低温溶剂热法制备新型四元二维含砷硫属化合物及其物理性能研究
发布时间：2019-04-24 08:38
【摘要】：多元硫属化合物是一类结构非常丰富的半导体材料,具有优良的物理化学性能,在非线性光学、光催化、太阳能电池等领域具有广泛的应用。因此,它们的合成研究已经成为目前无机化学合成方向的一个十分活跃的研究领域。近年来,因为含砷的硫属化合物具有新颖的结构类型和潜在的应用前景,吸引了越来越多人的关注。众所周知,表面活性剂具有蒸气压较低、热稳定性高、价格便宜等优点,且能够调节纳米晶体的尺寸、表面能、物理性质,以及调控多孔框架结构内部孔的尺寸等,在纳米晶和多孔框架材料的制备合成方面应用广泛,但其应用在制备合成新型多元硫属化合物方面的报道研究相对较少。本文以表面活性剂配合有机胺作为反应介质,通过对反应条件(反应物的种类及用量、溶剂种类和用量、反应温度、反应时间等因素)进行调控,成功制备出6种新型四元含砷的硫属化合物Cs3CuAs4S8(1)、Cs3CuAs4Se8(2)、NaAg2AsS3·H2O(3)、KAg2AsS3(4)、Cs2Ag2As2S5(5)和 Cs3AgAs4S8(6),该工艺过程简单,易于操作,且制得目标产物产率较高,晶体质量较好。通过SEM、EDS、单晶X射线衍射、XRD、UV、TG及理论计算等手段,对化合物进行结构与性能表征分析。发现这6种硫属化合物都具有二维层状的结构,且除化合物NaAg2AsS3·H20是间接带隙半导体材料外其他均为直接带隙半导体材料。
[Abstract]:Multi-sulfur compounds are a kind of semiconductor materials with very rich structure and have excellent physical and chemical properties. They are widely used in nonlinear optics, photocatalysis, solar cells and other fields. Therefore, their synthesis has become a very active research field in the direction of inorganic synthesis. In recent years, arsenic-containing sulfur compounds have attracted more and more attention because of their novel structural types and potential application prospects. It is well known that surfactants have the advantages of low vapor pressure, high thermal stability and low price, and can adjust the size of nanocrystals, surface energy, physical properties, and the size of pores in porous frame structure, etc. It has been widely used in the preparation and synthesis of nanocrystals and porous frame materials, but there are relatively few reports on the preparation and synthesis of new multi-element thiosulfide compounds. In this paper, surfactant and organic amine were used as the reaction medium, and the reaction conditions (such as the type and dosage of reactant, the type and amount of solvent, the reaction temperature, the reaction time and so on) were adjusted and controlled. Six new quaternary thiosulfide compounds Cs3CuAs4S8 (1), Cs3CuAs4Se8 (2), NaAg2AsS3 路H2O (3), KAg2AsS3 (4), Cs2Ag2As2S5 (5) and Cs3AgAs4S8 (6) were prepared successfully. The process is simple and easy to operate, and the yield of the target products is high. The crystal is of good quality. The structure and properties of the compounds were characterized by SEM,EDS, single crystal X-ray diffraction, XRD,UV,TG and theoretical calculation. It was found that the six thiosulfide compounds all have two-dimensional layered structures, and all of them are direct band-gap semiconductor materials except the compound NaAg2AsS3 路H _ 20 is an indirect band-gap semiconductor material.
【学位授予单位】：浙江大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O649
本文编号：2464307
[Abstract]:Multi-sulfur compounds are a kind of semiconductor materials with very rich structure and have excellent physical and chemical properties. They are widely used in nonlinear optics, photocatalysis, solar cells and other fields. Therefore, their synthesis has become a very active research field in the direction of inorganic synthesis. In recent years, arsenic-containing sulfur compounds have attracted more and more attention because of their novel structural types and potential application prospects. It is well known that surfactants have the advantages of low vapor pressure, high thermal stability and low price, and can adjust the size of nanocrystals, surface energy, physical properties, and the size of pores in porous frame structure, etc. It has been widely used in the preparation and synthesis of nanocrystals and porous frame materials, but there are relatively few reports on the preparation and synthesis of new multi-element thiosulfide compounds. In this paper, surfactant and organic amine were used as the reaction medium, and the reaction conditions (such as the type and dosage of reactant, the type and amount of solvent, the reaction temperature, the reaction time and so on) were adjusted and controlled. Six new quaternary thiosulfide compounds Cs3CuAs4S8 (1), Cs3CuAs4Se8 (2), NaAg2AsS3 路H2O (3), KAg2AsS3 (4), Cs2Ag2As2S5 (5) and Cs3AgAs4S8 (6) were prepared successfully. The process is simple and easy to operate, and the yield of the target products is high. The crystal is of good quality. The structure and properties of the compounds were characterized by SEM,EDS, single crystal X-ray diffraction, XRD,UV,TG and theoretical calculation. It was found that the six thiosulfide compounds all have two-dimensional layered structures, and all of them are direct band-gap semiconductor materials except the compound NaAg2AsS3 路H _ 20 is an indirect band-gap semiconductor material.
【学位授予单位】：浙江大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O649
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