strength of slightly higher than 680MPa could be reached. Additionally, the elongation values are a little bit lower for a quenching temperature of 750C due to a decreased potential for work hardening.

Table 47.
a) Gauge [mm] 1.20 1.20 1.20 1.20 1.20 1.20 b) Gauge [mm] 1.19 1.19 1.19 1.18 1.18 1.18

Mechanical results of both industrial trials: a) TQ=680C b) TQ=750C

Rp0.2 [ Pa] 640 635 643 645 624 624 Rp0.2 [MPa] 689 688 687 687 677 677 Rm [M a] 826 823 832 832 802 803 Rm [MPa 820 818 825 825 805 805 Ag [%] 9.1 9.2 9.0 8.7 9.4 9.7 Ag [% ] 7.7 7.9 7.3 7.1 8.0 7.8 A80 %] 15.2 15.8 15.8 15.5 15.0 15.7 A80 [%] 14.5 14.8 11.7 11.6 13.8 13.9 n2_4 0.097 0.099 0.093 0.093 0.096 0.097 n2_4 0.092 0.093 0.085 0.086 0.088 0.088 n4_6 0 1 3 0.105 0.098 0.098 0.104 0.104 n4_6 0.094 0.095 0.087 0.087 0.092 0.092 n6_10

Direction [ ] 0 0 90 90 45 45 Direction [ ] 0 0 90 90 45 45

0.100 n6_10

The results of the hole expansion tests can be found in Table 48. Both grades exhibit very good hole expansion ratios for the punched as well as for the machined edge condition. However, the CP800 grade produced with a quenching temperature of 750C shows slightly higher hole expansion ratios for both edge conditions. A reason for that could be that due to the elevated quenching temperature less ferrite has formed during cooling, yielding a smaller hardness contrast within the microstructure.

Table 48. Results of the hole expansion test for both industrial trials of CAL-GQ Grade Edge condition Hole expansion ratio [%] CP800-TQ680 Punched 47.5 CP800-TQ680 Machined 131.8 CP800-TQ750 Punched 60.2 CP800-TQ750 Machined 140.5
This assumption is confirmed by the micrographs of these grades (Figure 66). Both microstructures are consisting of ferrite (blue), bainite or tempered martensite (brown) and not tempered martensite (white). However, in the case of a quenching temperature of 680C more polygonal ferrite, less bainite or tempered martensite, and more untempered martensite is formed. Due to a lower quenching temperature, more polygonal ferrite is formed during soft cooling, leading to a higher degree of carbon redistribution. Hence, less bainite and more untempered martensite is formed. Due to the higher carbon content the martensite transforms at quite low temperatures during cooling after the overageing stage => no tempering. 76

a)

b)

Figure 66. Micrographs (Le Pera etching) of both industrially produced CP800 grades: a) Tq=680C; b) Tq=750C 2.7.3 Task 5.2 Critical evaluation of the results from WP4

As described earlier, the required properties from the initial project objectives; Rm>800MPa, Ri/t<1 and HE>35% have all been met for all production lines although the microstructures are different. Particularly difficult to produce is a bainitic microstructure in the continuously annealing line with water quenching. By comparing the forming limit diagrams of the initially delivered industrially produced steels, see Figure 67, and the steels from the final industrial trials based on the results of this project, see Figure 68, it is possible to draw some conclusions of other forming properties: Improved biaxial balanced stretch forming, plane strain and stretch-flangeability has been achieved for the steels produced through a hot dip galvanizing line and continuous annealing with gas section (steels R and V). This improvement is a result of a reduction of the size of the martensite grains, elimination of the soft ferrite phase and by replacing of hard martensite by tempered martensite or bainite. The continuously annealed and water quenched industrially produced materials have (steels S), however, better biaxial balanced stretch forming, plane strain, stretch-flangeability and uniaxial tensile properties in comparison with the results from the final industrial trails, due to a more homogeneous microstructure and smaller martensite grain size.

77

0,50

0,45

0,40

0,35

major strain 1 / -

0,30 R1 R1_mean R3 R3_mean V1 V1_mean V2 V2_mean S6-B1 S6-B1_mean S6-B2 S6-B2_mean

0,25

0,20

0,15

0,10

0,05

0,00 -0,15

-0,10

-0,05

0,00

0,05

0,10

0,15

0,20

0,25

0,30

0,35

0,40

0,45

minor strain 2 / -

Figure 67. Forming limited diagrams of industrially produced voest and Ruukki grades and industrially produced SSAB grades with varying texture.
0,5

0,45

0,4

0,35

major strain 1 / -

0,3

0,25

0,2

0,15

0,1

R7-F2 R7-F2_mean R7-F5 R7-F5_mean V2-F1 V2-F1_mean V2-F2 V2-F2_mean S9-F1 S9-F1_mean S9-F2 S9-B2_mean

0,05

0 -0,15

-0,1

-0,05

0,05

0,1

0,15 minor strain 2 / -

0,2

0,25

0,3

0,35

0,4

0,45

Figure 68. Forming limited diagrams of industrial produced materials from WP5

78

2.7.4

Task 5.3 Critical comparison of the objectives of the project and the results obtained in the project

This comparison between the objectives of the project and the results obtained is made in Table 49. The objectives are divided in main objectives and minor objectives, task by task.

Table 49. Comparison between objectives and results Project objectives Critical evaluation Main objectives To achieve an improved The activities and obtained results are in agreement with the scheduled strength-formability tasks and objectives. The stretch-forming and deep-drawing capacities balance with particular were analysed using forming limit diagrams. focus on bendability, Investigations in this project has shown, that reducing the hardness stretch-flangeability and contrast within the microstructure leads to a significant improvement in deep-drawing capacity. terms of bendability and stretch-flangeability. For the CAL_WQ process a new steel grade, DP1000 with low carbon equivalent (LCE), has been developed in the project. 1000LCE has a leaner chemical composition compared to DP1000, improved hole expansion due to less difference between the phase constituents and better weldability due to lower carbon equivalent. Results are satisfactory for hot dip galvanized material and a clear improvement in forming properties was achieved. To develop guidelines of Results show, that a homogeneous hardness distribution within the how to produce the microstructure can be reached by suppressing the formation of ferrite material, by an appropriate and/or tempering of martensite alloy design, and wellA working guideline was developed successfully for all production adjusted processing routes. parameters Dilatometer trials as well as annealing simulation trials have resulted in guidelines how to produce the 1000LCE in CAL. Annealing simulations are not directly translatable to the production in CAL (some adjustments are always needed), but the simulations still have saved SSAB a number of in-line trials.
To produce these steels, with equivalent properties, through different available processing routes, i.e. continuous annealing lines with either water or gas quenching facilities, or hot dip galvanizing lines. To characterise the material for the end user including constitutive equations for the performance of the material. A comparison of the mechanical, bending, and stretch-flanging properties reveal that equivalent materials can be produced, by adjusting the ally design to the specific production lines. The properties via hot dip galvanizing route are a bit inferior compared to other routes, especially hole expansion rate is lower, although they fulfil the target properties. There is still room for improvement.

The characterisation the materials for the end user were carried out. The activities and obtained results are in agreement with the scheduled tasks and objectives. The formability of materials in terms of roll-forming and stretchflanging can be described best by the minimal bending radius and the hole expansion ratio, respectively. The end user of 1000LCE is at present satisfied with the flatness and weldability of the material but the main properties at the end user is however the forming stability in their process. Minor objectives task by task WP1 Delivery of fully Fulfilled according to project plan industrially produced material Delivery of as cold-rolled Fulfilled according to project plan material 79

Production of material with different textures through variation in the rolling sequence Processing of lab material Characterisation of properties and structures of the starting materials WP2 Determination of the cementite dissolution and austenite formation kinetics Investigation of the transformation behaviour during cooling Calculations of phase transformations Delivery of know-how WP3 Producing different microstructures and texture based on industrial processed as cold-rolled material Producing different microstructures and texture based on lab processed material Producing microstructures and textures based on the results above WP4 Mechanical testing Fracture path Void nucleation and growth Correlation Evaluation of the correlation WP5 Processing of material with optimised microstructure and texture on industrial scale Characterisation of the formability Mechanical properties as a function of strain rate, temperature and stress state Flow curves Constitutive equations and material parameters for the stamping simulations Critical evaluation of the results obtained in the R&D project WP6

Fulfilled according to project plan but could not be implemented in the final on line trials.

Performed successfully Performed successfully

Performed successfully in time

Performed successfully in time

Performed successfully in time In meetings and in reports Fulfilled according to project plan but with a delay. Texture variation in the final products too small to be able to model.

Fulfilled according to project plan

The evaluation of the mechanical properties of the laboratory samples led into improved mechanical properties

Fulfilled according to project plan Performed Performed Performed Available in this final report

In-line full scale trials, with satisfying output. Fulfilled according to project plan

Fulfilled according to project plan using tensile testing, hole expansion, bending, complete FLDs, Available in this final report

Available in this final report Constitutive equations presented in this final report

See this table

80

To ensure that the project is carried out according to agreed time and cost schedules

Provision of interim and final reports on time

The project was delayed and granted an extension with one extra year. The reason for this was twofold: The tasks of WP3 and WP4 could not run in parallel with WP2, as was intended in the initial plan, since the transformation kinetics were needed to set up the laboratory trials The financial crisis during 2009 made all on line trials impossible All reports delivered on time

2.7.5

Task 5.4 Basic characterisation of the formability based on forming limit diagrams

In the following figures (from Figure 69 to Figure 74) the FLD curves are reported for each steel grade of the industrial trials for room temperature and for elevated temperature, 80C. The position of forming limit curve depends mainly on material strength and thickness. Necking in thicker plates extends over a larger area than in thinner plates. The thicker R- and V- grades elongate more before necking than the thinner S-grades. Higher strength gives poorer formability for the same thickness for grades S9-F1 and S9-F2. Independent on test temperature all grades have better formability under biaxial stress conditions followed by uniaxial forming. All grades have poor plane strain formability. The influence of test temperature on the formability of R7-F5- and V2-F1-grades is quite high in plane strain and stretch-forming areas. High influence of test temperature was also observed for R7-F2- and S9-F2-grades in the uniaxial forming area. For S9-F1 and S9-F2 grades is the temperature influence quite high in the area of biaxial forming. For R7-F2 is the temperature influence in the plane strain forming area also quite high.
0,50 2=0 0,45 0,40 0,35 1=-22 1=2

major strain, -

0,30 0,25 RT 0,20 0,15 0,10 0,05 0,00 -0,20 80 C

-0,10

0,00

0,10

0,20

0,30

0,40

0,50

minor strain, -

Figure 69. Forming limit diagram of the R7-F2 grade (HDG)

81

0,50 2=0 0,45 0,40 0,35 1=-22 1=2

major strain, -

0,30 0,25 RT 0,20 0,15 0,10 0,05 0,00 -0,20 80 C

-0,10

0,00

0,10

0,20

0,30

0,40

0,50

minor strain, -

Figure 70. Forming limit diagram of the R7-F5 grade (HDG)

0,50 =0 0,45 0,40 0,35 major strain, 0,30 0,25
RT 80 C

1= 2

1=-22

0,20 0,15 0,10 0,05 0,00 -0,20

-0,10

0,00

0,10

0,20

0,30

0,40

0,50

minor strain, -

Figure 71. Forming limit diagram of V2-F1 grade (CAL-GQ)

82

0,55 0,50 0,45 0,40 1=-22 2=0

1=2

major strain, -

0,35 0,30 0,25 RT 0,20 0,15 0,10 0,05 0,00 -0,20 80 C

-0,10

0,00

0,10

0,20

0,30

0,40

0,50

minor strain, -

Figure 72. Forming limit diagram of V2-F2 grade, (CAL_GQ)

0,50 2=0 0,45 0,40 0,35 1=-22 1=2

major strain, -

0,30 0,25 RT 0,20 0,15 0,10 0,05 0,00 -0,20 80 C

-0,10

0,00

0,10

0,20

0,30

0,40

0,50

minor strain, -

Figure 73. Forming limit diagram of S9-F1 grade, (CAL-WQ)

83

0,50 2=0 0,45 0,40 0,35 1=-22 1=2

major strain, -

0,30 0,25 RT 0,20 0,15 0,10 0,05 0,00 -0,20 80C

-0,10

0,00

0,10

0,20

0,30

0,40

0,50

minor strain, -

Figure 74. Forming limit diagram of S9-F2 grade, (CAL-WQ)

84

2.7.6 2.7.6.1

Task 5.5 impact of the strain rate and temperature on the mechanical properties samples from industrial trials Tensile testing, room temperature and at -40 C and 100 C

Tensile tests were carried out according to DIN EN 10002 at room temperature, at -40C and 100C. All results in both longitudinal and transversal rolling direction for tests at room temperature are given in appendix 6 in chapter 5.6. Results obtained in longitudinal direction for test temperatures -40C and 100c are given in appendix 7 in chapter 5.7. The mechanical properties of all complex-phase grades are strongly dependent on test temperatures, see Figure 75. The tensile strength of these grades decrease with increasing test temperature. For dual-phase grades (S9) the influence of test temperature on mechanical properties is not significant.

Tensile strength, Rm [MPa]

1200 1000 800 -40C 600 400 200 0 R7-F2 R7-F5 V2-F1 V2-F2 S9-F1 S9-F2
20C

100C

a)

Uniform elongation, Ag [%]

14 12 10 8 6 4 2 0 R7-F2 R7-F5 V2-F1 V2-F2 S9-F1 S9-F2
-40C

20C 100C

b)

Total elongation, A80 [%]

20 15 -40C 10 5 0 R7-F2 R7-F5 V2-F1 V2-F2 S9-F1 S9-F2
20C

100C

c) Figure 75. Mechanical properties at various temperatures for the steels from the final on line trials; a) tensile strength, b) uniform elongation, c) total elongation

85

2.7.6.2

Dynamic tensile tests

To examine the strain rate sensitivity of the steel grades the dynamic tensile tests were performed at strain rates in range between 20/s and 200/s.

Figure 76. Example of sample geometry

As shown in Figure 76 the measuring length region is 12mm in length and 6mm in width. The strain has been measured with an opto-electronic device on the sample. At strain rate 20/s the force has been measured with the piezoelectric load cell and at strain rate 200/s the force was measured with strain gages on sample to reduce the oscillations in the force signal. The effect of strain rate on yield strength (Rp0.2) and tensile strength (Rm) is presented in appendix 8 in chapter 5.7 and in Figure 77.

Yield Strength, Rp0.2 [MPa]

1200 1000 800 600 400 200 0 1500 1000
20s-1 200s-1

Tensile Strength, Rm [MPa]

500 0

20s-1 200s-1

Figure 77. Strain rate sensitivity for investigated steels, a) Rp0.2 and b) Rm.
In appendix 7 in chapter 5.7, the true stress-strain data are displayed. All tested materials show slight positive strain rate sensitivity.

2.7.7

Task 5.6 impact of the strain state on mechanical properties

The Bulge test is characterised by a biaxial stress and strain state and tensile test by uniaxial stress and strain state. Bulge test is frictionless and has the advantage of better comparability with practical processes of sheet metal forming by tensile loading. For the comparison of tensile tests flow curves with the flow curves after the bulge tests, the direction dependency of tensile tests flow curves should be found. That will be done through the evaluation of the equivalent stress v and equivalent strain v according to Hill yield criteria. For the samples in transverse direction the equivalent stress and equivalent strain can be expressed as: Eq. 1 V = TR B Z 90 Where
TR true stress and

BZ 90 =

r0 (r90 + 1) 3 2 r0 r90 + r0 + r90

Eq. 2

V = TR B Z 90 1
where TR true strain.

86

Results of bulge tests and tensile tests after conversion according to Hill yield criteria (Figure 78 to Figure 80) have been compared in order to find the impact of the strain state on mechanical properties. Hydraulic bulge test provides flow curves up to very high strains. The flow curves of steels from Ruukki (R7-F2, R7-F5) and voestalpine (V2-F1, V2-F2) after biaxial and uniaxial forming are in good agreement for the region of low strains. The flow curves of the SSAB-grades (S9-F1, S9-F2) are different because of the high strain hardening for the uniaxial tensile tests at the low strains.

1400

1200

Equivalent plastic stress, MPa

1000

800

600

400

200

0 0,0 0,1 0,2 0,3 Equivalent plastic strain , R7-F2_bulge test R7-F2_tensile test R7-F5_bulge test R7-F5_tensile test

0,4

0,5

0,6

Figure 78. Strain state of R7-F2 and R7-F5

1400

1200

Equivalent plastic stress, MPa

1000

800

600

400

200

0 0,0 0,1 0,1 0,2 0,2 0,3 0,3 0,4 0,4 0,5 Equivalent plastic strain,S9-F1_bulge test S9-F1_tensile test S9-F2_bulge test S9-F2_tensile test

Figure 79. Strain state of S9-F1 and S9-F2

87

1400

1200

Equivalent plastic stress, MPa

1000

800

600

400

200

0 0,0 0,1 0,2 0,3 0,4 0,5 0,6 0,7 Equivalent plastic strain,V2-F1_bulge test V2-F1_tensile test V2-F2_bulge test V2-F2_tensile test

Figure 80. Strain state of V2-F1 and V2-F2 2.7.8 Task 5.8 constitutive modelling and determination of the parameters relevant for the selected CP grades

The individual behaviour of the individual phases has been modelled. According to model based on the dislocation theory reported by Bergstrm and Rodriguez et al.[10, 11] for ferritic and martensitic phases the flow stress can be expressed as:

= 0 + + M b
where

1 exp(Mk2 ) k2 L

Eq. 3

- const, M - Taylor factor (M=3) - shear modulus ( = 80000MPa) B - Burgers vector (b=2,5*10-10) L - dislocation mean free path (for ferrite L=d-the ferrite mean linear intercept in m) k2 - recovery rate (for ferrite: k2=10-5/d) - additional strengthening with regard to the precipitation and carbon in solution (for ferrite =5000Css; for martensite =3065[C]-161) Css - carbon in solution [C] - martensite carbon content 0 - Peierls stress (a function of chemical constituents of material in solid solution ) 0= 77+80%Mn+750%P+60%Si+80%Cu+45%Ni+60%Cr+11%Mo+5000Nss Nss - nitrogen in solid solution

According to model based on the dislocation theory reported by Parker et. al [12] for bainite the flow stress can be expressed as:

= 0 + T + M b
where

1 exp( k2 M ) k2 d L

Eq. 4

- const, M - Taylor factor (M=3) - shear modulus ( = 80000MPa) B - Burgers vector (b=2,5*10-10 m) dL- bainitic grain size, m k2 - recovery rate 0 - Peierls stress (a function of chemical constituents of material in solid solution ), MPa 0= 77+80%Mn+750%P+60%Si+80%Cu+45%Ni+60%Cr+11%Mo

88

T - temperature dependent additional strengthening with regard to precipitates, dislocations and carbon in solution,C

Where:

T = 1,36 1011T 3, 205 (C )

Eq. 5

T - transformation temperature,C

The formulated flow curves of ferrite, martensite and bainite phases with regard to model mentioned above were found to be: Ferrite: (0,002%C): =87+5310, 26 Martensite: 1200M (0,11%C): =23720,14 Martensite: 1400M (0,17%C): =35900,16 Martensite: 1700M2 (0,28%C): =30210,13 Bainite: (0,14 %C): 290+12340,13 Bainite: (0,16%C): 304+1353 0,12 Experimental flow curves obtained with fully martensitic, ferritic and bainitic microstructures (delivered by the industrial partners) together with the predictions from the models using Equations 3 and 4 are outlined in Figure 81. The modelled flow curves are taking into account the carbon distribution in single phases. It can be observed that different carbon content has a strong influence on strength of martensite and bainite.
2000 1800 1600 1400 true stress, MPa 1200 1000 800 600 400 200 0 0 0,05 0,1 0,15 0,2 true strain,0,25 0,3 0,35 0,4

0,28%C 0,17%C 0,11 %C martensite

0,16%C 0,14%C

bainite

ferrite

Eq. 5
experimental data predictions from the model

Figure 81. Experimental flow curves obtained with fully martensitic, ferritic and bainitic microstructures together with the predictions from models using Equations 1 and 2.

89

2.8

CONCLUSIONS

The following conclusions can be drawn from the work performed in this project: General conclusions: The project objectives have been met; improving the properties of steel products from three different annealing lines to obtain a tensile strength of >800MPa, a bending radii <1 and a hole expansion ratio>35%. A new steel, SSABs LCE1000, has been the outcome of this project together with adjustments of the existing process parameters and compositions for the CP-steels with Rm 800MPa at Rautaruukki and voestalpine. The properties and microstructures are not identical between the three products so there is still room for improvement. It is very difficult to obtain a bainitic structure in the CAL-WQ process due to the lack of intermediate temperature holding zones. About alloy selection and laboratory simulations: Laboratory simulations of annealing cycles, using dilatometers (for precise control of temperature schedules) and annealing simulators are useful tools in steel product development but there is always need for on line trials to ensure that the results can be transferred to full scale. Very promising results were obtained in the laboratory tests by modifying the chemical composition using Nb microalloying for HDG steels. Some additional study is still needed, in order to reduce the amount of Mo. About phase transformations and kinetic of phase transformations: The carbide dissolution kinetics will control the rate of the phase transformation if the annealing temperature is low or the soaking time is short. The kinetics varies with the chemical composition of the steel and it was shown that a Cr-addition will slow down the dissolution rate. A phase transformation close to equilibrium was usually achieved at a soaking time of 80 s or more, although much of the phase transformation is done during the heating, before the actual annealing temperature is reached. The CCT diagrams determined in the dilatometry investigations show very different behaviour for the investigated steels. It seems that the additions of slowly diffusing elements (Mn, Mo and Cr) have a stronger impact on the transformation kinetics than C. The maximum continuous cooling rate used in the dilatometry investigations was 285C/s. This was enough to describe the transformation behaviour in a CAL (continuous annealing line) with gas quenching and HDG (hot dip galvanizing), but too low of a cooling rate for a CAL with water quenching. According to the dilatometry investigations, the steel from SSAB has the poorest hardenability, due to its lean alloy composition. It requires cooling rates of more than 285C/s to transform to martensite and/or bainite. The steel from voestalpine has the highest hardenability of the three investigated steels. This is due to the high Mn-content and the Mo-addition. Bainite can be achieved at cooling rates between 50C/s and 100C/s and the material will transform to martensite at rates over 100C/s. The steel from Ruukki has an intermediate hardenability. Full martensite transformation will only be achieved at rates above 285C/s, but bainite is formed between 50C/s and 285C/s. The hardenability can be explained by the chemical composition of the Ruukki steel, which is leaner compared to the steel from voestalpine, although the Crcontent may be responsible for the extended bainite field.

91

About fracture and damage mechanisms: Failure is initiated frequently by decohesion of the matrix from inclusions. When the hard phase (e.g. martensite) appears in bands, voids form by cracking of adjacent hard phase grains. The relative hardness of the constituting phases has a marked influence on the density of voids. In microstructures with moderate hardness ratio such voids appear at higher plastic strain. Plastic failure of the ductile ferritic matrix is observed only seldom and then it is correlated with the presence of non-metallic inclusions and decohesion of the matrix from these inclusions or hard second phase. About microstructure and hole expansion (stretch-flangeability) or bending: The strength/hardness difference between the matrix phases in the microstructure must not be high. This mechanical homogeneity prevents local hot-spots of stress and/or strain in the microstructure especially at phase boundaries which act as nucleation sites for voids. Several possibilities have been tried to reach this goal for CP-grades: Reducing the grain size of the hard martensite Replacing hard martensite by softer tempered martensite or bainite. Increasing the strength of the matrix by grain size reduction, other strengthening mechanisms (solution or precipitation hardening) and /or the introduction of more bainite. Reducing the amount of soft ferrite

The experimental findings regarding bending is not as obvious as for hole expansion but the best results were achieved with the following principles: Reducing the grain size of all constituents in the microstructure. Reduce the hardness difference between different phases Replacing hard martensite and/or soft ferrite by bainite or tempered martensite. Ferrite is not poor for bending but the required strength level will not be reached if too much ferrite is present at the same time as martensite is avoided. The experimental finding for nearly fully martensitic DP-grades TS1200M with 96.5% of tempered martensite have also established that the homogeneous microstructure of this material provides high strength and good hole expansion level although the tensile elongation is low, and that this steel shows better HE than a dual phase microstructure with ferrite and martensite.

About texture: The texture investigation implies that a strong {111}-texture should be beneficial for the hole expansion properties. Manipulating the texture was considered more difficult than changing the phase constituents. It was shown that the best texture was achieved annealing in the austenite-ferrite region, a processing condition that will be difficult to use in HDG or CAL-GQ. These processes normally use full austenitisation to achieve a bainitic transformation during the isothermal holding section. Without complete transformation during annealing it is likely that the yield strength level will be too low without more additions of alloying elements. Another possibility to improve the texture is to increase the cold rolling reduction, and this was shown in laboratory trials but could not be tested in full scale. The obtained variations in crystallographic texture have been very small in all experiments except for the specific tests performed under task 1.3.

92

2.9

EXPLOITATION AND IMPACT OF THE RESEARCH RESULTS

A new steel product, SSABs LCE1000, has been the outcome of this project together with adjustments of the existing process parameters and compositions for the CP-steels with Rm 800 MPa at Rautaruukki and voestalpine. One of the major goals of this project has been to develop guidelines of how to produce the material through several processing routes, i.e. continuous annealing and hot dip galvanizing, which should make the results transferable throughout Europe. This has been successful in the lines available in this project and since the main three commercial annealing processes are covered, the results of this project will be able to benefit not only the three industrial partners of this consortium, but many other steel producers in Europe. Only minor adjustments are intended in each type of facility to produce advanced high-strength CP material. No patents have been considered since the work performed has been more of incremental improvements.

93

3. 3.1

LIST OF FIGURES, TABLES, ACRONYMS AND ABBREVIATIONS LIST OF FIGURES

Two temperature schedules were selected; one with annealing in the two phase region and one in the austenite region............................................................................................ 15 The texture is weaker if the material is annealed in the austenite region or if the cold rolling reduction is reduced. ODF sections with 2=45 .................................................... 16 The microstructure is showing approximately the same level of martensite (here in dark grey or black) and there are unrecrystallised structures in the sample with 50% cold rolling and annealed in the two phase region...................................................................... 17 Hole expansion ratio of annealed SSAB-materials with different textures ........................ 17 True stress-true strain of the as hot rolled materials. .......................................................... 18 Microstructure of the as hot rolled materials. ..................................................................... 18 True stress-true strain of the cold rolled and annealed samples. ........................................ 19 Microstructure of the DP texture materials after cold rolling and annealing. ..................... 19 True stress strain curves for the high and low cold rolling reduction ................................. 20 Microstructure of TS800 with low (LR) and high (HR) cold rolling reduction. ................ 20 The crystallographic texture of the industrially produced coils with varying texture. ODF sections with 2=45 .................................................................................................. 21 EBSD maps of the a) 56% cold rolled and b) 69% cold rolled steel. Coiling temperature after hot rolling of 600C. The orientations are coloured relative to the end orientation of the -fibre, {001}<110>........................................................................ 21 Hole expansion tests of the various cold rolling reductions and coiling temperatures ....... 22 In a) an example of cold rolled Ruukki material and in b) after annealing, HR=20/s, Tan=760C, tan=0s. In a) Picral was used as etchant and the carbides appear white. In b) Cr-acid was used as etchant and carbides appear black. ............................................ 26 Dissolution time of carbides at different temperatures for the three steels, V1, R4 and S7 (voestalpine, Ruukki and SSAB)................................................................ 27 An example of the microstructure and tensile strength of the voestalpine grade as a function of the annealing time (0s and 80s) and annealing temperature (760C -840C) . 28 A Comparison between ThermoCalc calculations and results from dilatometry and microstructures after annealing simulations show that 80s of annealing is usually very close to equilibrium for all the investigated steel. .............................................................. 29 CCT diagram for the SSAB steel, S7.................................................................................. 30 CCT diagram for the voestalpine steel, V1 ......................................................................... 31 CCT diagrams for the Ruukki Steel, R4. ............................................................................ 32 Microstructures of the SSAB steel S7, temperature 860C, cooling rate a) 1C/s b) 20C/s c) 100C/s d) 200C/s, holding time 40s, heating rate 20C/s, etched with LePera. ........... 33 Microstructures of the voestalpine steel V1, temperature 860C, cooling rate a) 1C/s b) 20C/s c) 100C/s d) 200C/s s, holding time 40s, heating rate 20C/s, etched with LePera.............................................................................................................. 33 Microstructures of the Ruukki steel R4, temperature 860C, cooling rate a) 1C/s b) 20C/s c) 100C/s d) 200C/s s, holding time 40s, heating rate 20C/s, etched with LePera ......... 33 Microstructures of CP800 of a) SSAB b) voestalpine and c) Ruukki, temperature 780C, cooling rate 20C/s, holding time 40s, heating rate 20C/s, etched with LePera ................ 34 Schematic time-temperature cycle of the lab anneals simulating a continuous annealing line with gas quenching for steel V1................................................................................... 36 Schematic time-temperature cycle of the lab anneals simulating a continuous annealing line with water quenching for steel S7. ............................................................................... 36 Schematic time-temperature cycle of the hot dip galvanizing laboratory cycles for steel R4 ............................................................................................................................... 36 Simulations of a continuous annealing line with water quenching and separate overageing. Annealing both in the austenite region as well as in the intercritical range was performed and various overageing temperatures were tested. ........................... 38 Simulations of a continuous annealing line with water quenching, soft cooling in the gas jet section and overageing. Annealing was performed in the austenite region and the overageing temperatures were set to 200C. ....................................................................... 38 94

Figure 1. Figure 2. Figure 3.

Figure 4. Figure 5. Figure 6. Figure 7. Figure 8. Figure 9. Figure 10. Figure 11. Figure 12.

Figure 13. Figure 14.

Figure 15. Figure 16. Figure 17.

Figure 18. Figure 19. Figure 20. Figure 21. Figure 22.

Figure 23. Figure 24. Figure 25. Figure 26. Figure 27. Figure 28.

Figure 29.

Figure 30.

Simulations of a continuous annealing line with gas quenching or hot dip galvanizing line. Annealing was performed in the austenite region and various overageing temperatures were tested. .................................................................................................... 38 Figure 31. Time-temperature cycle 1, 2 and 3 for the continuous annealing line CALVAS ............... 41 Figure 32. Time-temperature cycle 4 and 5 for the continuous annealing line CALVAS ................... 41 Figure 33. Time-temperature cycle for the continuous annealing line with water quenching. ............ 42 Figure 34. Time-temperature cycle for the hot dip galvanizing lab anneals. ....................................... 43 Figure 35. Experimental setup of the hole expansion test a) before the test; b) after the test .............. 45 Figure 36. Mechanical properties of laboratory produced material as a function of annealing temperature ......................................................................................................................... 47 Figure 37. Microstructures of CP-steel R5 (Nb)(a, c, e), and R6 (Mo+Nb) (b, d, f) annealing temperature (a+b) 780 C(c+d) 805 C and (e+f) 830 C, etched with LePera. .................. 48 The bar is 20 m...................................................................................................................................... 48 Figure 38. Results from the initial laboratory annealing simulations showing a) tensile strength vs. overageing temperature for CAL GQ, b) tensile strength vs. quenching temperature for CAL WQ and c) hole expansion vs. annealing temperature for the hot dip galvanizing cycle. .............................................................................. Fel! Bokmrket r inte definierat. Figure 39. Microstructures after the laboratory simulations of task 3.1. The numbers indicate the cycle tested.......................................................................................................................... 50 Figure 40. Tensile strength for all steels and cycles in task 3.2 wide range of microstructures. The lighter colours indicate too low tensile strength. ......................................................... 52 Figure 41. Bending properties for all steels and cycles in task 3.2 wide range of microstructures. The lighter colours indicate too poor bending. ................................................................... 52 Figure 42. Hole expansion for all steels and cycles in task 3.2 wide range of microstructures. The lighter colours indicate too poor HE value. ................................................................. 52 Figure 43. Cycle 1-3. Simulations of continuous annealing in the austenite region (880C), water quenching and various overageing temperatures were tested (1=400C, 2=300C, 3=200C). The bar shows 1-3 m and all images have the same magnification. .............. 53 Figure 44. Cycle 4-6. Simulations of continuous annealing in the two phase region (780C), water quenching and various overageing temperatures were tested (4=400C, 5=300C, 6=200C). The bar shows 2-3 m and all images have the same magnification. .............. 54 Figure 45. Cycle 7 - annealing in the austenite region at 880C followed by soft cooling in the gas jet section to 450C. Quenching in water and overageing at 200C The bar shows 1-2 m and all images have the same magnification. .............................................. 54 Figure 46. Cycle 8, 9 and10 - annealing in the austenite region at 880C gas quenching to various overageing temperatures 550C, 450C and 350C gas quenching to room temperature. The bar shows 1-2 m and all images have the same magnification............ 55 Figure 47. In lens micrographs of the 5 samples subjected to the continuous annealing cycle with water quenching. ......................................................................................................... 57 Figure 48. In lens micrographs of the 5 samples subjected to the continuous annealing cycle with gas cooling. ................................................................................................................. 58 Figure 49. In lens micrographs of the 5 samples subjected to the galvanizing cycle. .......................... 59 Figure 50. Tensile strength of the steels from the on line trials ........................................................... 60 Figure 51. Hole expansion of the steels from the on line trials ............................................................ 60 Figure 52. Bending results of the steels from the on line trials ............................................................ 60 Figure 53. Micro void development at 5% prestraining in DP-Grade S6-B2 and CP-Grade V1; and at 2% pre-straining in fully martensitic grade S4 .............................................................. 61 Figure 54. Fracture surface of steel samples with different microstructures........................................ 62 Figure 55. Microstructure of investigated steel samples from the industrial trials beneath the punched edge surface after HE testing at 3000x-magnification ......................................... 63 Figure 56. Hole expansion versus bending for laboratory samples and the final industrial trials. The project goals are in the lower right corner of the graph; Ri/t<1, HE>35%. ........................ 64 Figure 57. Hole expansion and bending versus tempering temperature for steels with high martensite content. .............................................................................................................. 64 Figure 58. Hole expansion ratio versus martensite content.................................................................. 65 Figure 59. Bending versus martensite content. .................................................................................... 65

95

Figure 60. Figure 61. Figure 62. Figure 63. Figure 64. Figure 65. Figure 66. Figure 67. Figure 68. Figure 69. Figure 70. Figure 71. Figure 72. Figure 73. Figure 74. Figure 75. Figure 76. Figure 77. Figure 78. Figure 79. Figure 80. Figure 81.

Effect of ferrite on the hole expansion ratio in the alloy from Ruukki. The structures are of CP-type. .................................................................................................................... 66 Yield strength as a function of a) annealing and b) soft cooling temperatures. .................. 71 Hole expansion rate as a function of a) annealing and b) soft cooling temperature. .......... 71 Optical micrographs showing the general microstructure of microalloyed composition after each annealing cycle. .................................................................................................. 72 Complex phase microstructure ........................................................................................... 73 Microstructures of industrial trials of CAL-WQ at SSAB .................................................. 74 Micrographs (Le Pera etching) of both industrially produced CP800 grades: a) Tq=680C; b) Tq=750C .................................................................................................... 77 Forming limited diagrams of industrially produced voest and Ruukki grades and industrially produced SSAB grades with varying texture. .................................................. 78 Forming limited diagrams of industrial produced materials from WP5 ............................ 78 Forming limit diagram of the R7-F2 grade (HDG)............................................................. 81 Forming limit diagram of the R7-F5 grade (HDG)............................................................. 82 Forming limit diagram of V2-F1 grade (CAL-GQ) ............................................................ 82 Forming limit diagram of V2-F2 grade, (CAL_GQ) .......................................................... 83 Forming limit diagram of S9-F1 grade, (CAL-WQ)........................................................... 83 Forming limit diagram of S9-F2 grade, (CAL-WQ)........................................................... 84 Mechanical properties at various temperatures for the steels from the final on line trials; a) tensile strength, b) uniform elongation, c) total elongation .................................. 85 Example of sample geometry.............................................................................................. 86 Strain rate sensitivity for investigated steels, a) Rp0.2 and b) Rm. .................................... 86 Strain state of R7-F2 and R7-F5 ......................................................................................... 87 Strain state of S9-F1 and S9-F2 .......................................................................................... 87 Strain state of V2-F1 and V2-F2 ......................................................................................... 88 Experimental flow curves obtained with fully martensitic, ferritic and bainitic microstructures together with the predictions from models using Equations 1 and 2. ....... 89

96

3.2

LIST OF TABLES
Selected range for alloy composition .................................................................................... 7 Chemical analysis, laboratory annealing ............................................................................... 8 Tasks of WP1 ...................................................................................................................... 13 Selected materials, (wt%) .................................................................................................... 13 Annealing temperatures ....................................................................................................... 14 Chemical composition of the industrially cold rolled materials (wt%) ............................... 14 Task 1.3 Texture programme, chemical composition, coiling and cold reduction.............. 15 As hot rolled condition: ....................................................................................................... 18 Mechanical properties of the finished products (DP-steels) ................................................ 19 Comparison of tensile data for high and low cold rolling reduction ................................... 20 Chemical compositions of the investigated steels in wt%. .................................................. 22 Summary of the phase constituents (%) and properties of the different industrially produced steels.................................................................................................................... 23 Tasks of WP2 ...................................................................................................................... 25 Chemical composition of the industrially produced CP-grades (wt%) ............................... 26 Tasks of WP3 ...................................................................................................................... 35 Chemical analysis, laboratory annealing ............................................................................. 35 Properties of the first laboratory annealed samples ............................................................. 37 Properties and microstructures obtained in task 3.2 ............................................................ 39 Chemical composition of the lab annealed samples (wt%) ................................................. 40 Annealing parameters for the five time temperature cycles ................................................ 40 Chemical composition of the lab annealed samples (wt%) ................................................. 42 Annealing parameters for the five time temperature ........................................................... 42 Chemical composition of the lab annealed samples (wt%) ................................................. 43 Annealing parameters for the five time temperature cycles ................................................ 43 Tasks of WP4 ...................................................................................................................... 45 Mechanical Properties of the industrial samples ................................................................. 46 Microstructures of the industrial samples............................................................................ 47 Microstructures and properties of the samples in task 3.2 A wide range of microstructures.................................................................................................................... 51 Microstructures and properties of the samples in task 3.3 special microstructures .......... 56 Tasks of WP5 ...................................................................................................................... 69 Chemical compositions of the investigated steels in wt%. .................................................. 69 Mechanical properties of the investigated steels. ................................................................ 69 Results from the formability tests for the investigated steels. ............................................. 70 Chemical composition used in the industrial trials [wt%]. .................................................. 70 Annealing cycles used in line trials. .................................................................................... 70 Mechanical properties of the modified composition ........................................................... 70 Forming tests. ...................................................................................................................... 71 Table 1: Chemical composition and annealing temperatures .............................................. 73 Results from tensile testing ................................................................................................. 73 Table 3: Chemical composition for dilatometer trials, [wt%] ............................................. 73 Annealing conditions ........................................................................................................... 74 Results from mechanical testing .......................................................................................... 74 Chemical composition and annealing parameters, on line trials CAL-WQ ........................ 74 Mechanical properties, on line trials CAL-WQ................................................................... 74 Chemical composition of the industrially produced CP800 grades [wt%].......................... 75 Annealing parameters for the industrial trials ..................................................................... 76 Mechanical results of both industrial trials: a) TQ=680C b) TQ=750C............................ 76 Results of the hole expansion test for both industrial trials of CAL-GQ ............................ 76 Comparison between objectives and results ........................................................................ 79

Table 1. Table 2. Table 3. Table 4. Table 5. Table 6. Table 7. Table 8. Table 9. Table 10. Table 11. Table 12. Table 13. Table 14. Table 15. Table 16. Table 17. Table 18. Table 19. Table 20. Table 21. Table 22. Table 23. Table 24. Table 25. Table 26. Table 27. Table 28. Table 29. Table 30. Table 31. Table 32. Table 33. Table 34. Table 35. Table 36. Table 37. Table 38. Table 39. Table 40. Table 41. Table 42. Table 43. Table 44. Table 45. Table 46. Table 47. Table 48. Table 49.

97

3.3

LIST OF ACRONYMS AND ABBREVIATIONS

Total elongation Uniform elongation Continuous annealing line CAL with gas coolin CAL with water quenching Continuous cooling transformation diagrams Software for EBSD analysis Complex phase, the microstructure consists of minimum 3 phases Cold rolled Coiling temperature after hot rolling Software for calculations of diffusion kinetics Dual phase, microstructure with ferrite and martensite Electron back scatter diffraction Energy dispersive spectroscopy Field emission gun scanning electron microscope Forming limit diagram Hot dip galvanizing line Hole expansion ratio Swerea KIMAB, Coordinator of the project Low carbon equivalent Bending radius Tensile strength Yield strength Rautaruukki Oyj, partner in this project Rheinisch-Westflische Technische Hochschule, partner in this project Scanning electron microscope SSAB EMEA, partner in this project Temperature of annealing Transmission electron microscope Software for calculations of thermodynamic equilibrium Overageing temperature Overageing time Quenching temperature Tensile strength voestalpine Stahl GmbH, partner in this project Work package Yield strength

A80 Ag CAL CAL-GQ CAL-WQ CCT Channel 5 CP CR CT Dictra DP EBSD EDS FEG SEM FLD HDG HE KIMAB LCE Ri/t Rm Rp0.2 Ruukki RWTH SEM SSAB Tan TEM ThermoCalc TOA tOA TQ TS voest WP YS

98

4.

LIST OF REFERENCES 1. Hashimoto, S.: Materials Science and Technology 2005 Proceedings, Developments in Sheet Products for Automotive Applications, 107-114 (2005) 2. Garcia, C.I. et al.: Materials Science and Technology 2005 Proceedings, Developments in Sheet Products for Automotive Applications, 77-86 (2005) 3. Pyshmintsev, I. Y. et al.: Steel Research 73 (2002) No. 9, 392-402. 4. Bleck, W. Frehn, A. Ohlert, J.: International Symposium on Niobium 2001, 2001 cbmm.com.br, Niobium in dual phase and TRIP steels 5. Hebesberger, T. et al.: Int. Conf. on Steels in Cars and Trucks, Steel - Future for the Automotive Industry Proceedings, 57-65 (2005) 6. W. Bleck, Proc. Int. Conf. on TRIP-Aided High Strength Ferrous Alloys, Ed. B.C. DeCooman, Ghent, Belgium, GRIPS Sparkling World of Steel Vol. 1: Proceedings, 2002, pp. 13-23. 7. http://www.key-to-steel.com/Articles/Art51.htm 8. M.C. Somani, D.A. Porter, J. Pyykknen, J. Tarkka, J. Kmi and L.P. Karjalainen, Proc. Intl. Conf. Microalloyed Steels: Processing, Microstructure, Properties and Performance (MA07), AIST, University of Pittsburgh, Pittsburgh, 2007, pp.95-106. 9. C.I. Garcia, K. Cho, Y. Gong, T.R. Chen and A.J. DeArdo, Materials Science & Technology 2005, ASM, ACerS, AIST, AWS, TMS, Pittsburgh, 2005, pp. 77-86. 10. Bergstroem, Y.: A dislocation model for the stress-strain behaviour of polycrystalline -Fe with special emphasis on the densities of mobile dislocations. Material Science and Engineering 5 (1969/1970), pp. 193-200. 11. Rodriguez, R.M. and Guitierrez, I: Unified formulation to predict the tensile curves of steels with different microstructures. Material Science Forum 426-432 (2003), pp. 4525-4530. 12. Parker, S.V et al.: Property models for mixed microstructures. Technical Steel Research, European Commission, Final report, EUR20880EN, 2003.

99

5. 5.1

APPENDICES APPENDIX 1
Designation
R1 R2 R3 S1 S2 S3 S4 S5 V1 V2 S6-A S6-B1

ALL INCLUDED STEELS PER TASK AND ANNEALING SIMULATION SCHEDULES

Supplier
Ruukki Ruukki Ruukki SSAB SSAB SSAB SSAB SSAB Voest Voest SSAB SSAB SSAB SSAB SSAB

Grade
CP800-1 CP800-2 CP800-new TS 800 TS 1000-1 TS 1000-2 TS 1200 (M) TS 1200 (DP) VA CP800-Mo VA CP800 TS 800 TS 800 TS 800 TS 800 TS 800 LAB TS 800 LAB TS 800 LAB TS 800 LAB TS 800 LAB TS 800 LAB CP800-1 Ru-4 Ru-5 CP800-1 CP800-1 CP800-1 Ru-4 Ru-4 Ru-4 Ru-5 Ru-5 Ru-5 VA CP800-Mo CP800-1 TS 800 VA CP800-Mo VA CP800-Mo VA CP800-Mo VA CP800-Mo VA CP800-Mo CP800-1 CP800-1 CP800-1 CP800-1 CP800-1 TS 800 TS 800 TS 800 TS 800 TS 800

Gauge
1.19 2.50 1.19 1.50 1.80 1.00 1.60 1.65 1.50 1.50 1.5 1.5 1.5 1.5 3.4 1.7 1.36 1.02 0.92 0.54

Condition
HDG HDG HDG CAL CAL CAL CAL CAL CAL CAL CT 515C, CR 56% CAL CT 600C, CR 56% CAL CT 600C, CR 69% CAL CT 660C, CR 56% CAL HR, CT 600C CT 600C, CR 50% CT 600C, CR 60% CT 600C, CR 70% CT 600C, CR 77% CT 600C, CR 84% CR CR CR Task 1.4 Task 1.4 Task 1.4 Task 1.4 Task 1.4 Task 1.4 Task 1.4 Task 1.4 Task 1.4

C
0.17 0.17 0.17 0.144 0.172 0.170 0.178 0.135 0.11 0.14 0.13 0.13 0.13 0.13 0.144 0.144 0.144 0.144 0.144 0.144 0.17 0.17 0.17 0.17 0.17 0.17 0.17 0.17 0.17 0.17 0.17 0.17 0.11 0.14 0.135 0.11 0.11 0.11 0.11 0.11 0.14 0.14 0.14 0.14 0.14 0.135 0.135 0.135 0.135 0.135

Mn
1.7 1.7 1.7 1.52 1.59 1.63 1.41 1.53 2.1 2.1 1.51 1.51 1.51 1.51 1.52 1.52 1.52 1.52 1.52 1.52 1.7 1.7 1.7 1.7 1.7 1.7 1.7 1.7 1.7 1.7 1.7 1.7 2.1 1.7 1.5 2.1 2.1 2.1 2.1 2.1 1.7 1.7 1.7 1.7 1.7 1.5 1.5 1.5 1.5 1.5

Si
0.18 0.18 0.18 0.48 0.51 0.47 0.44 0.18 0.15 0.2 0.21 0.21 0.21 0.21 0.48 0.48 0.48 0.48 0.48 0.48 0.18 0.18 0.18 0.18 0.18 0.18 0.18 0.18 0.18 0.18 0.18 0.18 0.15 0.18 0.5 0.15 0.15 0.15 0.15 0.15 0.18 0.18 0.18 0.18 0.18 0.5 0.5 0.5 0.5 0.5

Cr
0.3 0.3 0.3

Mo
0.15 0.15 0.16

Nb

Industrial starting material

0 0.3

0.2 0

0.018 0.017 0.017 0.016 0.015 0.02 0.02 0.015 0.015 0.015 0.015 0.018 0.018 0.018 0.018 0.018 0.018

Texture, lab materials

S6-B2 S6-C S1-HR S1-Tex1 S1-Tex2 S1-Tex3 S1-Tex4 S1-Tex5 R1-CR R5-CR R6-CR R1-B1 R1-B2 R1-B3 R5-B1 R5-B2 R5-B3 R6-B1 R6-B2 R6-B3 V1-CR R4-CR S7-CR V1-A1 V1-A2 V1-A3 V1-A4 V1-A5 R4-A1 R4-A2 R4-A3 R4-A4 R4-A5 S7-A1 S7-A2 S7-A3 S7-A4 S7-A5

Ruukki Ruukki Ruukki Ruukki Ruukki Ruukki Ruukki Ruukki Ruukki Ruukki Ruukki Ruukki Voest Ruukki SSAB Voest Voest Voest Voest Voest Ruukki Ruukki Ruukki Ruukki Ruukki SSAB SSAB SSAB SSAB SSAB 1.50 1.2 1.23 1.50 1.50 1.50 1.50 1.50 1.2 1.2 1.2 1.2 1.2 1.23 1.23 1.23 1.23 1.23

0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0 0.3 0 0 0 0 0 0.3 0.3 0.3 0.3 0.3

Task 1.4, ann. temp 780,805,830

0.15 0.15 0.15 0.15 0.15 0.015 0.015

0.15 0.15 0.15 0.2 0.15 0.2 0.2 0.2 0.2 0.2 0.15 0.15 0.15 0.15 0.15

0.015 0.015 0.015 0.015 0.015 0.015 0.02 0.015 0.02 0.02 0.02 0.02 0.02

CR CR CR Task 3.1 Task 3.1 Task 3.1 Task 3.1 Task 3.1 Task 3.1 Task 3.1 Task 3.1 Task 3.1 Task 3.1 Task 3.1 Task 3.1 Task 3.1 Task 3.1 Task 3.1

First lab simulations, task 3.1

0.015 0.015 0.015 0.015 0.015

100

Designation
V1-CR R4-CR S7-CR V1-C1 V1-C2 V1-C3 V1-C4 V1-C5 V1-C6 V1-C7 V1-C8 V1-C9 V1-C10 R4-C1 R4-C2 R4-C3 R4-C4 R4-C5 R4-C6 R4-C7 R4-C8 R4-C9 R4-C10 S7-C1 S7-C2 S7-C3 S7-C4 S7-C5 S7-C6 S7-C7 S7-C8 S7-C9 S7-C10 V2-CR R6-CR S8-CR S9-CR V2-D1 V2-D2 V2-D3 V2-D4 V2-D5 R6-D1 R6-D2 R6-D3 R6-D4 R6-D5 S8-D1 S8-D2 S8-D3 S9-D1 S9-D2 V2-F1 V2-F2 R7-F1 R7-F2 R7-F3 R7-F4 R7-F5 S9-F1 S9-F2

Grade
VA CP800-Mo CP800-1 TS 800 VA CP800-Mo VA CP800-Mo VA CP800-Mo VA CP800-Mo VA CP800-Mo VA CP800-Mo VA CP800-Mo VA CP800-Mo VA CP800-Mo VA CP800-Mo CP800-1 CP800-1 CP800-1 CP800-1 CP800-1 CP800-1 CP800-1 CP800-1 CP800-1 CP800-1 TS 800 TS 800 TS 800 TS 800 TS 800 TS 800 TS 800 TS 800 TS 800 TS 800 VA CP800 Ru-5 C756598 C720009 VA CP800 VA CP800 VA CP800 VA CP800 VA CP800 Ru-5 Ru-5 Ru-5 Ru-5 Ru-5 C756598 C756598 C756598 C720009 C720009 VA CP800 VA CP800 TS800 CP Mo Nb TS800 CP Mo Nb TS800 CP Mo Nb TS800 CP Mo Nb TS800 CP Mo Nb C720009 C720009

Supplier
Voest Ruukki SSAB Voest Voest Voest Voest Voest Voest Voest Voest Voest Voest Ruukki Ruukki Ruukki Ruukki Ruukki Ruukki Ruukki Ruukki Ruukki Ruukki SSAB SSAB SSAB SSAB SSAB SSAB SSAB SSAB SSAB SSAB Voest Ruukki SSAB SSAB Voest Voest Voest Voest Voest Ruukki Ruukki Ruukki Ruukki Ruukki SSAB SSAB SSAB SSAB SSAB Voest Voest Ruukki Ruukki Ruukki Ruukki Ruukki SSAB SSAB

Gauge
1.50 1.2 1.23 1.50 1.50 1.50 1.50 1.50 1.50 1.50 1.50 1.50 1.50 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1.23 1.23 1.23 1.23 1.23 1.23 1.23 1.23 1.23 1.23 1.50

Condition
CR CR CR Task 3.2 Task 3.2 Task 3.2 Task 3.2 Task 3.2 Task 3.2 Task 3.2 Task 3.2 Task 3.2 Task 3.2 Task 3.2 Task 3.2 Task 3.2 Task 3.2 Task 3.2 Task 3.2 Task 3.2 Task 3.2 Task 3.2 Task 3.2 Task 3.2 Task 3.2 Task 3.2 Task 3.2 Task 3.2 Task 3.2 Task 3.2 Task 3.2 Task 3.2 Task 3.2 CR CR CR CR Task 3.3 Task 3.3 Task 3.3 Task 3.3 Task 3.3 Task 3.3 Task 3.3 Task 3.3 Task 3.3 Task 3.3 Task 3.3 Task 3.3 Task 3.3 Task 3.3 Task 3.3 Task 5.1, 680 Task 5.1, 750 Task 5.1 Task 5.1 Task 5.1 Task 5.1 Task 5.1 Task 5.1, 780 Task 5.1, 795

C
0.11 0.14 0.135 0.11 0.11 0.11 0.11 0.11 0.11 0.11 0.11 0.11 0.11 0.14 0.14 0.14 0.14 0.14 0.14 0.14 0.14 0.14 0.14 0.135 0.135 0.135 0.135 0.135 0.135 0.135 0.135 0.135 0.135 0.14 0.17 0.125 0.13 0.14 0.14 0.14 0.14 0.14 0.17 0.17 0.17 0.17 0.17 0.125 0.125 0.125 0.13 0.13 0.14 0.14 0.15 0.15 0.15 0.15 0.15 0.13 0.13

Mn
2.1 1.7 1.5 2.1 2.1 2.1 2.1 2.1 2.1 2.1 2.1 2.1 2.1 1.7 1.7 1.7 1.7 1.7 1.7 1.7 1.7 1.7 1.7 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 2.1 1.7 1.52 1.0 2.1 2.1 2.1 2.1 2.1 1.7 1.7 1.7 1.7 1.7 1.52 1.52 1.52 1.0 1.0 2.1 2.1 1.7 1.7 1.7 1.7 1.7 1.0 1.0

Si
0.15 0.18 0.5 0.15 0.15 0.15 0.15 0.15 0.15 0.15 0.15 0.15 0.15 0.18 0.18 0.18 0.18 0.18 0.18 0.18 0.18 0.18 0.18 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.2 0.18 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.18 0.18 0.18 0.18 0.18 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2

Cr
0 0.3 0 0 0 0 0 0 0 0 0 0 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3

Mo
0.2 0.15 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.15 0.15 0.15 0.15 0.15 0.15 0.15 0.15 0.15 0.15

Nb
0.02 0.015 0.02 0.02 0.02 0.02 0.02 0.02 0.02 0.02 0.02 0.02

Task 3.2, annealing simulator

0.015 0.015 0.015 0.015 0.015 0.015 0.015 0.015 0.015 0.015 0.3 0.3 0 0.15 0.02 0.015 0.015 0.015 0.02 0.02 0.02 0.02 0.02 0.015 0.015 0.015 0.015 0.015 0.015 0.015 0.015 0.015 0.015 0.02 0.02 0.01 0.01 0.01 0.01 0.01 0.015 0.015

Task 3.3, dedicated lab anneals

1.50 1.50 1.50 1.50 1.50

0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3

0 0 0 0 0 0.15 0.15 0.15 0.15 0.15

Final industrial trials

1.50 1.50 1.5 1.5 1.5 1.5 1.5

0.3 0.3 0.3 0.3 0.3 0.3 0.3

0 0 0.15 0.15 0.15 0.15 0.15

101

Task 3.1 See page 3536 Task 3.2 Annealing cycles

Cycle 1 Cycle 2 Cycle 3 Cycle 4 Cycle 5

t [s] 0 43 133 133 153 183 203

Cycle 6

T [ C] 25 880 880 25 400 400 25

t [s] 0 43 133 133 153 183 203

Cycle 7

T [ C] 25 880 880 25 300 300 25

t [s] 0 43 133 133 153 183 203

Cycle 8

T [ C] 25 880 880 25 200 200 25

t [s] 0 43 133 133 153 183 203

Cycle 9

T [ C] 25 780 780 25 400 400 25

t [s] 0 43 133 133 153 183 203

Cycle 10

T [ C] 25 780 780 25 300 300 25

t [s] 0 43 133 133 153 183 203

T [ C] 25 780 780 25 200 200 25

t [s] 0 43 133 154.5 154.5 164.5 184.5 194.5

T [ C] 25 880 880 450 25 200 200 25

t [s] 0 43 133 143 173 198

T [ C] 25 880 880 550 550 25

t [s] 0 43 133 143 173 198

T [ C] 25 880 880 450 450 25

t [s] 0 43 133 143 173 198

T [ C] 25 880 880 350 350 25

Task 3.3 Simulation of continuous annealing with gas quenching (V-materials)

Cycle 1 t [s] 0.00 261.16 377.75 389.49 400.25 409.80 821.03 916.42 924.44 T [ C] 20.00 840.00 840.00 680.00 680.00 350.00 350.00 150.00 20.00 Cycle 2 t [s] 0.00 261.16 377.75 389.49 400.25 409.80 821.03 916.42 924.44 T [ C] 20.00 840.00 840.00 680.00 680.00 375.00 375.00 150.00 20.00 Cycle 3 t [s] 0.00 261.16 377.75 389.49 400.25 409.80 821.03 916.42 924.44 T [ C] 20.00 840.00 840.00 680.00 680.00 400.00 400.00 150.00 20.00 Cycle 4 t [s] 0.00 261.16 377.75 389.49 400.25 409.80 821.03 916.42 924.44 T [ C] 20.00 840.00 840.00 750.00 750.00 350.00 350.00 150.00 20.00 Cycle 5 t [s] 0.00 261.16 377.75 389.49 400.25 409.80 821.03 916.42 924.44 T [ C] 20.00 840.00 840.00 750.00 750.00 400.00 400.00 150.00 20.00

Simulation of continuous annealing with water quenching (S-materials)

Steel S8 Cycle 1 t [s] 0 18 68 142 230 250 250 277 337 372 T [ C] 25 200 665 865 880 650 25 200 200 25 Cycle 2 t [s] 0 18 68 141 230 250 250 276 336 371 T [ C] 25 200 665 835 850 700 25 200 200 25 Cycle 3 t [s] 0 18 68 141 230 250 250 276 336 371 T [ C] 25 200 665 835 850 650 25 200 200 25 Steel S9 Cycle 1 t [s] 0 18 68 129 217 237 238 264 324 359 T [ C] 25 200 665 830 845 830 25 200 200 25 Cycle 2 t [s] 0 18 68 129 217 237 238 264 324 359 T [ C] 25 200 665 830 845 795 25 200 200 25

Simulation of hot dip galvanising (R-materials)

Cycle 1 t [s] 0 200 272 309 321 416 526 T [ C] 25 830 830 740 480 465 25 Cycle 2 t [s] 0 200 272 309 321 416 526 T [ C] 25 860 860 740 480 465 25 Cycle 3 t [s] 0 200 272 309 321 416 526 T [ C] 25 900 900 780 480 465 25 Cycle 4 t [s] 0 200 272 309 321 336 446 T [ C] 25 860 860 740 480 465 25 Cycle 5 t [s] 0 200 272 309 321 416 526 T [ C] 25 830 830 800 480 465 25

102

5.2

APPENDIX 2 RESULTS FROM INDUSTRIALLY PRODUCED MATERIAL WITH VARYING TEXTURE, TASK 1.3.
r n HE % 0.92 1.07 0.86 1.06 0.81 0.96 0.81 0.92 0.09 0.09 0.11 0.11 0.12 0.12 0.11 0.12 37 44 51 48

Mechanical Properties of the industrially produced material with varying texture Sample Dir Cold Coiling YS TS Ag A 80 remark rolling temperature MPa MPa % % C %
S6-A 0 90 S6-B1 0 90 S6-B2 0 90 S6-C 0 90 56 56 56 56 69 69 56 56 515 515 600 600 600 600 660 660 591 571 541 532 553 559 564 548 881 887 816 825 825 835 831 866 8.3 8.4 9.4 9.5 10.8 10.3 9.8 9.2 13 14 15 15 16 15 15 14 r8, n4-8 r8, n4-8 r8, n4-8 r8, n4-8 r8, n4-8 r8, n4-8 r8, n4-8 r8, n4-8

5.3

APPENDIX 3 Cycle

RESULTS FROM INITIAL LABORATORY SIMULATIONS, TASK 3.1 TQ [C] 700 700 700 700 700 Tan [C] 780 760 800 840 840 Tan [C] 830 830 780 780 805 TOA [C] 500 450 400 350 300 TQ [C] 730 710 400 680 400 tan [s] 48 95 48 95 95 Gauge [mm] 1.52 1.52 1.51 1.52 1.53 Rp0.2 [MPa] 509 411 437 466 478 Rm [MPa] 898 766 597 806 851 Ag [%] 8.3 12.7 13.0 10.2 9.1 A80 [%] 11.7 18.0 18.3 14.5 12.2 HE [%] 49 64 73 71 55

V1-A1 V1-A2 V1-A3 V1-A4 V1-A5

1 2 3 4 5

S7-A1 S7-A2 S7-A3 S7-A4 S7-A5

6 7 8 9 10

1.24 1.23 1.23 1.23 1.23

576 541 374 685 388

1143 1116 791 1078 790

4.9 7.5 15.8 2.3 16.2

5.6 8.7 19.8 3.5 21.8

16 14 23 10 29

R4-A1 R4-A2 R4-A3 R4-A4 R4-A5

11 12 13 14 15

1.24 1.18 1.18 1.18 1.18

530 529 438 422 498

812 801 821 807 801

9.3 8.3 8.1 7.1 7.3

13.3 11.2 11.6 10.3 11.1

59 60 36 32 64

103

5.4

APPENDIX 4 RESULTS FROM LABORATORY SIMULATIONS OF A WIDE RANGE OF MICROSTRUCTURES, TASK 3.2

Tensile test and HE results on the laboratory anneals of the R4 steel in task 3.2 Sample dir ReH ReL YS TS Ag A25 remark r -ID MPa MPa MPa MPa % % R4-C1 0 1216 1245 2.2 5 r2,n1,5-2,5 1.27 R4-C2 0 1230 1373 3.2 7.4 r2,n1,5-3,5 0.73 R4-C3 0 1211 1450 2.3 5.8 r2,n1-3 1.52 R4-C4 0 1190 1170 1171 1190 5.2 6.5 R4-C5* 0 1285 1376 2.5 2.9 R4-C6* 0 1241 1488 2.6 3.2 R4-C7* 0 705 1122 7.1 8.5 r4,n4-6 0.75 R4-C8 0 608 1046 10 16.1 r8,n4-8 0.82 R4-C9 0 658 851 8.3 13.4 r4,n4-8 0.93 R4-C10 0 690 920 5.7 10.5 r2,n2-4 1.33 Tensile test and HE results on the laboratory anneals of the V1 steel in task 3.2 Sampledir ReH ReL YS TS Ag A25 remark r ID MPa MPa MPa MPa % % V1-C1* 0 1220 1169 1172 1172 0.2 2.4 V1-C2** 0 0 0 859 898 1.4 3.5 V1-C3* 0 1159 1141 1141 1145 0.9 4.3 V1-C4 0 0 0 910 947 1.6 4.1 V1-C5* 0 0 0 900 950 0.2 0.2 V1-C6 0 0 0 907 1145 4.8 9.4 r4,n2-5 0.86 V1-C7 0 0 0 676 948 3.3 5.6 r2,n1-3 0.87 V1-C8 0 0 0 602 985 9.2 12.1 r8,n4-8 0.81 V1-C9 0 0 0 597 788 11.8 18.5 r8,n4-8 0.54 V1-C10 0 0 0 605 856 8.3 12.8 r4,n4-6 0.68 * - Fracture outside the gauge length ** - Values seems to be too low Tensile test and HE results on the laboratory anneals of the S7 steel in task 3.2 Sampledir ReH ReL YS TS Ag A25 remark ID MPa MPa MPa MPa % % S7-C1 0 962 941 938 973 3.6 8.7 S7-C2 0 0 0 911 930 5.2 7.3 S7-C3* 0 0 0 1181 1383 1.4 1.5 S7-C4 0 0 0 699 833 5.8 11.1 r2,n 4-6 S7-C5 0 0 0 872 1137 6.1 10.7 r4,n2-4 S7-C6* 0 0 0 551 962 9.5 10.8 r2,n4-6 S7-C7* 0 0 0 446 779 14.6 19.2 r8,n5-10 S7-C8* 0 506 520 499 603 11.3 13 r8,n4-8 S7-C9* 0 0 0 484 664 5.5 6.2 r2,n2-4 S7-C10* 0 0 0 391 665 5.1 5.1 R2,n2-4 * - Fracture outside the gauge length

n
0.03 0.05 0.07 0.14 0.15 0.10 0.09

HE
% 88 87 69 83 73 44 22 16 59 49

n
0.08 0.10 0.13 0.14 0.11

HE
% 52 73 72 42 33 29 38 24 71 45

r
0.65 0.7 0.71 0.76 0.83 0.51 0.59

n
0.09 0.08 0.08 0.16 0.13 0.13 0.24

HE
% 57 51 33 33 26 23 24 84 48 28

104

5.5

APPENDIX 5 RESULTS FROM LABORATORY SIMULATIONS OF DEDICATED MICROSTRUCTURES, TASK 3.3

Dir 90 0 45 90 0 45 90 0 45 90 0 45 90 0 45 Rp0.2 MPa 538 479 486 526 523 540 580 489 563 541 496 551 505 481 523 Rm MPa 789 819 808 777 767 798 790 804 802 825 826 810 798 843 802 Ag % 12.1 9.9 11.2 10.5 8.3 8.5 10.3 10.1 8 11.6 12.8 12.7 12.2 10.4 12.3 A80 % 15.9 12.5 13.8 14.5 11.9 9.5 15 14.1 12 16 17 19.2 16.2 14.1 15.5 remark r8, n5-10 r4, n4-8 r8, n5-10 r8, n5-10 r4, n4-8 r8, n4-8 r10, n4-8 r10, n 5-10 r6, n4-8 r4, n5-10 r10, n5-10 r4, n5-10 r10, n5-10 r8, n5-10 r8, n5-10 r 0.91 0.64 0.83 0.96 0.74 0.98 0.96 0.87 0.87 0.84 0.86 0.95 0.91 0.71 0.98 n 0.15 0.15 0.16 0.15 0.15 0.15 0.14 0.16 0.14 0.15 0.17 0.14 0.15 0.15 0.15 Ri/t HE % 32

Tensile test results on the laboratory anneals from task 3.3, hot dip galvanizing
Sample HDG R4-D1 R4-D1 R4-D1 R4-D2 R4-D2 R4-D2 R4-D3 R4-D3 R4-D3 R4-D4 R4-D4 R4-D4 R4-D5 R4-D5 R4-D5

0.3-1.3 40 0.3-0.7 44 0.3-0.7 40 0.3-0.7 39 0.3-0.7

Tensile test results on the laboratory anneals from task 3.3, CAL with gas quenching
Sample CAL-GQ V1-D1 V1-D1 V1-D1 V1-D2 V1-D2 V1-D2 V1-D3 V1-D3 V1-D3 V1-D4 V1-D4 V1-D4 V1-D5 V1-D5 V1-D5 Dir 90 0 45 90 0 45 90 0 45 90 0 45 90 0 45 Rp0.2 MPa 608 612 626 616 632 642 490 641 631 576 667 686 535 663 663 Rm MPa 885 842 848 804 803 801 803 819 815 877 831 865 866 812 815 Ag % 9.3 9.5 10.9 9.7 10.2 10.6 10.5 11.2 12.7 9.8 9.2 9.1 10.2 10.3 10.7 A80 % 11.0 13.8 16.2 14.3 14.0 14.6 14.8 15.7 18.8 14.2 13.2 13.4 12.1 15.2 15.6 remark r10, n5-10 r10, n5-10 r10, n5-10 r10, n5-10 r10, n5-10 r10, n5-10 r10, n5-10 r10, n5-10 r10, n5-10 r10, n5-10 r10, n5-10 r8, n4-8 R10, n5-10 r10, n5-10 r10, n5-10 r 0.66 0.86 0.88 0.89 0.87 0.82 0.66 0.86 0.87 0.75 0.77 0.84 0.82 0.84 1.23 n 0.13 0.12 0.12 0.12 0.13 0.12 0.13 0.16 0.14 0.13 0.11 0.11 0.14 0.13 0.13 Ri/t HE % 75

<0.5 84 <0.5 83 0.5-1.0 75 <0.5 79 <0.5

Tensile test results on the laboratory anneals from task 3.3, CAL with water quenching
Sample CAL-WQ S8-D1 S8-D1 S8-D1 S8-D2 S8-D2 * S8-D3 S8-D3 S8-D3 S9-D1 S9-D1 S9-D1* S9-D2 S9-D2 Dir 90 0 45 90 0 90 0 45 90 0 45 90 0 Rp0.2 MPa 685 588 601 1061 1062 521 532 529 654 663 557 521 617 Rm MPa 1020 1033 994 1273 1305 960 981 933 950 920 806 921 975 Ag % 5.6 6 6.8 2.1 2.9 10.7 7.4 9.7 2.3 3.7 3.6 2.2 2.1 A80 % 6.8 7.2 7.4 2.2 4.3 12.9 9.7 9.9 2.4 4.6 3.7 2.3 2.2 remark r4, n4-6 r6, n4-6 r6, n4-6 r2, n2,5-3,5 r10, n5-10 r6, n4-8 r8, n4-6 r8, n4-8 r 0.56 0.56 0.91 0.69 0.85 0.69 0.75 1.24 n 0.11 0.11 0.13 0.05 0.14 0.13 0.14 0.15 Ri/t HE % 25

1.7 34 1.7 23 1.7 44 1.0 48 0.5-1.0

* - fracture outside the gauge length

105

5.6

APPENDIX 6

RESULTS FROM FINAL ON LINE TRIALS, TASK 5.1

Tensile tests data from steels from the final industrial trial, T=296K Sample
R7_F2 R7_F2 R7_F5 R7_F5 V2_F1 V2_F1 V2_F2 V2_F2 S9_F1 S9_F1 S9_F2 S9_F2

Dir
90 0 90 0 90 0 90 0 90 0 90 0

Rp0.2 MPa 665 643 595 580 664 637 706 705 625 639 748 729

Rm MPa 814 809 790 789 867 851 855 847 1004 995 1101 1082

Ag % 8.6 9.2 10.9 12.0 8 9.1 6.7 7.2 7.6 8.4 5.5 6.7

A80 % 15.8 14.7 15.5 18.4 12.2 13.9 11.8 12.1 8.11 11 7.1 9.3

remark
r8, n4-8 r8, n4-8 r10, n5-10 r10, n5-10 r8, n4-8 r8, n4-8 r4, n4-6 r4, n4-6 r4, n3-5 r4, n3-5 r4, n 3-5 r4, n2-6

r
0.92 0.86 0.97 0.83 1.04 0.76 1.09 0.78 0.62 0.67 0.50 0.82

n
0.09 0.10 0.12 0.12 0.09 0.10 0.08 0.09 0.10 0.11 0.09 0.08

Ri/t
0.5 0.7 NA NA 0.5 0.8 0.5 0.8 NA NA 0.8 1.0

HE %
44 39 56 48 38 46

5.7

APPENDIX 7 RESULTS FROM FINAL ON LINE TRIALS; EFFECT OF STRAIN RATE AND TEMPERATURE, TASK 5.5

Tensile tests data on industrial trial materials measured at different test temperatures, -40C, 100C SampleID
R7_F2* R7_F2* R7_F5 R7_F5 V2_F1 V2_F1 V2_F2 V2_F2 S9_F1 S9_F1 S9_F2 S9_F2

Test temp K 233 373 233 373 233 373 233 373 233 373 233 373

dir
0 0 0 0 0 0 0 0 0 0 0 0

YS
MPa 671 648 560 576 670 687 679 693 697 636 769 721

TS
MPa 866 808 881 740 925 826 910 826 1070 1004 1117 1127

Ag
% 9,8 8,6 11,5 7,8 10,4 6,7 10,3 4,5 8,3 7,9 7,2 7,3

A80
% 16,4 8,6 18,1 12,2 18,2 12,0 18,5 7,3 11,5 9,6 10,5 8,1

remark
r8, n 4-8 r4, n 2-4 r6, n6-10 r4, n2-4 r8, n5-10 r4, n2-4 r8, n5-10 r4, n2-4 r6, n4-8 r4, n3-5 r6, n4-8 r4, n3-5

r
0,88 0,93 0,69 0,82 0,76 0,79 0,87 0,90 1,01 0,83 0,89 0,77

n
0,12 0,09 0,11 0,12 0,11 0,09 0,12 0,08 0,10 0,09 0,09 0,09

Tensile tests data on industrial trial materials measured at strain rate 20 s-1 and 200 s-1. Material Strain rate, s-1 Rp0.2, MPa Rm, MPa 20 660 842 R7-F2 200 745 923 20 569 833 R7-F5 200 656 877 20 700 888 V2-F1 200 870 978 20 732 879 V2-F2 200 805 926 20 799 1030 S9-F1 200 962 1120 20 893 1109 S9-F2 200 1050 1227

106

1200

1000

true stress, MPa

800

600

400

200

0 0 0,02 0,04 0,06 0,08 0,1 0,12 0,14 0,16

true plastic strain, flow curve spline (RUQA0001, 18.728/s) flow curve spline (RUQA0003, 22.253/s) flow curve spline (RUQC0002, 195.650/s) flow curve spline (RUQA0002, 22.997/s) flow curve spline (RUQC0001, 193.037/s) flow curve spline (RUQC0003, 185.164/s)

Smoothed flow curves of R7-F2 at strain rates 20 and 200/s

1200

1000

true stress, MPa

800

600

400

200

0 0 0,02 0,04 0,06 0,08 0,1 0,12 0,14 0,16

true plastic strain, flow curve spline (RUF1QA02, 20.556/s) flow curve spline (RUF1QA04, 17.574/s) flow curve spline (RUF1QC02, 181.402/s) flow curve spline (RUF1QA03, 20.149/s) flow curve spline (RUF1QC01, 181.467/s) flow curve spline (RUF1QC03, 182.501/s)

Smoothed flow curves of R7-F5 at strain rates 20 and 200/s

107

1200

1000

true stress, MPa

800

600

400

200

0 0 0,02 0,04 0,06 0,08 0,1 0,12

true plastic strain, flow curve spline (VAF1QA01, 17.047/s) flow curve spline (VAF1QA03, 21.051/s) flow curve spline (VAF1QC02, 187.795/s) flow curve spline (VAF1QA02, 17.816/s) flow curve spline (VAF1QC01, 196.401/s) flow curve spline (VAF1QC03, 195.142/s)

Smoothed flow curves of V2-F1 at strain rates 20 and 200/s

1200 1000 true stress, MPa 800 600 400 200 0 0 0,02 0,04 0,06 true plastic strain, flow curve spline (VAF4QA01, 21.061/s) flow curve spline (VAF4QA03, 19.909/s) flow curve spline (VAF4QC02, 201.678/s) flow curve spline (VAF4QA02, 17.351/s) flow curve spline (VAF4QC01, 217.686/s) flow curve spline (VAF4QC03, 194.605/s)

0,08

0,1

0,12

Smoothed flow curves of V2-F2 at strain rates 20 and 200/s

108

1400 1200 1000 800 600 400 200 0 0 0,01 0,02 0,03 0,04 0,05 0,06 0,07 0,08 0,09

true stress, MPa

true plastic strain, flow curve spline (SB1QA001, 18.614/s) flow curve spline (SB1QC001, 187.161/s) flow curve spline (SB1QC003, 191.838/s) flow curve spline (SB1QA002, 18.011/s) flow curve spline (SB1QC002, 191.116/s)

Smoothed flow curves of S9-F1 at strain rates 20 and 200/s

1400 1200 1000

true stress, MPa

800 600 400 200 0 0 0,01 0,02 0,03 0,04 0,05 0,06 0,07 0,08 0,09

true plastic strain, flow curve spline (SB2QA001, 21.554/s) flow curve spline (SB2QA002, 21.309/s)
flow curve spline (SB2QC001, 205.109/s) flow curve spline (SB2QC002, 214.881/s)

Smoothed flow curves of S9-F2 at strain rates 20 and 200/s

109

European Commission EUR 25041  Cold-rolled complex-phase (CP) steel grades with optimised bendability, stretch-flangeability and anisotropy (CP-Steels) L. Ryde, O. Lyytinen, P. Peura, M. Titova, Y. Vilander Granbom, T. Hebesberger Luxembourg: Publications Office of the European Union 2012 109 pp. 21 29.7 cm Research Fund for Coal and Steel series ISBN 978-92-79-22146-0 doi:10.2777/97678 ISSN 1831-9424

HOW TO OBTAIN EU PUBLICATIONS

Free publications: via EU Bookshop (http://bookshop.europa.eu); at the European Unions representations or delegations. You can obtain their contact details on the Internet (http://ec.europa.eu) or by sending a fax to +352 2929-42758. Priced publications: via EU Bookshop (http://bookshop.europa.eu). Priced subscriptions (e.g. annual series of the Official Journal of the European Union and reports of cases before the Court of Justice of the European Union): via one of the sales agents of the Publications Office of the European Union (http://publications.europa.eu/others/agents/index_en.htm).

This RFCS project started on 1 July 2006 and was coordinated by Swerea KIMAB. Other partners engaged in the project were Ruukki Metals Oyj (Ruukki), Rheinisch-Westflische Technische Hochschule (RWTH), SSAB EMEA (SSAB) and voestalpine Stahl GmbH (voest). This final technical report includes contributions from all partners and describes the results of the research carried out over the entire project. The overall goal of this project was to identify microstructures with optimised balance between strength, bendability and stretch-flangeability and to develop guidelines on how to produce this cold rolled sheet steel through three processing routes, i.e. by continuous annealing with gas cooling, continuous annealing with quenching, and the third route was hot dip galvanizing. The objectives were to produce material with the following properties: a tensile strength of more than 800 MPa, a hole expansion ratio (HE) of more than 35 % and a bending angle, Ri/t<1. This has been obtained through a sequential narrowing of the processing parameters and the chemical composition, using laboratory simulations in several steps in parallel with some on line trials. The final results were then achieved in full scale trials. The required property goals for the project were reached for all processing routes, although their different design has introduced differences in the microstructures that are reflected in the properties.

KI-NA-25041-EN-N