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Title: QUARTERLY METALLURGICAL PROGRESS REPORT NO. 5 FOR THE PERIOD OF OCTOBER 1, 1959 TO DECEMBER 1959

Technical Report ·
OSTI ID:4200762

Investigations are being made to develop new methods for preparing high- purity yttrium metal. Research during the past quarter centered largely on the development of methods for preparing pure anhydrous yttrium iodide and the subsequent reduction of the iodide to metal. Methods for preparing anhydrous yttrium bromide were also investigated. Fabrication studies were continued to determine further the working characteristics of high-purity yttrium. These studies included hammer and press forging, cold rolling, extrusion and annealing tests. A modified procedure for chlorinating calcined thorium oxalate was developed. Varying distillation temperature and retort pressure reduced the amount of entrained solids in purified thorium tetrachloride. Modifications in reduction equipment designed to prevent volatilization of sodium from the reaction crucible were partially successful. An ingot melted from selected material had an as-cast Brinell hardness (500 kg load) of 35 and an annealed hardness of 28. This material was cold-forged 68%. Attempts to reduce UF/sub 6/ with lithium, calcium, magnesium, and antimony failed to produce a satisfactory uranium metal sponge. Research was continued on the development of an economical process for the extraction of zirconium-hafnium values from zircon sand, and the preparation of an enriched hafnium fraction for feed to a suitable solvent extraction scheme. Studies on fluoride roasting of zircon followed by fractional crystallization of the zirconium fraction, and upgrading of hafnium tetrachloride by selective disproportionation are being conducted. Preliminary results from a set of 64 samples conducted on a statistical basis showed no further improvement was obtained in extraction efficiency. Approximately 50% of the combined zirconium and hafnium values were extracted by leaching a reacted mixture of zircon and K/sub 2/SiF/sub 6/ with dilute hydrofluoric acid solution. Results from three additional selective disproportionation tests showed that the hafnium content was enriched from 3.2 to 5.6% (based on a ratio expressed as Hf/Hf + Zr x 100). Hafnium-vanadium alloys were prepared by arc-melting and suction casting. The investigation of the zirconium-gadolinium phase diagram was completed. The diagram is a simple eutectic system with limited terminal solubility of gadolinium in alpha and beta zirconium phases, and of zirconium in gamma and delta gadolinium phases. The investigation of stainless steel (304)-gadolinium pseudo-binary phase diagram was initiated. No difficulty was encountered in consolidating selected alloy compositions by nonconsumable arc-melting. As-cast alloys are being subjected to melting point determinations and hot swaging. Investigation to determine phase diagrams for the binary systems, titaniumgadolinium, titanium-iridium, and titanium-europium were continued. A total of nine air-cooled arc melts completed in one of the herringbone-finned crucibles are being evaluated. Of these nine heats, six were iron, one was titanium, atd two were zirconium. Machined crucibles are being produced from the free machining copper-lead and coppertellurium alloys in an effort to determine the feasibility of producing machined crucibles for air cooling. Fifty air samples taken from the various thorium handling areas have been analyzed by decay count procedures. In addition, three representative samples have been sent to the University of California Lawrence Radiation Laboratory for alpha-pulse height analysis. Although no definite conclusions can be made as to hazards presented, an idea of the relative dangers of given operations can be drawn from the initial activities. Compression strength and density values were determined on eighty expendable graphite mold specimens and a series of castings is being produced using expendable material BW. (For preceding period see USBMU-647.) (auth)

Research Organization:
Bureau of Mines. Albany Metallurgy Research Center, Oreg.
DOE Contract Number:
AT(11-1)-599
NSA Number:
NSA-14-007704
OSTI ID:
4200762
Report Number(s):
USBM-U-672
Resource Relation:
Other Information: Orig. Receipt Date: 31-DEC-60
Country of Publication:
United States
Language:
English