Uranium Silicide/Nitride Pellet Fabrication Demonstration: Report on Powder Characteristics (Final CRADA Report)
This report details experimental procedures and results of work at the Idaho National Lab to fabricate U 3 Si 2 and UN ceramic powders from their basic elements. The reaction procedure centers on arc melting using a cold, copper hearth. The reacted "buttons" are then ground into powder, and the powder is characterized. The preliminary experiments utilized feeding pieces of metallic U and Si (in the proper ratio) into the arc-melting furnace for melting into "buttons." This melting was repeated several times with the intent of homogenizing the reaction to produce phase pure U 3 Si 2 powder. However, sintering of the pressed-powder at over 1400C showed partial melting and slumping of the pellets. Characterization of the powder using x-ray diffraction (XRD) indicated the crystalline portion of the powder was U 3 Si 2 . However, further investigations indicated a significant portion (12.4%) of the powder was amorphous Si that was transformed into crystalline Si after a period of annealing. Therefore, a greatly improved method of powder fabrication was developed using mixing fine powders of U and Si together, pressing into a pellet, followed by arc melting and grinding into U 3 Si 2 powder. This method was highly successful in producing high phase purity (>98.5% U 3 Si 2 ) powder. One feature of this method is that the fine U powder is made by a hydride/de-hydride cycle. The equipment available at INL only allows for fabrication of relatively small batches, and the method (using INL equipment) is somewhat labor intensive. The powder was used to successfully press and sinter U 3 Si 2 pellets ("Final Report on Pellet Fabrication," INL/LTD-13-29465). A limited attempt was made to fabricate high purity UN powder using the fine U powder made at INL (hydride/de-hydride method) and heating it under flowing nitrogen gas. X-ray diffraction was used to characterize the resulting powder, and a Rietveld refinement was performed on the data. The refinement showed a result of 70.0% UN and 30.0% U 2 N 3 . It is thought that the UN content can be easily increased