CENTRAL RESEARCH LIBRARY DOCUMENT COLLECTION = - OBNL 1463 Metallurgy m_t.l__,veralics b e R METHODS OF FABRICATION OF CONTROL AND SAFETY ELEMENT COMPONENTS FOR THE AIRCRAFT AND HOMOGENEOUS REACTOR EXPERIMENTS OAK RIDGE NATIONAL LABORATORY i] OFERATED BY " CARBIDE AND CARBON CHEMICALS COMPANY ] / A DIVISION OF UNION CARBIDE AND CARBON CORPORATION | e POST OFFICE BOX P OAK RIDGE. TENNESSEE ? ¥, ORNL-1463 This document consists of 18§ pages. Copy_5 of 159 copies. Series A, Contract No. W-7405, eng-26 METALLURGY DIVISION METHODS OF FABRICATION OF CONTROL AND SAFETY ELEMENT COMPONENTS FOR THE AIRCRAFT AND HOMOGENEOUS REACTOR EXPERIMENTS J. H. Coobs and E. S. Bomar Powder Metallurgy by J. H. Coobs and E. S. Bomar Welding and Brazing by G. M. Slaughter and P. Patriarca DE b lASS IFIED B ----AE[E T 557 ———i s Mmook ma & Sy FEB £ 6 1953 OAK RIDGE NATIONAL LABORATORY Operated by CARBIDE AND CARBON CHEMICALS COMPANY A Division of Union Carbide and Carbon Corporation Post Office Box P O0ak Ridge, Tennessee MARTIN MARIETTA ENERGY SYSTEMS LIBRARIES R 3 445k 03531485 4 | ORNL-1463 Metallurgy and Ceramics DISTRIBUTION 1. C. E. Center 27. A. Hollaender 2, Biology Library 28, M. T. 3. Health Physics Li 29, K. Z. 4, Metallurgy Libra 30. J. S. 9-6. Central Researc brary 31. A. S, 7. Reactor Experi al 32, C. S, Engineering rary 33. C. E. 8-13. Central Fil 34. D. S, 14, C. E. Lars 35. D. W, 15. W. B. (K-25) 36. E. M, 16. L. B. t (Y-12) 37. A. J 17. A, M, nberg 38. D owen 18. E. H4aWaylor 39. P Reyling 19. E hipley 40. . Williams 20, F VonderLage 41. Coobs 21. . Briant 42 . S. Bomar 22, J. Fretague . M. Slaughter 23 A. Swartout . Patriarca 2 . C. Lind . . Levy (on loan from A . L. Steahly Pratt and Whitney . H. Snell Aircraft) EXTERNAL DISTRIB 46-53. Aréonne National Labo 54-58. Atomic Energy Commi , Washington 59. Battelle Memoria titute 60-62. Brookhaven Natj Laboratory 63. Brush Beryllj 64. Bureau of ompany 65-66. Californg esearch and Development Company 67-68. d Carbon Chemicals Company (K-25 Plant) 69-72. ) nd Carbon Chemicals Company (Y-12 Plant) 13. i o Patent Group 4. ow Chemical Company (Rocky Flats) 75-77. duPont Company General Electric Company (ANPP) (1 copy ea. to W. Baxter, H. C. Brassfield, J. A. McGurty, and W. J. Koshuba) General Electric Company, Richland Hanford Operations Office aho Operations Office a State College s Atomic Power Laboratory amos Scientific Laboratory rodt Chemical Works etts Institute of Technology (Kaufmann) atory isory Committee for Aeronautics, Cleveland ory Committee for Aeronautics, Washington of Standards 90-9 94. 95-98. 99-.101. 102. Mal 103. Massa 104-106. Mound 107. Nationa 108. National 109. National B 110. National Lea 111. Naval Research 112. New Brunswick L 113-117. New York Operati 118-120. North American Avy 121. Patent Branch, Wash 122. Rand Corporation 123. San Francisco Operatio 124. Savannah River Operatio 125. Savannah River Operations 126. Sylvania Electric Products, 127-130. University of California Ra 131. Walter Kidde Nuclear Laborato 132-135. Westinghouse Electric Corporati 136-144. Wright Air Development Center (1 Pratt and Whitney Aircraft) 145-159. Technical Information Service, Oak Ri fice, Augusta ice, Wilmington n Laboratory Inc. to R. Strough, 111 i © i METHODS OF FABRICATION OF CONTROL AND SAFETY ELEMENT COMPONENTS FOR THE AIRCRAFT AND HOMOGENEOUS REACTOR EXPERIMENTS J. H. Coobs and E, S. Bomar SUMMARY This report contains, in two parts, the experimental work leading to the fabrication of control and safety components for the Aircraft and Homogeneous Reactor Experiments. The method evolved for preparation of cylindrical inserts for the ARE control and safety rods required the hot-pressing of mixtures of boron carbide with alumina and with 1iron. A technique for fabrication of control plates for the HRE was devised to minimize defects found in earlier sets of plates., The method involved closely packing pressed-powder com- pacts 1n a frame and then hot-rolling to bond protective cladding sheets to the core. INTRODUCTION The neutron-absorbing material selected for control and safety elements in both the ARE and HRE was boron in the carbide form. Cylinders with acceptable physical properties and the requisite amount of boron were made for the ARE safety rods by consolidating mixed iron and boron carbide powders. Consolidation was effected by pressing atan elevated temperature. Inserts for the control elements were prepared in a similar manner by using a dilute suspension of boron carbide in alumina as a carrier. The operating conditions to which the HRE control and safety plates are exposed require that the high cross- section material be completely enclosed in a protective envelope. Initially, efforts were directed toward the cladding of Boral with stainless steel as a protective covering. Later, pressed and sintered compacts of boron carbide suspended in copper were sub- stituted for the Boral to permit rolling at a higher temperature for bonding of cladding to core. ARE CONTROL AND SAFETY ROD COMPONENTS The design selected for the control and safety rods for the ARE called for the use of boron carbide as the high cross-section material. Inserts for the control rod were to be made in the form of cylinders and composed of a dilute suspension of boron carbide in alumina. These were later prepared with a minimum of difficulty. The boron carbide bearing components for the safety rods were to have es- sentially the same shape, but were to be made of pure boron carbide. The reply to an inquiry to a supplier of the special grade of boron carbide required for the pure boron carbide pressed cylinders indicated that the cost for these items would be quite high. Therefore experimental work was done which revealed that pressed cylinders containing an acceptable amount of boron carbide bonded with iron could be produced. Experimental Work on Safety Rod Inserts. Mixtures containing 80 vol % boron carbide (Norton, metallurgical grade, which analyzed 71 * 1% boron) and 20 vol % copper, nickel, and iron were hot-pressed to check the useful- ness of these materials as cementing agents. The powders used were all -325 mesh, and were milled together, using steel balls, for several hours. The results of these runs are tabulated in Table 1, The results of the first runs indicated that nickel did not promote especially desirable properties in the pressed compact. A liquid phase formed, but i1t did not wet the boron carbide particles and gave little cementing action, TABLE 1. PROPERTIES OF HOT-PRESSED NICKEL, COPPER, AND IRON PLUS BORON CARBIDE COMPACTS PRESSING DENSITY AS PERCENTAGE Cg?P?ffl;ION TEMPERATURE OF THEORETICAL REMARKS e (°C) DENSITY 20 Ni-80 B,C 1200 74.0 We ak, much nickel loss 20 Ni-80 B,C 1200 70.4 Weak, soft 20 Cu-80 B,C 1100 74.5 Fairly strong, loss of copper 20 Cu-80 B,C 1090 78.4 Fairly strong 20 Fe-80 B,C 1050 69.0 Soft, weak 20 Fe-80 B,C 1170 73.7 Soft, weak 20 Fe-80 B,C 1290 71.0 Soft, weak Copper gave somewhat better cementing effect than the nickel even though it did not dissolve appreciable amounts of boron or carbon. In every instance, however, a portion of the copper was lost by extrusion past the rams, and the resulting compacts were still too porous and weak to be useful. The 1nitial runs in which iron was used as the bonding agent were also being too soft and There was, unsatisfactory, porous. however, no evidence of loss of iron during the pressing cycle; the iron may have been converted to solid FeB or Fe,C. This is confirmed by the work of Nelson, Willmore, and Womeldorph,(l) who pressed and sintered mixtures of 20 wt % 1iron (7.5 vol %) and 80 wt % boron carbide at 1930°C for 30 minutes, These sintered bodies were fairly strong and underwent some shrinkage, with no loss of material. Examination by x-ray-diffraction techniques failed to detect iron, but revealed the presence of FeB, B,C, and graphite. It thus seems that the bonding phase is FeB formed by reaction of iron and (1)J Woneldo;ph, (1951). A. Nelson, T. A. Willmore, and R. C. J. Electrochen, Soc. 98, No. 12, 465 boron carbide cycle, during the sintering On the basis of these conclusions, several runs were made at higher temperatures; the results are shown in Table 2. After several runs a hot- pressing cycle of 5 min at 1525 to 1535°C was selected. This schedule gave well-bonded slugs having adensity close to 80% of theoretical with only 3 to 4% loss of material during press- ing, Production of Safety Rod Inserts. Having selected boron carbide and iron as the combination to be used, quanti- ties of the powders were prepared to give 80 vol % (56 wt %) boron carbide and 20 vol % iron. Coarse boron carbide powder was reduced to a fine powder by grinding for 16 hr in a steel ball mill with steel balls. The sieve analysis of this material 1is given in Table 3. The requisite amount of -325 mesh iron powder was then blended with the boron carbide by grinding for an additional 8 hr in the same mill, The mixture was consolidated by hot-pressing at 1520 to 1530°C and 2500-ps1 pressure in graphite dies. TABLE 2. ADDITIONAL PROPERTIES OF HOT-PRESSED IRON PLUS BORON CARBIDE COMPACTS PRESSIN , S PERCENTAGE COTE??I;:DN TEJ?%;:TJ;E DFNiflffifiZOBETICflL fi%fi? REMARKS (oG DENSITY 20 Fe-80 B,C 1520 77.6 Strong 20 Fe-80 B,C 1725 70.5 29 We ak 7.5 Fe-92.5 B,C 1740 68.2 6.0 | Fairly strong 20 Fe-80 B,C 1520 80.0 3.0 Strong 20 Fe-80 B,C 1520 77.8 4.2 | Strong 20 Fe-80 B,C 1525 80.3 5.5 | Strong 20 Fe-80 B,C 1530 77.8 6.5 | Strong 20 Fe-80 B,C 1525 79.0 6.5 | Strong 20 Fe-80 B,C 1520 78.3 8.0 Strong Densities approximately 80% of theo- retical for the mixture were obtained under these conditions, One of the assemblies used for the pressing operation is shown in Fig. 1. For assembly, the long punch and mandrel were placed in the die with TABLE 3. SIEVE BORON CARBIDE POWDER +100 mesh -100 +200 mesh -200 +325 mesh -325 mesh ANALYSIS OF 1. 2% 17. 2% 18.8% 62.8% UNCLASSIFIED ¥-TOB9 M dwfifié‘,{ Fig. 1. Graphite Die Assembly. the mandrel centrally located along the axis of the die., The punch extended out of the bottom of the die. A charge of 132 to 133 g of blended powder was then loaded into the annular space between the die and mandrel, the top punch put in place, and a load of 2000 psi applied to seat the punches prior to placing in the hot-pressing rig. The set-up for hot-pressing is shown 1in Fig. 2. The lower punch rested on a graphite block, which, in turn, was 1nsulated from a Transite base by two refractory bricks (Norton, RA 1190). A quartz liner served as a retainer for the bubble-alumina insulation poured 1in around the graphite die prior to heating. The quartz cylinder was, 1in turn, externally supported by a Transite sleeve that extended up to the induction coil. Power was supplied by an Ajax, 40-kw converter set at 30 kw for heat-up and at about 15 kw to hold at temperature. An argon atmosphere was introduced at the bottom of the assembly to decrease the rate of oxidation of the graphite dies. It was found necessary to use additional graphite spacers, as shown in Fig. 2, to prevent excessive heating of the press ram because of coupling with the magnetic field of the induction coil. A prism was mounted over the sight tube of the die so that optical temperature readings could be made in a horizontal position. Also, a low- pressure gage was added to the press for this work, This gage, which 1is not shown in Fig. 2, 1s connected to the hydraulic line above the gage shown, It was found necessary to push the mandrel out of the slug at high temper- ature to avoid cracking during cooling because of a marked difference in expansion coefficients for the boron carbide compacts and graphite. The mandrel was pushed out of the compact into the lower punch by using an undersize mandrel, The hot-pressed slugs were ground to within the limits of tolerance for length with a diamond wheel and brazed into a finished azsembly, as shown 1in Fig. 3. The brazing operation was carried out in a hydrogen atmosphere, and Nicrobraz alloy was used. Experimental Work om Control Rod Inserts. The first step 1n the work on control rod inserts was toestablish the compatibility of aluminum oxide and boron carbide at the elevated temperature used for fabrication. A preliminary slug, less than full size, was hot-pressed at 1750°C for 5 min from a mixture of 90 vol % aluminum oxide {(Norton, grade 38-500) and 10 vol % boron carbide (Norton, metal- lurgical grade). The powder was con- tained in a graphite die and con- solidated at a pressure of 2500 psi. Metallographic examination revealed that the two materials were compatible. A second slug containing the prescribed amount of -325 mesh boron carbide had a density 86% of theoretical and possessed satisfactory physical properties, A full-size alumina-boron carbide cylinder was pressed by using the above conditions of temperature and pressure. Considerable difficulty was encountered in ejecting the slug from the die. There was also a marked tendency for the bubble-alumina in- sulation to sinter at this temperature. Subsequently, another full-size slug was pressed, and a maximum temperature of 1650°C was used. The compact was removed without difficulty, and sintering of the i1nsulating material was minimized. The density of the second compact dropped to 80% of theoretical but the physical properties were still acceptable. The boron carbide investment was increased proportionately to compensate for the decreased density. Production of Control Rod Inserts. The hot-pressing equipment used for making the boron carbide-iron parts was also employed for producing inserts UNCLASSIFIED Y-7059 & ¥ Hot-Pressing Rig. 2. Fig. Fig. 3. Assembly for for the control rods. New dies were used, however, to avoid additional boron pickup. Inserts for two rods were to be made; one set with a boron carbide content of 0,022 to0.024 g/cm?, the other with a boron carbide content of 0.005 to 0.006 g/cm?. A special grade of alumina was used (Norton, grade 38-500). Batches of about 1 1b were prepared by mixing appropriate quantities of the alumina and =325 mesh boron carbide (Norton, metallurgical grade). Fine boron carbide powder was obtained by ball- milling relatively coarse stock and screening out the desired fraction, Blending was carried out by tumbling in a glass jar for approximately 8 hours. The boron carbide additions were such as to give the correct boron investment for a hot-pressed compact having a density 80% of theoretical. The technique for hot-pressing the alumina-boron carbide powder es- sentially duplicated that used on the UNCLASSIFIED Y-7080 Boron Carbide-Iron Slug. boron carbide-iron powder, except for an increase in maximum temperature to 1650°C, Components for an assembly and a completed unit are shown in Fig. 4. The brazing operation was again done by using Nicrobraz alloy in a hydrogen atmosphere. HRE CONTROL ELEMENTS The design of the control elements for the HRE calls for plates bent into semicircular shapes. The plates will be exposed during operation of the HRE to high-pressure water and gas. The plates are to be made of a high cross- section material contained in a stain- less steel jacket., For the first set of elements built, sheet stock of boron carbide dispersed in aluminum was canned in type 347 stainless steel by covering the boron carbide stock with the steel and edge-welding. Several of these plates were found to distend following return to atmospheric UNCLASSIFIED Y=-7T0814 DUTER TUBE & INNER TURE ™ Fig. 4. pressure after exposure to operating pressures, Failure was accredited to an accumulation, as aresult of leakage through porous welds, of high-pressure gas 1n the space between the cladding and insert. The porosity may have been caused by melting and alloying of the aluminum with the weld metal. The purpose of this investigation was to determine a procedure of fabri- cation that would minimize the defects found in the first set of plates. Hot-rolling was employed to eliminate the void by bonding the cladding to the core. In an effort to use ma- terials readily available, bonding of the boron carbide-aluminum sheet with stainless steel was attempted first. Work was later shifted to the cladding of pressed-powder mixtures of boron carbide suspended in copper, since this method appeared to offer a better chance for success in the limited time available for the work. Reproducibility of the quality of the edge weld was assured by using a straight-line arc-welding train. Conditions were determined for operation of the arc welder to obtain sound welds without melting of the aluminum core. Assembly for Boron Carbide—Aluminum Oxide Slugs. Experimental Work on Stainless Steel—Boral. A preliminary check on the feasibility of bonding stainless steel to boron carbide-aluminum sheet stock was carried out on material com- posed of 37 vol % boron carbide and 63 vol % aluminum (35 wt % boron carbide and 65 wt % aluminum). This material is called Boral and is of the same composition as the stock used 1in the preparation of the original set of control plates., Cores measuring 3/4 in. in diameter were prepared for small samples by pressing =100 +200 mesh boron carbide and =100 mesh atomized-aluminum powders, in the volume ratio given above, at a pressure of 50 tons per square inch, These compacts were placed in frames blanked from type 347 stainless steel, Cladding plates for the cores were prepared as indicated in the following groups: Group 1. Thin layer of type 302 stain- less steel powder sintered at 1150°C to the inside sur- face of cladding. Group 2. Thin layer of copper powder sintered at 1020°C to inside surface of cladding, Plain cladding, bright annealed in a dry hydrogen atmosphere, The cladding and frames were spot welded to hold them together, heliarc welded around the edges, and given the treatments listed in Table 4, Group 3. TABLE 4. TEMPERATURES AND PERCENTAGE REDUCTIONS FOR EXPERIMENTAL ROLL-CLADDING OF BORAL WITH STAINLESS STEEL TOTAL CLADDING ROLLING REDUCTION GROUP TEMPERATURE (%) 1 600°C, 3 passes 32.5 1 600°C, 1 pass; 31 500°C, 2 passes 2 600°C, 3 passes 35 2 600°C, 1 pass; 34 500°C, 2 passes 3 600°C, 3 passes 33 3 600°C, 1 pass; 37 500°C, 2 passes Group 3 claddings were prepared to check straight metallurgical bonding of stainless steel to aluminum. The copper layer of Group 2 was introduced as an ald to bonding, for possible use in case a bond was not obtained between stainless steel and aluminum. The sintered layer of stainless steel powder 1n Group 1 was 1introduced to offer a rough surface for mechanical keying in the event metallurgical bonding could not be obtained at the rolling temperatures employed. After the specimens were rolled, samples were taken from each of the three groups for metallographic exami- nation, thermal cycling, and autoclave tests. Metallographic examination indicated that bonding had occurred at the Boral-to-cladding interface in each group. No cladding-to-core reaction zone was evident in those samples rolled partially at 500°C, Samples reduced entirely at 600°C did show a region of interaction between the Boral and the cladding stock, Bonding of cladding to the picture frame occurred in the Group 2 samples that had the sintered-copper layer. Figure 5 shows the interface region for a sample from each group rolled at 600°C. Neither cycling 25 times between room temperature and 500°F nor exposure to helium for 18 hr at 1500 psi following sudden pressure release was found to affect the samples. Several samples, measuring 2 by 8 i1in., with Boral cores and copper- coated stainless steel cladding were next prepared. Rolling was carried out at 600°C to ensure bonding. At this temperature, the Boral was reduced preferentially and presumably built up sufficient pressure ahead of the rolls to burst an end from each of the laminates after four or five passes, Altering the per cent reduction per pass seemed 1lneffective as long as the total reduction exceeded 30%. Subse- quently, two laminates similar to the above were processed by using three passes at 600°C to obtain 20% reduction and two additional passes at 500°C to obtain a total reduction of 30%. These plates rolled very satisfactorily, and there was no evidence of the end rupture experienced with earlier samples, The edge-welding problem was 1in- vestigated by using a 6-in, length from one of the 2- by 8-in. plates prepared as outlined above. The excess stock along the length of the sample was sheared off at an angle to the core so that the core-to-edge distance varied from 3/8 to 1/16 inch. The plate was sealed along this sheared edge by using the straight-line arc- welding train, The arc was observed for any irregularity in appearance, and irregularity was detected for edge- stock thicknesses of the order of 1/8 inch., Examination of the edge of the plate under the microscope after the welding operation showed defects at ——— - UNCLASSIFIED ¥=-5573 —=— TYPE 347 STAINLESS STEEL CLADDING -s— SINTERED LAYER OF TYPE 302 STAINLESS STEEL Rl b e aghe U e R (a}-'-“":v':.;fitlt‘:"{{é &:‘;"3 Tl NS y s H“u"*#%fi i %"P-‘.h-- VT MG S Y Lt A ™ .:'}'*".‘:T__fi_*a‘..fifim UNCLASSIFIED ¥-5574 - ® < - . & -— TYPE 347 STAINLESS STEEL ok ; CLADDING -%— SINTERED LAYER OF COPPER -=— BORAL UNCLASSIFIED ’ Y-55T72 . -%— TYPE 347 STAINLESS STEEL CLADDING ==— STAINLESS STEEL-ALUMINUM REACTION ZONE - = . - g - . i .- ‘l "~ ¢ . . I . A b * Ly ." LA PR el . ) - . ¢ . & Fig. 5. (a) Interface of Stainless Steel Cladding with Sintered Stainless Steel Powder Against Boral Core. 500X (b) Interface of Stainless Steel Cladding with Sintered-Copper Powder Against Boral Core. 500X (c¢) Interface of Stainless Steel Cladding Against Boral Core. 750X thicknesses up to 3/16 inch. At best, the 1/8-in.-wide frame requested for the stainless steel clad Boral 1s a border-line requirement for sound edge welds. The results of the experimental vork on Boral-stainless steel laminates indicate that full-size plates can probably be prepared by using the procedure outlined above, Experimental Work on Stainless Steel-Borcu. Stainless steel laminates rolled at 600°C work-hardened quite rapidly, and the resulting plate was very rigid. Since the plates were to be formed into semicircular shapes after rolling, with a radius of about 7 3/4 in., for the smallest-diameter pair, it would be helpful if the rolling process could be carried out at somewhat above 600°C. Obviously, this would necessitate replacing the aluminum with some other carrier for the boron carbide. Screening of Potential Core Metallics. Iron, nickel, types 302 and 410 stain- less steel, and chromium powders were considered as substitutes for aluminum. Coarse evaluation tests were made by pressing compacts containing 37 vol % boron carbide with each of these metals. The compacts were sintered at 1150°C for 30 min with the results listed 1in Table 5. These tests indicated that in all cases the boron carbide reacted with the matrix metal to formabrittle intermetallic or low-melting eutectic phase, with accompanying detrimental effects to the physical properties of the compacts. Laminates containing cores of the above compositions gave uniformly poor results after hot-rolling. Several laminates containing iron or type 302 stainless steel inthe cores wererolled at 1225°C; at this temperature the cladding was attacked by the core material and most of the center portion melted away. Several other laminates containing iron, type 410 stainless steel, and chromium matrices were rolled at 1050 to 1125°C; all these laminates blistered badly because of ruptures within the cores, Copper was considered next for the metallic of the core. Information from the literature indicated that copper does not react with or dissolve appreciable amounts of boron or carbon at temperatures far above i1ts melting point, TABLE 5. PROPERTIES OF SINTERED COMPACTS OF NICKEL, IRON, TYPE 302 STAINLESS STEEL, TYPE 410 STAINLESS STEEL, AND CHROMIUM PLUS BORON CARBIDE DENSITY AS PERCENTAGE COMPOSITION OF THEORETICAL DENSITY PROPERTIES Green Sintered Ni-B,C Ni-B eutectoid formed and flowed out of compact Fe—B4C 76.5 70.0 Brittle, fairly strong, liquid phase formed Type 302 stainless 74.0 59.5 Very brittle, liquid steel-B,C phase formed Type 410 stainless steel-B,C Very brittle, weak Cr-B,C Brittle, poorly sintered 10 A compact of copper and coarse boron carbide was prepared by sintering a mixture of the powders and then cold- pressing, resintering, and cold- rolling the mixture. The compact was successfully clad by hot-rolling at 1000°C, with a 50% reduction in seven passes., Figure 6 shows the interface between type 347 stainless steel cladding and the boron carbide-copper core. The finished laminate could be bent to a l-in. radius without failure. When bent further, failure occurred through the core and not at the bond surface. A revision in the scheduled time for completion of the full-size plates for the HRE forced an early decision as to which fabrication method would be used. The copper-bearing core was chosen as STAINLESS o 0 & e, .-1‘ -eas . T & ) ! 4 Fig. 6. Core. 250X the material most likely to fabricate satisfactorily. Preparation of Boron Carbide-Copper Cores. The boron carbide bearing section for each plate was assembled by using multiple inserts. A press with 150-tons capacity was available with which to consolidate the powders. Since a considerable amount of wear caused by the hard boron carbide particles was anticipated, it was decided to form the compacts in a die at 25 tsi, sinter, and coin the sintered compacts between hardened-steel plates at 50 tsi, in an effort to minimize die wear. A hardened-steel die was there- fore made to form 1- by 3-in. compacts of the required thickness. Stock for cores was prepared as a mixture of 41 vol % (16.3 wt %) boron carbide (Norton, metallurgical grade, Rl 4 - NyncLassiFien) Y-5692 e - - N o . wr ». : R Interface of Stainless Steel Cladding Against Boromn Carbide-Copper 11 which analyzed 71 * 1% boron) in copper powder (U. S. Metals Refining Company, type C). Two per cent of stearic acid dissolved 1n acetone was added to minimize classification of the boron carbide during handling of the mixture. The acetone was driven off by gentle heating prior to com- pacting. The compacts were pressed at 25 tsi, heated in air at 400°C to remove the binder, and sintered at 950°C for 2 hours. The compacts were then repressed at 50 tsi between hardened-steel plates and resintered for 15 min at 950°C to promote densi- fication. Preparation prior to cladding was then completed by cold- rolling to the desired thickness, loading the laminates into the frames, edge welding, and evacuating. Finally, the composite plates were hot-rolled at 1000°C, as described above. It was discovered during the preheating period for rolling the large plates that an outward distortion of the cladding occurred. The cause could not be determined with certainty. The edge welds on all plates were checked for soundness prior to rolling by a test of ability of the laminate to hold a vacuum. The possibility of a volatile residue from the binder after firing at 950°C does not seem likely. By delaying sealing of the exhaust tube for the laminates and applying vacuum to the core during the preheating cycle, the difficulty with swelling was eliminated. Subsequently, camphor was substituted for stearic acid as a binder to help minimize residual con- tamination following sintering. Components for preparation of a laminate are shown in Fig. 7. The rolled laminates were x rayed to locate the cores and the excess stainless steel stock was sheared from the edges to leave aminimum of 1/8-in. border, which was sealed by using the automatic argon-arc welder. In this UNCLASSIFIED ¥Y-T284 Hot Rolled Composite Pressed 8 Sintered Cu B4C Fig. 7. 12 347 Picture Frame 347 Cladding Components for HRE Control Plate. operation, the boron carbide-copper mixture possesses an additional advantage over Boral in that its higher melting point reduces the chances of melting of the core and the associated contamination of the weld. The actual core area for each plate, except plate 8, was determined from the x-ray pictures; plate 8 was delivered for a bending experiment before an x~ray picture was taken. The edges of plate 8 were trimmed by using the outline of the core that was visible on the cladding surface as a guide, The level of the boron carbide content of these plates was slightly below the 100-mg minimum requested, except for plate 16. The deficiency may be accredited to a lack of famili- arity with the properties of the powder mixture. 13 APPENDIX A. HRE CONTROL PLATE DATA PLATE NUMBER 6 10 5 9 1 14 12 16 Over-all length, in. | 16 1/8 16 1/8 17 1/8 17 3/16 18 1/8 19 11/16 | 19 3/16 13 13/16 Over-all width, 1in. 1 1 1/32 15/16 15/16 19/16 6 1/14 6 1/16 9 5/16 Core length, in. 15 3/4 15 3/4 [16 5/8 16 11/16 | 17 3/4 19 5/6 18 9/16 13 5/16 Core width, in. 11/16 21/32 15/16 15/16 11/8 53/4 513/16 | 9 1/32 Core area, in.? 10.8 10.3 15.6 15.65 20.0 111.0 107.9 120.3 B,C-Cu investment, g | 56.3 53.7 82.8 82.9 108.3 596.3 599.3 744 B,C investment, g 9.17 9.08 13.5 13.5 17.565 ar1.2 97.7 122 B investment, g 6.46 6.46 9.62 9.62 12.56 69.2 69.5 87.6 B per cm? of core, g |92.8 97.3 95.7 95.4 97.5 97 100 113 *Plate deliveared for bending experiment before x-ray picture could be taken for determination of aize. Equipment: Material: Welding Conditions: 14 APPENDIX B. WELDING CONDITIONS HRE CONTROL PLATES G-E, WD4200, d-c welder Linde, CM 37, machine carriage Airco, machine heliweld holder G-E, hi-thoria, 0.040-1in.-dia tungsten electrode Nine stainless steel clad boron carbide and copper sheets, 1/8 in. thick, in varying widths of 1 to 9 1/4 in.; accumul ated edge welding required was approximately 27 ft for the nine plates and varied in length from 13 to 19 inches. Shielding gas, Gas flow, 25 ft®/hr Generator open-circuit voltage, 70 volts Arc voltage, 10 volts Arc current, 46 amp Welding speed, 10 in./min argon