ENGINEERING RESEARCH INSTITUTE THE UNIVERSITY OF MICHIGAN ANN ARBOR, MICH. REPORT ON INFLUENCE OF PROTECTIVE COATINGS ON THE RUPTURE PROPERTIES OF '111722-A"V,, MODIFIED TYPE 403, AND 422 ALLOYS IN SHEET FORM (PHASE IV) by K, P. MacKay J, W., Freeman Project 2536 December 31, 1957 Curtis s-Wright Corporation Wright Aeronautical Division Wood-Ridge, New Jersey

INFLUENCE OF PROTECTIVE COATINGS ON THE RUPTURE PROPERTIES OF "17-22-A"'V9 MODIFIED TYPE 403, AND 422 ALLOYS IN SHEET FORM (PHASE IV) IThe influence of protective coatings on the properties of three heattreatable ferritic alloys in sheet form was evaluated by rupture tests, Two coatings, Solar Alcote and Al'=Dip Coating by Arthur Tickle Engineering Company processes9 were used on- "17-22-A"V steel sheet for test temperatures of 1100', 1200' and 1300'F, Modified Type 403 stainless steel sheet was evaluated at I 100' and 1200'F with these two coatings plus a sprayed Colmonoy coating applied by Metallizing Engineering Company, The investigation also included 422 stainless steel sheet at 1100' and 1200'F with Solar Alcote, Comparative properties were established for the uncoated condition at the same temperatures and at 900' and 1000'F for the Modified Type 403 and 422 alloys, The evaluations were based on rupture strengths for 209 80 and 300 hours, Standard heat treatments were applied to the specimens of uncoated alloys, For the coated specimens, the thermal treatments required for applying the coatings occurred after the standard heat treatments,

2 SUMMARY AND CONCLUSIONS There was surprisingly little difference in strength and ductility between coated and uncoated specimens for 20, 80 and 300 hours, The two largest exceptions wereo 1, The slopes of the stress-rupture time curves at 1300'F were considerably less for the coated than for uncoated condition in " 17-22 A"V sheet, Presumably this resulted from protection against the rather rapid rate of oxidation of this steel at 1300"F, However, the material coated by the Arthur Tickle Al-Dip process was considerably stronger than that with the Solar Alcote, The uncoated condition was equal in strength to the Arthur Tickle coated material at 20 hours and fell to that of the Solar Alcote at 300 hours. Thus the influence of the coatings between 20 and 300 hours at 1300'F was no larger than the influence of thermal treatments during coating on the properties of the alloy 2, The 422 alloy sheet with the Solar Alcote was substantially lower in rupture strength at 1100' and 1200'F than the uncoated condition, Presumably this was due to the effects of the thermal treatments during coating on the properties of the base material, The information supplied, however, did not explain why a similar effect was not evidenced for the Modified Type 403 steel, The data indicated that the Solar Alcote condition would have had inferior properties to the Arthur Tickle coated and uncoated conditions of 't17-22-A"V sheet for time periods longer than 300 hours at 1100' and 12001F. Presumably this was mainly due to structural differences in the base material caused by thermal treatment conditions during coating, The evidence is not, however, definite and there may have been factors associated with the coatings themselves involved, Aluminum coatings would be expected to have major benefits where their high oxidation resistance protected the specimens during testing from surface oxidation, Because '' 17.-22PA"'V steel is a less oxidation resistant than the two

3 12 Cr type steels in the investigation and because it was tested at 1300'F, it would be expected to be most improved by the coatings, as was found, It appeared, however, that even in this case for time periods up to 300 hours other factors were just as effective in altering properties as the coatings. The Modified Type 403 and 422 sheet probably had sufficient oxidation resistance so that the protection from the coatings had little effect in time periods up to 300 hours at 1 100 and 1200F6,

4 EXPERIMENTAL MATERIALS The materials used to evaluate the -effects of protective coating are described in Table 1, The heat numbers, chemical compositions and thickness values are those reported to the University by the Wright Aeronautical Division, It was further reported that the sheets had been heat treated as listed in Table 1,, Specimens were taken transverse to the direction of rolling of the sheet. The specimens were 22-inches long with a 0, 5-inch wide by 2-inch long gage length at the center, WAD machined and heat treated the specimens and carefully measured the dimensions of the gage section before coating, Both coated and uncoated specimens were supplied for the investigation, The information supplied regarding the three types of coatings investigated was as follows: 1, Solar Alcote by the Solar Aircraft Company, San Diego, California, Coating S1099A was applied by dipping for 25 minutes at 1400'F and then "diffusing'" for 15 minutes at 1250'F, 2, Al-Dlp Coating by Arthur Tickle Engineering Works9 Brooklyn9 New York, The coating was a 12-percent silicon alloy per WAD 5757 diffused at 1250'F, 3,, Metallizing Engineering Company9 Westburg, Long Island, New York Colmonoy alloy (AMS 4775) was sprayed and fused at approximately 2000'F, The coatings were applied to the alloys investigated as follows: I, Solar Alcote " 17 -22 -A"V Modified Type 403 (WAD 8105) 422 Alloy (WAD 8107) 2, Arthur Tickle Engineering Works Al-Dip 1t 17,-22 A t"V Modifled Type 403 (WAD 8105) 3, Metallizing Engineering Company's Colmonoy Coating Modified Type 403 (WAD 8105)

5 The original program included the A-Dlp coating (by Arthur Tickle Engineering Works) for the 422 alloy. This material was deleted from the program due to procurement difficulty. The Metallizing Engineering Company coating was only planned for the Modified Type 403 material. A coating by the Chicago Vitreous Company was to be included for all three alloys; but was deleted when the coated specimens were found to have numerous flaws, PROCEDURE Evaluation of the coatings was based on rupturetest results for uncoated and coated specimens, Both coated and uncoated specimens of "17-22-A"V steel were tested at 1100, 1200' and 1300'F, The Modified Type 403 and the 422 steels were tested at 1100 and 1200OF in both conditions and at 900 and 1000QF in the uncoated condition, The rupture tests were conducted in single-specimen units, Stresses were applied by simple beams except for those test conditions in which the required load was so low that direct dead.weight loading could be used, In conducting the tests the following general procedure was used~ 1, The specimens were set-up in the rupture units and the furnace brought to within 50-'F of the test temperature between 4:00 and 5:00 p, m, 2, The temperature was equalized overnight and adjusted the next day so that variation along the gage length and from the nominal test temperature was less than +3'F. 3, Temperature adjustments were completed so that the stress was applied by 1:00 p0 m, The stress and required loads were based on the dimensions of the specimens before coating as supplied by WAD,

4, An automatic timer was started at the time the load was applied to measure the rupture time, 5, Elongation values were obtained by measuring the change in the gage length after rupture, Punched gage marks were not used, the changes in the measured length of the 0. 5-inch wide portion of the gage length being used instead. No creep data was taken, RESULTS The data from the rupture tests on "17-22-A"V steel, Table 2, were used to plot the stress-rupture time curves of Figure 1. Similar curves for the Modified Type 403 steel, Figure 2, were based on the data in Table 3, The data in Table 4 was used to plot the curves of Figure 3 for the 422 alloy. Rupture strengths for 20, 80 and 300 hours derived from the curves of Figures 1, 2 and 3 are included in Tables 29 3 and 4 and are shown graphically as a function of temperature by Figures 4, 5 and 6, The results for each alloy are presented in detail in the following three sections of the report, "'17-22HA"V Alloy Sheet The rupture strengths for the uncoated and coated sheet were established (Table 2 and Fig, 1) at 1100', 1200' and 1300'Fo The results show that: 1, Rupture strengths decreased markedly with increasing temperature (Fig, 4), 2, Over the time range of 20 to 300 hours at 1 100 F there was very little difference in rupture strength and ductility between uncoated and coated specimens9 or between Solar Alcote or Arthur Tickle Al-Dip coatings. The coated specimens were slightly weaker at short time periods, Those coated by the Solar Alcote process appeared to be falling off in strength more than the other coating or the uncoated material at the longer-time periods,

7 3,, When tested at 1200*F, the drop in strength at the longer-time periods for the Solar Alcote specimens was more marked than at 1100F. The Al-Dip coating by the Arthur Tickle process also appeared to have a steeper stressrupture time curve at the longer time periods so that a slight superiority in strength between 20 and 300 hours, disappeared at 300 hours, There was no marked difference in ductility and all three conditions had high ductility in the rupture tests, 4, When tested at 1300'F, the AlDip coating by the Arthur Tickle process had a stress -rupture time curve parallel to that for the Solar Alcote but at a substantially higher stress level, The uncoated condition started out with high strength but had a steeper stress-rupture time curve than for the coated specimens, Thus the uncoated had rupture strength equal to that of the Arthur Tickle Al-Dip coated specimens at 20 hours and fell to the strength of the Solar Alcote specimens at 300 hours. Again all three materials had high and similar ductilities, 5, The differences in rupture strength for 20, 80 or 300 hours ranged between 1000 and 3000 psi with the most common difference being about 2000 psi, Modified Type 403 Sheet The rupture properties of the uncoated condition were evaluated at 900, 1000, 1. 00 and 1200~F (Table 3 and Fig. 2). All three coatings were evaluated at 1100' and 1200F,. Rupture strength decreased quite uniformly over this temperature range (Fig, 5), Rupture strength differences between uncoated and coated specimens or between the three-coating processes were of the order of 2500 psi or less at 1100 -and 1200~F, The curve of Figure 2 at 12001F for the Solar Alcote process was drawn to show the lowest possible strength indicated by the data,

8 Ductility of the uncoated specimens increased from about 12 percent at 900'F to about 25 percent at 1200'F, The Solar Alcote did not change ductility at 1100' and 1200'F, The Arthur Tickle Al-Dip coating tended to increase ductility particularly at 1200 F,. The Metallizing Engineering Company Colmonoy coating increased ductility substantially, except for one specimen tested at 1200'F which had both low strength and ductility, 422 Alloy Sheet The rupture strength of the uncoated sheet (Table 4 and Fig, 3) decreased directly with increasing temperature (Fig. 6), The material with the Solar Alcote coating had substantially lower strength than the uncoated condition at 1100 and 1200'F, There was not much change in ductility in the rupture tests with test temperature or as a result of coating, The stress dependency of rupture time was very small at 900' and 1000'F, At 1200'F. there was a considerable increase in the slope of the stress-rupture time curves for both uncoated and coated specimens, at least for time periods longer than 50 to 80 hours, DISCUSSION The Solar Alcote and Al-Dip coating by Arthur Tickle Engineering Company were definitely in the class of so-called aluminum coatings. It is understood that the Colmonoy coating applied by the Metallizing Engineering Company was also an aluminum base coating, Aluminum coating could be expected to influence rupture properties by prevention of reduction in strength and ductility associated with ductility, In the test results, however, consideration must be given to the possible alteration of properties of the base material as a result of the thermal treatments required to apply the coatings changing the metallurgical structure from that of the uncoated condition,

9 The only case where there was a substantial effect on rupture strength was the lower strength of the 422 material with the Solar Alcote. Because it is presumed that the coating would tend to offset damage from oxidation, it is presumed that the strength of the base material must have been reduced by the thermal treatments during application of the coating. Yet it is difficult to understand why the thermal treatment associated with coating of this material should have had so much effect on the 422 alloy when there was little apparent effect on the Modified Type 403 material, The reported conditions of heating for coating was the same in both cases and both alloys would be expected to respond in a similar manner, The slopes of the curves for the tests on "l7-22-A"V material at 1300'F indicated that the coatings were probably helping to maintain strength by reducing surface deterioration by oxidation, The issue is, however, clouded by the apparent breaks in the curves at 1100- for Solar Alcote specimens and at 1200-F for both coated materials, The only case where appreciable beneficial effects seemed indicated by the data.was "17-22-A"V sheet at 1300F,e Oxidation of this alloy would be expected to be quite rapid at 1300'F and protection against oxidation would be expected to show benefits, Even in this case, however, alteration of properties of the base metal by thermal treatments associated with coating had as much effect as oxidation protection, This latter observation was based on the differences in strength between the samples coated by the Solar Alcote and Arthur Tickle processes, Other factors could be involved, It is known that exclusion of oxygen during tests often results in lower creep-rupture properties than for tests conducted in air, A highly oxidation resistant coating could act in this way, The authors, however, know of no case where this effect has been proven for aluminum coating,, Also, the coatings would be expected to be weak and possibly brittle, Thus deterioration of the coating by creep might influence results,

10 Stress for the tests were based on specimen dimensions before coating, So far as is known, this provided a fair basis of evaluation, Certainly it would be better than using dimensions after coating with the increase in thickness due to the weak aluminum alloy coatings. Only three or four rupture tests were used to evaluate the materials at each temperature, In a number of cases the data were erratic, Both the few tests and the erratic results tended to cast doubt on the exact rupture strengths, However, the results are valid for evaluating the effects of the coatings,

TABLE 1 DESCRIPTION OF EXPERIMENTAL MATERIALS Modified t"17-22-A'"V Type 403 Rezistal 422 Material (AMS 6436) (WAD 8105) (WAD 8107) Heat N6,, D 14468 4566 142761 Sheet Thickness (inch) 0, 062 0, 063 0, 049 Chemical Composition (Percent) C 0, 20 - 0,25 0, 18 0,22 Cr 1,00 1- 50 12,28 11,71 W o 0.93 Si 0.,55 0,75 0,46 0,36 Ni d 0,50 max, 0, 12 0 69 Mn 0. 60 - 0 90 0, 48 0, 68 Mo d 0 40 - 0 60 1, 09 0. 94 P O., 040 max. 0, 019 S 0,. 040 max, 0, 015 0.018 Va ' i 0.75 - 0,95 0,22 0,26 Cu ~ 0,50 max. Note- Actual composition of the " 17-22-A"V was not available, The analysis given is the range in AMS 6436. Specified Heat Treatments for Experimental Materials Normalizing Conditions Tempering Conditions Temperature Time Temperature Time Rockwell C Material ('F) (hours) (F) (hou)L Hardness 17-22A(V) 1775 0,5 1200 6 26/32 (AMS 6436) Mod, Type 403 1800 0,5 1100 2 35 (WAD 8105) Rezistal 422 1900 0.5 1150 2 34 (WAD 8107)

TABLE 2 RUPTURE PROPERTIES OF UNCOATED AND COATED ''17-22-A"V STEEL SHEET (Heat D1-4468 AMS 6436) Test Rupture Coating Temperature Stress Time Elongation Process (-F) (psi) (hours) (% in 2 in. ) Uncoated 1 100 40,000 0,.3 30 35,000 2,4 27 35, 000 2., 5 36 28,500 24.2 22 26,000 35.5 32 21 500 184.9 37 Solar Alcote 1100 29 000 5,0 32 23,500 120,2 32 20,000 275.0 39 18,000 293.5 30 Arthur Tickle 1100 29,000 5,2 35 23, 500 66.6 44 20,000 272.3 38 19% 000 451.,3 26 Uncoated 1 200 18, 000 18. 9 36 13,000 107, 1 30 11,000 233.9 28 Solar Alcote 1200 19,000 8, 7 29 14, 000 66.9 41 12, 000 112, 3 32 9,000 169.0 42 Arthur Tickle 1200 20,000 6,3 42 16,000 57, 4 56 14,000 104.7 34 11,000 267,5 32 Uncoated 1300 9,500 23,8 54 6,500 100.0 69 5,.000 203.0 36 Solar Alcote 1300 8,500 16,9 46 7,9000 30.7 52 4,500 140, 9 42 3, 500 812,7 - Arthur Tickle 1300 9,500 27,2 26 7,000 135,5 54 5,800 536, 0 43

TABLE 2 (Concluded) RUPTURE PROPERTIES OF UNCOATED AND COATED " 17.22AA"V STEEL SHEET (Heat D14468 - AMS 6436) R uptur e Str engths Test Coating Temperature Stress for Rupture (psi) Process (~.F) 2Ohrr 80-hr 30..."00hr Uncoated 1 100 29,000 24,000 (20, 000) Solar Alcote 1100 26, 700 24,500 18,800 Arthur Tickle 1100 26,000 23,000 19, 500 Uncoated 1200 17,800 13, 500 (10,500) Solar Alcote 1200 16,800 13,000 ( 7,800) Arthur Tickle 1200 17,800 15,100 (10,500) Uncoated 1 300 (10,000) 6,900 ( 4,400) Solar Alcote 1300 7,600 59700 4,300 Arthur Tickle 1300 ( 9,800) 7,800 6, 300

TABLE 3 RUPTURE PROPERTIES OF MODIFIED TYPE 403 STEEL SHEET (Heat 4566 - WAD 8105) Test Rupture Coating Temperature Stress Time Elongation PrdoRess (*F) (psi) (hours) (% in 2 in) Uncoated 900 85,000 30.0 14 77,500 102. 1 12 72, 000 358. 4 12 Uncoated 1000 63,000 25.3 17 60, 000 29. 5 18 56,000 152. 8 16 52,000 706, 1 13 Uncoated 1 100 48,000 1.7 18 35, 000 45. 0 14 30, 000 70. 0 21 22,500 1309, 3 10 Solar Alcote 1100 37,000 5,3 22 31,000 74.9 16 26 500 138.4 17 Arthur Tickle 1100 38,000 8.2 22 33,000 36, 5 19 30, 000 171, 0 14 27, 000 303, 4 16 Metallizing Eng. Co. 1100 35,000 18.8 18 32 500 14, 6 18 27,000 111, 1 17 22,500 782 17 Uncoated 1200 26,000 2, 5 28 15,000 103,7 24 12,500 130,6 23 12, 000 171,4 28 Solar Alcote 1200 18,000 19. 3 32 14,000 24.5 20 11, 000 141, 0 22 9s500 38303 31 Arthur Tickle 1200 17,000 25.9 16 14,000 70.9 27 11,000 189,1 36 9, 500 392, 0 42 Metallizing Eng. Co, 1200 20,000 11, 9 40 15,000 72, 3 40 11,500 191, 2 41 99 500 233, 9 26

TABLE 3 (Concluded) RUPTURE PROPERTIES OF MODIFIED TYPE 403 STEEL SHEET (Heat 4566 - WAD 8105) R uptur e Strengths Test Coating Temperature Stress for Rupture (psi) Process (~F) Z0.*hr 80-hr 300hr Uncoated 900 (86,500) 79,000 73,000 Uncoated 1000 (62,500) 58,000 54,000 Uncoated 1100 37,000 31,500 27, 000 Solar Alcote 1100 34,000 30,500 (21, 500) Arthur Tickle 1100 35, 000 31,000 28, 000 Metallizing Eng, Co. 1100 34,000 29,000 24, 500 Uncoated 1200 17, 500 13, 800 (11,000) Solar Alcote 1200 16, 500 129 800 10, 000 Arthur Tickle 1200 189 500 13,500 10,000 Metallizing Engo Co. 1200 18,500 14,800 99 500

TABLE 4 RUPTURE PROPERTIES OF 422 ALLOY STEEL SHEET (Heat 142761 - WAD 8107) Test Rupture Coating Temperature Stress Time Elongation Process ('F) (psi) (hours) (% in 2 in ) Uncoated 900 90,000 20,7 12 85, 000 69,7 10 80,000 487,2 11 76, 000 2356, 6 10 Uncoated 1000 70,000 11, 0 13 64,000 140,8 11 60,000 1171,4 10 Uncoated 1100 51,000 21,.4 9 47, 000 70,6 8 43,000 174,2 10 40,000 303, 5 8 Solar Alcote 1100 47,000 3. 1 16 38,000 75.0 10 34,000 272, 1 8 Uncoated 1200 32,500 7.9 10 26,000 78,1 10 19v500 143.5 8 15,9000 446.1 10 Solar Alcote 1200 25,000 16, 1 12 21, 000 46.2 12 17, 000 94.0 10 12, 000 357, 6 10 Rupture Strengths Test Coating Temperature Stress for Rupture (psi) Process ('F) 0hr 83-hr 300-hr Uncoated 900 90, 000 86,000 82,000 Uncoated 1000 68,000 65,500 62,500 Uncoated 1100 52, 000 46, 000 40,000 Solar Alcote 1100 41,500 38,000 33,500 Uncoated 1200 29,500 26,000 17,000 Solar Alcote 1200 24,000 18,000 12,600

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