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用热分析、程序升温超高真空质谱、真空原位红外光谱等技术研究了属于Vaska Ⅱ_b型4:2钼、钨过氧配合物K_4Mo_4O_(12)(0_2)_2、K_4W_4O_(12)(O_2)_2·4H_2O的热分解行为,前者中两个过氧基同时分解(278℃),后者分两步进行(180和342℃),每步分解一个过氧基。4:2钨过氧配合物出现在180℃分解的原因是由于结晶水的作用。比较钼、钨过氧配合物的分解温度,发现Vaska Ⅱ_b型配合物的热稳定性都比Vaska Ⅱ_a型的高。
The effects of Vaska Ⅱ_b type 4: 2 molybdenum, tungsten peroxo complexes K_4Mo_4O_ (12) (0_2) _2, K_4W_4O_ (12) (O_2) and their complexes were investigated by means of thermal analysis, temperature programmed ultrahigh vacuum mass spectrometry and vacuum in situ IR spectroscopy. _2 · 4H_2O thermal decomposition behavior, the former two peroxide decomposition (278 ℃), the latter in two steps (180 and 342 ℃), each decomposition of a peroxy. The reason why 4: 2 tungsten peroxygen complex was decomposed at 180 ℃ is due to the effect of crystal water. Comparing the decomposition temperatures of the perovskite and tungsten perovskite complexes, the thermal stability of the Vaska Ⅱ_b complex was found to be higher than that of Vaska Ⅱ_a.