利用草酸还原五氧化二钒的方法制备系列低价钒氧化合物。将混匀的原料置于高纯N2洗气后的石英管中,600℃反应2h,nV2O5:nH2C2O4在1:0.5至1:2.5范围变化时,可以分别得到单一物相的V6O13,VO2和V2O3粉体。通过XRD,XPS,EPR,电阻测量及磁性测试等手段对VO2样品进行了表征,结果显示VO2样品在65℃附近发生从半导体到金属的相变,并且其电学和磁学性质变化与文献报道基本一致。
Oxalic acid reduction method was developed for preparing vanadium oxides with various low vanadium valence states by heating the mixture of vanadium pentoxide(V2O5) with suitable amounts of oxalic acid(H2C2O4) in sealed quarts tube under high-purity N2 at 600 ℃ for 2 h.When the molar ratio of V2O5 to H2C2O4 was varied from 1:0.5 to 1:2.5,pure phase samples V6O13,VO2 and V2O3 could be obtained.The VO2 sample was characterized by XRD,XPS,EPR as well as electric and magnetic measurements.The title material has a structure phase transition around 65 ℃,corresponding to a semiconductor-to-metal transition.With this transition,the resistivity and magnetic susceptibility are with discontinuous change near the phase transition temperature,in reasonable agreements with the reported data.