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納米結(jié)構(gòu)氧化錫的離子熱合成及氣敏特性研究

發(fā)布時(shí)間:2019-03-01 07:24
【摘要】:SnO是一類p型半導(dǎo)體材料,因其廣泛的應(yīng)用而得到大量的關(guān)注,特別是其可作為制備n型半導(dǎo)體SnO2的前軀體。本論文提出一種簡單環(huán)保的離子熱途徑制備具有納米結(jié)構(gòu)的SnO粉體,對(duì)粉體的微觀結(jié)構(gòu)、形成機(jī)理以及退火獲得SnO2的結(jié)構(gòu)演變過程進(jìn)行了詳細(xì)表征,并分析了納米結(jié)構(gòu)氧化錫材料的微觀結(jié)構(gòu)與化學(xué)組成對(duì)氣敏特性的影響規(guī)律。以氯化膽堿與尿素構(gòu)成的深共熔溶劑(CU)作為反應(yīng)介質(zhì)和反應(yīng)物,在其中溶解SnCl2,通過調(diào)節(jié)反應(yīng)時(shí)間和水分含量,對(duì)SnO產(chǎn)物的微觀形貌進(jìn)行調(diào)控。在水量為1%的CU溶劑中,反應(yīng)時(shí)間為1 min時(shí)制備出顆粒大小為4-6 m的SnO顆粒;反應(yīng)時(shí)間為60 min時(shí),得到大小為1-1.5um的繡球狀SnO顆粒。當(dāng)CU溶劑中的含水量為5%和15%時(shí),SnO顆粒呈多層片狀,并且隨含水量增大,SnO顆粒構(gòu)成的納米片越少,比表面積更大。透射電子顯微鏡表明CU中水分含量的增加有助于SnO介晶的形成。對(duì)SnO介晶進(jìn)行退火,得到由正交相和四方相混合構(gòu)成的SnO2介晶結(jié)構(gòu),同時(shí)兩相的成分比例取決于退火溫度和反應(yīng)溶液中的水分含量。對(duì)復(fù)合相SnO2進(jìn)行氣敏性能測試,發(fā)現(xiàn)正交相SnO2含量較多的復(fù)合相SnO2材料具有較高的乙醇?xì)饷粜阅?并且對(duì)乙醇具有較高的選擇性。在制備SnO粉體的反應(yīng)體系中加入Co2+,獲得了Co304/Sn02復(fù)合的空心納米結(jié)構(gòu)。研究發(fā)現(xiàn)當(dāng)反應(yīng)溶液中的Co2-的濃度為0.01 molL-1時(shí),能制備出由正八面體和立方體混合的空心多面體結(jié)構(gòu)Sn02。當(dāng)Co2+的濃度為0.03molL-1和0.05molL-1時(shí),僅有少量多面體結(jié)構(gòu)生成。多面體結(jié)構(gòu)SnO2材料表現(xiàn)出較高的乙醇?xì)饷粜阅堋?br/>[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.
【學(xué)位授予單位】:浙江大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2015
【分類號(hào)】:TB383.1;O614.432

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