Journal of Materials Processing Technology 212 (2012) 18021809

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Journal of Materials Processing Technology

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Effect of carburising on geometrical control during quenching of martensitic sheet steel channels
D.M. Fabijanic a , T.B. Hilditch b,
a b

Institute for Technology Research and Innovation, Deakin University, Waurn Ponds, Victoria 3217, Australia School of Engineering, Deakin University, Waurn Ponds, Victoria 3217, Australia

a r t i c l e

i n f o

a b s t r a c t
The impact of component orientation and selective carburising is examined on the distortion during quenching of post-forming heat-treated (PFHT) channels using three different strength martensitic steel grades. The results show that the minimal, though unpredictable distortion that occurred during quenching of uncarburised channels was conned to either an opening or closing of the channel wall angle. It is also shown that selective carburising on a given surface of the channel will cause a signicant change in the shape of the channel during quenching, which is related to the depth of carburising. 2012 Elsevier B.V. All rights reserved.

Article history: Received 30 September 2011 Received in revised form 29 March 2012 Accepted 31 March 2012 Available online 10 April 2012 Keywords: Martensitic steel Post form heat treat Carburizing Springback Quench distortion

1. Introduction Recent trends in the automotive industry have been to use increasingly stronger steels in body structure applications to allow weight and fuel savings. The classes of sheet steels that have been typically introduced to the automotive industry include both advanced high strength steels (AHSS) and ultra high strength steels (UHSS). While AHSS such as TRIP and dual-phase can be stamped at room temperature, there are issues related to die wear based on the high forming loads as shown by Pereira et al. (2008) and dimensional accuracy of components, including springback and curl as shown by Granzow (1983). The drawback of ultra high strength steels (UHSS), such as Martensitic steels, is that they have very limited formability at room temperature. This limited formability means that they can only be formed at room temperature into relatively simple geometries. To allow more complex component geometries to be formed from martensitic sheet steels, hot stamping is conventionally used, in either the direct or indirect method. Direct hot stamping is a process where the sheet steel is austenitised at approximately 950 C and subsequently formed. At this elevated temperatures the formability of the steel is signicantly enhanced. The formed component is then quenched in the die/press to obtain a martensitic microstructure. In the indirect hot stamping method the

Corresponding author. Tel.: +61 3 52272265; fax: +61 3 72272028. E-mail address: tim.hilditch@deakin.edu.au (T.B. Hilditch). 0924-0136/$ see front matter 2012 Elsevier B.V. All rights reserved. http://dx.doi.org/10.1016/j.jmatprotec.2012.03.026

component is partially cold-formed before austenitising and subsequently placed in a die for calibration and quenching. As oxidation and decarburisation of the steel is a signicant factor at these temperatures, a coating is typically applied as shown by Karbasian and Tekkaya (2010). Further, to extend the life of the tooling, it is common for a wear and oxidation resistant die coating to be applied. While hot stamping is currently used in the automotive industry, it does require expensive and specialised equipment. A potential alternative to hot stamping for martensitic sheet steels is the post-forming heat treatment (PFHT) process. In this process the steel is formed at room temperature while the microstructure is in an annealed, or softened state. The formed component is subsequently heat-treated and quenched to form a high strength microstructure. This process is similar to the indirect hot stamping method; however, dies are not used for nal forming at elevated temperature or for quenching. Another benet is that it is easier to use a protective atmosphere while heat treating than for hot stamping, removing the need for expensive coatings. While this process is not commonly used in sheet forming, Shanmugam and Karthikeyan (2004) have successfully used PFHT in the tube-forming of dual-phase steels. One potential issue for PFHT is that of shape change, or distortion, during the quench. In the hot-stamping process, the component is quenched in the die, which prevents distortion from occurring. Hilditch et al. (2007a) have recently shown during PFHT of dual-phase sheet steels without the use of dies or xtures during heat treating that quench distortion is an important factor and dependent on the orientation

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of the component during the quench. The cause of this behaviour can be linked to quenching process parameters such as the heat transfer coefcient, which Li et al. (2006) have shown can have a signicant effect on residual stress and consequently component distortion. This current study will examine the PFHT of martensitic sheet channels, proposing a novel method to control shape deviation by selectively introducing surface compressive stresses via a short carburisation process during heat treating. Acht et al. (2007) have shown that distortion caused by compressive residual stresses in carburising processes are strongly inuenced by the carburising depth and component thickness. Henriksen et al. (1992) showed that increased carbon concentration generated a competing effect on the magnitude of compressive residual stress by increasing both the lattice strain and amount of retained austenite in the carburised layer. A simple channel section component was used in the current study as it represents the geometry of reinforcement components typically manufactured from martensitic sheet steels in the automotive industry.

2.3. Post form heat treatment and carburising Table 2 outlines the experimental conditions used in this study. Specimens were heated in a uid bed furnace to a temperature of 925 C using a bed of aluminium oxide sand uidised with high purity nitrogen for 30 min and immediately quenched by dropping vertically into a bath of water at ambient temperature. The austenitising temperature for the three martensitic steels was kept constant and not optimised as a function of carbon content. Channels were loosely xed in the uid bed with wire to maintain a specic orientation during heat-treating and quenching without being constrained enough to restrict part distortion. Channels were quenched in two different orientations as shown in Table 2; crowndown and crown-up. 20 70 mm at strips of each martensitic grade were carburised on one side only for 10 and 30 min (at strip selective carburising). Carburising was performed in the same uid bed using an atmosphere of 15 vol.% propane, balance nitrogen. Selective carburising was achieved by the use of a water-based ceramic stop-off slurry painted on one side which formed an effective barrier to carbon diffusion. After carburising the strips were quenched in water. The radius of curvature (R) was calculated using Eq. (1) by measuring the height of the arc (h) for each strip over a nominal chord length (C) of 50 mm. h (C/2) + 2 2h
2

2. Methodology 2.1. Material and annealing treatment Three commercially produced martensitic steels were used in this study. Table 1 shows the chemical composition and nominal thickness of each. To achieve the softened state for cold forming, the steels were annealed at 1000 C for 15 min to ensure the martensitic microstructure transformed to austenite. After annealing, the specimens were slow cooled to room temperature in order to avoid the martensitic transformation. Note that in an industrial application it would obviously be ideal to receive the sheet in an already annealed condition.

R=

(1)

2.2. Channel forming 175 mm by 37 mm blanks in the as-received and annealed condition were formed into a simple channel sections using an Erichsen sheet metal former with a square 55 mm punch and square 60.25 mm die. Both the punch and die had 6 mm radius corners. A blank-holder force of 5 kN was used and the depth of draw was set at 45 mm. To reduce friction and prevent damage to the punch and die, the blanks were brushed with oil and a thin layer of plastic sheet material adhered to the blanks utilising the adhesive properties of the oil. To measure springback, trace outlines of the channels sections were prepared by digitally scanning a painted edge. Springback was measured as the angular deviation, , from the ideal channel shape (90 angle between crown and wall), neglecting the effects of sidewall curl. The measurement process is described in detail in Hilditch et al. (2007b) with the measurement uncertainty for the springback angle approximately 0.5 . It should be noted that a negative change in channel wall angle corresponds to a decrease in the springback angle, and vice versa for a positive change. The maximum press force required to form the specimens was also recorded for evaluation.
Table 1 Chemical composition of the examined steel in wt%. C Mart900 Mart1300 Mart1500 0.08 0.16 0.23 Mn 0.50 0.50 0.40 Si 0.00 0.19 0.20 Al 0.06 0.06 0.06 Cr 0.02 0.02 0.02 Nb 0.000 0.002 0.070

Two methods were utilised to achieve selective carburising for the channels; directional gas ow and selective masking. The directional gas ow method was based on the principle that the faces of the channel directly in the path of the gas ow (gas bubbled from bottom of uid bed reactor) would experience a higher carburising effect than the other faces. Selective carburising by directional gas ow was performed on Mart900 channels for 30 min in both crown-down and crown-up orientations and 10 min in the crowndown orientation. Selective masking was performed on Mart900 channels orientated in the crown down position only for 10 min, where alternatively only the inside or outside faces were masked. The total depth of the carburised case was determined by hardness proles (FutureTech microVickers, 50 gf, 10 s dwell time). Cross-sectional optical micrographs were prepared by standard metallographic techniques and then etched with 2% nital solution. The carbon concentration prole in the surface region was determined by Glow Discharge Optical Emission Spectroscopy (GDOES). At least two channels or strips were tested in each condition.

2.4. Tensile testing Tensile tests were conducted on an Instron screw-driven test frame in accordance with ASTM E8M, using a 6 mm specimen width and constant crosshead speed of 2 mm/min. Three replicates were used for each of three conditions; as-received, softened and rehardened. Strain was measured using a video extensometer on a nominally 25 mm gauge length.

Ti 0.04 0.00 0.00

V 0.03 0.00 0.00

B 0.002 0.002 0.000

N 0.14 0.05 0.02

P 0.01 0.01 0.01

Thickness (mm) 1.6 2.0 2.0

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Table 2 Details of the post form heat treatment and carburising trials performed. Treatment Quench distortion Austenitise 30 min + Water Quench Materials Mart900 Mart1300 Mart1500 Crown down Crown up

Flat strip selective masking Carburise one side 10 and 30 min + Water quench

Mart900 Mart1300 Mart1500

Directional gas ow Fully carburise 30 min + Water quench

Mart900

Directional gas ow Fully Carburise 10 min + Water quench

Mart900

Channel selective masking Carburise one side only 10 min + Water quench

Mart900

2.5. Residual stress measurement The residual stress measurements were carried out using a Panalytical Diffractometer equipped with Cu K radiation. Measurements were made at regular intervals of approximately 15 m from the carburised surface by systematically polishing back the surface using 3 m diamond paste and ops polishing. 15 measurements were made at each depth to calculate the residual stress. The peak examined for all measurements was the 1 1 2 peak which was centred at a 2 angle of 82.2 . This peak gave the best compromise between angular resolution and number of counts. The peaks were tted assuming a Gaussian distribution. The measurements were made between tilt angles of 70 and +70 degrees, and calculations of stress made assuming equal biaxial stress in the sheet. 3. Results and discussion 3.1. Tensile and channel forming behaviour Fig. 1 shows engineering stressstrain plots for the three martensitic steels in the as-received, annealed and rehardened conditions. The as-received tensile strength of these steels were approximately 950, 1300 and 1550 MPa, which is related to the amount of carbon (Table 1). In each case, annealing reduced the tensile strength to approximately one third of the as-received value while providing a signicant increase in ductility.

Fig. 1 also shows engineering stress-strain curves for the rehardened conditions, which were the annealed samples that had been heat-treated at 925 C for 30 min and water quenched. The rehardened tensile properties are indicative of the mechanical

Fig. 1. Engineering stress-strain curves for the Mart900, Mart1300 and Mart1500 in the as-received, annealed and rehardened conditions.

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Fig. 2. Average punch force during channel forming for the different martensitic steel grades in (a) as-received and annealed conditions; and, (b) springback angle due to forming for the different martensitic steel grades in the as-received and annealed conditions.

properties of the steel in the post-formed heat-treated channels. The rehardened tensile properties of the Mart1300 and Mart1500 steels suggest almost complete restoration of the original martensitic microstructure. The Mart900 steel in the rehardened condition had a slightly lower tensile strength and higher ductility than the as-received condition, suggesting that the original martensitic microstructure was not fully restored (potentially due to the quench rate for this lower carbon steel not being high enough). The heat treatment and quench schedule for the Mart900 was not optimised to restore the as-received properties as this was not the primary objective of the study. Fig. 2 shows that the average punch force and springback values are signicantly lower for the annealed steels, particularly Mart1500 and Mart1300. It should be noted that while martensitic sheet steels are not commonly cold-formed using the stamping process, all three grades in the as-received condition were able to be formed into the relatively simple channel shape used in this study. The excessive springback measured for the as-received steels, however, highlights one of the major difculties in forming steels of this strength (due to the dependence of springback on strength). The as-received Mart900 steel had the highest springback despite being the lowest strength grade as there is also a strong inverse correlation between thickness and springback as shown by Granzow (1983). The signicant reductions in punch force demonstrate another advantage in stamping softer steel, as punch force has a high correlation with die wear rates, which has become a signicant issue recently in sheet metal stamping of high strength steels as highlighted by Pereira et al. (2008). 3.2. Effect of post form heat treatment channel shape The shape of the quenched channels were compared to asreceived formed channels and it was found that differences were predominantly conned to either an opening or closing of the channel wall angle with respect to the channel crown. The channel wall angle is the exact same shape deviation as the springback angle. Fig. 3 plots the change in channel wall angle for the heat-treated and quenched channels relative to the springback angle of the asformed channels for the crown-down orientation. To eliminate the possibility that the channel wall movement was related to the relaxing of forming stresses, channels were heated to the same austenitic temperature and slow cooled to room temperature. No change in springback angle was detected, conrming that the shape change is quenching related. Surprisingly there was only a minimal effect of quench distortion for the PFHT of the channels used in this study. For all three martensitic steels quenched in both orientations, there was a deviation of less

than 2 due to quenching from the as-formed springback angle. However, the channel wall deviation was not consistent in terms of increasing or decreasing the channel wall angle and there was no obvious relationship with material strength, material thickness or quench orientation. This lack of apparent predictability is potentially related to the quenching process parameters such as the heat transfer coefcient that have been shown by Li et al. (2006) to have a signicant impact on distortion. Although the springback angle change due to quenching was minimal, a 1.5 uncertainty in nal springback angle is signicant to component design and assembly. The following section describes an initial investigation into the use of selective carburising to impart residual stresses that allow greater predictability in quenching shape movement and also to determine if as-formed springback can be corrected. 3.3. Flat strip selective carburising In addition to the variable quench distortion of the channel wall angle of 12 , the cold forming of the annealed steel resulted in a shape deviation due to springback of approximately 67 . A potential method to reduce variability and remove these shapedeviations during the PFHT process is the introduction of residual compressive stress into the outer layers of the sheet via carburising. To demonstrate this principle, at strips of all three steels were carburised on only one side for two different time intervals, 10 and 30 min, before quenching. The strip curved away from the side that

Fig. 3. Plot showing change in channel wall angle due to quenching in the crowndown orientation (left) and the crown-up orientation (right) for the three steels; insets showing the direction of shape deviation for a positive and negative change.

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Fig. 4. Proles of the at strips after selective carburising for each of the martensitic steels showing the curvature resulting from the introduction of compressive residual stresses into the outer layers on one side of the sheet. The top surface of each strip was carburised.

was carburised in all instances, though the curvature was negligible for the Mart1300 after 10 min and Mart1500 at both time intervals (Fig. 4). It is clear from Fig. 4 that the carburising causes relatively uniform curvature in the strip, and the curvature is more pronounced in the thinner lower strength material and with increasing carburising time. The explanation for the effect of the carburising treatment on the shape of the channel radii is similar to that used in shotpeen forming by Kopp and Schulz (2002). In shot-peen forming, a compressive layer is introduced to the surface of the sheet due to plastic deformation caused via the repeated impingement of steel balls. The depth of the plastic deformation layer, and hence compressive layer, is related to the shot velocity and mass ow. A shallow compressive stress layer will cause the sheet to curve away from the deformed side of the sheet (convex), with an increase in the deformed layer depth increasing the curvature. Microstructural analysis showed that carburising occurred on one side only and that case depth increased with time (Fig. 5). Microhardness proles (Fig. 6) also indicate that the depth of carburising increases with time, and that very high hardness levels are attained in the carburised region. Quantitative depth proles of carbon obtained by GDOES (Fig. 7) show that a consistent carbon concentration was achieved for all materials and that carbon concentration increased with time. The hardness levels correlate with work by Grange et al. (1977) that examined the effect of carbon on martensite hardness. By assuming that the carburised layer is a thin strip rigidly connected to a softer substrate, a modied version of Stoneys equation (Eq. (2)) from Jiang et al. (2006) was used to estimate the compressive residual stress that is causing the curvature:
c

Et 2 6(1 )R

(2)

where E is the Youngs modulus and is the Poissons ratio of the substrate, R is the radius of the curved strip; is the thickness of the carburised layer and t is the thickness of the substrate (sheet thickness minus thickness of carburised layer). The results of the compressive stress calculations suggest that there is a higher compressive residual stress in the Mart900 strip after 10 min carburising (380 MPa) than there was after 30 min carburising (255 MPa). The uncertainty associated with these calculated values is approximately 50 MPa. The measured residual stresses proles showed an increase in compressive stress to a peak value; at a depth of 55 m from the surface for the 10 min strip and

Fig. 5. Light optical micrographs showing selective carburising, 50, etched with 2% nital solution. The carburised depth is the distance between the specimen bottom edge and the dotted line indicated on the micrographs.

15 m for the 30 min strip. The peak compressive residual stresses measured in the strips showed a similar trend with 670 MPa in the 10 min strip and 395 MPa in the 30 min strip. Longer carburising times, and subsequent higher carbon contents, can increase the fraction of retained austenite. An increase in retained austenite in a carburised case has been reported by Parrish (1999) to reduce compressive stress due to the change in volume compared to martensite, perhaps explaining the lower peak compressive stress with increased carburising time in the present study as well as the

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Fig. 6. Microhardness proles for the investigated martensitic steels carburised for 10 and 30 min.

under prediction of Eq. (2). Despite the lower compressive peak stress more geometrical change (smaller radius) occurred in the sample carburised for a longer time, indicating that case depth is important in regard to the resulting radius of curvature for a particular material. The calculated compressive residual stress for the Mart1300 after 30 min (375 MPa) showed a similar level to the Mart900 after 10 min, despite having an increased carburising depth and carbon content, and the radius of curvature was larger. Also the highest strength MART1500 strips displayed no geometrical change, despite an obvious carburised region. These results suggest that the resulting shape change is a complex interaction between carburising depth, carbon content, material thickness and strength. However, for the same material the degree of shape change can be related to carburised case depth. 3.4. Control of channel shape via directional gas ow Since the gas ow during carburising was from the bottom of the uid bed, the surface of the channel facing down will be carburised more than the surfaces of the channel facing up. Carburising for 30 min had a signicant effect on the quench distortion for the Mart900 steel grade in the crown-down orientation, with the channel wall angle decreasing by approximately 11 . This large decrease shown in Fig. 8 meant that the nal channel shape had an angle less than 90 between crown and wall. As with the crown-down orientation, carburising caused a signicant difference in wall angle for both the Mart900 channels in the crown-up orientation. In this orientation, the channel wall angle increased by approximately 4 ,

meaning that the springback present from forming was amplied and the shape deviated further from the ideal 90 wall angle (Fig. 8). In the crown-down orientation, the outside of the channel crown had a carburised depth of 210 m while the inside of the crown had a carburised depth of 140 m. Similarly in the crownup orientation, the inside of the channel crown had a carburised depth of 200 m and a carburised depth on the outside of the channel crown of 150 m. Thus rather than the introduced compressive stresses of the two carburised surfaces cancelling each other out, the differential in compressive layer depths causes a net movement in the channel. As the channel-down orientation showed a drastic tendency to close up (reduce the springback angle) after 30 min carburising, this orientation was used at a shorter carburising time. Channels carburised for only 10 min showed an inclination to decrease in wall angle (close-up) by an average of approximately 1 (Fig. 8). This was signicantly lower than after 30 min, where the decrease was approximately 11 . The average carburising depth in the crown-down orientation on the outer layer was 200 m for 30 min and 165 m for 10 min, while the inner layer remained relatively constant at approximately 140150 m. Thus at the shorter carburising time there was a relatively small difference between the outer and inner layer depths, explaining the small resultant decrease in wall angle. 3.5. Control of channel shape via selective masking The selectively masked channels also showed a signicant change in channel wall angle after being quenched. The channels that had been carburised only on the outer wall closed up (reduction in wall angle) as shown in Fig. 8 by an average of approximately 12 . This meant that the nal channel shape had an angle less than 90 between crown and wall. It should also be noted that there was noticeable variation between the replicate channels tested at this condition. The channels that were only carburised on the inner wall also showed a signicant change in channel wall angle; however, these channels opened up, or increased the channel wall angle by an average of 9 as shown in Fig. 8. 3.6. Relationship between shape change and carburising depth Both methods for selective carburising, directional gas ow and selective masking, showed signicant effects on the channel wall angle for Mart900 due to carburising causing a change to the curvature of the crown-wall radius (punch radius). Carburising on the outer bre of the curved radius caused the radius to close-up (increase in curvature), while carburising on the inside of a curved radius caused the radius to open-up (decrease in curvature). The selectively carburised at strips showed that carburising depth was a signicant factor in the resultant curvature. By examining Eq. (2), it can be expected that the change in channel wall angle will be related to the carburising depth divided by the square of the substrate thickness (since channel wall angle is related to inverse of the curvature, R), which is plotted in Fig. 9 for Mart900. Fig. 9 shows data for Mart900 channels using both selective carburising methods, where the x-axis is the difference resulting from the competing effects of the carburised layers on each side of the 2 ) ( /t 2 )) where ( ) is the carburising depth on channel ((0 /t0 0 i i the outer wall and (i ) on the inner wall. The relationship between channel wall angle and carburising layer depth in Fig. 9 for the Mart 900 channels is supported by the work of Acht et al. (2007) who found carburizing depth and component thickness were signicant variables in distortion resulting from carburising. Comparison of the data to the trendline, however, shows some noticeable deviation, which suggests that there are other variables that are inuencing the change in curvature of

Fig. 7. Quantitative depth proles of carbon for the investigated martensitic steels carburised for 10 and 30 min.

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Fig. 8. Proles of the formed channels after selective carburising for Mart900 showing the shape change resulting from the quench orientation, method of selective carburising and carburising time. For each channel shown is the angle between the dotted lines. The uncertainty is the standard deviation of all channels tested in that specic condition.

the radius. The selective carburising of the at strips suggested that the carbon concentration has an effect on the resultant curvature. For the 30 min carburised channel the average carbon concentration was 1.2 wt.% on the outside of the crown and 0.5 wt.% on the inside, whereas for the 10 min carburised channel the average carbon concentration was 0.7 wt.% on the outside of the crown and 0.3 wt.% on the inside. The measurement of carbon concentration in the carburised layers for all channels showed signicant variation, however, of up to 0.5 wt.% on channel walls facing the gas ow, and 0.2 wt.% on channel walls facing away from the gas ow. The effect of carbon concentration may be important as there is an accompanying volume increase with the transformation from austenite to martensite during quenching. Higher carbon concentration reduces the temperature that martensite starts to form and will result in a larger volume change, hence larger compressive residual stress as found by Henriksen et al. (1992). As the increase in carbon concentration may also increase the amount of austenite that is retained in the microstructure after quenching, there could

effectively be competing effects on the compressive residual stress in the carburised layer. It is expected that a careful characterisation of the effect of carbon concentration would be necessary for a given steel composition to understand these competing factors to enable selective carburising to be used as a reliable processing method. It is also apparent that further development of this processing method would require excellent control of the carburising environment to achieve highly reproducible depths and carbon concentrations. This study has shown that selective carburising can be used to inuence the nal geometry of formed ultra high strength sheet steel channels, with potential to remove any shape deviations caused during forming. Although only at the initial stages, it is conceivable that a developed version of this PFHT process could have industrial application, as there are signicant advantages compared to hot stamping in terms of reduced requirements for tooling and press equipment.

4. Conclusions From this study on the post-forming heat treatment of three martensitic steels it can be concluded that: Cold forming annealed steel leads to signicantly reduced springback and punch force, while there was minimal quench distortion (less than 2 in terms of channel wall angle) after post form heat treatment for the tested materials. Orientation of the channel (crown-up or crown-down) was not a signicant variable in the direction or magnitude of the quench distortion for the uncarburised channels. Selective carburising of the outer surface of at martensitic steel strips caused curvature away from the induced compressive layer. Higher carburising depth and smaller sheet thickness caused greater curvature. Selective carburising of channel sections via both directional gas ow and selective masking methods led to a signicant change in the channel wall angle after quenching for Mart900. The change in

Fig. 9. Plot of change in channel wall, or springback angle after quenching versus 2 ) (i /ti2 )) for Mart900. Each data point represents a channel, with the x-axis ((0 /t0 uncertainty based on measurement error for the carburised depth.

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channel wall angle was dependent on the difference in carburised layer depth from the outer and inner walls of the channel. Acknowledgements The authors would like to acknowledge the work of Colin Whibley and Jamie Lee Gilbert in the specimen preparation and data measurement phases of this study, as well as Dr. Nicole Stanford in residual stress measurements. References
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