多元硫砷金属化合物的溶剂热合成

【作者】 李雪峰；

【导师】 安永林；

【作者基本信息】 大连理工大学 ， 无机化学， 2003， 硕士

【摘要】 硫族金属化合物具有多种多样的结构，是近年来研究的越来越多的无机多功能材料。这一类化合物的合成，并正在成为无机化学研究的热点。溶剂热（水热）合成方法是一种容易产生新相，获得新结构的有效无机合成方法。利用此方法，可以得到许多新颖，特殊结构的金属硫族化合物。 本文中，开发出了一条合成多元金属硫砷化合物的溶剂热合成路线。利用这条路线合成出了新颖的化合物[NH₃CH₂CH₂NH₃]AgAsS₄。该合成反应路线简单易操作，得到的产物纯，晶体质量好。 合成出来的化合物[NH₃CH₂CH₂NH₃]AgAsS₄，单晶结构分析属于单斜晶系，C2／c空间群，a=1.35805（8）nm，α=90°，b=0.65331（3）nnq，β=106.42（3）°，c=2.27711（9）nm，γ=90°，Z=8，V=1.93795（16）nm³，Dc=2.558g／cm³，μ=6.256mm^-1，F（000）=1440，R=0.0340，wR=0.0859。化合物具有有趣的一维无限链状结构，结构单元由[AgAsS₄]^2-与质子化的乙二胺构成。同时对该化合物还进行了SEM，IR，DSC-TGA表征。 对合成路线的影响因素进行了探讨，发现溶剂影响着合成反应。对于上述化合物最适合的乙醇／水体体积比为5／1～8／1，而当乙醇／水体积比为4／1时，则合成出了另外一种新的银的硫砷化合物。该合成路线有普遍的适用性，还可以用于合成其他金属的硫砷化合物。更多还原

【Abstract】 Chalcogenidometalates is one kind of inorganic multifunctional materials. The design and synthesis of the chalcogenidometalates have been motivated, and the study on novel structure of chalcogenidometalates is one important research in modern inorganic synthesis. Solventothermal (hydrothermal) synthesis technique is easy to synthesize new phases with novel structures, and some novel chalcogenideometalates can be produced by this techniques.In this thesis, a solventothermal synthetic route is developed successfully in synthesizing silver thioarsenate. In this method, a mixture of the ethanol and water (volume ratio 6:1), was used as solvent for the synthesis. This route is also characterized by mild reaction condition, and general utilty to synthesis of other chalcogenides.Well-formed yellow single crystal with light green color was obtained, this compound [NH3CH2CH2NH3]AgAsS4 crystallizes in the monoclinic system, space group C2/c; with a=1.35805(8)nm, a=90, b= 0.65331(3) nm, B= 106.42(3), c= 2.27711(9) nm, r= 90, Z=8, V=1.93795(16)nm3, Dc= 2.558g/cm3, u=6.256mm-1, F(000)= 1440, R=0.0340, wR=0.0859 The building block comprises of mainly [AgAsS4]2- and ethylenediammonium cations, and the total anion chain structure of crystal is similar to one ladder. The compound was also characterization by SEM, IR, DSC-TGA.Some key factors for the synthesis have been discussed, and the factor of solvent is the most important among these factors. The suitable volume ratio of ethanol and water for the mixture used in synthesis is from 5/1 to 8/1, while the ratio descends to 4/1, another new compound can be obtained. The synthetic route is applicable to synthesize other metal thioarsenates.更多还原