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以MoCl_3(OC_2H_5)_2为原料,应用溶胶-凝胶法制备了透明均匀的氧化钼薄膜。实验发现,合适的工艺条件为:浸透液浓度0.1～1.0mol/L,浸透湿度40～60％,H_2O/MoCl_3(OC_2H_5)_2摩尔比2～4,热处理温度300℃。薄膜在300℃以下热处理是非晶态的,加热到350℃时,有MoO_3晶相出现。应用红外吸收光谱、X-射线衍射对干凝胶的结构和组成进行了研究,在空气气氛中热处理干凝胶,主晶相是MoO_3,加热到600℃时,存在Mo_9O_(26)晶相;在氩气中,300℃是MoO_2晶相,400℃以上则为MoO_2和η-Mo_4O-(11)两种晶相,在1Pa真空中,300～400℃有MoO_2、Mo_8O_(23)和MoO_(28)三种晶相,600℃则转化为MoO_2和ν-Mo_4O_(11)两种晶相。应用DTA对凝胶进行热分析表明:在98℃左右,溶剂C_2H_5OH和吸附水挥发,加热到400℃以上,残余有机物开始氧化分解。
Using MoCl_3 (OC_2H_5) _2 as raw material, a transparent and uniform molybdenum oxide film was prepared by sol-gel method. The experimental results showed that the optimum conditions were as follows: the concentration of infiltration liquid was 0.1-1.0 mol / L, the infiltration humidity was 40-60%, the molar ratio of H 2 O / MoCl 3 (OC 2 H 5) 2 was 2-4, and the heat treatment temperature was 300 ℃. The film is heat-treated at 300 ℃ below the amorphous state, heated to 350 ℃, there MoO_3 crystal phase appears. The structure and composition of the xerogel were studied by infrared absorption spectroscopy and X-ray diffraction. The xerogel was heat-treated in the air atmosphere with the main phase being MoO_3. When heated to 600 ℃, the Mo_9O_ (26) In argon, 300 ℃ is the MoO_2 phase and 400 ℃ is the MoO_2 and η-Mo_4O- (11) phases. In 1Pa vacuum, MoO_2, Mo_8O_ (23) and MoO_ 28) three kinds of crystal phase, 600 ℃ is transformed into MoO_2 and ν-Mo_4O_ (11) two crystal phase. The thermal analysis of the gel by DTA showed that the solvent C_2H_5OH and adsorbed water volatilized at about 98 ℃ and heated to above 400 ℃. The residual organic compounds began to oxidize and decompose.