Manufacturing of heavy tungsten alloys from nano-sized metal oxides via simultaneous reduction-sintering powder treatments

Heavy tungsten alloys are of great importance in the engineering and mining industries as well as the military and medical applications because of their stability at high temperatures, high strength and dense structures. The present study develops a novel technology for the production of heavy tungsten alloys via thermal treatment of nano-sized metal oxides based on simultaneous reduction and sintering processes. Heavy tungsten alloy (95W-3Ni-2Fe) was produced from the reduction of mixed nano-sized metal oxides precursor in H₂ at 1000 ^o C followed by sintering at 1350–1450 ^o C for 30–90 min. The reduced and sintered samples were characterized by XRD to follow up the crystallinity, total porosity measurement was used to find out the densification properties, the grain structure and morphology were examined by RLM and SEM attached with EDAX. Micro-hardness tester was also used to investigate the influence of sintering conditions on the grain densification. A fundamental study on the kinetics of reduction of mixed nano-sized metal oxides precursor was performed by isothermal and non-isothermal techniques. Both results from isothermal and non-isothermal tests were used to calculate the activation energy which was correlated with macro- and micro-structures to predict the corresponding reduction mechanism. However, the influence of sintering temperature and time on the crystallinity of the produced phases, grain structure, morphology, total porosity, pore-size distribution, bulk and apparent densities, and the hardness of sintered compacts was extensively investigated. The results revealed that the presence of NiO and/or Fe₂O₃ in the mixed metal oxides precursor was very important to ease the reducibility of WO₃ as the metallic phases of Ni and/or Fe act as a catalyst for the reduction of WO₃. The rate of reduction proceeds faster in the following order: NiO > Fe₂O₃ > mixed oxide > WO₃. In non-isothermal experiments, it was found that the heating rate has a considerable effect on the reduction of precursor, i.e., the lower the heating rate, the higher the degree of reduction. It might be reported that the use of nano-sized metal oxides particles in the fabrication of heavy tungsten alloys greatly affects the main properties of the produced alloy. With the increase in sintering time, larger sizes of dense grains were developed, and the matrix became denser as a result of sintering and re-crystallization effects. The higher the sintering time, the higher the grain densification and the less pores formed in the matrix. On the other hand, with the increase in the sintering temperature, the grain boundaries were well defined in which the grains were composed of tungsten metal and surrounded by inter-metallics. The higher the temperature, the higher the XRD peak intensities of metallic tungsten and intermetallics as a result of sintering and re-crystallization.