Hanford Laboratories Operation Monthly Activities Report December 1956 (Deleted)

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,Route To: P.R. No. Location Route Date Work performed under Contra.ct No. W-31-109-Eng-52 between the Atomic Energy Commission and General Electric Compa.ny Signature and Date THIS DOCUMENT HAS BEEN SCANNED AND IS STORED ON THE OPTICAL DISK DRIVE

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19 - 20. Atomic Energy Commission, Hanford Operations Office, Attn: J. E. Travis

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FORCE REPORT AND PERSONNEL STATUS CHANGES Metallurgy and Reactor Fuels Physics and Instrumentation Chemistry and Separations Processes Operations Research and Synthesis INVENTIONS OR DISCOVERIES

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Manager, Hanford Laboratories. ......... Chemical Research and Development ........... Physics and Instrument Research and Reactor and Fuels Research and Development. .....

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METALLURGY AND REACTOR FUELS Preparation of High-Purity Uranium. Small quantities of high-purity uranium for USC 'in single crystal preparation have been obtained through electrowinning from a molter salt bath. A ternary consisting of potassium chloride, lithium chloride, and uranium trichloride is used, together with reactor-grade uranium rods for the electrodes. The salt mixture has been made by introducing uranous oxide into the molten binary o potasslkXi chloride and lithium cljoride. Electrolysis reduced the higher uranium chlorides to the trichlorides. Investigations a r e being made to determine the effect of varying operational temperatures, cathodic current densities, and cathode shape on the size and shape of the electrodeposited Chlorination proceeds at 700-800 C. Low Temperature Irradiation of Uranium Tensile Samples. Specimens prepared fron beta-annealed dingot uranium sheet were exposed for short periods in a HAP0 Reacto using the poison column facility. mately one year before being tested. observed, even for the shortest exposure. Several samples were than annealed t o determine whether the damage observed could be removed. at room temperature for the one year period, and it w a s tested without further annealing. The yield strength of this sample w a s considerably lower than the "asirradiated" yield strength for samples held in the refrigerator, indicating that appreciable recovery occurs at room temperature. at 200, 300, and 400 C for periods of 10 hours. the yield strength to pre-irradiation values for the samples with the lowest exposure but caused only varying degrees of recovery in the highest exposure material. Static Corrosion Tests in Organic Coolants. uranium metal by MfPb at 40~ O Confirm e dby static corrosion tests in laborator: no visible attack of the uranium after one day at 400 C. There was considerable spalling evident after four days and fairly complete disintegration after six days. Aftt 19 days the uranium was converted t o UC, and the MIPB was very dark in color and about the fluidity of 20-weight motor oil. The estimated exposures were 1 x 1016' and 1 x 1017 A significant increase in yield strength was The samples were stored in a refrigerator f o r approxiOne sample had remainec Additional samples were annealec These anneals produced a lowering of The absence of rapid corrosion of bare Contrary t o previous tests conducted at 450 C, there was essentially Cathodic Vacuum Etching of U 0 2 . 1s first necessary to develop its structure by suitable etching methods. vacuum etching has proved itself for both optical and electron microscope examinatior This etch developed differences inthe topography of the specimen. etching has been successfully applied to sintered UO which is extremely difficult to etch by chemical o r electrolytic means. The grain s3ructure and porosity of sintered U 0 2 has been photographed in the optical and electron microscope. The applicability of cathodic vacuum etching to other cermets will be investigated. TO examine the microstructure of a material, it This type of

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All five KAPL powder metallurgy U-Mg samples have been received at the HAP0 radiometallurgy facility after irradiation at the MTR. Three of the irradiated sample and two unirradiated control samples have been bend tested. The bend test data indicate that irradiation has had a sintering effect on the powder metallurgy compacts and has increased the mechanical properties. material are poor a s shown in the following table. The properties of the unirradiated Effects of Exposure on the Bend Strength Estimat ed Particle Size Maximum Deflections One of the remaining two unexamined irradiated pieces will be studied for interdiffusion between the A1 cladding and the U-Mg core material. bend tested. These two will be the study of plutonium or other radioactive surfaces. to studies of machined plutonium surfaces. were in some respects more useful than profilometer readings. this method can also be used for micrographic examination of cathodically etched metallographic samples of plutonium o r other radioactive materials. A Faxfilm replication technique has been developed for The method has been applied Replicas made by Data obtained by examination of replicas Barrel plating techniques a r e being investigated f o r use in the electrodeposition of nickel on P u - A l alloy monitor foil discs for reactor monitoring experiments. Modification of the barrell plater has been completed and further plating tests will Thickness standards have been completed f o r calibration of an eddy current thickness gage being developed for determination of can thickness. Mandrels were plated with nickel or copper and ground to uniform thickness. The specimens were then accurate gaged so that the thickness of the electrodeposited coating would be known for use as The feasibility of coating uranium or other materials with plutonium metal is being studied. Production of stable plutonium films 1 mil in thickness appears feasible. There is cause for optimism. A vacuum system was designed for cold "coating" The apparatus is being constructed and should be completed by The equipment can be converted t o "hot" work if necessary.

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Temporary plutonium corrosion testing facilities are being installed in the 234- 5 Building. The experimental test chamber is being fabricated from monolithic lucite. Molds for casting a criticality part were fabricated and a good casting f o r the segments was made after two failures. mold and furnace troubles on filling the second. three pours and is still usable. Failures were due to a metal leak in the first The same mold was used for all A program to determine the accuracy of the Monarch lathe and the t r a c e r system is and is being fabricated. This template will be inspected by the sine bar method and on the 30" Kodak comparator. similarly inspected. A system utilizing a microformer capable of measuring lit,ear displacements on the order of microinches will be mounted below the t r a c e r heau to measure null balance variations in the tracer valve. A special template having a variety of radii and angles has been designed Parts machined using this template will also be Tooling and gages required f o r the fabrication of two large plutonium parts a r e now metal frits at the vacuum ports. during machining is also included in the design. installed to regulate coolant temperature and a sump pump has been obtained to recycle the coolant to the bath in case a large coolant flow is required. control is critical in order to achieve the extreme accuracies required. Full support vacuum chucks a r e being designed utilizing powder Temperature indication and regulation of the chucks A constant temperature bath is being Design of a hood f o r the polar thickness gage being supplied by UCRL has been completed. The 30" Kodak optical comparator has been checked and adjusted. lation of the inspection hood and the portable comparator box is about 7 5 per cent cast, radiographed, sampled, analyzed and prepared for canning. The 190 aluminum cans f o r these slugs have been machined and anodized. assembles have been completed. inch) which a r e t o be placed between the cap assembles and the slugs is in progress. All of the simulated 1000 MWD/T uranium PCTR slugs have been The initial group of 45 cap Fabrication of the aluminum foil wafers (0. 0015 Two irradiated samples and two control pieces of Th-2 w / o U-235 alloy have been bend tested. The control pieces bent to the limit of the test apparatus at about 3500 pounds load without breaking. load and only 0. 004-inch.deflection. t o irradiation and the ductility has been reduced markedly. a / o burnup, appreciable irradiation and fission product damage is to be expected. The irradiated pieces broke at about 5000 pounds The strength of the material has increased due However, at 0. 5 and 1.0 Recrystallization and Recovery of Zirconium Alloys. The electrical resistivity values of 224 specimens from the "Recrystallization and Recovery of Zirconium Alloys" project show an excessive scatter. degree of anneal s o the observed scatter could be due to a non-uniform rolling texture To check this, a control experiment w a s initiated utilizing a series of single specimer Separate specimens were used in each

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measured before and after annealing. Electrical resistivity measurements have beel completed on 24 Zircaloy-2 and Zircaloy-3 specimens where material examined w a s 50 p e r cent cold worked, then annealed in air, helium, or vacuum f o r 10, 100, and 1000 minutes at 300, 400, 500, and 700 C. Several general observations can be madc concerning electrical resistivity data (at -195 C) from this portion of the experiments (1) the 50 per cent cold worked Zircaloy-2 has a value of 44 micro-ohm-cm in the as-worked condition compared to 20 micro-ohm-cm f o r Zircaloy-2 (2) after anneals f o r 1000 minutes at 300, 400, and 500 C recovery is not complete (3) a 700 C anneal causes a minimum electrical resistivity in ten minutes followed by an increase to near or above the as-worked value in 1000 minutes (4)the 1000-minute value is great6 f o r the air anneal than for the helium, and greater for the helium anneal than f o r the vacuum ( 5 ) of the factors that contribute to this increase in electrical resistivity, contamination by hydrogen and oxygen a r e considered dominant and ( 6 ) the maximum spread of electrical resistivity values, as a function of annealing temperature, occur at a ten-minute anneal and is greater for Zircaloy-2 than for Zircaloy-3. Tensile Properties of Zircaloy-2. Post-irradiation examination w a s continued of tstimated neutron exposure of the material w a s 1.4 x 10'' nvt (a1 MeV) and 7 x 10 changes in tensile properties in the "as-irradiated" specimens were determined. During the past month several samples have been given post -irradiation vacuum hour anneals a r e underway. ircaloy-2 tensile specimens exposed two operating cyc s in the MTR. The 2o Both annealed and cold worked material was irradiated and the Annealing for 10 hours at 250, 300, and 350 C has been completed and 100B, D, F Reactor Zircaloy Process Tubes. The experimental fabrication of zirconiur welded process tubing is in progress. Defective areas in the zirconium and Zircaloy strip have been removed, and the usable strip lengths were butt welded together by the Trent Tube Company. The rod will be resistance welded t o the strip prior to roll forming and welding of the tubing. welded using the "Thermatool" welding process. will be evaluated. Samples from the welded tubes KER Size Zircaloy-2 Process Tubes. obtain tube blanA's for the fabrication of ribless KER size m o c e s s tubes. Three Zircaloy-2 billets were extruded to extrusion of two of the billets was successful. Formability Test f o r Zirconium Alloys. tubes have resulted from fractures which occur across the r i b s during the tube of fracture a r e being conducted. rolled on a grooved, hardened steel block. the r i b was reduced somewhat l e s s than that of the flat pprtion of the plate. fractures observed at the root and crest of the r i b were very similar to those commonly encountered in tube reducing. from the differential reduction of a r e a between the r i b and the flat plate portion. Additional tests a r e planned to determine quantitatively the magnitude of the differential reduction of area at the point where fractures are observed. Low fabrication yields of Zircaloy process Formability studies which are designed to reproduce this type In all cases the cross sectional area of Ten Zircaloy-2 plates with premachined ribs were The observed fractures apparently resulted

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Magnesium Alloy Tubing f o r Organic Coolant Materials The possibility of using magnesium alloy tubing to contain organic coolant materials has been suggested. indicates that presently-available alloys do not possess adequate elevated temperature A survey of the engineering properties of magnesium alloys However, there is a possibility that new experimental alloys may be Tensile Properties of Aluminum Alloy M-388 A study is being made of several variables that affect the tensile properties of an aluminum-1 w/o Ni alloy, M-388, in preparation for tests to determine the extent of radiation damage in this material. Material cold-worked to 10, 25, and 50 per cent reduction in a r e a w a s annealed for 1, 7 , 100, and 1000 hours at 150 and 200 C and 1, 7 . and 100 hours at 250, 300, 350, and 400 C to determine recovery and recrystallizatioi through tensile property measurements. microstructure of the specimens is being examined. cold worked 10, 25, and 50 per cent and annealed for 30 to 1000 minutes at 400, 500, and 600 C to determine the influence of fabrication and annealing conditions upon the grain size. There was very little difference in grain size with time at temperature. Increasing the temperature from 400 to 500 C did not produce a significant change. The p r i o r cold work appears to be the governing factor. conditions the average grain diameter of the 10 per cent cold worked material w a s approximately a factor of six larger than that of the 50 per cent cold worked material. These tests have been completed and the Another group of samples were For the same annealing Optical and Electron Micrography In many instances optical and electron micrography of identical areas .is desirable in order that results by optical methods can be referred directly t o the equivalent results by electron microscope methods and t o permit examination at any level of accomplishing this a r e impossible. A satisfactory method for examining a given, preselected a r e a in a radioactive specimen and its electron microscope replica has use of a mechanical stage for manipulating the non-radioactive replica. ing grid required for electron microscopy is placed in a special holder on the stage of the microscope and so oriented to permit positioning of a grid opening above any rack mechanism and the grid is cemented t o the replica with dilute adhesive solution. This method can also be used for non-radioactive specimens. In the case of radioactive materials, conventional techniques for The substage of a petrographic microscope w a s modified to permit Contact between grid and replica is achieved with the substage Diffusion in non-irradiated U/AlSi and U/Z r couples is being investigated to provide a …