硫化锑微纳米材料的合成及其性能研究

发布时间：2018-06-27 18:15

本文选题：Sb2S3 + 海胆结构　；参考：《东北电力大学》2017年硕士论文

【摘要】：微纳米结构材料由于融合了微米材料和纳米材料的特点,在光学、电学、声学等诸多方面表现出独特的性能。而带隙窄,且能充分利用太阳光的硫化物半导体材料,在光催化领域受到了研究者的青睐。此外,石墨烯具有吸附能力强,具有大的比表面积,电子迁移率快等特点,可改善半导体光催化剂的光催化性。因此,制备具有协同效应的石墨烯/硫化物复合微纳米材料成为光催化材料领域的研究重点之一。本文的主要研究内容如下所述:(1)采用湿化学法,以酒石酸锑钾、硫代乙酰胺为原料,合成出由长约10μm,单根直径约100 nm的纳米棒组装成的海胆结构Sb2S3微纳米材料。系统探索了反应物摩尔比、反应时间和反应温度对产物形貌的影响。结果表明当酒石酸锑钾和硫代乙酰胺摩尔比为1:2,160℃油浴加热5 h,可合成出均一海胆结构的Sb2S3微纳米材料。根据晶体分裂机制,详细推测了海胆结构Sb2S3微纳米材料的生长机理,并对产物的光学性能进行了相关测试。(2)采用微波法,以酒石酸锑钾、硫脲为原料,合成出一维的管状Sb2S3微纳米材料,长约20μm,孔径约为2.5μm。系统探索了微波功率,反应物摩尔比、反应时间和反应温度对产物形貌的影响,结果表明当酒石酸锑钾和硫脲摩尔比为1:6,180℃微波加热3h,可制得均一形貌的管状结构Sb2S3微纳米材料。初步推测了管状结构Sb2S3微纳米材料的生长机理,并对其光学性能进行了测试。(3)采用改良的Hummers法制备了氧化石墨,并在湿化学法制备Sb2S3的基础上加入氧化石墨,以硼氢化钠(NaBH4)作还原剂进行化学还原,Sb2S3形成的同时氧化石墨也被还原成石墨烯(rGO)。X射线衍射分析确定材料的组成为斜方晶系Sb2S3与rGO。扫描电子显微镜显示材料中Sb2S3保持了原有的海胆结构形貌,同时石墨烯包裹在Sb2S3海胆结构外,形成石墨烯/硫化物复合结构。(4)以氙灯作为光源,亚甲基蓝为目标降解物,分别考察了上述两种结构以及相应的Sb2S3/石墨烯复合材料在可见光下的光催化活性。结果表明,采用海胆状Sb2S3作为光催化剂,当投加量为0.03 g时,降解30 mg/L的MB,在130 min内其降解率可达99.32%。管状Sb2S3光催化剂投加量为0.05 g时,降解50 mg/L的MB,在130 min内其降解率可达98.87%。此外,相比纯Sb2S3微纳米材料,在相同实验条件下Sb2S3/石墨烯复合材料达到相同降解效果时,降解时间缩短了50 min,表明复合材料具有更高效的光催化降解能力。
[Abstract]:Because of the characteristics of micronanomaterials and nanomaterials, micronanomaterials exhibit unique properties in many aspects, such as optics, electricity, and acoustics, which have a narrow band gap and can make full use of solar light sulphide semiconductors, which have been favored by researchers in the field of photocatalysis. In addition, graphene has a strong adsorption capacity and has a large capacity. The specific surface area and fast electron mobility can improve the photocatalytic activity of semiconductor photocatalyst. Therefore, the preparation of graphene / sulfide composite micronanomaterials with synergistic effects has become one of the key topics in the field of photocatalytic materials. The main contents of this paper are as follows: (1) using wet chemical method, antimony potassium tartrate, sulfur The synthesis of Sb2S3 micro nanomaterials composed of a nanorod with a length of about 10 m and a single diameter of about 100 nm was synthesized from acetamide. The effect of the molar ratio of reactants, reaction time and reaction temperature on the morphology of the products was systematically explored. The results showed that the molar ratio of antimony potassium tartrate and thioacetamide was 5 h at 1:2160 C for oil bath. Sb2S3 micro nanomaterials with homogeneous sea urchin structure were synthesized. According to the mechanism of crystal splitting, the growth mechanism of Sb2S3 micro nanomaterials in sea urchin structure was speculated and the optical properties of the products were tested. (2) a one-dimensional tubular Sb2S3 micro nanomaterial was synthesized by microwave method, using potassium antimony potassium tartrate and thiourea as raw material, which was about 20 m long. The effect of microwave power, molar ratio of reactant, reaction time and reaction temperature on the morphology of the product was explored. The results showed that the tubular structure Sb2S3 micro nano material could be prepared by microwave heating 3H at the molar ratio of antimony potassium tartrate and thiourea at 1:6180 C, and the tubular structure Sb2S3 micro nanomaterials were preliminarily speculated. The growth mechanism was tested and its optical properties were tested. (3) graphite oxide was prepared by improved Hummers method, and graphite oxide was added to Sb2S3 by wet chemical method. Sodium borohydride (NaBH4) was used as reducing agent for chemical reduction. The formation of Sb2S3 was also reduced to graphene (rGO).X ray diffraction analysis. The composition of the material is the trapezoid Sb2S3 and the rGO. scanning electron microscope. Sb2S3 maintains the original structure of the sea urchin, and the graphene is wrapped in the structure of the Sb2S3 sea urchin to form a composite structure of graphene / sulfide. (4) the xenon lamp is used as the light source and Ya Jiaji blue is the target degrading object, and the above two structures are investigated respectively. As well as the photocatalytic activity of the corresponding Sb2S3/ graphene composite under visible light, the results show that the degradation rate of 50 mg/L in the 130 min is degraded by the degradation rate of 30 mg/L MB when the dosage is 0.03 g, and the degradation rate of the 99.32%. tubular Sb2S3 photocatalyst is up to 0.05 g in 130 min. Up to 98.87%., compared with pure Sb2S3 micro nano materials, the degradation time of Sb2S3/ graphene composite has been reduced by 50 min under the same experimental conditions, which indicates that the composite has more efficient photocatalytic degradation ability.
【学位授予单位】：东北电力大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O614.531;TB383.1

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