溶膠—凝膠法制備納米ATO粉體和薄膜及其結(jié)構(gòu)與性能的研究
發(fā)布時間:2018-04-01 10:10
本文選題:sol-gel法 切入點(diǎn):納米ATO粉體和薄膜 出處:《蘭州理工大學(xué)》2011年碩士論文
【摘要】:二氧化錫(SnO_2)是一種具有直接帶隙的寬禁帶N型半導(dǎo)體材料,300K時其禁帶寬度為3.62eV,室溫下電阻率較高,當(dāng)產(chǎn)生氧空位或摻雜元素后形成N型半導(dǎo)體,具有導(dǎo)電性能。銻摻雜二氧化錫(Antimony doped Tin Oxide, ATO)作為透明導(dǎo)電薄膜由于具有優(yōu)良的導(dǎo)電性能、光學(xué)性能、穩(wěn)定性好和靈敏度高等優(yōu)點(diǎn),廣泛應(yīng)于太陽能電池、電致變色材料、防輻射抗靜電材料、氣敏元件、電極材料等方面。 以SnCl_4·5H_2O和SbCl_3為主要原料,采用溶膠-凝膠(sol-gel)法制備了球形納米ATO粉末。分別用XRD、FTIR、XPS、FESEM及四探針電阻率/方阻測試儀對粉體的晶體結(jié)構(gòu)、元素組成、表面形貌和粉末電阻進(jìn)行了表征和分析,系統(tǒng)考察了煅燒溫度、煅燒時間和Sb摻雜量對ATO粉末晶體結(jié)構(gòu)、晶粒尺寸、形貌和導(dǎo)電性能的影響。 采用sol-gel旋涂法,以SnCl_4和SbCl_3為主要原料,制得了光、電性能優(yōu)良的納米ATO薄膜。分別利用XRD、FESEM、紫外/可見分光光度計、熒光光譜儀及四探針電阻率/方阻測試儀對薄膜的晶體結(jié)構(gòu)、表面形貌、光透過率、光致發(fā)光性能和方塊電阻進(jìn)行了分析表征,系統(tǒng)考察了無水乙醇的加入量、溶劑的種類、超純水的加入量、煅燒溫度、Sb摻雜量和薄膜厚度對ATO薄膜結(jié)構(gòu)及其光、電性能的影響。 XRD結(jié)果表明所制得的ATO為(110)面擇優(yōu)取向的四方相錫石結(jié)構(gòu)的納米顆粒,沒有出現(xiàn)銻的氧化物的峰,說明Sb的摻雜并沒有改變SnO_2的晶體結(jié)構(gòu),所有的Sb離子進(jìn)入到SnO_2晶格中取代了部分的Sn離子,形成了固溶體。確定了ATO納米粉體的最佳制備條件:Sb摻雜量為15 mol%,所得前軀體在1000℃煅燒3.0 h。所得ATO納米粉體的壓片電阻率最小為10.18Ω·cm。 納米ATO薄膜的最佳制備條件為:Sb摻雜量為10 mol%,加入2倍理論量的無水乙醇作溶劑,再滴加1.5倍理論量的超純水,涂膜5次在650℃煅燒2.0 h。所得淡藍(lán)色納米ATO薄膜的綜合性能最佳,膜厚為787.5 nm左右,方塊電阻率為60.1Ω/□,可見光透過率大于80%,且具有熒光性能。最后,探討并提出了sol-gel法制備ATO可能的反應(yīng)機(jī)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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