摘要
应用ＤＴＡ／Ｔ／ＥＧＤ／ＧＣ在线联用技术，在空气气氛中对Ｇｅ－１３２的热氧化分解反应历程（室温～９２５°Ｃ）进行了研究，应用Ｘ－ｒａｙ仪对Ｇｅ－１３２在不同温度（４５０°Ｃ、６５０°Ｃ、７２０°Ｃ、８００°Ｃ、９２５°Ｃ）下的热氧化分解反应残物作了物相鉴定；测定了Ｇｅ－１３２的ＴＧ／ＤＴＧ曲线（室温～９７０°Ｃ）；在ＤＴＡ／Ｔ／ＧＣ联用曲线的ＧＣ谱图上，检出了各反应温度下的Ｏ２、ＣＯ２和Ｈ２Ｏ及其热氧化分解产物（逸出气）的组成演变规律。从各残物的ＸＲＤ谱图上可观察到，Ｇｅ－１３２的晶相结构破坏到７２０°Ｃ时才析出微量Ｇｅ、ＧｅＯ２，并发现Ｇｅ在８００°Ｃ时被氧化为ＧｅＯ２，至９２５°Ｃ时形成为高纯度ＧｅＯ２。ＴＧＡ定量计算表明，Ｇｅ－１３２在空气气氛中被氧化为ＧｅＯ２的得率与理论计算值相当。综合上述的实验结果与数据分析，对ＤＴＡ曲线上呈现的二个吸热效应和三个放热效应的性质作出了判断和验证，并得出了Ｇｅ－１３２在空气气氛中被氧化为ＧｅＯ２的反应历程。
Based on the experimental results of previous work, XIII, the reaction mechanism of the thermal oxidation decomposition in air atmosphere (ambient temperature￣925℃) of Ge 132 was studied by applying DTA/T/EGD/GC on line coupled simultanious technique. By using XRD the substance phase of the residue of Ge 132 at different temperature (450℃、650℃、720℃、800℃ and 925℃) was identified. TG/DTG curves of Ge 132 was detected from ambient temperature to 970℃. In the GC gram of DTA/GC coupled curves, O 2,CO 2 and H 2O of the decomposition product of thermal oxidation (evolved gas) at different reaction temperature have been detected. Also its variational law of the composition was traced. From XRD gram of the residues, it is observed that the crystal Ge and crystal GeO 2 are not released until 720℃. It was discovered that Ge was oxidized to GeO 2 at 800℃ and high purity GeO 2 was obtained at 925℃. It is shown by the quantitative calculation of TGA, that the percentage of GeO 2 oxidized from Ge * 132 in the air is approximate to the theorical calculative value. The characteristic of two endothermal effects and three exothermal effects presented on the DTA curve is determined and verified by the above experimental results and data analysis, and the reaction mechanism of Ge 132 oxidized to GeO 2 in the air atmosphere is obtained.
作者
蔡根才
钱延龙
黄吉玲
黄家桢
沈明赓
钱义祥
Cai, Gencai; Qian, Yanlong; Huang, Jiling; Huang, Jiazhen; Shen, Minggeng; Qian, Yixiang
出处
《华东理工大学学报（自然科学版）》
EI
CSCD
北大核心
1997年第1期121-126,共6页
Journal of East China University of Science and Technology
关键词
差热分析
逸出气检测
气相色谱
锗有机化合物
carboxyethylgermanium sesquioxide
organic germanium(Ge 132)
differential thermal analysis(DTA)
evolved gas detector(EGD)
gas chromatography(GC)
on line coupled simultaneous technique
