oo A B — o iy 0 - C-84 - Reactors-Specm res %AII‘CI‘G“’ Reucf&rs > AEC RESEARCH AND DEVELOPMENT REPORT - i T iy 3 4456 035029y & "1 F ] - A kL f , f" f;, -&»‘ ‘s M fre "\‘él (e “ ' v m g o oz @ on R RATRELY) m-r* LTS e COMPATIBILITY TESTS OF MATERIALS FOR USE IN BEARINGS, SEALS, AND VALVES IN FUSED FLUORIDE SALTS AT 1200°F ¥.p To; W. C. Tunnell QaserricaTioN CHANG LIBERARY DO NOT TRANSFER 10 If you wish someone else « . i send in name with docume it arrange a loan. A Division of'il on Carporation . TENNESSEE [ LEGAL NOTICE This report was prepared as an account of Government sponscred work. Neither the United States, nor the Commission, nor any person acting on behalf of the Commission: A. Magkes any warranty or representation, express or implied, with respect to the accuracy, completeness, or usefulness of the information contained in this report, or that the use of any information, apparaotus, method, or process disclosed in this report moy not infringe privately owned rights; or B. Assumes any licbilities with respect to the use of, or for damages resulting from the use of any information, apparatus, method, or process disclosed in this report. As used in the ocbove, '‘person acting on behalf of the Commission®' includes any employee or contractor of the Commission to the extent that such employee or contractor prepares, handles or distributes, or provides access to, any information pursuant to his employment or contract with the Commission. ORNL-2103 This document consists of 74 pages. Copy /’36 of 250 copies. Series A, Contract No. W-7405-eng-26 AIRCRAFT REACTOR ENGINEERING DIVISION COMPATIBILITY TESTS OF MATERIALS FOR USE IN BEARINGS, SEALS, AND VALVES IN FUSED FLUORIDE SALTS AT 1200°F W. C. Tunnell DATE ISSUED SEP 271 190a OAK RIDGE NATIONAL LABORATORY Operated by UNION CARBIDE NUCLEAR COMPANY A Division of Union Carbide and Carbon Corporation Peost Office Box P Oak Ridge, Tennessee MARTIN MARIETTA ENERGY SYSTEMS LIBRARIES AR 3 4yy5k 0350294 & :OCO:\ICJ'\U'ikaM——- MEOEOECPPIMEIZTCPOCEMIMEIAINTI-OAOT>METZOEOMMDEON . G. . J. . Bender . Billington . Blankenship . Blizard . Borkowski . Boudreau . . Boyd ? . Bredig \ . Browning . Bruce . Callihan D . Cardwell % . Center (K-25) . Charpie . Clifford . Cottrell . Cowen OwImpPpm=oomPmm-~ovmy¥ . Cromer . S, . L. H. . Doney . Douglas . Dytko . Eister . Emlet (K-25) . Ferguson . Froas . Furgerson . Gray . Grimes . Hoffman . Hoffman g . Hollaender , =smoO-LFomomXxIP>ZT ORNL-2103 C-84 — Reactors-Special Features of Aircraft Reactors INTERNAL DISTRIBUTION Affel Barton Coobs Crouse Culler DeVan Frye 49, R. B indauer 50. R. S@ ivingston 51, R. 4"" Lyon 52. F.fi_ . Maienschein 53. W¢D. Manly 54, F. R. Mann 554 L. A, Mann . W. B. McDonald 7. F.R. McQuilkin 58. R. V. Meghreblian 59. R. P. Milford 60. A. J. Miller 61. R. E. Moore 62. J. G. Morgan 63. K. Z. Morgan 64. E. J. Murphy 65. J. P. Murray (Y-12) 66. M. L. Nelson 67. G. J. Nessle 68. R. B. Oliver 69. L. G. Qverholser 70. P. Patriarca 71. R. W, Peelle 72. A. M. Perry 73. J. C. Pigg 74. H. F. Poppendiek 75. P. M. Reyling 76. A. E. Richt 77. M. T. Robinson 78. H. W. Savage 79. A. W. Savolainen 80. R. D. Schultheiss 81. E. D. Shipley 82. A. Simon 83. 0. Sisman 84. J. Sites 85. M. J. Skinner A 86. G. P. Smith N\ 87. A. H. Snell ¥8. C. D. Susano 2. J. A. Swartout 98, E. H. Taylor 91%R. E. Thoma 92. & B. Trauger 93. '\;,‘R- Van Artsdalen 94. G. M. Watson 95. A. M:Weinberg A 96. J.%. White 112, R. G acPherson 97. G. B Whitman 113. W. l "Osborn 98. E. PRWigner (consultant} 114. W Scott 99. G. C.Williams 115. #_""‘" Smith 100. J. C. Wlson 116. .‘ K. Stair 101, C. E. Weaters 1174BE. Storto 102. E. S. Belis ] ;” W. C. Tunnell 103. R. B. Bridfs .ff" D. R. Ward 104. A, A, AbbaRello p/0. J. Zasler 105. L. P. Carperfar 121, H. Inouye 106. W. G. Cobb & 122. W. H. Cook 107. J. A, Conlin . -]24 ORNL - Y-12 Technical Library 108. G. A, Cristy p Document Reference Section 109. S. M. DeCamp 25-]34 Laboratory Records Department 110. B. L. Greenstreet J 135, Laboratory Records, ORNL R.C, 111, J. W. Kingsley ’ 136-137. Central Research Library EXTERNAL DIZERIBUTION P lant Represeny ive, Baltimore flant Represeffitive, Burbank 140, AF { Repre ' ahve, Marietta 141-143, AF PRt Repre; tohve, Santa Monica 144-145. AF Pl Repr il nfcmve, Seattle 146. AF PlarfiRen entofive, Wood-Ridge 147. Air Mater(@l 148. Air ReseaNillhnd Development Command (RDGN) 149, Air Technif® Intelligence Center 150. Allison Djn 151-153. ANP Proj £t Wifice, Fort Worth 154. Albuque ; e (QRerations Office 155. Argonn /" ationq@l aboratory 156. Armed bial Weapons Project, Sandia 157. Armeg ; Forces Spe lWeapons Project, Washington 158. Assi #a Secretaryqt the Air Force, R&D 159-164. Atofllt Energy ComnW@sion, Washington 165. Ba ’f le Memorial Insflite 166-167. Bffs Plant (WAPD) W& 168. feau of Aeronautics W& 169. Jeau of Aeronautics (CE v 170. 171.4 138. A 139. AF i;." e a fbrces Spigl e 24) Blrcau of Aeronautics Genflnl Representative Thicago Operations Office ¥ 17 '_,-"7: hicago Patent Group ":1;.,\ 1748 Chief of Naval Research % f Convair-General Dynamics Corf b. Engineer Research and DevelopM@int Laboratories ; General Electric Company (ANPDY@ #4380, Hartford Area Office : .',{;T; Headquarters, Air Force Special Weains Cenfter ‘:;’.'"i 182. ldaho Operations Office B & 183. Knolls Atomic Power Laboratory § % 184. Lockland Area Office R 185. 186. 187. 188. 189, 190. 191, 192, 193. 194, 195. 196-199, 200. 201. 202. 203. 204, 205-222. 223-247. 248, 249, 250, Los Alamos Je National Advidk National Advisily Naval Air Deve \@ Naval Research & North American Aviltion, 4 % (Aerophysics Division) ¢, (Canoga Park) Nuclear Development} ation of America Office of the Chief of ' Patent Branch, Washig USAF Project R o Wright Air Devg ;pment Cenf'_ Division o ' . hhent, AEC, ORC Richard G. J& Technical | _search Group, New CONTENTS A B SIIACT oottt ettt e e e a e e s e b e bt Materials Requirements ........ccoiiiiiiiiiiiiiiicer et ere e Self-Welding and Friction Effects ... T @St APPAFGIUS ooviuiiiiieieeeeieieie e et sstrasesereetebes e se e e et e s st b ettt Selection of Materials ..o e ettt e aa et b etr e e et e rea et rnes T @5t PrOCEAUIE oottt ettt et s e n et e b e eenen e ebe e ebaeebneente e Criteria for Rating Materials ...t e Evaluation of ResuUlEs ..ot Conclusions and Recommendations .o e Ot W W LW N et aad e Acknowledgment ... Appendix A. Index for Tests of Various Pin and Plate Combinations..........cccooocoo. 19 Appendix B. Material Compatibility Tests — Correlation Series ..o, 23 Appendix C. Photographic Record of Wear Patterns ..., 29 COMPATIBILITY TESTS OF MATERIALS FOR USE IN BEARINGS, SEALS, AND VALVES IN FUSED FLUORIDES AT 1200°F W. C. Tunnell ABSTRACT A series of tests were made for selecting combinations of materials compatible for possible use in journal bearings, face seals, and valve seats operating in fused fluoride salts at 1500°F. The test apparatus was designed to impose on the test specimen conditions similar tc those that will be encountered in starting journal bearings and face seals from rest or in opening valves which have been seoted for a considerable time. These conditions are considered to be those most likely to cause damage to the working surfaces. Thirty=six combinations of ten different materials were tested in fused fluoride salts at 1200°F with the use of an apparatus consisting of a pin sliding against a rotating plate under a fixed [oad. The following combinations of materials showed sufficient promise to warrant further testing at higher temperatures: Kennametal 151A vs Adamas A Adamas A vs Kennametal 138A Kennametal 151A vs Norbide B4C Kennametal 151A vs Carboloy 608 Kennametal 151A vs Kennametal 151A Kennametal 151A vs High-Density Graphite MATERIALS REQUIREMENTS A basic requirement of materials used for pump journal bearings, face-type shaft seals, and valve seats in contact with fused fluoride salts at high In addition the materials must resist wear, galling, and self- welding under severe operating conditions. There- temperatures is corrosion resistance. fore screening tests were developed to ascertain the design limitations that materials might impose on the Aircraft Reactor Test, in which a fused salt mixture i s to be circulated at 1500°F, The selected corrosion-resistant materials were screened for compatibility under conditions that simulated, in a general way, the operation of journal bearings, face-type seals with boundary lubrication, or valve seats under load in fused fluoride salts at 1200 to 1500°F. It was originaily planned that the materials would be given a preliminary screening test at 1200°F, that those proving to be compatible would then be further tested at 1350 and 1500°F, and that any material proving to be compatible at 1500°F would be tested as actual bearing pump and valve components. However, tests at 1200°F were the only ones performed, because the work was stopped by higher priority projects. SELF-WELDING AND FRICTION EFFECTS In considering materials for high-temperature ap- plication, it is recognized that any formed, smooth surface has microscopic asperities. Also, it has been reliably demonstrated that two such surfaces in intimate sliding contact will generate sufficient heat to cause welding and shearing of these minute asperities as they come in contact under the ex- treme unit pressures, or that the asperities will shear without welding, or that they will slide “‘up and over'’ each other and create frictional forces, metal transfer, and/or surface damage. A similar condition exists in a valve poppet and seat, and it is intensified when the assembly is subjected to a high temperature with high unit pressures at the minute contact points; that is, a *‘weld'’ forms through diffusion bonding of the metals. When the valve is to be opened, the welds must be broken; surface damage and metal transfer result, metal Some combinations apparently resist diffusion bonding, or welding, but such resistant combi- nations can be determined only through tests. In a study of the friction of metals the conclusion has been that the magnitude of the frictional forces and the extent and type of surface domage caused by sliding are determined primarily by the relative physical properties of the two sliding surfaces.! In particular, the behavior is very dependent upon the relative hardnesses of the sliding surfaces, and, if the sliding speed is high, the relative softening or melting points are quite important. Properly designed, hydrodynamically lubricated bearings operate with a thin layer of the lubricant separating the two sliding surfaces, except in cases of extreme loads or of starting and stopping under load, when the thin film may be destroyed or interrupted and metal-to-metal contact may occur. The bearing then operates in what is called a '‘boundary region’’ of lubrication, and an analy- sis of the friction developed becomes complicated. The phenomena invelved cannot be explained by any presently known lubrication theory. Surface finish and the chemical and physical properties of the. sliding surfaces become critical in this situation, and hardnesses, shear strengths, and melting points of the materials are important. TEST APPARATUS The test apparatus, which was modified from apparatus previously used for testing seals, con- sisted of an Inconel sump tank, an Inconel operat- ing pot, and a concentric spindle shaft and sliding shaft arrangement inserted in the operating pot and externally supported by ball bearings (Fig. 1). The 2%4“' specimen plate was rotated in the operating pot and was held against a ]/2-in.-dia stationary pin specimen. The contact pressure of the plate on the pin couid be adjusted by on external spring. The surface of the plate speci- men was lapped flat, to within three light bands, and the end of the stationary pin specimen was ground to a Y%-in.radius cylindrical surface so that theoretical line contact between the speci- mens could be obtained. The pin was mounted so that contact would occur at a mean radius of 1 in. from the center of the plate. The mean slid- ing speed (7.4 fps) used by Vail at KAPL? was selected for use in these tests, At the specified sliding speed of 7.4 fps, the plate rotated at 850 rpm. The test apparatus was calibrated {tests Nos. 1 and 2) by use of acetylene tetrabromide (1.1-2,2 TEB) as the liquid, a Graphitar 14 plate, and an 1F. P. Bowden and D. Tabor, The Friction and Lubri- cation of Solids, p 78, Clarendon Press, Oxford, 1950. 2p, B. Vail, Compatibility of Materials in Liquid Metal, KAPL-589 (Aug. 18, 1951). UNCLASSIFIED DWG 22338 LOADING SPRING ——— DRIVE WHEEL -BALL BEARINGS SPINDLE SHAFT SLIDING SHAFT ROTATING PLATE — Fig. 1. Bearing Materials Compatibility Tester, [nconel pin. Contact pressure was applied in vary- ing steps until, with a 10-lb load on the load spring and an initial Hertz stress of about 15,000 psi, the hydrodynamic film was interrupted and a With the load requirement established, a series of six cor- relation tests {tests Nos. 3 through 8, Appendix B) were conducted in which type 416 stainless steel plates were used in combination with six different boundary lubricated condition existed. pin materials: babbit, die steel, high-speed tool steel, Stellite 6, Stellite Star J, and Superoilite. The fluid used was regular-grade Texaco Regal ““A’ oil, without additives, which has a viscosity of 40 to 44 SSU at 210°F. The correlation tests were run at room temperature and were each of 2-hr duration. agreement with the KAPL data for the same ma- terial combinations. A pin-wear classification guide (Fig. 2) was prepared by taking cuts of known amounts off the wearing nose of an unused test pin and then photo- graphing the pin. The photographs provided a reference to which photographs of the tested pins could be compared to determine visually the extent of wear, The results were in reasonable SELECTION OF MATERIALS An examination of work by Vail® with sodium and sodium-potassium alloy at temperatures up to 950°F and recommendations made by the Materials Chemistry Section and the Ceramics Department of ORNL were used as the basis for selecting materials, Samples of materials that were ex- pected to be corrosion resistant were obtained and were exposed to the fluoride salt in static capsule or seesaw tests? for 100 hr, The ma- terials selected and the results of the corrosion tests are presented in Table 1, TEST PROCEDURE The test specimens were cleaned with alcohol and then slowly heated to 1200°F in a purging stream of dry, pure helium, After the operating pot and specimens were heated, a fluoride mixture at 1200°F was introduced into the pot and brought to the level-control probe. The rotation of the submerged plate specimen was started, and the system temperature was allowed to come to equi- librium at 1200°F, Contact was then established between the pin and plote specimens, with a 10-Ib contact load being applied for 120 min, during which time the specimens remained sub- merged in the molten fluoride salt, The load was released, and the fluoride mixture was allowed to drain back into the sump pot and freeze. The 3p. B. Vail, Compatibility of Materials in Liquid Metal, Second Report, KAPL-1021 (Jan. 5, 1954). 4A. desS. Brasunas, A Simplified Apparatus for Making Thermal Gradient Dynamic Corrosion Tests, ORNL CF- 52-3-123 (March 13, 1952). system was allowed to cool to room temperature under a helium atmosphere before the specimens were removed for examination. Photographs were taken of the pin and the plate after each run (see Appendix C), and enlargements were made of the pin-surface and plate-surface photographs to show the wear pattern. A Faxfilm replica was also made of each plate and pin. The process consisted in applying a clear solvent to the surface to be recorded, pressing a piece of soluble plastic tope against the solvent and surface, allowing a few seconds for reaction and drying, and then mounting the tape in slides for projection. A sample of the fluoride was recovered after each run, and a spectrographic analysis was made, with special emphasis given to the constituents of the compatibility specimens., There was no in- crease of metal content, except in the case of the oxides, which were recognized as being soluble in the fluoride. CRITERIA FOR RATING MATERIALS The compatibility of pairs of materials operating in contact with each other was established as a relative measure of resistance to mechanical dam- age, such as wear, galling, and self-welding. For the purpose of classifying materials according to test results, arbitrary group standards were estab- lished, as follows: Group A ~ Only slight wear on the narrow-band pin specimen; no spalling of either specimen; no galling or smearing tendency; no appreciable change in surface flatness of the plate; no change in surface finish, except an improvement (polishing or superfinishing); no appreciable reduction in hardness as indicated by the Rockwell hardness tester; and no evidence of erosion or corrosion by spectrographic or visual means. Group B ~ Slight wear indications on either specimen; no spalling; no smearing or metal pickup; slight scoring and surface roughening; no appreci- able reduction in Rockwell hardness; no evidence of erosion or corrosion by spectrographic or visual means. Group C — More extensive wear than on speci- mens of Group B; some possible roughening of either surface or of both; some metal pickup, smear- ing, scoring, or spalling readily apparent; no evidence of erosion or corrosion by spectrographic or visual means. UNCLASSIFIED PHOTO 18266 0.001-IN. CUT 0.002-IN, CUT 0.003-IN. CUT 0.005IN. CUT 0.010-IN. CUT 0.015IN. QUT 0.030-IN. CUT Fig. 2. Pin-Wear Classification Guide. Machine cuts of various amounts on an Inconel pin specimen. Group D -~ Excessive wear of either specimen; metal pickup; scoring or smearing; roughening of surfaces; reduction in hardness; deterioration of surface finish; corrosion or erosionreadily apparent. EVALUATION OF RESULTS From the post-test photographs (presented in Appendix C), a very clear indication of the com- patibility of the test materials was obtained. Wear, smearing, or metal buildup, galling or self-welding, spalling, and cracking are all identifiable in the photographs. The extent of pin wear may be ob- served by comparison of the test photograph with Fig. 2. The hardness readings and the spectro- graphic analyses were effective in indicating the compatibility of the specimens, The test data, presented in Tables 2 and 3, showed that, in general, pairs of unlike materials were more compatible than pairs of like materials. Thirty-six combinations of ten different materials were tested, and the following were considered suitable for further testing at higher temperature: Kennametal 151A vs Adamas A Adamas A vs Kennametal 138A Kennametal 151A vs Norbide B4C Kennametal 151A vs Carboloy 608 Kennametal 151A vs Kennametal 151A Kennametal 151A vs High-Density Graphite The repetition of various tests showed that the results were reproducible and indicated that the test apparatus and methods used were consistent and reliable. No single property or combination of properties, such as surface finish, hardness, or chemical composition, was found which was characteristic of the best materials. It is felt that tests of ad- ditional combinations of carbides would be produc- tive and that tests of available borides, nitrides, and silicides would greatly increase the chances of finding ideal combinations of materials for the desired applications. CONCLUSIONS AND RECOMMENDATIONS From the results obtained at 1200°F it is con- cluded that several of the combinations of ma- terials tested were sufficiently compatible under the conditions imposed on them to warrant further testing at 1350 to 1500°F, as was originally planned (see ‘‘Materials Requirements'’). There- fore the following recommendations are made: 1. Resume the compatibility screening tests reported herein and test additional promising com- binations of carbides, as well as combinations of borides, nitrides, and silicides, which alsc offer promise, 2. Run a series of tests on the screened com- binations at 1350 and 1500°F, successively screen- ing and retaining the most promising. 3. Test the material combinations which show promise at 1500°F as journal bearings, face seals, and valve seats in apparatus designed to simulate operation in an actual reactor circuit. ACKNOWLEDGMENT The work of D. B, Vail of the Knolls Atomic Power Laboratory (reports KAPL-58% and - 021) on the compatibility of materials in sodium and in NaK was of considerable value in the initial selection of materials to be tested. It was also used to check and to validate the calibration of the apparatus used. The data presented herein were obtained by P. G. Smith and J. W, Kingsley of ORNL and by W. K. Stair, consultant, the University of Tennessee, TABLE 1. CONDITIONS AND RESULTS OF CORROSION TESTS OF SELECTED ALLOYS, CERMETS, AND CERAMICS IN FUSED FLUORIDE SALTS Fluoride Salt Mixtures Used: 1. NuF-ZrF4-UF4 (50-46-4 mole %) 2. NoF-ZrF4-UF4 {46-50-4 mole %) , 3. NaF-ZrF4-UF4 (53.5-40-6.5 mole %) 4. NaF-KF-LiF-UF, (10.9-43.5-44.5-1.1 mole %) Material Typical Composition Fl-uoride Salt Type Depth of Corrosion Manufacturer Mixture Used of Attack Comments ldentification {wt %) a ) Reference (see above) Test (mils) Adamas Carbide Corp. AA 97 WC=3 Co 1 Seesaw 0 Hot zone, 1500°F; cold zone, b 1328°F A 94 WC—6 Co 1 Seesaw 0 Hot zone, 1490°F; cold zone, b 1355°F 66 60 WC=12 Co-28 TaC 1 Seesaw 1 Hot zone, 1500°F; cold zone, b 1319°F Borolite Corp. MoSi2 Nickel-bonded 3 Seesaw 0 c SiC 3 Static 0 d TiB2 3 Seesaw 2 d ZrB2 3 Seesaw 2 d Carboloy Dept., General 44A 94 WC=6 Co 2 Static 0 e Electric Co. 55A 87 WC-13 Co 2 Static 0 e 608 83 CryCy~2 WC=15 Ni 2 Static Some surface roughening e 1 Seesaw 4 Attack on exposed surface / 779 91 WC~9 Co 2 Static 0 Some evidence of spalling e 907 74 WCa6 Co-20 TaC 2 Static 0 Some evidence of spalling e X350S 98 Cr3C2—2 wC 1 Seesaw 0 Specimen extremely brittle f The Carborundum Company BN 3 Static 2to 5 d Mo,B 501 3 Seesaw 16 d Electro Metallurgical Cr3C2 3 Static 0 CraC, particles did not d Company appear well bonded in as-received condition 5i3N4 3 Static 2tc 5 d TiC 3 Static 0 TiC particles did not appear d to be formed or bonded as well as could have been TABLE 1. (continued) ) ) . Fluoride Salt Type Depth of ) Manufacturer M?f?”al, Typical Composition Mixture Used of Attack Comments Corrosion ldentification (wt %) a ) Reference (see above) Test {mils) Electro Metallurgical ZrC 3 Static Penetrated Small incipient cracks in d Company ZrC particles throughout specimen Firth Sterling, Inc. FS 27 43 TiC-50 Ni-7 Cr,0, 1 Seesaw 2to5 e Haynes Stellite Company 1 46 Co-31 Cr=13 W— 1 Static 10 € 1 Ni~3 Fe-2.45C 3 46 Co=31 Cr=13 W~ 4 Static 6 e 3 Ni-3 Fe-2.45C 2 Static 29 6 56 Co~30 Cr=5 W= 1 Static 15 e 3 Ni~3 Fe-1,25C 12 56 Co=31 Cr=8 W- 1 Static 13 e 2 Fe-1.35C 19 52 Co~31 Cr=10 W= 4 Static 2 e 3 Fe-1.8C 2 Static 29 e 21 65 Co—25 to 30 Cr-4.5 to 1 Static 5 e 6.5 Mo-=2 Fe=1.5 to 3.5 Ni-=0.2 C 25 40 Co=20 Cr—-15 W- 4 Static 0 e 10 Ni—3 Fe~1 Mo~ 0.1C ] Static 5 e 40 13.5 Cr—4.5 Fe—4 Si- 1 Static 5 e 1 Co=3.2 B=Bal Ni 41 12 Cr~4.5 Fe—~4 Si- 1 Static 23 e 1 Co-2.25 B~Bal Ni Hastelloy B 63 Ni—=28 Mo—6 Fe=1 Cr 4 Static 5 e 1 Static 5 e Hastelloy C 55 Ni~17 Mo—16 Cr— 4 Static 2 e 6 Fe—4 W7 to 10 5i 1 Static 1 e TABLE 1. (continued) _ . . Fluoride Salt Type Depth of Manufacturer Material Typical Composition Mixture Used of Atrock Commente Corrosion ldentification (wt %) a . Reference (see above) Test {mils) Haynes Stellite Company Hastelloy D 83 Ni~4 Ca=1 Fe=1 Cr 1 Static 1.5 e Kennametal, Inc. 138A 65 TiC=20 Co= 1 Seesaw 0.5 to 1 May have been slight attack g 15 NbTiTcC3 on binder 150A 80 TiC~10 Ni-~ 1 Seesaw 4 / 10 NbTiTaC, 3 Seesaw 0 c 3 Seesaw 0 d 151A 70 TiC=20 Ni~ Seesaw 1to2 f 10 NbTiTaC3 1 Seesaw 6 Blisters on surface c 3 Seesaw 0 d 3 Seesaw 0 d 1528 64 TiC-30 Ni- 1 Seesaw 2 f 6 NbTiTaC, 1 Seesaw 4t07 Erratic attack c 3 Seesaw 0 d 3 Seesaw 0 d 153B 54 TiC—-40 Ni- 1 Seesaw 3 Uniform attack above TiC g 6 NbTiTaC3 particle surface 1618 ? TiC=? Ni=? Mo 1 Seesaw 0 Only 208°F temperature dif- g ferential on capsule 1628 64 TiC=25 Ni—=5 Mo~ ] Seesaw 9 Portions of surface appeared f 6 NbTiTaC3 to be ploted 3 Seesaw 0 d 3 Seesaw 0 d D4675 97.5 WC=-2.5 Co 1 Seesaw 1 Slight subsurface voids c 3 Seesaw 0 d Metamic LT-1 77 Cr-~23 A|203 1 Seesaw Completely penetrated b Norton Company Norbide B,C 3 Static 5 One side of specimen d showed unidentified phase 14 mils deep TABLE 1. (continued) . . . Fluoride Salt Type Depth of ) Manufactorer Mcrh.enu! Typical Composition Mixture Used of Attack Commente Corrosion Identification (wt %) Reference (see above) Test? (mils) ORNL Ceramics Laboratory SiC-Si Sintercast Corp. of America 1 50 TiC=50 Co-base 1 Seesaw 0.5 to 2 Random penetration, voids g binder between TiC and binder 4 48 TiC-52 Co-base 1 Seesaw 1 Possible phase change g binder within particle 5 48 TiC=52 Ni-base 1 Seesaw 0 g binder 8 48 TiC=52 Ni-base 1 Seesaw 2 Some TiC without binder g binder observed; not attacked 10 47 TiC=53 Ni-base 1 Seesaw 5 Some attack on binder; g binder TiC particles separated Vascoloy-Ramet Corp. EE 80 WC=-10 TiC=10 Co 1 Seesaw 0 Hot zone, 1500°F; cold zone, b 1346°F EH 54 WC—40 TiC=6 Co 1 Seesaw 0 Hot zone, 1500°F; cold zone, b 1445°F 2A3 89 WC-11 Co 1 Seesaw 0 Hot zone, 1500°F; cold zone, b 1328°F (55 hr only) 2A7 95.5 WC~4.5 Co 1 Seesaw 0 Hot zone, 1500°F; cold zone, b 1355°F; spalling to a depth of 1 to 1.5 mils Unidentified TiN 3 Static 2 d Copper 4 Static 0 Negligible attack i Graphite 4 Static 0 Negligible attack i Graph-i-tite 1 Static 2 d 3 Static 2 d NOTE: See following page for references. oL 9Static tests: specimen submerged in fluoride salt sealed in Inconel capsule for 100 hr at 1500°F. Seesaw test: tilting Inconel capsule filled with fluoride salt; temperatures of specimen end (hot zone) and other end (cold zone), as specified; tests of 100-hr duration. bMemorandum, D. C. Vreeland to W. D. Manly, Results of Corrosion Tests with Various Tungsten Carbide Cermets (Nov. 25, 1953). “Data presented at conference at ORNL, May 25, 1954, by ORNL Metallurgy Division representatives. dPersoncfl communication from W. H, Cook. (Dec. 22, 1953). “Memorandum, D. C. Vreeland to W. D. Manly, Summary of Corrosion Resistance of Some Hard Facing Alloys, Cermets, and Ceramics in Various Media fMemorandum, E. E. Hoffman to W. D. Manly, Cermets Seesaw Tested in Fluoride #30 in Inconel Containers. EMemorandum, W. H. Cock to W. D. Manly, Dynamic Testing of Some Nickel-Base Bonded and Cobalt-Base Bonded Litanium Carbide Specimens in Fluo- ride #30 (April 20, 1954). Memorandum, D. C. Vreeland to W. D. Manly, Results of Corrosion Tests with Metamic LT-1 Cermet (Nov. 24, 1953). 'D. C. Vreeland, E. E. Hoffman, and L. D. Dyer, Met. Quar. Prog. Rep. Oct. 31, 1952, ORNL-1437, p 25. TABLE 2. SUMMARY OF DATA OF MATERIALS COMPATIBILITY TEST I Metal Pin Plate Plate Surface Pickup, Test Pin Plate Hardness* Pin Wear Hardness Finish** Spalling, Group - e —_— . Remarks No. Identification \dentification Before After Resistance PBefore After Before After and Classification Test Test Test Test Test Test Galling Resistance ] Incone! Graphitar 14 Calibration run for load reguirement using TEB 2 Copper Graphitar 14 One-hour operatiaon, 10-1b load, room temperature TEB 3 Babbit Type 416 Good 18-20 18 Good Correlation test in oil, stainless steel 2 hr at 850 rpm, room temperature 4 Ontario die Type 416 Poor 1820 150=160 Poor Correlation test in oil, steel stainless steel 2 hr at 850 rpm, room tempetature 5 Stellite 6 Type 416 Poor 18-24 175-225 Poor Correlation test in oil, stainless steel 2 hr at 850 rpm, room temperature 6 Stellite Type 416 ' Poor 20-28 125-150 Poor Correlation test in oil, Star J stainless steel 2 hr ot 850 rpm, room temperature 7 High-Speed Type 416 Poor 2432 160 Poor Correlation test in oil, tool steel stainless steel 2 hr at 850 rpm, t;oom temperature 8 Superoilite Type 416 Goed 16--24 30--35 Fair Correlation test in oil, stainless steel 2 hr at 850 rpm, room temperature 9 Inconel Graphitar 14 Good Friction test, 18°F temperature rise in oil *Hardness determined on Rockwell Hardness Tester. This machine was not available for use from the beginning of investigation. **Surface finish determined by use of The Brush Development Co. Profilometer in pin. rms. Zt TABLE 2. (continued) Metal Pin Plate Plate Surface Pickup, & . Test Pin Plate Hardness Pin Wear Hardness Finish** Spalling, Group No. ldentification ldentification Before After Resistance Before After Before After and Remarks Classification Test Test Test Test Test Test Galling Resistance 10 Inconel Graphitar 14 Good Operation for 20 hr, 10-1b load, oil, room temperature 1 inconel Graphitar 14 Good Good First test using fuel C No. 30, metal buildup on pin 12 Carboloy 608 Kennametal 71 Rc 4 Excessive metal 135A buildup preventing contact 13 Kennametal Kennametal 71 Rc Excessive metal 138A 138A buildup preventing contact 14 Inconel Graphitar 14 Goced Good Temperature calibra- C tion; pin 38°F cooler than liquid 15 Carboloy 608 Kennametal 10-12 Metal buildup investi- 151A gation; Ni plate pot, Inconel sump 16 Carboloy 608 Kennametal 70 Rc 10 Metal buildup investi- 151A gation; type 316 stainless steel pot, Inconel sump 17 Carboloy 608 Kennametal 72 Rc 7=10 Metal buildup investi- 151A gation; Ni pot, Ni sump 18 Carboloy 608 Kennametal 71 RC 7-10 Metal buildup investi- 151A gation; Incenel pot, *Hardness determined on Rockwell Hardness Tester. **Surface finish determined by use of The Brush Development Co. Profilometer in fin. rms. incone! sump This machine was not available for use from the beginning of investigation. £l TABLE 2. (continued) Metal Pin Plate Plate Surface Pickup, Test Pin Plate Hardness* Pin Wear Hardness Finish** Spalling, Group No. Identification Identification Befere After Resistance Before After Before After and Remarks Classification Test Test Test Test Test Test Galling Resistance 19 Coarboloy 608 Kennametal 65 RC Fair 70 Rc 6—=7 67 Goed Slight taper wear on C 151A pin; plate alignment good 20 Kennametal Adamas A 72 R_ Good 79 R, 5-7 2-3 Good Corner wear on B 15TA misaligned pin; plate wear gocd 21 Adamas A Adamas A 77 R, 78 R, Fair 78R_ 78R, 7-10 16--18 Fair Like materials ex- C pected to wear; plate may be warped 22 Carboloy 608 Adamas A 70 Rc Fair 79 Rc 72 Rc 5.7 7-8 Good Good pin pattern; C plate may be warped 23 Adamas A Kennametal 79 R. Good 73R, 66 R, 5~7 5-7 Good Good wear patterns; B 151A slight material buildup 24 Adamas A Kennametal 79 Rc Good 73 R. 4-5 4-5 Good Good wear pattern; B 138A very slight buildup 25 Adamas A Norbide B,C 73R, Excellent 8--10 15-20 Fair Plate scored and C excessive spalling 26 Kennametal Kennametal 5-7 Specimens reground ? 151A 138A before photos made; data destroyed 27 ARE moder- Adamas A 72 RC 5.7 Surface Pin reacted with fuel; D ator BeO scale no contact existed 28 Adamas A High-Density 65 Good 1012 Fair Good wear pattern; C Graphite some material buildup *Hardness determined on Rockwell Hardness Tester. This mechine was not available for use from the beginning of investigation. **S, 1 face finish determined by use of The Brush Development Co, Profilometer in gin. rms, r1 TABLE 2. (continued) Metal Pin Plate Plate Surface Pickup, Test Pin Plate Hardness* Pin Wear Hardness Finish** Spalling, Group P ipe an = — , Remarks No. Identification |dentification Before After Resistance Before After Before After and Classification Test Test Test Test Test Test Galling Resistance 29 ARE moder- ARE moder. 15-18 Pin and plate reacted; D ator BeQ ator BeO fuel plate cracked 30 Adamas A Kearfoot A|203 70 15-18 Plate reacted with D fuel; plate cracked 31 Adamas A Graphitar 14 7 57 Good 3-5 Fair Good wear pattern; some material buildup 32 Carboloy 608 Carboloy 608 58 64 Fair 61 R, 72 Rc 1-2 2-3 Good 33 Carboloy 608 Norbide B,C 58 R, Fair 2-3 Poor Material buildup; D plate misaligned; smearing 34 Carboloy 608 Kennametal 59 R, 70R_ Fair 59 R, 1-2 Good Pin and plate wear C 138A pattern even and concentric 35 Adamas A Norbide B4C 68 Good 2-3 Good Dry run; inert atmos- C phere; 900°F noted even though no heat had been applied 36 Kennametal Norbide B4C 56 67 Good 2-3 Fair Some scoring of plate; B 151A pin wear good 37 Kennametal Carboloy 608 57 68 Good 61 1-2 Good Only slight scoring of B 151A plate; pin wear very good 38 Kennametal Kennametal 58 66 Good 61 1-2 Good Slight scoring; may be B8 151A 151A warping of plate; pin weaqr even *Hardness determined on Rockwell Hardness Tester. This machine was not available for use from the beginning of investigation. **Surface finish determined by use of The Brush Development Co. Profilometer in pgtin. rms. TABLE 2, (continued) Metal Pin Plate Plate Surface Pickup, Test Pin Plate Hardness* Pin Wear Hardness Finish*~ Spalling, Group Ne. Identification Identification Before After Resistance PBefore After Before After and Remarks Classification Test Test Test Test Test Test Galling Resistance 39 Kennametal Graphitar 14 57 53 Fair 5=6 Fair Spalling of plate; C 151A material buildup 40 Kennametal High-Density 56 66 Good 50-60 Good Slight scoring of B 151A Graphite plate; even wear pattern 41 Carboloy 608 Graphitor 14 50 70 Fair 5~7 Good Some smearing on C pin; plate wear good 42 Carboloy 608 High-Density 58 68 Fair 5060 40-50 Good Slight wear on plate; C Graphite pin pattern even 43 Norbide BAC Adamas A Fair 72 79 1-2 1-2 Good Pin misaligned; high C stress on plate but no wear 44 Norbide BAC Norbide B4C Fair 2-3 40 =50 Fair Pin spalled and worn; D little plate wear; material buildup 45 Norbide B ,C Carboloy 608 Fair 60 70 4-5 45 Good Pin spalled; mis- C aligned plate; wear uneven 46 Norbide B ,C Kennametal Good 59 71 1-2 1-2 Good Plate misaligned or C 151A warped; high stress; no wear 47 Norbide B,C Kennametal Good 58 72 1-2 2-3 Good Pin and plate wear C 138A even; slight spalling of pin 48 Kennametal Adamas A 59 58 Fair 72 71 1-2 4.5 Fair Some smearing and C 138A plate may have warped *Hardness determined on Rockwell Hardness Tester, This machine was not available for use from the beginning of investigation, 5l **Surface finish determined by use of The Brush Development Co. Profilometer in pin, rms. 91 TABLE 2, (continued) Metal Plate Plate Surface Pickup, Test Pin Plate Hardness* Pin Wear Hardness Finish** Spalling, Group No. Identification ldentification Before After Resistance Before After Before After and Remarks Classification Test Test Test Test Test Test Galling Resistance 49 Kennametal Norbide B4C 60 71 Good 2--3 100150 Poor Plate scored and 138A smeared 50 Kennametal Inconel 53 65 Poor 84 RB 84 RB 4-5 200=225 Poor Pin worn excessively; D 151A plate roughened but showed little wear 51 Adamas A Inconel 57 77 84 Rp 4=5 52 Kennametal inconel 58 66 84 RB 45 151A 53 Adamaos A Inconel 70 4-5 54 Kennametal Kennametal 61 59 2-3 138A 138A 55 (7) *Hardness determined on Rockwell Hatdness Tester. This machine was not available for use from the beginning of investigation. **S rface finish determined by use of The Brush Development Co. Profilometer in pin. rms. TABLE 3. RESULTS OF SPECTROGRAPHIC ANALYSIS OF THE FLUORIDE AFTER VARIOUS TESTS Impurities in Flucride Mixture (wt %)* Test No, Specimen Materials Al B Co Cr Fe Ni Si Ti W Sump Pot No. 1 39 TiC-Ni and graphite <0.1 <0.01 <0.05 <0.05 <0.05 <0.05 <0.01 <0.05 <0.2 32 Cr,C, <0.01 T <0.05 <0.05 0.2 <0.05 0.1 £0.05 <0.02