溶胶—凝胶法制备纳米ATO粉体和薄膜及其结构与性能的研究

发布时间：2018-04-01 10:10

  本文选题：sol-gel法　切入点：纳米ATO粉体和薄膜　出处：《兰州理工大学》2011年硕士论文

【摘要】：二氧化锡(SnO_2)是一种具有直接带隙的宽禁带N型半导体材料,300K时其禁带宽度为3.62eV,室温下电阻率较高,当产生氧空位或掺杂元素后形成N型半导体,具有导电性能。锑掺杂二氧化锡(Antimony doped Tin Oxide, ATO)作为透明导电薄膜由于具有优良的导电性能、光学性能、稳定性好和灵敏度高等优点,广泛应于太阳能电池、电致变色材料、防辐射抗静电材料、气敏元件、电极材料等方面。 以SnCl_4·5H_2O和SbCl_3为主要原料,采用溶胶-凝胶(sol-gel)法制备了球形纳米ATO粉末。分别用XRD、FTIR、XPS、FESEM及四探针电阻率/方阻测试仪对粉体的晶体结构、元素组成、表面形貌和粉末电阻进行了表征和分析,系统考察了煅烧温度、煅烧时间和Sb掺杂量对ATO粉末晶体结构、晶粒尺寸、形貌和导电性能的影响。 采用sol-gel旋涂法,以SnCl_4和SbCl_3为主要原料,制得了光、电性能优良的纳米ATO薄膜。分别利用XRD、FESEM、紫外/可见分光光度计、荧光光谱仪及四探针电阻率/方阻测试仪对薄膜的晶体结构、表面形貌、光透过率、光致发光性能和方块电阻进行了分析表征,系统考察了无水乙醇的加入量、溶剂的种类、超纯水的加入量、煅烧温度、Sb掺杂量和薄膜厚度对ATO薄膜结构及其光、电性能的影响。 XRD结果表明所制得的ATO为(110)面择优取向的四方相锡石结构的纳米颗粒,没有出现锑的氧化物的峰,说明Sb的掺杂并没有改变SnO_2的晶体结构,所有的Sb离子进入到SnO_2晶格中取代了部分的Sn离子,形成了固溶体。确定了ATO纳米粉体的最佳制备条件:Sb掺杂量为15 mol%,所得前躯体在1000℃煅烧3.0 h。所得ATO纳米粉体的压片电阻率最小为10.18Ω·cm。 纳米ATO薄膜的最佳制备条件为:Sb掺杂量为10 mol%,加入2倍理论量的无水乙醇作溶剂,再滴加1.5倍理论量的超纯水,涂膜5次在650℃煅烧2.0 h。所得淡蓝色纳米ATO薄膜的综合性能最佳,膜厚为787.5 nm左右,方块电阻率为60.1Ω/□,可见光透过率大于80%,且具有荧光性能。最后,探讨并提出了sol-gel法制备ATO可能的反应机理。
[Abstract]:SnO _ 2) is a wide bandgap N-type semiconductor material with a direct band gap of 3.62 EV at 300K. The resistivity is high at room temperature. When oxygen vacancies or doped elements are produced, N-type semiconductors are formed. Antimony doped doped doped Tin oxide (ATO) is widely used in solar cells and electrochromic materials because of its excellent conductive properties, optical properties, good stability and high sensitivity. Anti-radiation anti-static materials, gas sensors, electrode materials and so on. Spherical nanometer ATO powders were prepared by sol-gel method using SnCl_4 5H_2O and SbCl_3 as main raw materials. The crystal structure and elemental composition of the powders were characterized by X-ray diffraction FTIR FE-SEM and four-probe resistivity / square resistance tester, respectively. The effects of calcination temperature, calcination time and SB doping amount on the crystal structure, grain size, morphology and conductivity of ATO powder were investigated. Nanocrystalline ATO thin films were prepared by sol-gel spin-coating method using SnCl_4 and SbCl_3 as main raw materials. The crystal structure, surface morphology, photoluminescence, photoluminescence and square resistance of the films were characterized by fluorescence spectrometer and four-probe resistivity / square resistance tester. The amount of anhydrous ethanol and the kinds of solvents were systematically investigated. The effects of the addition amount of ultra-pure water, calcination temperature and SB doping amount and film thickness on the structure, optical and electrical properties of ATO thin films were investigated. The XRD results show that the prepared ATO is tetragonal cassiterite nanoparticles with preferred orientation on the ATO (110) plane, and there is no peak of antimony oxide, indicating that SB doping does not change the crystal structure of SnO_2. All SB ions enter the SnO_2 lattice and replace some of the Sn ions. A solid solution was formed. The optimum preparation conditions of ATO nano-powders were determined as follows: the doping amount of ATO was 15 mol / mol, and the precursor was calcined at 1000 鈩，

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