离子液体中纳米氧化铟、氧化锡和ITO粉末的制备及性能研究
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摘要
离子液体由于具有一些优异性能,如可忽略的蒸汽压、低熔点、很宽的液相温度、低毒性、不燃性、很宽的电势窗和对有机物及无机物良好的溶解性等,而广泛应用于化学合成、分离和电化学等方面。在无机领域,从离子液体中合成微/纳米材料的研究已经获得一些突破,引起国内外科学研究者的广泛关注。本论文中,通过微波加热的方式,在室温离子液体中制备了纳米氧化铟、氧化锡和氧化铟锡粉末材料,提出了一种无机纳米材料新的制备方法。
对制备的纳米粉末材料采用X射线衍射(XRD)、差示扫描量热(DSC)、傅里叶红外分析光谱(FT-IR)、紫外.可见分析光谱(UV-Vis)和电泳测试(Zeta电位)及电阻率性能测试等手段进行了分析和表征,结果表明:氧化铟为立方型结构,粒径在31.4nm,氧化锡为四方型结构,粒径在21.0nm,ITO粉末为立方铁锰矿结构,粒径在21.6nm;DSC测试发现氧化铟的前驱物比较接近与氧化铟本体,氧化锡粉末为单—晶型,没有晶型的转化,ITO粉末材料的晶型完全转化温度在480℃;Zeta电位测试表明氧化铟在pH=2.6处和pH=9.8处有两个等电点,氧化锡pH=3.1处、pH=8.9处和pH值=10.2处有三个等电点;光谱性能测试表明氧化铟出现部分红移现象,氧化锡的光学带隙变窄,ITO粉末的在可见光区平均透过率88%以上;电学性能测试表明制备的三种纳米材料的电阻均随着热处理温度的升高而降低。
Room Temperature Ionic Liquids (RTILs) have been widely used in the organic chemical reactions, separations, and electrochemical for their negligible vapor pressure, low melting points, wide range of liquid temperatures, low toxicity, non-flammability, large electrochemical window, good solvents for many organic and inorganic materials, high ionic conductively and thermal stability. In contrast to their successful applications in organic and materials chemistry, the use of RTILs in micro-nanostructres synthesis has acquire some success, and has brought more attention of scientists .In this paper, nanometer indium oxide, tin dioxide and ITO powder were prepared in ionic liquids with the assistant of microwave heating, which was a new way of preparation of inorganic nanomaterials .
The powders of the nanomaterial were analyzed and characterized by XRD, DSC, FT-IR, UV-Vis , Zeta potential and electrical performance, the results showed that: Indium oxide has the cubic structure, and size of particle is 31.4 nm, tin dioxide has the square structure, size of the particle is 21.0 nm, while the ITO powder for the cubic structure of iron, 21.6 nm in diameter; DSC showed that the precursor of indium and indium oxide close to the body, tin dioxide powder is a single crystal without crystal transformation, and the ITO powder fully transformant crystal temperature needs above 480℃; Zeta potential showed that the indium oxide material has two equipotential points at the pH = 2.6 and the pH = 9.8, while the tin dioxide material has three equipotential points at pH = 3.1, pH = 8.9 and the pH = 10.2; Optical performance showed that indium oxide displays part of a red shift, and the tin dioxide band gap becomes narrows, the ITO powder showed 88 percent above the average transmittance at visible light distrect; Electrical performance showed that the resistance of the three powders become lower while temperature increased.
对制备的纳米粉末材料采用X射线衍射(XRD)、差示扫描量热(DSC)、傅里叶红外分析光谱(FT-IR)、紫外.可见分析光谱(UV-Vis)和电泳测试(Zeta电位)及电阻率性能测试等手段进行了分析和表征,结果表明:氧化铟为立方型结构,粒径在31.4nm,氧化锡为四方型结构,粒径在21.0nm,ITO粉末为立方铁锰矿结构,粒径在21.6nm;DSC测试发现氧化铟的前驱物比较接近与氧化铟本体,氧化锡粉末为单—晶型,没有晶型的转化,ITO粉末材料的晶型完全转化温度在480℃;Zeta电位测试表明氧化铟在pH=2.6处和pH=9.8处有两个等电点,氧化锡pH=3.1处、pH=8.9处和pH值=10.2处有三个等电点;光谱性能测试表明氧化铟出现部分红移现象,氧化锡的光学带隙变窄,ITO粉末的在可见光区平均透过率88%以上;电学性能测试表明制备的三种纳米材料的电阻均随着热处理温度的升高而降低。
Room Temperature Ionic Liquids (RTILs) have been widely used in the organic chemical reactions, separations, and electrochemical for their negligible vapor pressure, low melting points, wide range of liquid temperatures, low toxicity, non-flammability, large electrochemical window, good solvents for many organic and inorganic materials, high ionic conductively and thermal stability. In contrast to their successful applications in organic and materials chemistry, the use of RTILs in micro-nanostructres synthesis has acquire some success, and has brought more attention of scientists .In this paper, nanometer indium oxide, tin dioxide and ITO powder were prepared in ionic liquids with the assistant of microwave heating, which was a new way of preparation of inorganic nanomaterials .
The powders of the nanomaterial were analyzed and characterized by XRD, DSC, FT-IR, UV-Vis , Zeta potential and electrical performance, the results showed that: Indium oxide has the cubic structure, and size of particle is 31.4 nm, tin dioxide has the square structure, size of the particle is 21.0 nm, while the ITO powder for the cubic structure of iron, 21.6 nm in diameter; DSC showed that the precursor of indium and indium oxide close to the body, tin dioxide powder is a single crystal without crystal transformation, and the ITO powder fully transformant crystal temperature needs above 480℃; Zeta potential showed that the indium oxide material has two equipotential points at the pH = 2.6 and the pH = 9.8, while the tin dioxide material has three equipotential points at pH = 3.1, pH = 8.9 and the pH = 10.2; Optical performance showed that indium oxide displays part of a red shift, and the tin dioxide band gap becomes narrows, the ITO powder showed 88 percent above the average transmittance at visible light distrect; Electrical performance showed that the resistance of the three powders become lower while temperature increased.
引文
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[19]Yongzhong Wu,Xiaopeng Hao.Ultrasound-assisted synthesis of nanocrystalline ZnS in the ionic liquid[BMIM]BF_4[J].Materials Letters,2006(23):519-522
[20]杨振兴,王广健,刘义武.室温离子液体在无机纳米材料合成中的应用[J].淮北煤炭师范学院学报(自然科学版),2006,27(4):21-28
[21]刘浪,俞建伟.超细氢氧化铟的研制[J].广东化工,2003,2:8-9
[22]庄子栋,李延生.沉淀法制备氧化铟锡超细材料的研究进展[J].山西化工,2005,25(3):1-5
[23]段学臣,陈振华.超细In_2O_3粉末的研制[J].粉末冶金技术,2007,15(6):52-54
[24]裴小苗,司文元,刘欣,等.超声场中溶胶凝胶法制备纳米氧化铝粉体的研究[J].金刚石与磨料磨具工程,2005,6:71-74
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[30]赵杰,赵经贵,高山,等.SnO_2纳米薄膜的制备,显微结构及气敏性能[J].应用化学,2004,21(2):122-125
[31]阎军锋,何崇斌,张志勇,等.MOPECVD法制备超微颗粒SnO_2薄膜[J].西北大学学报,2000,30(3):185-188
[32]LIU Ying,KOEP E,LIU Mei-lin.A highly sensitive and fastresponding SnO_2 sensor fabricated by combustion chemical vapor deposition[J].Chem Mater,2005,17(6):3997-4000
[33]Fujihara S,Maeda T,Ohgi H,et al.Hydrothermal routes to prepare nanocrystalline mesoporous SnO_2 having high thermal stability[J].Langmuir,2004,20(15):6476-6481
[34]Chen D I,Gao L.Facile synthesis of single-crystal tin oxide nanorods with tunable dimensions via hydrotherm alprocess[J].Chem,Phys,Lett,2007,398(1-3):201-206
[35]Tanaka S,EsakaT.High Nox sensitivity of oxide thin films prepared by RF sputtering [J].Materials Research Bullitin,2000,35(14-15):2491-2502
[36]Sberveglieri G,FagliaagG,Garoppelli S.A new technique for preparing SnO_2 sputtered thin films as gas sensor.Proe 6th Int.Conf Solid-state Sensors and Actuators(Transducers 1),San Francisco,CA,USA,June 23-27,2006,165
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