Effect of Cold Work and Heat - Tratment On The High Temp Rupture Properties of 91

Effect of Cold Work and Heat Treatment on the Elevated-Temperature Rupture Properties of Grade 91 Material
Technical Report
Effective December 6, 2006, this report has been made publicly available in accordance with Section 734.3(b)(3) and published in accordance with Section 734.7 of the U.S. Export Administration Regulations. As a result of this publication, this report is subject to only copyright protection and does not require any license agreement from EPRI. This notice supersedes the export control restrictions and any proprietary licensed material notices embedded in the document prior to publication.
Effects of Cold Work and Heat Treatment on the ElevatedTemperature Rupture Properties of Grade 91 Material
1011352
Final Report, January 2005
EPRI Project Manager K. Coleman
EPRI 3412 Hillview Avenue, Palo Alto, California 94304 PO Box 10412, Palo Alto, California 94303 USA 800.313.3774 650.855.2121 askepri@epri.com www.epri.com
DISCLAIMER OF WARRANTIES AND LIMITATION OF LIABILITIES

THIS DOCUMENT WAS PREPARED BY THE ORGANIZATION(S) NAMED BELOW AS AN ACCOUNT OF WORK SPONSORED OR COSPONSORED BY THE ELECTRIC POWER RESEARCH INSTITUTE, INC. (EPRI). NEITHER EPRI, ANY MEMBER OF EPRI, ANY COSPONSOR, THE ORGANIZATION(S) BELOW, NOR ANY PERSON ACTING ON BEHALF OF ANY OF THEM: (A) MAKES ANY WARRANTY OR REPRESENTATION WHATSOEVER, EXPRESS OR IMPLIED, (I) WITH RESPECT TO THE USE OF ANY INFORMATION, APPARATUS, METHOD, PROCESS, OR SIMILAR ITEM DISCLOSED IN THIS DOCUMENT, INCLUDING MERCHANTABILITY AND FITNESS FOR A PARTICULAR PURPOSE, OR (II) THAT SUCH USE DOES NOT INFRINGE ON OR INTERFERE WITH PRIVATELY OWNED RIGHTS, INCLUDING ANY PARTY'S INTELLECTUAL PROPERTY, OR (III) THAT THIS DOCUMENT IS SUITABLE TO ANY PARTICULAR USER'S CIRCUMSTANCE; OR (B) ASSUMES RESPONSIBILITY FOR ANY DAMAGES OR OTHER LIABILITY WHATSOEVER (INCLUDING ANY CONSEQUENTIAL DAMAGES, EVEN IF EPRI OR ANY EPRI REPRESENTATIVE HAS BEEN ADVISED OF THE POSSIBILITY OF SUCH DAMAGES) RESULTING FROM YOUR SELECTION OR USE OF THIS DOCUMENT OR ANY INFORMATION, APPARATUS, METHOD, PROCESS, OR SIMILAR ITEM DISCLOSED IN THIS DOCUMENT. ORGANIZATION(S) THAT PREPARED THIS DOCUMENT Alstom Power, Inc.
ORDERING INFORMATION
Requests for copies of this report should be directed to EPRI Orders and Conferences, 1355 Willow Way, Suite 278, Concord, CA 94520, (800) 313-3774, press 2 or internally x5379, (925) 609-9169, (925) 609-1310 (fax). Electric Power Research Institute and EPRI are registered service marks of the Electric Power Research Institute, Inc. EPRI. ELECTRIFY THE WORLD is a service mark of the Electric Power Research Institute, Inc. Copyright 2005 Electric Power Research Institute, Inc. All rights reserved.
CITATIONS
This report was prepared by Alstom Power, Inc. Materials Technology Center 1119 Riverfront Parkway Chattanooga, TN 37402 Principal Investigator J. Henry This report describes research sponsored by EPRI. The report is a corporate document that should be cited in the literature in the following manner: Effects of Cold Work and Heat Treatment on the Elevated-Temperature Rupture Properties of Grade 91 Material, EPRI, Palo Alto, CA: 2005. 1011352.
iii
PRODUCT DESCRIPTION
For many years it has been understood that straining austenitic materials reduces their hightemperature properties. Recognizing this, ASME added a section (PG-19) to the Boiler Code, SC-I, which requires heat treatment after the forming of austenitic materials. The industry has experienced failures of newer creep-enhanced ferritic materials like Grade 91 that indicate these materials suffer from the same type of degradation mechanism as austenitic materials. Boiler manufacturers have implemented guidelines for heat treating these alloys, but there is no consensus among manufacturers as to the proper heat treatments for different strain levels. The goal of the project described in this report is to develop a technical basis for rules that will be added to PG-19 for Grade 91 material. Results and Findings Large test coupons were marked with grids to make measurements of strain possible, then the coupons were bent to induce strain. Rupture coupons were removed from locations within the block where the material had experienced specific strain levels. These coupons were then tested to determine the amount of degradation resulting from each level of strain. Subsequent samples received heat treatments to determine the appropriate levels of heat treatment needed to restore rupture properties. Challenges and Objectives The goal of this project is to provide technical justification and rules for heat treatment of Grade 91 materials after forming. Methods to develop a specific strain level throughout the entire test specimen were developed. This required having a large block of Grade 91 material forged into 6-in. x 6-in. x 30-in. (152-mm x 152-mm x 762-mm) pieces that could be strained. A method of measuring strain using grid markings on the blocks was developed. With the correlation between strain level and required heat-treatment temperatures that was developed by this project, premature failures resulting from strain-induced material degradation will be minimized. Applications, Value, and Use Many new creep-strength-enhanced ferritic alloys are currently under development or have recently started to be used in fossil boiler applications. These include T23, T24, P91, and P92. Methods developed by this project to test the effect of strain-induced degradation of these materials can be used to develop guidelines for post-strain heat treatment. The elimination of premature failures caused by strain will allow utilities to realize the full benefit from upgrades and retrofits on new construction using these alloys.
EPRI Perspective EPRI has been at the forefront of new alloy development for high-temperature boiler applications. Because these alloys are much stronger than the low-alloy ferritic materials (P11 and P22) commonly used for boiler pressure parts, thinner components can be used. This results in initial material savings and improvements in component life. Thinner components are also more resistant to thermal fatigue damage, allowing utilities more flexibility in dispatching units. Higher operating pressures and temperatures are possible with these materials, thereby resulting in more-efficient power plants. Approach This program first developed a method to test the effect of strain on the high-temperature performance of materials. Next, an alloy that is being widely used for replacement and new fabrication was tested to see what level of degradation resulted in degraded material properties. Finally, heat treatments were evaluated to determine if properties could be restored through a subcritical or normalization heat treatment. Keywords P91 Fabrication Advanced materials Headers Piping Heat treatment
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ACKNOWLEDGMENTS
EPRI acknowledges the contribution of J. C. Hitchcock, Alstoms principal manufactory engineer, for his assistance in the preparation and production of the cold-bent test blocks.
vii
CONTENTS
1 BACKGROUND AND INTRODUCTION ................................................................................1-1 2 STRAIN DEVELOPED DURING THE COLD-BENDING OF GRADE 91 TUBING AS A FUNCTION OF R/D RATIOS .................................................................................................2-1 2.1 Deformation/Strain Determination Using the Grid Method ..............................................2-1 2.2 Deformation/Strain Determination Using the Wall Thickness Method.............................2-7 2.3 The Effect of Heat Treatment on Cold-Worked Grade 91 Microstructure .....................2-13 3 REVIEW OF CREEP RUPTURE TEST RESULTS USING COLD-ROLLED GRADE 91 STRIPS .................................................................................................................................3-1 4 EVALUATION OF COLD-WORK AND HEAT TREATMENT ON THE ELEVATEDTEMPERATURE CREEP RUPTURE PROPERTIES OF GRADE 91 MATERIAL USING COLD-BENT BLOCKS..............................................................................................................4-1 4.1 Material Preparation for Creep Rupture Testing .............................................................4-1 4.2 Scale Model Study of the Bending Procedure for Preparation of Test Coupons ............4-3 4.3 Bending the 6" x 6" x 30" Test Coupons .........................................................................4-5 4.4 Determination of Local Strain and Strain Distribution for Preparation of Creep Rupture Test Specimens.......................................................................................................4-9 4.5 Creep Rupture Testing ..................................................................................................4-10 4.5.1 Creep Rupture Behavior of Unstrained Grade 91 Material....................................4-11 4.5.2 The Effect of Cold-Work on Creep Rupture Behavior of Grade 91 Material..........4-13 4.5.3 The Effect of Heat Treatment on Creep Rupture Behavior of Cold-Worked Grade 91 Material...........................................................................................................4-15 4.5.4 The Relationship Between Cold-Work-Induced Hardness Increase and Creep Life Reduction......................................................................................................4-17 5 CONCLUSIONS .....................................................................................................................5-1 6 RECOMMENDATIONS ..........................................................................................................6-1 7 FUTURE WORK .....................................................................................................................7-1
ix
8 REFERENCES .......................................................................................................................8-1 A MEASURED AND CALCULATED STRAINS FOR BENT TUBES USED IN THE STUDY...................................................................................................................................... A-1
LIST OF FIGURES
Figure 2-1 Locations of Measured and Calculated Strains Using the Grid Method ...................2-3 Figure 2-2 Calculated Strain Levels at Seven Locations Around the Tube Bend for Nominal 33% Level (Based on Grid Method L/Li) ............................................................2-4 Figure 2-3 Calculated Strain Levels at Seven Locations Around the Tube Bend for Nominal 25% Level (Based on Grid Method L/Li) ............................................................2-5 Figure 2-4 Calculated Strain Levels at Seven Locations Around the Tube Bend for Nominal 20% Level (Based on Grid Method L/Li) ............................................................2-6 Figure 2-5 Calculated Strain Levels at Seven Locations Around the Tube Bend for Nominal 15% Level (Based on Grid Method L/Li) ............................................................2-7 Figure 2-6 Locations of Measured and Calculated Strains Using the Wall Thickness Method ...............................................................................................................................2-8 Figure 2-7 Calculated Strain Levels at the 90 Location of the Tube Bend at Eight Locations Around the Circumference, for the Nominal 33% Strain Level (Based on Wall Thickness Method t/ti) ..............................................................................................2-9 Figure 2-8 Calculated Strain Levels at the 90 Location of the Tube Bend at Eight Locations Around the Circumference, for the Nominal 25% Strain Level (Based on Wall Thickness Method t/ti) ............................................................................................2-10 Figure 2-9 Calculated Strain Levels at the 90 Location of the Tube Bend at Eight Locations Around the Circumference, for the Nominal 20% Strain Level (Based on Wall Thickness Method t/ti) ............................................................................................2-11 Figure 2-10 Calculated Strain Levels at the 90 Location of the Tube Bend at Eight Locations Around the Circumference, for the Nominal 15% Strain Level (Based on Wall Thickness Method t/ti) ............................................................................................2-12 Figure 2-11 Example of the Effect of Heat Treatment on the Microstructure of ColdFormed Tubing.................................................................................................................2-14 Figure 3-1 Summarized Creep Rupture Test Results Using Cold-Rolled Grade 91 Strips at Test Temperatures of 600C and 650C and at Various Stress Levels in the Range of 81190 MPa .......................................................................................................3-3 Figure 3-2 Summarized Creep Rupture Test Results as a Function of Cold-Work Levels ........3-4 Figure 4-1 Sketch Showing the Center Thermocouple Location ...............................................4-2 Figure 4-2 Typical Microstructural Condition of the Grade 91 Material in the Re-Heat Treated Condition...............................................................................................................4-3 Figure 4-3 Typical Results of Single-Step 3-Point Bending and Multiple-Step 3-Point Bending ..............................................................................................................................4-4
xi
Figure 4-4 Example of the 6" x 6" x 30" Test Blocks and the Grids Inscribed on the Surface of the Blocks Prior to Bending ..............................................................................4-6 Figure 4-5 Bending Status After Completion of the First Stage in the Bending Process ...........4-7 Figure 4-6 Bending Status After Completion of the Second and Third Stages of the Bending Process ................................................................................................................4-8 Figure 4-7 Final Condition of the Bent Test Coupons, with the Inscribed Grid Patterns Shown in the Bend Zone....................................................................................................4-9 Figure 4-8 Photo Showing Orientation of Test Specimens ......................................................4-10 Figure 4-9 Documentation of the Creep Rupture Behavior of the Unstrained Grade 91 Test Material as Compared to the Imputed Mean and Minimum Properties for Grade 91 Material ............................................................................................................4-12 Figure 4-10 Documentation of the Effect of Cold-Work on the Creep Rupture Behavior of the Grade 91 Test Material, Based on Comparison with the Behavior of the Unstrained Base Metal .....................................................................................................4-14 Figure 4-11 The Effect of a Post-Forming Subcritical Heat Treatment on the Creep Rupture Behavior of the Cold-Worked Grade 91 Test Material Compared with the Behavior of the Unstrained Base Metal and the Cold-Worked Material with No PostForming Heat Treatment ..................................................................................................4-16 Figure 4-12 Creep Life Reduction as a Function of Hardness Increase Induced by ColdWorking ............................................................................................................................4-19
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LIST OF TABLES
Table 1-1 Chemical Composition of Wrought Modified 9Cr and Standard 9Cr-1Mo Steels ......1-2 Table 2-1 Chemistry for Two Heats Used in the Deformation Study .........................................2-1 Table 2-2 Tube Identification .....................................................................................................2-2 Table 2-3 The Ratio t / L ........................................................................................................2-12 Table 2-4 Hardness Values of Specimens...............................................................................2-15 Table 3-1 Chemical Composition for the Two Heats Used for Simulated Creep Rupture Testing ...............................................................................................................................3-1 Table 3-2 Material Hardness Values as a Function of the Level of Cold-Work .........................3-2 Table 4-1 Chemical Composition of the Grade 91 Heat for the Test Program ..........................4-1 Table 4-2 Mechanical Composition of the Grade 91 Heat for the Test Program .......................4-2 Table 4-3 Hardness Measurements from the Surface to the Center of the Block .....................4-3 Table 4-4 Cold-Work-Induced Hardness Increase and Creep Life Reduction.........................4-18
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BACKGROUND AND INTRODUCTION
The efficiency of fossil power plants is a direct function of both the temperature and the pressure of the product steam. Strategies for improving overall power plant efficiency have received attention worldwide since the first of the energy crises in the 1970s, and an inevitable focus of that attention has been an increase in the operating parameters (steam pressure and temperature). Of course, such an increase requires the selection of materials for critical pressure part components that can operate reliably under the more rigorous operating conditions. One group of materials that has shown substantial promise for operation in the intermediate temperature regimes of advanced-cycle steam generators has been the creep-strength-enhanced ferritic alloys, among which the modified 9Cr alloy (Grade 91) has seen the most extensive use in existing plants. The Grade 91 alloy was developed by the then Combustion Engineerings (CEs) Metallurgical and Materials Laboratory under U.S. Department of Energy (DOE) sponsorship from 1969 to 1977. Beginning in 1969, a series of proposals for the development of a super 9Cr alloy for use in the liquid metal fast breeder reactor (LMFBR) was submitted to DOE (and to its predecessor organizations, AED and ERDA) by CE. Approval was granted to begin the hardware development work at CE in early 1975 under the administration of Oak Ridge National Laboratorys (ORNLs) Metals and Ceramics Division. The alloy composition and favorable mechanical properties, including high creep rupture strength coupled with satisfactory fracture toughness at temperatures below ambient, had been established by the year 1977. Subsequently, ORNL participated actively in the commercialization and ASME Code approval of what today is known as Grade 91. It should be recognized that the composition and properties of Grade 91 were optimized for the LMFBR application, particularly for the steam tubing and other structural material for the sodium-steam generator components. This alloy was not optimized for fossil boiler or petrochemical applications [16]. With the loss of funding support for the LMFBR program that occurred in the late 1970s, the program sponsors looked toward other possible applications of the alloy, and fossil-fired steam generators were identified as potential users. Grade 91 gained its initial acceptance as boiler tubing suitable for use in ASME Boiler and Pressure Vessel Code Section I construction in Code Case 1943 in 1983. The ensuing years have seen widespread usage of the material, largely in the power and petrochemical industries. In addition, there have been further developments in the advanced 9-12Cr ferritic steels, leading to new alloys with service temperature advantages over Grade 91. Among these new alloys are Grade 92 (Code Case 2179), Grade 122 (Code Case 2180), and Grade 911 (Code Case 2327). Included among the new boiler steels has been an enhanced version of the standard 2-1/4Cr-1Mo alloy, known as Grade 23 in Code Case 2199.
1-1
Background and Introduction
The modified 9Cr alloy represents a reengineering of the standard 9Cr-1Mo alloy, which is identified as T9 in the ASME SA-213 tubing specification. The principal modification consists of controlled additions of vanadium, niobium, and nitrogen, which substantially increase the creep strength of the alloy through the precipitation of M23C6 carbides and MX (Nb, V) carbonitrides, in addition to the lesser solution strengthening effects. Like its lower-strength predecessor, the modified 9Cr alloy exhibits superior hardenability and, within the specified chemical composition range, will transform to 100% martensite upon air cooling, even in thick sections. Table 1-1 compares the specified chemical compositions for the standard 9Cr-1Mo alloy and the modified 9Cr material [7].
Table 1-1 Chemical Composition of Wrought Modified 9Cr and Standard 9Cr-1Mo Steels Element
Standard 9Cr-1Mo Modified 9Cr
C
0.15 max. 0.08 0.12
Mn
0.30 0.60 0.30 0.60
P
0.025 max. 0.020 max.
S
0.025 max. 0.010 max.
Si
0.25 1.00 0.20 0.50
Cr
8.00 10.00 8.00 9.50
Mo
0.90 1.10 0.85 1.05
Ni
0.40 max.
V
0.18 0.25
Nb
0.06 0.10
N
0.030 0.070
Al
0.04 max.
From the standpoint of designing pressure part components for operation at elevated temperatures in boilers, creep is one of the primary damage mechanisms that must be considered in determining the serviceability of those components. In common engineering practice, the effect of creep is simply taken into account through the allowable stresses, which are established by Subcommittee II of the ASME Code based on the tested creep properties of the material. The data from which the allowable stresses are derived are typically based on the testing of fully heat-treated base material samples using uniaxial test specimens. The effects of fabrication processes, such as welding and forming, on the creep behavior of the materials, as that behavior compares to the unprocessed material (base metal), are generally not considered. That these processes may adversely affect the properties of the material is well known, as the premature failures of high-energy piping at longitudinal seam welds have demonstrated. There is no doubt, therefore, that an understanding of the possible effects of fabrication on the creep properties of materials is essential to predicting the serviceability of the components fabricated from these materials. With regard to the creep-strength-enhanced ferritic steels, the critical dependence of these materials on the ability of the carbonitride particles precipitated during tempering to stabilize the disordered martensitic structure suggests that they may be particularly vulnerable to processing effects. Certainly the well-known susceptibility of these materials to the Type IV effect is evidence of this vulnerability. Because of their strong microstructural dependence, the modified 9Cr alloys typically have fabrication requirements that are more stringent than those of the standard boiler alloys. Material vendors, regulatory groups, and construction companies have established these requirements in attempts to address the unique characteristics of the modified 9Cr alloy and thereby ensure optimum serviceability of the components. However, long-term service experience with the material is limited, so all effects of processing are not known at this time. As a result, the requirements imposed by various organizations are not consistent, and in some cases are contradictory. Fabrication difficulties and recent service failures have indicated that the requirements associated with cold-forming of modified 9Cr material should be better understood. 1-2
For example, concerns have arisen that some forming requirements are too conservative with regard to the application of heat treatment, that some post-forming heat treatment is actually deleterious, and that forming limits are inconsistent. A few preliminary studies have been conducted to investigate the effects of cold-working on the creep properties of Grade 91 by ORNL, Sumitomo, and Stork Boiler/TNO Research Institute in the Netherlands [810]. From these studies it appears certain that there is a significant reduction in the creep rupture strength of Grade 91 material when strained beyond certain limits. However, there are not sufficient data to establish what the limits are and whether the degree of reduction is a direct function of the amount of working, or whether there exists some threshold level of strain below which there are no significant effects. Since modified 9Cr steel is being used more extensively by boiler manufacturers due to its excellent elevated-temperature properties, it is essential that the effects of cold-forming and subsequent heat treatment on the creep properties of modified 9Cr steel be quantified to the extent possible. In order to provide a more sound technical basis for assessing the effects of cold-forming and subsequent heat treatment on the creep properties of modified 9Cr steel, a program of testing has been initiated by Alstom Powers Materials Technology Center under the sponsorship of EPRI. This program has been designed to address the issues outlined above by providing additional data that will make it possible to devise technically defensible cold-forming requirements. The objective of this program is to more accurately characterize the magnitude of the effect of coldworking on the elevated-temperature properties of Grade 91, recognizing that not all possible combinations of composition, heat treatment, strain, and operating conditions can be evaluated. Should effects be uncovered during this program that have not been anticipated, then supplementary efforts may be advisable. The first stage of the program involved more accurately determining the deformation/strain patterns that develop in boiler tubing during bending. Accurate strain measurements were made on etched bend samples in both the circumferential and longitudinal directions, with special attention given to the extrados and intrados of the bends. Common sizes of Grade 91 tubing were purchased, and the tubes were cold-formed into bends using R/D ratios commonly used for boiler tubing. The cold-forming procedures used to bend the tubing mirrored the standard procedures used at Alstoms Chattanooga tubular production site for many years. Once the deformation/strain data obtained from the T91 tube bends were evaluated, test coupons representing several different deformation/strain levels were produced using cold-bent Grade 91 wrought plate (6" [152 mm] thick). Creep rupture specimens were extracted from the tension side of the bent coupons to simulate the extrados condition of cold-formed tubing. In order to provide baseline data, creep rupture specimens also were prepared from the as-received base material. For the program, four simulated cold-bent coupons (6" x 6" x 30" [152 mm x 152 mm x 762 mm]) of Grade 91 material were produced. The strain pattern developed in each of the test coupons during cold-bending was based on the evaluation of a matrix consisting of 0.25" x 0.25" (6.35 mm x 6.25 mm) cells inscribed into the surface of each coupon prior to bending. Over 1200 measurements were made and the appropriate calculations performed to define the strain pattern. The creep rupture test specimens were then removed from the test coupons to represent specific strain levels. Creep rupture test conditions were designed based on the imputed creep rupture 1-3
properties of unstrained Grade 91 material calculated from ASME SCI allowable stresses for sections above and below 3" (76 mm) in thickness, along with test data from ORNL, V&M Tubing, EPRI, MPC, and Mitsubishi Heavy Industries (MHI) The test stress levels for the program ranged from 8.7 ksi (60 MPa) to 20.3 ksi (140 MPa); this range spans the design stress levels for most applications in boilers. Test temperatures were selected to yield rupture times for the unstrained base metal between 300 and 10,000 hours. In this report, the results of the program are reviewed and the implications of the results to the more general issue of coldforming of Grade 91 material are discussed in detail.
1-4
STRAIN DEVELOPED DURING THE COLD-BENDING OF GRADE 91 TUBING AS A FUNCTION OF R/D RATIOS
The purpose of this portion of the study was to more accurately determine the cold-working strains developed in the process of tube bending when using bending techniques that represent standard practice in the industry. As part of this evaluation, the strains estimated by standard design formulas were compared to the actual strains developed in a tube during bending in both the longitudinal and transverse directions. Obviously, the ability to accurately quantify the level of strain developed in a cold-bent tube is essential in establishing the relationship between coldworking effects and creep rupture life. Grade 91 tubing was purchased for use in sizes commonly adopted for superheater or reheater applications, and tube bends were cold-formed to several different R/D ratios typically used in the production of superheater or reheater bends. The bending practice reflected common shop procedures, such as those that have been used at Alstoms Chattanooga tubular production site for many years. The deformation/strain pattern along the length of the cold-formed T91 tubing was determined in both the circumferential and longitudinal directions, with the focus of attention being the extrados and intrados of the bends, where the maximum strain was expected to occur. A grid pattern was inscribed on the outer diameter surface of each tube along the length of tubing to be bent. The etching was applied around the full circumference of the tube for a length of 20" (508 mm). The grid pattern itself consisted of a 0.25" (6.35 mm) square with four circles 0.1" (2.54 mm) in diameter inside the square. A deep etching pattern was used to ensure survival of the pattern during the bending operation.
2.1 Deformation/Strain Determination Using the Grid Method

As a preliminary step in the study of cold-work effects on Grade 91 tubing, efforts were made to accurately determine the amount of strain developed in a cold-formed Grade 91 tube bend. Two heats of the material were selected for this purpose, and these were identified as heats B9832-01 and B9833-01. The compositions of these two heats are recorded in Table 2-1.
Table 2-1 Chemistry for Two Heats Used in the Deformation Study Heat # C Mn P S Si Ni Cr M V Nb Ti Co Cu Al B W As Sn Zr N
Heat B 9832-01 .094 .39 .023 .001 .39 .08 8.28 .99 .21 .077 .002 .009 .02 .013 <.001 <.01 <.001 .003 <.001 .040 Heat B 9833-01 .094 .39 .024 .001 .39 .08 8.34 .98 .21 .077 .002 .01 .02 .013 <.001 <.01 <.001 .003 <.001 .044
2-1
Strain Developed During the Cold-Bending of Grade 91 Tubing as a Function of R/D Ratios
A total of 23 tubes were included in this portion of the study. As previously mentioned, a grid pattern was first etched onto the outer diameter surface of the tube in the area to be bent, the grid consisting of 0.25" (6.35-mm) squares, with each square containing four 0.1" (2.54-mm) diameter circles. All 23 tubes were then bent to one of four estimated strain levels, 15%, 20%, 25%, and 33%. The bend radius was determined using the formula for strain, D/2R, with D being the original tube outer diameter (D = 2.125" [53.975 mm]) and R being the nominal bend radius. To evaluate possible effects of heat treatment on the cold-worked microstructures, eight tubes, two from each estimated strain level and one from each heat, were stress relieved at 1350F (732C) for 30 minutes. In addition, eight tubes, two from each estimated strain level and one from each heat, were stress relieved at 1425F (774C) for 60 minutes. Table 2-2 lists the tube identifications, nominal bending strains, and post-bending stress relief conditions.
Table 2-2 Tube Identification Tube # 11A 11B 12A 12B 13A 13B 15A 15B 16A 16B 17A 17B 19A 19B 20A 20B 21A 21B 24A 24B 25A 25B 26A Heat # B 9832-01 B 9833-01 B 9832-01 B 9833-01 B 9832-01 B 9833-01 B 9832-01 B 9833-01 B 9832-01 B 9833-01 B 9832-01 B 9833-01 B 9832-01 B 9833-01 B 9832-01 B 9833-01 B 9832-01 B 9833-01 B 9832-01 B 9833-01 B 9832-01 B 9833-01 B 9832-01 Estimated Strain Level 33% 33% 33% 33% 33% 33% 25% 25% 25% 25% 25% 25% 20% 20% 20% 20% 20% 20% 15% 15% 15% 15% 15% Heat Treatment As Bent As Bent 1350F 30 minutes 1350F 30 minutes 1425F 60 minutes 1425F 60 minutes As Bent As Bent 1350F 30 minutes 1350F 30 minutes 1425F 60 minutes 1425F 60 minutes As Bent As Bent 1350F 30 minutes 1350F 30 minutes 1425F 60 minutes 1425F 60 minutes 1350F 30 minutes 1350F 30 minutes 1425F 60 minutes 1425F 60 minutes As Bent
2-2
After the tubes were bent, the grid pattern on each tube was measured at seven locations around the bend, as indicated in Figure 2-1. Each square etched onto the tube surface was originally 0.25" (6.35 mm), and the L was calculated by subtracting 0.25" from the measured length. Actual strain was defined as L = L/Li. These calculated strain values then were compared with the nominal strain. The data are represented in graphical form in Figures 2-2 through 2-5, and individual values are presented in Appendix A. As shown in Figures 2-2 through 2-5, the measured axial strain was in all cases somewhat higher than the strain estimated by the D/2R formula. At all four strain levels, certain locations on the bend extrados exceeded the estimated strain. The magnitude of the difference depended on the applied strain and the location within the bend. For a nominal strain of 33%, the measured strain was up to 1.2 times higher than the nominal value. In fact, the maximum strain measured at all strain levels was between 1.2 and 1.3 times the nominal strain value. However, the location within the bend where the maximum strain occurred varied to a small extent, although the variations appeared to be within the normal scatter of the data. In general, as can be seen in Figures 2-2 through 2-5, at each of the four strain levels for both heats of material the measured strains were very consistent.
Figure 2-1 Locations of Measured and Calculated Strains Using the Grid Method
2-3
45 40 35 30 25 20 15 10 5 0 0 30 60 90 Tube Location (degrees) 120 150 180
Calculated Strain (in./in.)
As-Bent Condition (Heat A and B) 1350F 30 Minutes (Heat A and B) 1425F 60 Minutes (Heat A and B) Figure 2-2 Calculated Strain Levels at Seven Locations Around the Tube Bend for Nominal 33% Level (Based on Grid Method L/Li)
2-4
35 30 Calculated Strain (in./in.) 25 20 15 10 5 0 0 30 60 90 Tube Location (degrees)

120
150
180
2-5
30
25
20
15
10
0 0 30 60 90 Tube Location (degrees) 120 150 180
2-6
20 18 16 Calculated Strain (in./in.) 14 12 10 8 6 4 2 0
30
60
90
Tube Location (degrees)
120
150
180
2.2 Deformation/Strain Determination Using the Wall Thickness Method

The data reported above pertained to the strains developed in the axial direction, as quantified using the grid method. Another aspect of the deformation study was to study strain in the transverse, or through-thickness, direction and to evaluate the ovalization of the tubing that occurred as a result of the bending process. To quantify this deformation, ring sections were cut from each tube at the midpoint of the bend, as indicated in Figure 2-6. Wall thickness was then measured at eight locations around the circumference of the tubing in these ring sections and compared to an average wall thickness value obtained outside of the bend area. The locations for wall thickness measurements are shown in Figure 2-6. The calculated strain levels, using the formula t = t/ti based on wall thickness, are represented graphically in Figures 2-7 through 2-10.
2-7
Figures 2-7 through 2-10 demonstrate that, as expected, the extrados position at the midpoint of the bend is consistently the location of maximum tensile strain, while the intrados position at the midpoint of the bend generally is the location of maximum compressive strain. The graphs also illustrate that, as expected, the measured strain on the intrados side is higher than that experienced on the extrados. Finally, all four wall thickness graphs show that the strain measured in the transverse directions was lower than the maximum strain measured in the axial direction. The relationship between maximum strain in the transverse (wall thickness) direction and maximum strain in the longitudinal (grid) direction are shown in Table 2-3. To obtain the ratios (t / L), only the as-bent data were used, and only the maximum strain, regardless of tube location. There is some degree of error inherent in these calculations. For example, the unstrained wall thickness was assumed to be equal to the original wall thickness in the bend, and there is a degree of error associated with this assumption. In general, the strain in the transverse direction was approximately 0.59 times the strain in the longitudinal direction.
Figure 2-6 Locations of Measured and Calculated Strains Using the Wall Thickness Method
2-8
20 15 10
Extrados
Intrados
5 0 -5 -10 -15 -20 -25 -30 30 45 60 75 90 105 120 135 150 165 180 195 210 225 240 255 270 285 300 315 330
Location Around Circumference (degrees)
As-Bent Condition (Heat A and B) 1350F 30 Minutes (Heat A and B) 1425F 60 Minutes (Heat A and B) Figure 2-7 Calculated Strain Levels at the 90 Location of the Tube Bend at Eight Locations Around the Circumference, for the Nominal 33% Strain Level (Based on Wall Thickness Method t/ti)
2-9
20 15 10
E x tra d o s In tra d o s
5 0 -5 -1 0 -1 5 -2 0 -2 5 -3 0 30 45 60 75 90 105 120 135 150 165 180 195 210 225 240 255 270 285 300 315 330 L o c a tio n A ro u n d C irc u m fe re n c e (d e g re e s )
2-10
20 15 10 Extrados Intrados
5 0 -5 -10 -15 -20 -25 -30 30 45 60 75 90 105 120 135 150 165 180 195 210 225 240 255 270 285 300 315 330
2-11
20 15 10 5 0 -5 -10 -15 -20 -25 -30
Extrados
Intrados
30
45
60
75
90 105 120 135 150 165 180 195 210 225 240 255 270 285 300 315 330
As-Bent Condition (Heat A and B) 1350F 30 Minutes (Heat A and B) 1425F 60 Minutes (Heat A and B) Figure 2-10 Calculated Strain Levels at the 90 Location of the Tube Bend at Eight Locations Around the Circumference, for the Nominal 15% Strain Level (Based on Wall Thickness Method t/ti) Table 2-3 The Ratio t / L Estimated Nominal Strain 33% 25% 20% 15% Maximum Transverse Strain Using Wall Thickness (t in./in.) 27.4% 18.4% 11.9% 11.7% Maximum Longitudinal Strain Using the Grid Method (L in./in.) 40.4% 32.6% 24.8% 19.0% Ratio t / L .68 .56 .48 .62
2-12
2.3 The Effect of Heat Treatment on Cold-Worked Grade 91 Microstructure

In order to evaluate in a qualitative manner the possible effects of heat treatment on the coldworked microstructures, a total of 16 tube bends were given a post-forming heat treatment. Eight of the sixteen bends (two from each estimated strain level and one from each heat) were stressrelieved at 1350F (732C) for 30 minutes, and the other eight bends (two from each estimated strain level and one from each heat) were stress-relieved at 1425F (774C) for 60 minutes. The heat treatment parameters had been selected to bracket the range of tempering parameters commonly used in manufacturing for the processing of Grade 91 tubing. The microstructural examination was focused on nominal strain levels of 20%, 25%, and 33%. For each nominal strain level and heat treatment condition, metallographic specimens were removed from the bend extrados to provide both the longitudinal and circumferential views of the structure. For comparison, specimens were also removed from the bend extrados on the as-bent tubes. The metallographic examination established that for the 1350F treatment for 30 minutes, the first traces of recrystallization could be seen in the cold-worked Grade 91 material, when viewed by light optical microscopy at magnifications up to 1000x. The degree of recrystallization was limited at all three nominal strain levels. For the 1425F heat treatment for 60 minutes, the degree of recrystallization was more advanced, and evidence of significant recrystallization was observed in specimens representing all three nominal strain levels. In all cases, the grain structure had been refined in comparison with the cold-worked condition. Surprisingly, however, there appeared to be no significant difference in the degree of recrystallization that occurred when comparing the three nominal strain levels, at least as the recrystallization amount could be determined by optical microscopy at magnifications as high as 1000x. The example for the effect of heat treatment on the microstructure of cold-formed tubing is shown in Figure 2-11 for the strain level of 33%.
2-13
Figure 2-11 Example of the Effect of Heat Treatment on the Microstructure of Cold-Formed Tubing
Hardness measurements were obtained using a Vickers hardness tester with a 20-kg test load from specimens representing nominal strain levels of 20% and 33%. The measured hardness values are summarized in the Table 2-4.
2-14
Strain Developed During the Cold-Bending of Grade 91 Tubing as a Function of R/D Ratios Table 2-4 Hardness Values of Specimens Nominal Strain Level 20% 33% As-Bent 251 HV / 239 HB 255 HV / 243 HB 1350F for 30 minutes 237 HV / 225 HB 234 HV / 223 HB 1425F for 60 minutes 227 HV / 216 HB 227 HV / 216 HB Base Metal (0% Strain) 225 HV / 214 HB 225 HV / 214 HB
As can be seen, tempering at both conditions reduced the hardness measurably. At 1425F for 60 minutes, the heat treatment reduced the hardness value of the cold-worked Grade 91 to a level that is approximately equal to that of the original base metal with 0% cold-work. The hardness testing results were generally consistent with the metallographic examination. It should be pointed out that the same tempering parameters (1350F for 30 minutes and 1425F for 60 minutes) will be used in the program to further evaluate the effects of heat treatment on coldworked Grade 91 material.
2-15
REVIEW OF CREEP RUPTURE TEST RESULTS USING COLD-ROLLED GRADE 91 STRIPS
Prior to the beginning of the current test program, limited creep rupture testing had been conducted on cold-formed Grade 91 material, in which the cold-deformation had been induced by cold-rolling flattened strips of the material. This testing involved two separate heats (Heats A and B). The chemical composition for the two heats is presented in Table 3-1.
Table 3-1 Chemical Composition for the Two Heats Used for Simulated Creep Rupture Testing Heat # Heat A Heat B C .094 .086 Mn .38 .38 P .020 .020 S <.001 .001 Si .29 .26 Ni .14 .06 Cr 8.64 8.25 Mo .86 .88 V .21 .22 Nb .06 .07 Cu .02 <.01 Al .03 .03 N .041 .046
Cold-rolling is an easily controlled method of inducing a specific level of deformation, and it has been the method of choice in several of the studies on the effects of cold-work that have been conducted to date. However, the manner in which the material is deformed during cold-rolling only introduces compressive deformation to the material, which is significantly different than the manner in which the material is deformed in both tension and compression at certain critical locations in a tube during bending. Questions have been raised regarding the validity of the data obtained from the testing of cold-rolled strip, and it has been this uncertainty that served as the basis for the current study. For the earlier study, coupons were rolled to five different levels of cold-work (10%, 15%, 20%, 25%, and 30%). At the time of the study, Grade 91 plate was not available, and therefore Grade 91 tubes were used instead. Strips were cut from the tubing so that the longitudinal axis was oriented perpendicular to the intended rolling direction. These strips were flattened and then normalized and tempered at Alstoms Chattanooga manufacturing facility. The flattened strips were then sent to the Oak Ridge National Laboratory to be cold-rolled to the desired level of cold-strain for each of the two material heats. To serve as control samples, several of the specimens were normalized and tempered, but were not cold-worked. Prior to conducting creep rupture testing, hardness was measured on all simulation coupons using a Vickers hardness tester with a 20-kg test load. The results of the hardness testing are summarized in Table 3-2.
3-1
Review of Creep Rupture Test Results Using Cold-Rolled Grade 91 Strips Table 3-2 Material Hardness Values as a Function of the Level of Cold-Work Vickers (20-kg Load) Hardness of Grade Heat # Heat A Heat B N&T 215 204 10% Cold-Work 231 271 15% Cold-Work 231 251 20% Cold-Work 312 224 25% Cold-Work 307 276 30% Cold-Work 338 338
A total of 36 specimens, including 21 specimens at 0% and 15 specimens at 1030%, were machined for creep rupture testing. Creep rupture testing was conducted at two different temperatures, 600C and 650C, and at various stress levels in the range of 81190 MPa. Test results are presented in Figures 3-1 and 3-2 as the Larson-Miller Parameter (LMP = [T(K) * (35.0 + Log time(hrs))] / 1000) plotted against the various stress levels. In Figure 3-1, the creep rupture test results of 0% specimens (shown in the plot as solid symbols with trend lines) are compared with those of various levels (1030%) of cold-strained specimens (shown as open symbols). In Figure 3-2, the same creep rupture test results are further detailed as the function of cold-strain levels.
3-2
Review of Creep Rupture Test Results Using Cold-Rolled Grade 91 Strips
225
200
175 Stress (MPa)
150
125
100
75 31 32 33 34 35 36 LMP T (K) * (35.0 + Log time(hrs)) / 1000
Heat A, 0% Heat B, 0% Heat A, 1030% Cold-Work Heat B, 1030% Cold-Work Figure 3-1 Summarized Creep Rupture Test Results Using Cold-Rolled Grade 91 Strips at Test Temperatures of 600C and 650C and at Various Stress Levels in the Range of 81190 MPa
3-3
Review of Creep Rupture Test Results Using Cold-Rolled Grade 91 Strips
225
200
175 Stress (MPa)
150
125
100
75 31 32 33 34 35 36 LMP T (K) * (35.0 + Log time(hrs)) / 1000
Heat A: Blue Heat B: Green 10% Cold-Work 15% Cold-Work 20% Cold-Work 25% Cold-Work 30% Cold-Work Figure 3-2 Summarized Creep Rupture Test Results as a Function of Cold-Work Levels
Despite the anomalous behavior of the Heat B material, this preliminary study indicated that for the Grade 91 material there was a definite effect of cold-working by rolling on the creep rupture behavior of the material, especially at strain levels above 10%. The results further indicated that the greater the cold-strain level, the more significant the adverse effect on creep rupture properties. Questions remained, however, over the possible influence of the manner in which the material was strained on the material behavior, and over the magnitude of the effect at intermediate strain levels where, at present, there exists some confusion regarding the appropriate heat treatment practice. It was as an attempt to answer these questions that the current, more detailed study of cold-working effects was initiated.
3-4
EVALUATION OF COLD-WORK AND HEAT TREATMENT ON THE ELEVATED-TEMPERATURE CREEP RUPTURE PROPERTIES OF GRADE 91 MATERIAL USING COLD-BENT BLOCKS
The test program has been designed to obtain information on two unresolved questions. First, it is hoped that evaluating material that has been cold-deformed in a manner approximating the strain behavior of a tubular bend will answer the question of whether the method of straining substantially alters the response of the material to cold-working effects. Second, it is intended that the testing will more accurately characterize the response of Grade 91 material to cold-work effects at intermediate levels of strain as a basis for formulating technically defensible heat treatment requirements. Although the scope of the project has limited the evaluation to one heat of Grade 91 material, sufficient material is available to support a larger test matrix than originally proposed.
4.1 Material Preparation for Creep Rupture Testing

Four forged blocks of Grade 91 material, measuring 6" x 6" x 30" (152 mm x 152 mm x 762 mm) and representing one heat of material, were purchased for the program, because 6" (152-mm) thick plate of the Grade 91 material was not available at the time of the program start. The use of a 6" thick block was intended to minimize the through-thickness strain gradient, so that the local strain within the gage section of the creep rupture specimens could be maintained at a relatively uniform level. In comparison with the strain induced by the cold-rolling of plate, strain induced by bending provides a closer approximation of both the tension and compression strain patterns that develop during the cold-bending of tubing and piping. The chemical composition and mechanical properties of the Grade 91 heat are presented in Tables 4-1 and 4-2.
Table 4-1 Chemical Composition of the Grade 91 Heat for the Test Program Heat #
66071 (Alstom Lab) 66071 (Mill Report)
C
.085 .090
Mn
.44 .48
P
.014 .015 .020 max .025 max
S
.001 .001 .010 max .025 max
Si
.33 .33 .20-.50 .20-.50
Ni
.14 .16 .40 max .40 max
Cr
8.11 8.35 8.00-9.50 8.0-9.5
Mo
.93 .92
V
.21 .21
Nb
.07 .075 .06-.10 .06-.10
Cu
.13 -------
Al
.013 .017
N
.047 .049
ASME .08-.12 .30-.60 SA-387 Gr.91 ASTM A336-F91 .08-.12 .30-.60
.85-1.05 .18-.25 .85-1.05 .18-.25
.04 max .030-.070 .04 max .03-.07
4-1
Evaluation of Cold-Work and Heat Treatment on the Elevated-Temperature Creep Rupture Properties of Grade 91 Material Using Cold-Bent Blocks Table 4-2 Mechanical Composition of the Grade 91 Heat for the Test Program Heat # Tensile Strength (ksi) 106 85110 85110 Yield Strength (ksi) 87 60 min. 60 min. Elongation in 2" (%) 23 18 min. 20 min. Reduction in Area (%) 66 --40 min. Normalizing (F/h) 1900/5 19002000 19002000 Tempering (F/h) 1400/8 1350 min. 1350 min.
66071 (Mill Report) ASME ASTM
The as-received Grade 91material (four separate blocks) had been normalized and tempered by the mill after forging. To ensure uniformity of the microstructure throughout the 6" x 6" (152-mm x 152-mm) cross-sectional area of the blocks and to eliminate any coarse carbides that may have formed near the center of the blocks during slow cooling from the normalizing temperature, all four pieces were re-heat treated. The re-heat treatment consisted of austenitizing at 1940F (1060C) for 1 hour, quenching in oil, and tempering at 1436F (780C) for 1 hour. It should be noted that the tempering parameter for the re-heat treatment was adjusted to simulate V&M Tubings tempering practice for Grade 91 tubing. This re-heat treated structure then became the base condition for all subsequent testing in the program. During the entire course of the re-heat treatment, two pairs of thermocouples were attached to one of the four pieces so that the center and surface temperatures of the blocks could be monitored. The center thermocouple was installed into a 0.125" (3.2-mm) diameter x 3" (76-mm) deep centerline hole, located 6" (152 mm) from the end of the block, as shown in Figure 4-1. The holding time was recorded once the center of the block had reached the designated heat-treating temperature.
1 inch = 25.4 mm Figure 4-1 Sketch Showing the Center Thermocouple Location
After the re-heat treatment, a through-thickness hardness survey was conducted to verify the uniformity of the microstructure across the entire cross-section of the block. The hardness test results are summarized in Table 4-3, where it may be seen that the hardness was consistent throughout the cross section. Examination of the microstructure after the re-heat treatment using optical microscopy showed that the microstructure was uniform from the surface to the center of the test blocks and also confirmed the absence of coarse grain boundary carbides. A typical area of the microstructure of the Grade 91 test material after the re-heat treatment is shown in Figure 4-2. 4-2
Evaluation of Cold-Work and Heat Treatment on the Elevated-Temperature Creep Rupture Properties of Grade 91 Material Using Cold-Bent Blocks Table 4-3 Hardness Measurements from the Surface to the Center of the Block Location Near Surface Hardness (HB) 217 1" from Surface 212 2" from Surface 212 Center 212
Figure 4-2 Typical Microstructural Condition of the Grade 91 Material in the Re-Heat Treated Condition
4.2 Scale Model Study of the Bending Procedure for Preparation of Test Coupons
Based on the results of the tube bend strain measurements as described above, it was known that the actual strain levels in cold-bent tubing are typically 1.21.3 times the nominal strain level predicted using D/2R. In order to determine the most appropriate bending procedure to produce the desired levels of strain in 6" x 6" x 30" (152-mm x 152-mm x 762-mm) forged blocks, scale models of the blocks, measuring 1" x 1" x 5" (25.4 mm x 25.4 mm x 127 mm), were constructed 4-3
Evaluation of Cold-Work and Heat Treatment on the Elevated-Temperature Creep Rupture Properties of Grade 91 Material Using Cold-Bent Blocks
from Grade 91 plate material and bent using several different bending procedures. For the bending of these models, both 2" (50.8-mm) and 3.75" (92.25-mm) diameter dies were evaluated, coupled with 3-point bending, 4-point bending, and combination bending techniques. Prior to bending the scale models, 0.25" x 0.25" (6.35-mm x 6.35-mm) grids were marked on their surface to permit determination of the local strain after bending. A total of four scale models were made and evaluated, with extensive measurements and strain calculations obtained from each model. The results of the scale model study are summarized as follows: No cracking or tearing developed on the tension surface of the scale models to a maximum strain of 73%. Single-step 3-point bending caused a peaking effect, which resulted in a steep strain gradient in the longitudinal direction, as shown in Figure 4-3. 4-point bending required too high a bending force. Approximately 43 tons (39,000 kg) of bending force was needed to bend the 1" x 1" (25.4-mm x 25.4-mm) cross-section scale model. Multiple-step 3-point bending with various-size dies (upper and lower dies) created a desirable bend profile, as shown in Figure 4-3.
Figure 4-3 Typical Results of Single-Step 3-Point Bending and Multiple-Step 3-Point Bending
4-4
4.3 Bending the 6" x 6" x 30" Test Coupons

After reviewing the results of the scale model study with a manufacturing engineer familiar with the bending of heavy section components, a three-step 3-point bending procedure with varioussize upper and lower dies was selected to produce the cold-bent coupons for the program. The target maximum strain level on the tension surface was 34%. This target strain was identified based on the results of an evaluation of strain patterns recorded on a large group of cold-bent tubes, which represented a wide range of bend radii and tube diameters in common use for boiler applications. The evaluation showed that in cold-bent tubing the local strain produced on the outer fibers of the bend extrados would not normally exceed 35%. Prior to the bending, all side-surfaces of the blocks were mechanically cleaned and blue-inked. Then, 0.25" x 0.25" (6.35-mm x 6.35-mm) grids were marked over a 10" (254-mm) section near the center of the blocks, with 0.5" x 0.5" (12.7-mm x 12.7-mm) grids marked on 5" (127-mm) extensions from the center area. In addition, 1" x 1" (25.4-mm x 25.4-mm) grids were marked over a 20" (508-mm) center portion on the tension surface of the blocks. The change in the size of the grids permitted a determination to be made of the local strain level and strain distribution through the entire block, so that creep rupture test specimens could be removed from specific locations with the desired amount of strain. An example of the blocks ready for bending is shown in Figure 4-4.
4-5
Figure 4-4 Example of the 6" x 6" x 30" Test Blocks and the Grids Inscribed on the Surface of the Blocks Prior to Bending
The bending of the blocks was carried out in Alstoms header shop in Chattanooga, Tennessee, using a 6000-ton press. The bending sequence is documented in Figures 4-5 and 4-6, and an example of the cold-bent coupons is presented in Figure 4-7. During the bending, the metal temperature of the blocks was monitored using a laser-guided infrared thermometer. The maximum metal temperature of the coupons was controlled to maintain the metal temperature of the blocks below 150F (66C).
4-6
Figure 4-5 Bending Status After Completion of the First Stage in the Bending Process
4-7
Figure 4-6 Bending Status After Completion of the Second and Third Stages of the Bending Process
4-8
Figure 4-7 Final Condition of the Bent Test Coupons, with the Inscribed Grid Patterns Shown in the Bend Zone
4.4 Determination of Local Strain and Strain Distribution for Preparation of Creep Rupture Test Specimens
To accurately characterize the local strain produced during the bending of the blocks, 1200 separate measurements were obtained from the grid-matrix inscribed on the surfaces of each block. Based on these measurements, a strain matrix was generated for the entire bending zone produced on each block. Then, a specimen removal plan was formulated, identifying the location 4-9
for each creep rupture specimen that would represent the desired level of strain. All creep rupture specimens used in the test program were produced with a 0.505" (12.827 mm) diameter in the gage length. The orientation of the specimens relative to the test block was such that the specimens were removed from the tension side of the bend with the axis of the specimen transverse to the straining direction and parallel to the tension surface (as shown in Figure 4-8). Based on the results of the strain measurements across the entire bending zone, the variation in strain level within the gage section of any of the creep rupture specimens was calculated to be less than 5%.
Figure 4-8 Photo Showing Orientation of Test Specimens
It was possible to remove approximately 35 creep rupture specimens from each coupon, including 15 specimens with 1030% tension strain and 8 specimens with 1025% compression strain, in addition to 12 base metal specimens with 0% strain.
4.5 Creep Rupture Testing

Creep rupture testing was conducted on specimens obtained from the test blocks that represented the following conditions: Material with no cold-strain (0%) Material embodying various levels of cold-strain, but with no post-forming heat treatment Material embodying various levels of cold-strain, plus one of two post-forming subcritical heat treatments
The tests of the cold-strained material focused on tensile strains ranging from 10 to 30%. The test stress levels for the program ranged from 8.7 ksi (60 MPa) to 20.3 ksi (140 MPa), a range which spans the design stress levels for most applications in boilers. Test temperatures were selected to yield rupture times for the unstrained base metal between 300 and 10,000 hours. The time-to-rupture for unstrained base metal was estimated based on the imputed creep rupture properties for Grade 91 material calculated from the ASME SC I allowable stresses for sections above and below 3" in thickness, along with test data from ORNL, V&M Tubing, EPRI, MPC, and MHI [2, 8, 1114].
4-10
4.5.1 Creep Rupture Behavior of Unstrained Grade 91 Material The initial creep rupture tests were designed to locate the unstrained test material within the database population. That is, the test results for unstrained material were compared with the imputed mean and minimum properties calculated from the ASME SC I allowable stresses for section thickness above and below 3" (76 mm). As shown in Figure 4-9, the Larson-Miller plot of the results indicates that the creep strength of the unstrained material falls between the mean values for Grade 91 above and below 3" in section thickness.
4-11
100.0
Imputed Mean for Grade 91 (<3 in.)
Imputed Mean for Grade 91 (>3 in.)
Imputed Minimum for Grade 91 (<3 in.)
Imputed Minimum for Grade 91 (>3 in.)
Grade 91 Base Metal with 0% Cold-Work
Stress (ksi)
10.0
Note: Imputed Mean and Minimum Properties are Calculated Based on ASME SC I Allowable Stresses
1.0 57.00
58.00
59.00
60.00
61.00
62.00
63.00
64.00
65.00
66.00
67.00
68.00
69.00
LMP=(T+460)(36+logt)/1000
Figure 4-9 Documentation of the Creep Rupture Behavior of the Unstrained Grade 91 Test Material as Compared to the Imputed Mean and Minimum Properties for Grade 91 Material
4-12
4.5.2 The Effect of Cold-Work on Creep Rupture Behavior of Grade 91 Material The evaluation of the effect of varying levels of cold-work, specifically 10%, 20%, and 30%, on the creep rupture behavior of the Grade 91 material focused on two stress levels, 8.7 ksi (60 MPa) and 14.5 ksi (100 MPa). These stresses were chosen because they represented typical reheater and superheater design values. The test results are presented in Figure 4-10, where they are compared with the results obtained for the unstrained base metal (0%) as well as the imputed mean and minimum properties calculated from the ASME SC I allowable stresses for section thickness above and below 3" (76 mm). Based on the results obtained to date, it is clear that the cold-work induced during bending has had a significant and adverse effect on the creep rupture behavior of the Grade 91 material. The magnitude of the effect appears to be directly proportional to the amount of cold-strain, so that as the strain increases the creep rupture life decreases.
4-13
100.0 Imputed Mean for Grade 91 (<3 in.) Imputed Mean for Grade 91 (>3 in.) Imputed Minimum for Grade 91 (<3 in.) Imputed Minimum for Grade 91 (>3 in.) Grade 91-Base Metal (0% Cold-Work) Grade 91-30% Cold-Work Grade 91-20% Cold-Work Grade 91-15% Cold-Work Grade 91-10% Cold-Work Stress (ksi)
10.0
Note: Imputed Mean and Minimum Properties are Calculated Based on ASME Maximum Allowable Stress 1.0 57.00
58.00
59.00
60.00
61.00
62.00
63.00
64.00
65.00
66.00
67.00
68.00
69.00
LMP=(T+460)(36+logt)/1000
Figure 4-10 Documentation of the Effect of Cold-Work on the Creep Rupture Behavior of the Grade 91 Test Material, Based on Comparison with the Behavior of the Unstrained Base Metal
4-14
4.5.3 The Effect of Heat Treatment on Creep Rupture Behavior of Cold-Worked Grade 91 Material Two subcritical heat treatments, representing a low and a high tempering parameter (1350F [732C] for 30 minutes and 1425F [774C] for 60 minutes), were selected for evaluation. These heat treatments fairly represent typical postfabrication (tempering) heat treatment practice for Grade 91 tubular components. The creep rupture tests for the specimens representing these heat treatment conditions were conducted at a stress level of 14.5 ksi (100 MPa), with the cold-strain levels of 15%, 20%, and 25%. The creep rupture test results are shown in Figure 4-11, where they are compared with the results for the unstrained base metal (0%) and the cold-strained material at the 10%, 20%, and 30% levels.
4-15
100.0
Heat Treatment 1: 1350F for 30 Minutes Heat Treatment 2: 1425F for 60 Minutes
Imputed Mean for Grade 91 (<3 in.) Imputed Mean for Grade 91 (>3 in.) Imputed Minimum for Grade 91 (<3 in.) Imputed Minimum for Grade 91 (>3 in.) Grade 91-Base Metal (0% Cold-Work) Grade 91-30% Cold-Work Grade 91-20% Cold-Work Grade 91-15% Cold-Work Grade 91-10% Cold-Work Grade 91-25% Cold-Work + Heat Treatment Grade 91-20% Cold-Work + Heat Treatment Grade 91-15% Cold-Work + Heat Treatment
Stress (ksi)
10.0
Note: Imputed Mean and Minimum Properties are Calculated Based on ASME Maximum Allowable 1.0 65.00 65.20 65.40 65.60 65.80 66.00 66.20 66.40 66.60 66.80 67.00 67.20 67.40 67.60 67.80 68.00 68.20
Figure 4-11 The Effect of a Post-Forming Subcritical Heat Treatment on the Creep Rupture Behavior of the Cold-Worked Grade 91 Test Material Compared with the Behavior of the Unstrained Base Metal and the Cold-Worked Material with No Post-Forming Heat Treatment
4-16
The limited test results obtained indicate that post-forming heat treatment of the cold-worked Grade 91 material in the range of 1350F (732C) for 30 minutes and 1425F (774) for 60 minutes provides no significant increase in the creep rupture time. Comparing the results for the specimens heat treated at 1350F for 30 minutes with the results for specimens heat treated at 1425F for 60 minutes suggests a slight improvement in creep strength with a higher tempering parameter. 4.5.4 The Relationship Between Cold-Work-Induced Hardness Increase and Creep Life Reduction Hardness measurements were conducted on the Grade 91 material in all test conditions, including unstrained base metal (quenched and tempered), cold-worked (1030%), and coldworked plus post-forming heat treatment, using a Brinel hardness tester with the standard test condition (10-mm ball and 3000-kg load). The results of the measurements are recorded in Table 4-4. As expected, the increase in hardness stemming from the cold-work was found to be directly proportional to the amount of cold-strain. Also as expected, the post-forming heat treatments reduced the cold-worked hardness by an amount that was consistent with the tempering parameter for the specific heat treatment applied. What was not expected, but what is potentially of considerable practical interest, was the fact that the magnitude of the creep life reduction was directly proportional to the increase in hardness caused by the cold-work, as shown in Figure 4-12.
4-17
Evaluation of Cold-Work and Heat Treatment on the Elevated-Temperature Creep Rupture Properties of Grade 91 Material Using Cold-Bent Blocks Table 4-4 Cold-Work-Induced Hardness Increase and Creep Life Reduction Sample ID Hardness (HB) Hardness Difference (HB-HB0) 0
+
Life Reduction (%) Relative to Base Metal 0
Relative to Imputed Mean1
Grade 91 BM (0%) (HB0) Grade 91 (30% CW) Grade 91 (25%CW+1350F/30 min.) Grade 91 (25%CW+1425F/60 min.) Grade 91 (20% CW) Grade 91 (20%CW+1350F/30 min.) Grade 91 (20%CW+1425F/60 min.) Grade 91 (15% CW) Grade 91 (15%CW+1350F/30 min.) Grade 91 (15%CW+1425F/60 min.) Grade 91 (10% CW)
1
218 240 225 210 228 224 212 224 223 206 220
16+144% 6280%

22 7
5980%

+ +
65% 60%

56% 50%
10 6
46 54%

4250%
36% 25% --
20% 7%
6 6 5
+ +
4659%
+
5%
18% 6%
12 2
25%
490%
718%
Imputed mean value was calculated based on ASME SC I allowable stresses for Grade 91 with thickness greater than 3".
4-18
80
70
60
Life Reduction (%)
50
40
30
20
10
0 0 5 10 15 20 25
Cold-Work-Induced Hardness Increase (HV)
Figure 4-12 Creep Life Reduction as a Function of Hardness Increase Induced by Cold-Working
4-19
CONCLUSIONS
Principal conclusions of the study are as follows: Testing of Grade 91 material that had been cold-worked to approximate the strain induced during typical cold-bending of boiler tubes has confirmed that this cold-work does have a significant and adverse effect on the creep rupture strength of the material. Results to date indicate that there is no obvious threshold value below which the effect is absent, but that the magnitude of the effect increases with the level of cold-strain induced. Based on limited test results, a post-forming subcritical heat treatment conducted at tempering parameters commonly used in the fabrication of Grade 91 tubular components provided no significant benefit with regard to restoration of the creep rupture strength of cold-worked Grade 91 material. This is consistent with the explanation that attributes the degradation in properties induced by cold-work to accelerated recovery/recrystallization and the consequent reduction in the obstacles to dislocation movement. As expected, the increase in the material hardness due to cold-work was proportional to the amount of strain, and the tempering effect of the post-forming heat treatment was consistent with the relative magnitude of the tempering parameter. What was not expected was a possible relation between the magnitude of the creep life reduction and the increase in the material hardness caused by the cold-work. In general, the results of this study are in broad agreement with the results obtained from prior studies in which the cold-work was induced in the material through the cold-rolling reduction of plate specimens. Inconsistencies have been noted with the results of a recent V&M Tubing study, in which the impact of post-forming subcritical heat treatment on the rupture properties of the material included beneficial effects in some instances, apparently related to the magnitude of the tempering parameter. It will be necessary to resolve this question through additional testing, since the apparent benefits do not appear to be consistent with the mechanism by which it is assumed the degradation due to cold-work takes place.
5-1
RECOMMENDATIONS
Recommendations arising from the study include the following: Based on the information available to date, if the full strength of the Grade 91 material is required to ensure satisfactory service life, then when the amount of tensile strain induced during bending exceeds 20%, the full length of the tubing should be renormalized and tempered. Similar proposals currently are being considered by an ASME SCII Task Group, and action on this matter is expected in the near future. The benefits of post-forming subcritical heat treatments of cold-formed bends in Grade 91 material are minimal with respect to improvements in creep rupture life, and, therefore, they need not be applied for that purpose. Results of the recent V&M Tubing study indicate that under certain circumstances these heat treatments may, in fact, be damaging. However, other potential benefits of the post-forming subcritical heat treatment, such as a reduction in hardness or residual stress to avoid corrosion-related damage, may dictate that they be performed for a specific application.
6-1
FUTURE WORK
Alstom intends to continue the current program in order to confirm results obtained through relatively short-term tests by comparing them with the results of longer-term tests intended to run up to 10,000 hours. Additional creep rupture tests are planned to focus on intermediate strain levels in an effort to identify a threshold value below which the effect on properties is not practically significant. Tests also will be performed on specimens removed from the compression side of the bends to compare the effects on rupture strength of compressive and tensile strains of a similar magnitude. Duplicate specimens will be tested for all material conditions. Further validation of the effects of the cold-work will be obtained through the performance of carefully selected pressurized tubular creep rupture tests. The range of variations in response to cold-work between different heats of the material should be investigated in a systematic fashion, but there is currently no provision for such work to be carried out. Finally, microstructural studies will be conducted on material in all conditions represented in the creep rupture tests in order to correlate the loss of strength and the effect of post-forming heat treatment with the change in substructure.
7-1
REFERENCES
1. Contract AT (30-1)-4004 Correspondence: CEND-355 June 1969 (First Proposal for Development of 912%Cr for BRP Applications), CEND-360 December 1970. R&PD 960003-1 July 1970. 2. G. C. Bodine, Jr., B. Chakravarti, S. D. Harkness, C. M. Owens, B. W. Roberts, D. M. Vandergriff, and C. T. Ward, The Development of a 9Cr Steel with Improved Strength and Toughness. Paper 25 in International Conference on Ferritic Steels for Fast Reactor Steam Generators, British Nuclear Society, London, May/June 1997. 3. B. Chakravarti, G. C. Bodine, and C. T. Ward, Development of a Ferritic Steel for High Temperature Power Plants. Paper Presented at Materials Show and Conference of American Society of Metals, Chicago, October 2527, 1977. 4. G. C. Bodine, Jr., B. Chakravarti, S. D. Harkness, C. M. Owens, B. W. Roberts, D. M. Vandergriff, and C. T. Ward, A Program for the Development of Advanced Ferritic Alloys for LMFBR Structural Applications. TR-MCD-015, September 1977, Combustion Engineering, Inc., 1000 Prospect Hill Road, Windsor, Connecticut. 5. C. T. Ward, C-E Power Systems, Part I: Modified 9Cr-1Mo Steel Development Program Progress Report for Period Ending September 30, 1978, ORNL/BRP-79/2. Oak Ridge National Laboratory, Oak Ridge, Tennessee. 6. V. K. Sikka, Oak Ridge National Laboratory, Part II: Modified 9Cr-1Mo Steel Development Program Progress Report for Period Ending September 30, 1978, ORNL/BRP-79/2. Oak Ridge National Laboratory, Oak Ridge, Tennessee. 7. ASME, Specification for Seamless Ferritic and Austenitic AlloySteel Boiler, Superheater, and Heat-Exchanger Tubes, ASME Boiler and Pressure Vessel Code, Section II, Part A, SA213-2001. 8. Private Communication, C. T. Ward, Alstom Power, to R. W. Swindeman, ORNL. 9. A. Iseda, M. Kubata, Y. Haynase, S.Yamamoto, and K. Yosikawa, The Sumitomo Search, May 1988, pp. 1730. 10. F. Arav, H. J. M. Lentferink, C. F. Etienne, and J. C. Van Wortel, Effect of Fabrication Processes on the Creep Behavior of 9-12% Chromium Steels. Proceedings of the International Conference on Creep of Materials, Lake Buena Vista, Florida, May 121, 1992. 11. Vallourec Industries, The T91 Book. Revision 2, March 1994.
8-1
References
12. C. D. Lundin, P. Liu, G. V. Thorwald, and T. L. Anderson, Determination of Creep Behavior of Singular HAZ Regions to Model the Behavior of the Entire HAZ of Cr-Mo Steels (ASME T/P11, T/P91, T/P92, T/P122) In Elevated Temperature Service. Welding Research Council Bulletin 475, September 2002. 13. Mitsubishi Heavy Industries, ORNL/SMI/MHI/CE Joint Meeting on Super 9Cr (Modified 9Cr-1Mo). March 29, 1983. 14. Sumitomo Metals, Creep Data Sheets, Sumitomo Seamless Tubes and Pipe. December 1993.
8-2
MEASURED AND CALCULATED STRAINS FOR BENT TUBES USED IN THE STUDY
Location along Bend 0 30 60 90 120 150 180 11B B 9833-01 33% As Bent 0 30 60 90 120 150 180 Square after Bend (in.) 0.253 0.341 0.351 0.351 0.351 0.351 0.253 0.253 0.336 0.351 0.351 0.351 0.351 0.253 Calculated Strain (L / Li) 1.4 36.5 40.4 40.4 40.4 40.4 1.4 1.4 34.6 40.4 40.4 40.4 40.4 1.4
Tube # 11A
Heat # B 9832-01
Estimated Strain 33%
Heat Treatment As Bent
Tube # 12A
Heat # B 9832-01
Heat Treatment 1350F * 30 minutes
Location along Bend 0 30 60 90 120 150 180
Square after Bend (in.) 0.253 0.331 0.351 0.351 0.351 0.321 0.253 0.253 0.341 0.351 0.351 0.356 0.356 0.253
Calculated Strain (L / Li) 1.4 32.6 40.4 40.4 40.4 28.7 1.4 1.4 36.5 40.4 40.4 42.4 42.4 1.4
12B
B 9833-01
33%
1350F * 30 minutes
0 30 60 90 120 150 180
A-1
Measured and Calculated Strains for Bent Tubes Used in the Study
Location along Bend 0 30 60 90 120 150 180 13B B 9833-01 33% 1425F * 60 minutes 0 30 60 90 120 150 180 Square after Bend (in.) 0.253 0.341 0.341 0.341 0.346 0.331 0.253 0.253 0.336 0.351 0.341 0.351 0.336 0.253 Calculated Strain (L / Li) 1.4 36.5 36.5 36.5 38.5 32.6 1.4 1.4 34.6 40.4 36.5 40.4 34.6 1.4
Tube # 13A
Heat # B 9832-01
Tube # 15A
Heat # B 9832-01
15B
B 9833-01
25%
As Bent
0 30 60 90 120 150 180
A-2
Tube # 16A
Heat # B 9832-01
16B
B 9833-01
25%
1350F * 30 minutes
0 30 60 90 120 150 180
Tube # 17A
Heat # B 9832-01
17B
B 9833-01
25%
1425F * 60 minutes
0 30 60 90 120 150 180
A-3
Tube # 19A
Heat # B 9832-01
19B
B 9833-01
20%
As Bent
0 30 60 90 120 150 180
Tube # 20A
Heat # B 9832-01
20B
B 9833-01
20%
1350F * 30 minutes
0 30 60 90 120 150 180
A-4
Tube # 21A
Heat # B 9832-01
21B
B 9833-01
20%
1425F * 60 minutes
0 30 60 90 120 150 180
Tube # 24A
Heat # B 9832-01
24B
B 9833-01
15%
1350F * 30 minutes
0 30 60 90 120 150 180
A-5
Tube # 25A
Heat # B 9832-01
25B
B 9833-01
15%
1425F * 60 minutes
0 30 60 90 120 150 180
Tube #
26A
Heat #
B 9832-01
Estimated Strain
15%
Heat Treatment
As Bent
Location along Bend

0 30 60 90 120 150 180
Square after Bend (in.)

0.250 0.297 0.292 0.292 0.292 0.292 0.250
Calculated Strain (L / Li)

0.0 19.0 17.0 17.0 17.0 17.0 0.0
Note: There was not enough of Heat B 9833-01 to make 24 tubes. Therefore, this heat was not tested at 15% strain as bent.
A-6
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Effect of Cold Work and Heat - Tratment On The High Temp Rupture Properties of 91

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Effect of Cold Work and Heat Treatment on the Elevated-Temperature Rupture Properties of Grade 91 Material

Final Report, January 2005

EPRI Project Manager K. Coleman

DISCLAIMER OF WARRANTIES AND LIMITATION OF LIABILITIES

BACKGROUND AND INTRODUCTION

Background and Introduction

Background and Introduction

Background and Introduction

2.1 Deformation/Strain Determination Using the Grid Method

45 40 35 30 25 20 15 10 5 0 0 30 60 90 Tube Location (degrees) 120 150 180

Calculated Strain (in./in.)

35 30 Calculated Strain (in./in.) 25 20 15 10 5 0 0 30 60 90 Tube Location (degrees)

Calculated Strain (in./in.)

0 0 30 60 90 Tube Location (degrees) 120 150 180

2.2 Deformation/Strain Determination Using the Wall Thickness Method

Calculated Strain (in./in.)

Location Around Circumference (degrees)

Calculated Strain (in./in.)

Calculated Strain (in./in.)

Location Around Circumference (degrees)

20 15 10 5 0 -5 -10 -15 -20 -25 -30

Calculated Strain (in./in.)

2.3 The Effect of Heat Treatment on Cold-Worked Grade 91 Microstructure

REVIEW OF CREEP RUPTURE TEST RESULTS USING COLD-ROLLED GRADE 91 STRIPS

Review of Creep Rupture Test Results Using Cold-Rolled Grade 91 Strips

175 Stress (MPa)

75 31 32 33 34 35 36 LMP T (K) * (35.0 + Log time(hrs)) / 1000

Review of Creep Rupture Test Results Using Cold-Rolled Grade 91 Strips

175 Stress (MPa)

75 31 32 33 34 35 36 LMP T (K) * (35.0 + Log time(hrs)) / 1000

4.1 Material Preparation for Creep Rupture Testing

ASME .08-.12 .30-.60 SA-387 Gr.91 ASTM A336-F91 .08-.12 .30-.60

.85-1.05 .18-.25 .85-1.05 .18-.25

.04 max .030-.070 .04 max .03-.07

66071 (Mill Report) ASME ASTM

4.3 Bending the 6" x 6" x 30" Test Coupons

Figure 4-8 Photo Showing Orientation of Test Specimens

4.5 Creep Rupture Testing

Life Reduction (%) Relative to Base Metal 0

Relative to Imputed Mean1

Life Reduction (%)

Cold-Work-Induced Hardness Increase (HV)

Estimated Strain 33%

Heat Treatment As Bent

Estimated Strain 33%

Heat Treatment 1350F * 30 minutes

Location along Bend 0 30 60 90 120 150 180

0 30 60 90 120 150 180

Estimated Strain 33%

Heat Treatment 1425F * 60 minutes

Estimated Strain 25%

Heat Treatment As Bent

Location along Bend 0 30 60 90 120 150 180

0 30 60 90 120 150 180

Estimated Strain 25%

Heat Treatment 1350F * 30 minutes

Location along Bend 0 30 60 90 120 150 180

0 30 60 90 120 150 180

Estimated Strain 25%

Heat Treatment 1425F * 60 minutes

Location along Bend 0 30 60 90 120 150 180

0 30 60 90 120 150 180