T. Sekino et al., Reduction and sintering of alumina/tungsten nanocomposites - Powder processing, reduction behavior and microstructural characterization, J CERAM S J, 108(6), 2000, pp. 541-547
Reduction behavior of tungsten oxide mixed with alumina powder and its sint
ering processes were investigated to fabricate Al2O3/W nanocomposites, Subm
icron-sized WO3 powder could be obtained by a conventional ball-milling tec
hnique. Hygrometry analysis of Al2O3/WO3 mixture revealed that WO3 powder w
as reduced in two steps at 873 and 973 K, X-ray diffraction and transmissio
n electron microscopy (TEM) analysis confirmed that Magneli phases, such as
WO2 and WOx (n=2.89 to 2.92), were obtained by the reduction of WO3 at 873
K. However, WO3 was completely reduced to metallic W when the reduction te
mperature was higher than 1173 K, A thermodynamic analysis qualitatively ag
reed with the experimental result that WO2 and WO, coexisted at intermediat
e temperatures. Reduction followed by hot-press sintering of Al2O3/WO3 mixt
ures was carried out to obtain Al2O3/W nanocomposites. Agglomeration and/or
incomplete reduction was found at high W content; however, dense Al2O3/W c
omposites with >98% of their theoretical density were obtained at low W con
tent (i.e., < 10 vol%). A microstructural investigation of the dense compos
ite revealed that it consisted of both micro- and nano-sized W dispersions.
Furthermore, a large number of W particles of around 40 nm were found to b
e homogeneously dispersed in the Al2O3 matrix. These particles were much fi
ner than the WO3 particles obtained by ball-milling.