The University of Michigan * Office of Research Administration Ann Arbor, Michigan A SURVEY OF CREEP-RUPTURE PROPERTIES AT 1100~F OF 2 1/4 Cr 1 Mo STEEL TUBES MADE BY MICHIGAN SEAMLESS TUBE COMPANY by R. Jackowski J, W. Freeman Project 05007-30-T July 31, 1964 MICHIGAN SEAMLESS TUBE COMPANY 400 WEST AVENUE SOUTH LYON, MICHIGAN

A SURVEY OF CREEP-RUPTURE PROPERTIES AT 1100~F OF 2 1/4 CriMo STEEL TUBES MADE BY MICHIGAN SEAMLESS TUBE COMPANY The Michigan Seamless Tube Company produces 2 1/4 CrAiMo steel tubes for use in superheaters and other high temperature applications. This report presents the results of a limited number of creep-rupture tests at 11000F designed to survey the high temperature strength of the tubing. The data obtained were to be used to select tubes for the 5000 to 10, 000 hour test now required for evaluation of superheater tubing, The samples were taken from production processed tubing so that the data would be representative of the tubes as supplied to customers. This insured that effects of prior processing, if any, unique to Michigan Seamless Tubing Company production would thereby be included in the investigation. Samples of 14 tubes were supplied, The production of all the tubing involved a cold working process prior to a final heat treatment. Of the 14 tubes, nine were annealed at 1450F., two were normalized and tempered, and two were annealed at 1750'F Tests were not carried out on a quenched and tempered tube. The steel for manufacturing the tube is purchased from steel producers. The investigation accordingly included tubes from different suppliers, A major objective of the investigation was to determine if the tubing as produced had the properties expected by the Table P7 stresses of the Power Boiler (Section I) Code of the ASME Boiler and Pressure Vessel Committee. While prolonged rupture tests were not included, the data were extrapolated in accordance with the general trend of data for 2 1/4 CrlMo steel to obtain approximate values for comparison with the Code values. The heat treatment preferred by Michigan Seamless Tube Company was an anneal at 1450~F. During the course of the investigation, the heat treatment clause in ASTM Specification A213 was changed, to cast doubt on the treatment at 1450~F meeting the requirements. When this became known, prolonged tests were postponed pending clarification of the heat treatment. 1

SUMMARY AND CONCLUSIONS Survey type rupture tests at 1100~F were carried out on 14 samples of production superheater tubing from Michigan Seamless Tube Company. Extrapolation of the stress-rupture time curves to 100, 000 hours indicated the following approximate rupture strengths (psi): Number of Maximum Average Minimum Tubes Tested Annealed 1450~F 9600 7080 6000 9 Normalized and --- 7400-6600 --- 2 Tempered Annealed 1750 F --- 7000-6800 --- 2 ASTM STP No. 151 8500 7700 6350 Limited tests on barstock ASME Boiler --- 4200 --- Based on "average" Code Stress creep strength The present Code stress of 4200 psi was based on an average stress of 4200 psi for 0. 01 percent per 1000 hours.creep rate. This was the controlling factor in that 60 percent of the average and 80 percent of the minimum stress for rupture in 100, 000 hours were both higher than 4200 psi.'The above tabulation shows that 80 percent of minimum rupture strengths were above 4200 psi. The average strengths were somexiat below the average used in evaluating data for the present Code stress but certainly well within the range of strengths. One prolonged creep test at 4200 psi was conducted on a sample from Tube 1 (Ann, 1450~F). This test indicated a stress of 3800 psi for a minimum creep rate of 0 01 percent per 1000,hour's, This is slightly below but certainly within the range of rates in which the Code stress of 4200 psi was set. It is, however, "low" in that prolonged testing usually results in creep strengths considerably higher than those of the short time tests on which the present Code stress was set. The tubes annealed at 1450~F had a wide range range in rupture strengths including high values for Tubes 12, 13 and 14 which were specially processed 2

to produce high rupture strengths. It also resulted in the lowest strength measured, Normalizing and tempering or annealing at 1750~F resulted in near average values. Microstructures varied sufficiently to preclude their use as a means of identifying high or low strength material. The source of steel showed no significant effect although the data were too few to be certain. DESCRIPTION OF TUBES The information supplied describing the samples of tubes submitted is summarized in Table 1. Most of the tubes were finished by cold working and "annealing" at 1450~F. Two tubes (No.'s 6 and 9), however, were given a "full" anneal at 1750~F and two tubes (No's. 2 and 10) were normalized and tempered. Tube No. 11 was submitted after water quenching from 1700~F and tempering at 1450~F, although no testing was carried out in view of the general concensus that tempered martensite would have poor properties,, Tube 2 was made by normalizing and tempering Tube 1 stock which had been prior annealed at 1450 ~F Tubes 4 and 5 were tested to compare material for tubes from two sources of supply. Tube 6 was included to provide comparative data for full annealing using the same material as Tube 5. Tubes 7 through' 11 were submitted to evaluate manufacturing variables using one heat of steel. They included tube reducing versus cold drawing, as well as heat treatment variables. Tube 7 had both an unusual microstructure and an unusual stressrupture time curve. Tube 12 was submitted to check the unusual characteristics of Tube 7, Tube 12 had unusually high rupture strength. Tubes 13 and 14 were submitted to determine if the high strength of Tube 12 could be duplicated. 3

RESULTS The data from the rupture tests at 1100 F are given in Table 2. The stress-rupture time curves defined by the data are shown as Figures 1 through 3. Plates 1 through 14 show the microstructures prior to testing. Boiler Code stresses at temperatures where creep controls strength are based on the following properties: (1) The stress for rupture in 100, 000 hours, (2) The stress for a creep rate of 0. 00001 percent per hour (usually extrapolated as the stress for a creep rate of 001 percent per 1000 hours and sometimes as the stress for 1 percent creep in 100, 000 hours), The Code stress is the lowest of the following: (a) 60 percent of the average stress for rupture in 100, 000 hours, (b) 80 percent of the minimum stress for rupture in 100, 000 hours. (c) 100 percent of the average creep strength for 0, 01 percent per 1000 hours. Accordingly, the stress-rupture time curves obtained were extrapolated to 100, 000 hours, recognizing that the testing was less than that considered necessary for reliable extrapolation to 100, 000 hours. The extrapolations were based on the curves defined by the test points, a reasonably reliable procedure because 2 1/4 Cr.lMo steel usually has stress-rupture time curves which do not change slope, The rupture strengths for 100, 000 hours derived by extrapolation are given in the following tabulation: 4

Extrapolated 100,000-hour Tube Rupture Strength No. Heat Treatment (psi) 1 Anneal at 1450 F 6400 3 Anneal at 1450 F 7500 4 Anneal at 1450~F 6000 5 Anneal at 1450~F 6400 7 Anneal at 1450~F 6700 8 Anneal at 1450 F 6200 12 Anneal at 1450~F 9600 13 Anneal at 1450~F 7000 14 Anneal at 14500F 8000 Average Anneal at 1450~F 7080 2 Normalize 1650~ - temper 1375~F 6600 10 Normalize 1750~ - temper 1375~F 7400 6 Annealed 1750 F 7000 9 Annealed 1750~F 6800 11 Water quench 1700~F + temper at 1450~F No tests, The comments regarding these rupture strengths are as follows: 1. The range in strengths for rupture in 100, 000 hours obtained by extrapolation are as follows: Annealed at 1450~F -- 6000 to 9600 psi (9 tubes) Full annealed 1750~F ----- 6800 to 7000 psi (2 tubes) Normalized and tempered ----- 6600 to 7500 psi (2 tubes) These data would seem to indicate that annealing at 1450~F can produce as high or higher rupture strength as a full anneal or a normalize and temper as well as very low strengths. 2, The range of rupture strengths for an anneal at 1450~F apparently is not a "statistical" scatter but involves changes in prior processing to alter properties when heat treated at 1450 F. 3, Tubes 13 and 14 were submitted to verify that the high strength of Tube 12 could be reproduced. They were higher than average but below the 5

high value for Tube 12. 4. A full anneal of Tube 6 at 1750~F compared to Tube 5 with a 1450~F anneal only raised the strength from 6400 to 7000 psi. This is hardly a significant change. In the case of Tube 9, the anneal again resulted in only slightly higher strength than for Tubes 7 and 8 from the same heat. There is only a slight superiority indicated for the full anneal but it should be noted that in both cases it led to a higher strength than the 1450~F treatment. 5, Normalizing and tempering of Tube 1 rra terial after the original treatment at 14500~F to produce Tube 2 material hardly changed the strength at long time periods. It did, however, raise strengths at short time periods (See Fig. 3). Tube 10 had a 100, 000 hour strength of 7400 psi while Tube 7 and 8 annealed at 14500F or Tube 9 annealed at 17500F had slightly lower strengths. Again short time strengths were high for normalizing and tempering. 6. Tubes 4 and 5 did not show a significant difference between suppliers of steel. Tube 14 also did not show a significant difference which could be attributed to the steel producer. 7. Tube 7 had a microstructure (Plate 5) of fine pearlite in coarse grains. This was a considerably different structure than the other tubes heat treated at 1450~F. The stress-rupture time curve was also high at short times with a relatively steep slope reducing long time strength. 8. Tube 12 made as a check on Tube 7 had the usual microstructure expected (Plate 7) for annealing at 1450~F after cold work. The available data showed less slope and extrapolated to the highest stress for rupture in 100, 000 hours of all tubes tested. 9. Tubes 13 and 14 were used to check the reproducibility of the high strength of Tube 12 using steel from two suppliers. The results of the tests resembled those of Tube 7 more than they did those for Tube 12 - i. e., higher strengths at short time periods and steeper curves than the other curves for tubes heat treated at 1450~F, The duplication was not too good although the extrapolated stresses for rupture in 100, 000 hours were higher than the other tubes heat treated at 1450 F. 6

Creep Test A creep test on a specimen from Tube 1 was run for 4242 hours (Fig. 4) at 1100~F under 4200 psi, the present Code stress. At this time the creep rate had become essentially constant (Fig. 5) at 0. 000015 percent per hour (0.015 percent per 1000 hours). The creep rates used in Fig. 5 were obtained from a working curve drawn to a scale more consistent with the sensitivity of the creep measuring equipment than could be drawn in the condensed scale of Fig. 4. Extrapolation of this rate to 0. 01 percent per 1000 hours by using a curve with a slope usually exhibited by this steel (Fig. 6) indicates a creep strength of 3800 psi. The error in this procedure should be small because the rate of the actual test was so close to 0. 01 percent per 1000 hours. Because the creep rate had not changed for a considerable period of time, continuing the test to longer times would not have changed the strength significantly. Microstructures The microstructures of the tubes (Plates 1 through 14) indicate the following: 1. The material annealed at 1650~F prior to cold working and annealing at 1450~F had a structure of fine ferrite grains slightly elongated along the axis of the tube with spheroidized carbides (Plate 1). 2. When annealed at 14500F prior to cold working and then again annealed at 1450~F after cold working resulted in considerable variation in microstructures. Tube 3 (Plate 2) had a structure which was a combination of coarse ferrite grains and what appeared to be tempered bainite. Tubes 4 and 5 had structures (Plates 3 and 4) similar to Tube 3, Tube 7, however, had a structure (Plate 5) that appeared to be bainite or extremely fine pearlite in ferrite. Tube 8 (Plate 6) had a structure of ferrite plus highly spheroidized carbide particles. The only reported difference between Tubes 7 and 8 was cold drawing rather than tube reducing prior to the final heat treatment at 1450~F. Tube 12 (Plate 7) was more like Tube 8 than Tube 7 although there were a few small areas of the "bainite like" structure in Tube 12, Tubes 13 and 14 (Plates 8 and 9), however, had structures similar to Tube 7, 3. Normalizing Tube 2 at 16500F and tempering at 1375~F produced a structure (Plate 10)of fine ferrite grains with small areas of spheroidized 7

carbides which apparently had formed in the austenite transformed during treatment at 1650~F. Evidently 1650~F was below the upper critical temperature and transformation was only partially complete. Increasing the normalizing temperature to 17500F (Tube 10 and Plate 11) evidently caused complete transformation to austenitea On air cooling this produced a structure of bainite or very fine pearlite which was not appreciably changed by the temper at 1375~F. 4. A full anneal of Tube 6 at 1750~F resulted in fine ferrite, some imperfect pearlite grains and extensive carbide spheroidization (Plate 12). Tube 9 (Plate 13) had a considerably coarser grain size and no evidence of pearlite. For reasons not understood from the available information, there was a marked difference in microstructure for these two full annealed tubes, 5. As expected the structure of Tube 11 (Plate 14) was tempered martensite. The structures seem to indicate that the 1700~F treatment caused complete transformation before quenching to martensite. The treatment at 14500F tempered the martensite and caused precipitation and some agglomeration of carbides. The number of variations in the microstructures of the tubes for a heat treatment at 1450~F indicates prior history effects. The variation in structure for the two normalized and tempered tubes was not unexpected due to the difference in normalizing temperature. Also the normalize was applied to tubing which had primarily been annealed 14500F for Tube 2 while it was applied to a cold worked structure for Tube 10. The difference in microstructure for the two fully annealed tubes was unexpected. It must reflect a difference in response to heat treatment between heats if the conditions of heat treatment were the same as the data indicate. Reviewing these microstructures in relation to the results of the rupture tests seemingly leads to two conclusions: (1) Rupture strengths could not be predicted from the microstructures, (2) Microstructures would not identify the heat treatments. It would only be fair, however, to point out that the reported conditions of heat treatment also did not define the rupture strengths. 8

DISCUSSION The investigation was undertaken with the objective of defining the creep-rupture strength of tubes made for superheater service by Michigan Seamless Tube Company under ASTM Specification A213. Fourteen samples of tubing were submitted. All were hot pierced and hot rolled, annealed, cold worked to final size and then finally heat treated. Nine of the samples were annealed at 14500F as a final heat treatment; two tubes were normalized and tempered; two tubes were full annealed at 17500F; and one was quenched' and "tempered" at 1450 ~F The survey rupture tests at 11000F gave data which can be evaluated as follows: Extrapolated 100, 000-Hour Rupture Strengths (psi) Maximum Average Minimum Annealed 1450~F 9600 7080 6000 9 tubes Normalized + Tempered 7400-6600 2 tubes Full annealed 1750~F 7000-6800 2 tubes ASTM STP No. 151 8500 7700 6350 Limited tests on barstock Present Code Stress 4200 (based on "average" creep strength) The 100, 000-hour rupture strengths at 11000F for the tubes annealed at 1450~F cover the range for the steel. The data for Tubes 12, 13 and 14 suggest that prior history control might keep strengths at or above average. The low values are within the range which the present Code stress would accept (i. e., 60 percent of the "average" for tubes treated at 1450~F was 4248 psi and 80 percent of the minimum was 4800 psi. From this viewpoint the tubes treated at 14500F had rupture strength meeting the Code stress minimum criteria. No tests were conducted on the quenched tube due to tue to the general opinion that tempered martensite would have low strength. 9

The tubes which were full annealed or normalized and tempered had near average and well above minimum rupture strengths. The 3800 psi creep strength after annealing at 1450~F for the only tube tested was on the low side of the range for creep strength in STP No. 151 but within the range of data. One creep test does not define the creep strength for treatment at 1450~F and therefore the significance of the test is uncertain. Another objective of the tests was to survey the product and select tubes for the 10, 000-hour rupture and creep tests generally considered necessary to properly determine superheater tube strengths. The alteration in the heat treatment clause of the ASTM A213 specification after the investigation was started and the subsequent disagreements in interpretation had been a major factor in not proceeding with the prolonged tests. It should be recognized, however, that for T22 material the justification for requiring an anneal from near or above the upper critical temperature was largely based on creep strengths (not rupture strengths). In this report the relatively low strength of the one creep test on Tube 1 supports the probability of creep strength on the low side of the range for sub critical temperature heat treatments after cold work. This again is subject to the qualification that Tubes 12, 13 and 14 suggest that there are conditions of prior treatment which could if properly controlled yield average or better strengths The lack of a correlation of microstructure with either heat treatment of creep-rupture properties suggests that factors other than heat treatment were influencing properties. This would not be surprising for annealing at 1450~F. It was, however, surprising for the other two heat treatments, Examination of the data show no significant differences in tubes made from steel from two sources. 10

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Table 2 STRESS-R.UPTUR.E TIME DATA AT 1100~F FOR MICHIGAN SEAMLESS TUBE COMPANY 2 1/4 Cr - 1 Mo STEEL TUBING Rupture Elongation Reduction of Tube No, Stress(psi) Time(hours) (% in 2 inches) Area (%) Heated for one hour at 1450~F, air cooled, 1 20,000 25,,9 63, 5 870, 17,000 63 72.0 84..5 15,000 155 71, 0 84. 5 13,000 560 74,5 81.0 11, 000 1664 62.5 77, 0 3 17,000 86.2 47.0 83 0 15,500 174 71.0 84.0 14,000 562 52 5 81.0 12, 500.1187 69., 5 83, 5 4 16,000 106 54,0 59.0 14,800 151 45.5 60.0 13,000 401 39.0 55 5 5 16,000 187 38,5 53.5 14, 500 280 33.5 46.5 13,500 410 35.5 49 5 12,000 974 38.5 50, 0 7 19,000 238 49. 0 80.0 17,000 384 68, 5 81,0 15,500 814 55,5 77, 5 8 17,000 79 4 67.0 87. 5 14,000 265 59,0 86.5 12,000 1005 68.5 86 5 12 16,000 123 51 0 55 5 14, 500 449 50.0 70.0 13,500 1063 56.0 62 5 13 16, 500 369 59. 5 65 5 14, 500 905 41. 0 66 0 13,500 1516 45,0 61.5 14 16,500 864 43,5 63.5 14,500 1575 43,5 67.5 13,500 3225 36,5 56.0

Table 2 (continued) Rupture Elongation Reduction of Tube No. Stress(psi) Time(hours) (% in 2 inches) Area (%) Heated for one hour at 16500~E air cooled and tempered for one hour at 1375LF, air cooled. 2 17,000 180 55.0 81.0 15,000 393 58.0 82. 5 12,000 1924 55.0 74.0 Heated for one hour at 1750~F, air cooled and tempered for one hour at 1375~F 10 17,000 299 60. 5 85.0 15,000 726 49.0 82. 5 14,000 1181 50.5 83.0 Furnace cooled 50 /hour from 1750~F 6 17,000 70.5 85.0 76 5 14,000 335 59.5 70.5 12,500 799 60,0 61. 0 9 17, 000 62.2 76, 5 91 5 14,000 305 72 0 89. 0 12,500 697 62.5 90.0

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