A Nanosized WO3 and CuO powder mixture is prepared using novel high-energy ball milling in a bead mill to obtain a W-Cu nanocomposite powder, and the effect of milling time on the structural characteristics of WO3-CuO powder mixtures is investigated. The results show that the ball-milled WO3-CuO powder mixture reaches at steady state after 10 h milling, characterized by the uniform and narrow particle size distribution with primary crystalline sizes below 50 nm, a specific surface area of 37 m2/g, and powder mean particle size (D50) of 0.57 μm. The WO3-CuO powder mixtures milled for 10 h are heat-treated at different temperatures in H2 atmosphere to produce W-Cu powder. The XRD results shows that both the WO3 and CuO phases can be reduced to W and Cu phases at temperatures over 700oC. The reduced W-Cu nanocomposite powder exhibits excellent sinterability, and the ultrafine W-Cu composite can be obtained by the Cu liquid phase sintering process.
Fe3O4/Fe/graphene nanocomposite powder is synthesized by electrical wire explosion of Fe wire and dispersed graphene in deionized water at room temperature. The structural and electrochemical characteristics of the powder are characterized by the field-emission scanning electron microscopy, X-ray diffraction, Raman spectroscopy, field-emission transmission electron microscopy, cyclic voltammetry, and galvanometric discharge-charge method. For comparison, Fe3O4/Fe nanocomposites are fabricated under the same conditions. The Fe3O4/Fe nanocomposite particles, around 15-30 nm in size, are highly encapsulated in a graphene matrix. The Fe3O4/Fe/graphene nanocomposite powder exhibits a high initial charge specific capacity of 878 mA/g and a high capacity retention of 91% (798 mA/g) after 50 cycles. The good electrochemical performance of the Fe3O4/Fe/graphene nanocomposite powder is clearly established by comparison of the results with those obtained for Fe3O4/Fe nanocomposite powder and is attributed to alleviation of volume change, good distribution of electrode active materials, and improved electrical conductivity upon the addition of graphene.
Ultrasonic-milling of metal oxide nanopowders for the preparation of tungsten heavy alloys was investigated. Milling time was selected as a major process variable. XRD results of metal oxide nanopowders ultrasonic-milled for 50 h and 100 h showed that agglomerate size reduced with increasing milling time and there was no evidence of contamination or change of composition by impurities. It was found that nanocomposite powders reduced at in a hydrogen atmosphere showed a chemical composition of 93.1W-4.9Ni-2.0Fe from EDS analysis. Hardness of sintered part using 50 h and 100 h powder samples was 399 Hv and 463 Hv, respectively, which is higher than the that of commercial products (330-340 Hv).
Ultrasonic-milling of metal oxide nanopowders for the preparation of tungsten heavy alloys was investigated. Milling time was selected as a process variable. XRD results of metal oxide nanopowders ultrasonic-milled for 50 and 100h showed that mean crystallite size reduced with increasing milling time and there was no evidence of contamination or change of composition by impurities. It was found that nanocomposite powders reduced at in atmosphere had a composition of 93.1W-4.9Ni-2.0Fe by EDX analysis. Hardness of sintered samples of 50 and 100h was 390 and 463 Hv, respectively, which corresponds to the hardness of commercial products.
Recently, the fabrication process of W-Cu nanocomposite powders has been researched to improve the sinterability by mechanochemical process (MCP), which consists of ball milling and hydrogen-reduction with W- and Cu-oxide mixture. However, there are many control variables in this process because the W oxides are hydrogen-reduced via several reduction stages at high temperature over 80 with susceptive reduction conditions. In this experiment, the W-15 wt%Cu nanocomposite powder was fabricated with the ball-milling and hydrogen-reduction process using W and CuO powder. The microstructure of the fabricated W-Cu nanocomposite powder was homogeneously composed of the fine W particles embedded in the Cu matrix. In the sintering process, the solid state sintering was certainly observed around 85 at the heating rate of 1/min. It is considered that the solid state sintering at low temperature range should occur as a result of the sintering of Cu phase between aggregates. The specimen was fully densified over 98% for theoretical density at 120 for 1 h with the heating rate of 1/min.
The effects of residual impurities on solid state sintering of the powder injection molded (PIMed) W-15wt%Cu nanocomposite powder were investigated. The W-Cu nanocomposite powder was produced by the mech-ano-chemical process consisting of high energy ball-milling and hydrogen reduction of W blue powder-cuO mixture. Solid state sintering of the powder compacts was conducted at for 2~10 h in hydrogen atmosphere. The den-sification of PIM specimen was slightly larger than that of PM(conventional PM specimen), being due to fast coalescence of aggregate in the PIM. The only difference between PIM and PM specimens was the amount of residual impurities. The carbon as a strong reduction agent effectively reduced residual W oxide in the PIM specimen. The formed by reduction of oxide disintegrated W-Cu aggregates during removal process, on the contrary to this, micropore volume rapidly decreased due to coalescence of the disintegrated W-Cu aggregates during evolution of CO.It can be concluded that the higher densification was due to the earlier occurred Cu phase spreading that was induced by effective removal of residual oxides by carbon.
MgO based nanocomposite powder including ferromagnetic iron particle dispersions, which can be available for the magnetic and catalytic applications, was fabricated by the spray pyrolysis process using ultra-sonic atomizer and reduction processes. Liquid source was prepared from iron (Fe)-nitrate, as a source of Fe nano-dispersion, and magnesium (Mg)-nitrate, as a source of MgO materials, with pure water solvent. After the chamber were heated to given temperatures (500~), the mist of liquid droplets generated by ultrasonic atomizer carried into the chamber by a carrier gas of air, and the ist was decomposed into Fe-oxide and MgO nano-powder. The obtained powders were reduced by hydrogen atmosphere at 600~. The reduction behavior was investigated by thermal gravity and hygrometry. After reduction, the aggregated sub-micron Fe/MgO powders were obtained, and each aggregated powder composed of nano-sized Fe/MgO materials. By the difference of the chamber temperature, the particle size of Fe and MgO was changed in a few 10 nm levels. Also, the nano-porous Fe-MgO sub-micron powders were obtained. Through this preparation process and the evaluation of phase and microstructure, it was concluded that the Fe/MgO nanocomposite powders with high surface area and the higher coercive force were successfully fabricated.