纳米结构氧化锡的离子热合成及气敏特性研究
发布时间：2019-03-01 07:24
【摘要】：SnO是一类p型半导体材料,因其广泛的应用而得到大量的关注,特别是其可作为制备n型半导体SnO2的前躯体。本论文提出一种简单环保的离子热途径制备具有纳米结构的SnO粉体,对粉体的微观结构、形成机理以及退火获得SnO2的结构演变过程进行了详细表征,并分析了纳米结构氧化锡材料的微观结构与化学组成对气敏特性的影响规律。以氯化胆碱与尿素构成的深共熔溶剂(CU)作为反应介质和反应物,在其中溶解SnCl2,通过调节反应时间和水分含量,对SnO产物的微观形貌进行调控。在水量为1%的CU溶剂中,反应时间为1 min时制备出颗粒大小为4-6 m的SnO颗粒；反应时间为60 min时,得到大小为1-1.5um的绣球状SnO颗粒。当CU溶剂中的含水量为5%和15%时,SnO颗粒呈多层片状,并且随含水量增大,SnO颗粒构成的纳米片越少,比表面积更大。透射电子显微镜表明CU中水分含量的增加有助于SnO介晶的形成。对SnO介晶进行退火,得到由正交相和四方相混合构成的SnO2介晶结构,同时两相的成分比例取决于退火温度和反应溶液中的水分含量。对复合相SnO2进行气敏性能测试,发现正交相SnO2含量较多的复合相SnO2材料具有较高的乙醇气敏性能,并且对乙醇具有较高的选择性。在制备SnO粉体的反应体系中加入Co2+,获得了Co304/Sn02复合的空心纳米结构。研究发现当反应溶液中的Co2-的浓度为0.01 molL-1时,能制备出由正八面体和立方体混合的空心多面体结构Sn02。当Co2+的浓度为0.03molL-1和0.05molL-1时,仅有少量多面体结构生成。多面体结构SnO2材料表现出较高的乙醇气敏性能。
[Abstract]:SnO is a kind of p-type semiconductor material, which has attracted much attention because of its wide application. Especially, it can be used as the precursor of preparing n-type semiconductor SnO2. In this paper, a simple and environmentally friendly ion-thermal method is proposed to prepare nano-structured SnO powder. The microstructure, formation mechanism and structure evolution of SnO2 obtained by annealing are characterized in detail. The effects of microstructure and chemical composition on gas sensing properties of nano-structured tin oxide materials were also analyzed. The anatexic solvent (CU), composed of choline chloride and urea, was used as the reaction medium and reactant, in which the SnCl2, was dissolved by adjusting the reaction time and moisture content to regulate the micro-morphology of the SnO product. In CU solvent with water content of 1%, SnO particles with particle size of 4 渭 6 m were prepared when the reaction time was 1 min, and when the reaction time was 60 min, embroidered globular SnO particles with 1-1.5um size were obtained. When the water content in CU solvent is 5% and 15%, the SnO particles are multilayered, and the smaller the water content, the larger the specific surface area of SnO particles. Transmission electron microscopy (TEM) showed that the increase of moisture content in CU contributed to the formation of mesocrystalline SnO. The SnO mesocrystalline structure composed of orthogonal phase and tetragonal phase was obtained by annealing, and the proportion of the two phases depends on the annealing temperature and the water content in the reaction solution. The gas sensing properties of the composite phase SnO2 were tested. It was found that the composite phase SnO2 material with more SnO2 content in the orthogonal phase had higher ethanol gas sensitivity and higher selectivity to ethanol. The hollow nano-structure of SnO composite was obtained by adding Co2 into the reaction system of preparing Co304/Sn02 powder. It is found that when the concentration of Co2- in the reaction solution is 0.01molL- 1, the hollow polyhedral structure Sn02. with the mixture of regular octahedron and cube can be prepared. When the concentration of Co2 is 0.03molL-1 and 0.05 mol / L ~ (- 1), only a few polyhedral structures are formed. Polyhedral SnO2 exhibits high ethanol gas sensitivity.
【学位授予单位】：浙江大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TB383.1;O614.432
本文编号：2432207
[Abstract]:SnO is a kind of p-type semiconductor material, which has attracted much attention because of its wide application. Especially, it can be used as the precursor of preparing n-type semiconductor SnO2. In this paper, a simple and environmentally friendly ion-thermal method is proposed to prepare nano-structured SnO powder. The microstructure, formation mechanism and structure evolution of SnO2 obtained by annealing are characterized in detail. The effects of microstructure and chemical composition on gas sensing properties of nano-structured tin oxide materials were also analyzed. The anatexic solvent (CU), composed of choline chloride and urea, was used as the reaction medium and reactant, in which the SnCl2, was dissolved by adjusting the reaction time and moisture content to regulate the micro-morphology of the SnO product. In CU solvent with water content of 1%, SnO particles with particle size of 4 渭 6 m were prepared when the reaction time was 1 min, and when the reaction time was 60 min, embroidered globular SnO particles with 1-1.5um size were obtained. When the water content in CU solvent is 5% and 15%, the SnO particles are multilayered, and the smaller the water content, the larger the specific surface area of SnO particles. Transmission electron microscopy (TEM) showed that the increase of moisture content in CU contributed to the formation of mesocrystalline SnO. The SnO mesocrystalline structure composed of orthogonal phase and tetragonal phase was obtained by annealing, and the proportion of the two phases depends on the annealing temperature and the water content in the reaction solution. The gas sensing properties of the composite phase SnO2 were tested. It was found that the composite phase SnO2 material with more SnO2 content in the orthogonal phase had higher ethanol gas sensitivity and higher selectivity to ethanol. The hollow nano-structure of SnO composite was obtained by adding Co2 into the reaction system of preparing Co304/Sn02 powder. It is found that when the concentration of Co2- in the reaction solution is 0.01molL- 1, the hollow polyhedral structure Sn02. with the mixture of regular octahedron and cube can be prepared. When the concentration of Co2 is 0.03molL-1 and 0.05 mol / L ~ (- 1), only a few polyhedral structures are formed. Polyhedral SnO2 exhibits high ethanol gas sensitivity.
【学位授予单位】：浙江大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TB383.1;O614.432
【参考文献】
相关期刊论文 前6条
1 田立强,潘国峰,赵彦晓,王静,孙以材;TiO_2薄膜氧敏元件的研究与发展[J];传感器世界;2002年07期
2 常剑,蒋登高,詹自力,宋文会;半导体金属氧化物气敏材料敏感机理概述[J];传感器世界;2003年08期
3 徐甲强,闫冬良,王国庆,田志壮,江青萍;WO_3基H_2S气敏材料的研究[J];硅酸盐学报;1999年05期
4 石家华,孙逊,杨春和,高青雨,李永舫;离子液体研究进展[J];化学通报;2002年04期
5 周雅文;邓宇;尚海萍;韩德新;;离子液体的性质及其应用[J];杭州化工;2009年03期
6 张丽萍;;气敏传感器研究新进展[J];吉林工商学院学报;2012年02期
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