退火制备不同晶相WO_3的光催化降解性能研究
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摘要
采用水热法制备了正交相的WO_3·0.33H_2O纳米粉末,通过对水热产物在不同温度下进行真空退火1h后得到不同晶相的WO_3纳米粉末。对退火所得的不同的WO_3纳米粉末用X射线衍射、扫描电镜和拉曼光谱仪进行了晶相分析,微观形貌表征,化学键的表征。并且在紫外灯光照下,测试了通过退火所得不同晶相的WO_3纳米粉末对亚甲基蓝(MB)溶液的光催化降解效果,并通过脱色率公式对光催化降解效果进行了定量分析。结果表明,不同晶相的WO_3纳米粉末对MB溶液的光催化降解性能存在差异,其中不同晶相的WO_3纳米粉末对MB溶液的光催化降解效果由低至高为六方相<正交相<四方相,文中从晶体结构角度对此光催化降解的结果进行了分析。
Orthogonal WO_3·0.33H_2O nanopowders were prepared by hydrothermal method,and WO_3 nano materials with different crystalline phases were obtained by vacuum annealing of hydrothermal products at different temperatures for 1h.The obtained nano materials were characterized by X-ray diffraction,scanning electron microscopy and UV-Vis analysis.A methylene blue(MB)solution under UV irradiation was used to determine the photocatalytic activity of WO_3 photocatalyst with different crystalline phases.The effect of WO_3 with different crystalline phase on photocatalytic degradation of methylene blue under UV irradiation was investigated.Quantitative analysis of photocatalytic effect was carried out by degradation rate formula.The results of photocatalytic degradation test show that the photocatalytic degradation of WO_3 nanoparticles with different crystalline phases had different photocatalytic degradation performance in MB solution,and the photocatalytic degradation effect of WO_3 nanometers with different crystalline phases to MB solution ranged from low to high:hexagonal phase< orthorhombic phase< tetragonal phase.The results of photocatalytic degradation were analyzed in terms of crystal structure.
Orthogonal WO_3·0.33H_2O nanopowders were prepared by hydrothermal method,and WO_3 nano materials with different crystalline phases were obtained by vacuum annealing of hydrothermal products at different temperatures for 1h.The obtained nano materials were characterized by X-ray diffraction,scanning electron microscopy and UV-Vis analysis.A methylene blue(MB)solution under UV irradiation was used to determine the photocatalytic activity of WO_3 photocatalyst with different crystalline phases.The effect of WO_3 with different crystalline phase on photocatalytic degradation of methylene blue under UV irradiation was investigated.Quantitative analysis of photocatalytic effect was carried out by degradation rate formula.The results of photocatalytic degradation test show that the photocatalytic degradation of WO_3 nanoparticles with different crystalline phases had different photocatalytic degradation performance in MB solution,and the photocatalytic degradation effect of WO_3 nanometers with different crystalline phases to MB solution ranged from low to high:hexagonal phase< orthorhombic phase< tetragonal phase.The results of photocatalytic degradation were analyzed in terms of crystal structure.
引文
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[19]Zhou L,Zou J,Yu M M,et al.Green synthesis of hexagonal-shaped WO3·0.33H2O nanodiscs composed of nanosheets[J].Crystal Growth&Design,2008,8(11):3993-3998.
[20]Guéry C,Choquet C,Dujeancourt F,et al.Infrared and X-ray studies of hydrogen intercalation in different tungsten trioxides and tungsten trioxide hydrates[J].Journal of Solid State Electrochemistry,1997,1(3):199-207.
[21]Xie Y P,Liu G,Yin L,et al.Crystal facet-dependent photocatalytic oxidation and reduction reactivity of monoclinic WO3for solar energy conversion[J].Journal of Materials Chemistry,2012,22(14):6746-6751.
[2]Inoue Y.Photocatalytic water splitting by RuO2-loaded metal oxides and nitrides with d0-and d10-related electronic configurations[J].Energy and Environmental Science,2009,2(4):364-386.
[3]Bi Dongqin,Xu Yiming.Influence of iron oxide doping on the photocatalytic degradation of organic dye X3Bover tungsten oxide[J].Acta Phys-Chim Sin,2012,28(7):1777-1782(in Chinese).毕冬琴,许宜铭.Fe2O3掺杂对WO3光催化降解有机染料X3B的影响[J].物理化学学报,2012,28(7):1777-1782.
[4]Kumagai N,Matsuura Y,Kumagai N,et al.Kinetic and structural studies of the electrochemical insertion of lithium into hexagonal-type x(A2O)·WO3(A=Na+,K+,NH4+)[J].Journal of the Electrochemical Society,1992,139(12):3553-3558.
[5]Kumagai N,Yu A,Yashiro H.Thermodynamics and kinetics of electrochemical intercalation of lithium into Li0.50WO3.25,with a hexagonal tungsten bronze structure[J].Solid State Ionics,1997,98(3-4):159-166.
[6]Duncan J F,Kepert D L.Polyanion equilibria in aqueous solution.Part I.the quantitative analysis of acidified tungstate solutions[J].Journal of the Chemical Society,1961:5317-5325.
[7]Duncan J F,Kepert D L.Polyanion equilibria in aqueous solution.Part II.a thermodynamic study of the paratungstate A anion[J].Journal of the Chemical Society,1962,68(3):205-214.
[8]Chojnacka J.Application of isomatrix electromigration to the investigation of the condensation of WO42-ions[J].Journal of Inorganic&Nuclear Chemistry,1971,33(5):1345-1363.
[9]Xu Huili.Synthesis and characterization of transition metal oxide nanomaterials[D].Hangzhou:Zhejiang University,2007(in Chinese).许慧丽.过渡金属氧化物纳米材料的合成及其表征[D].杭州:浙江大学,2007.
[10]Mo Ruofei,Jin Guoqiang,Guo Xiangyun.Synthesis of monodisperse tungstic acid nanoparticles by UV irradiation method[J].Chinese Journal of Inorganic Chemstry,2008,24(1):111-116(in Chinese).莫若飞,靳国强,郭向云.紫外辐照法合成单分散钨酸纳米颗粒[J].无机化学学报,2008,24(1):111-116.
[11]Chang K H,Hu C C,Huang C M,et al.Microwave-assisted hydrothermal synthesis of crystalline WO3-WO3·0.5H2O mixtures for pseudocapacitors of the asymmetric type[J].Journal of Power Sources,2011,196(4):2387-2392.
[12]Shi J,Hu G,Cong R,et al.Controllable synthesis of WO3[round bullet,filled]nH2O microcrystals with various morphologies by a facile inorganic route and their photocatalytic activities[J].New Journal of Chemistry,2013,37(5):1538-1544.
[13]Peng Zhihong,Wu Xu,Zhou Qiusheng,et al.Preparation of ultrafine pyrochlore-type tungsten trioxide powder by hydrothermal method and its characterization[J].The Chinese Journal of Nonferrous Metals,2012,22(2):579-584(in Chinese).彭志宏,吴旭,周秋生,等.水热法制备超细焦绿石型三氧化钨及其表征[J].中国有色金属学报,2012,22(2):579-584.
[14]Gao X Q,Yang C,Xiao F,et al.WO3·0.33H2O nanoplates:hydrothermal synthesis,photocatalytic and gassensing properties[J].Materials Letters,2012,84:151-153.
[15]Frey G L,Rothschild A,Sloan J,et al.Investigations of nonstoichiometric tungsten oxide nanoparticles[J].Journal of Solid State Chemistry,2001,162(2):300-314.
[16]Zhang X,Lu X,Shen Y,et al.Three-dimensional WO3nanostructures on carbon paper:photoelectrochemical property and visible light driven photocatalysis[J].Chemical Communications,2011,47(20):5804-5806.
[17]Pecquenard B,Lecacheux H,Livage J,et al.Orthorhombic WO3formed via a Ti-stabilized WO3·{1/3}H2O phase[J].Journal of Solid State Chemistry France,1998,135(1):159-168.
[18]Sungpanich J,Thongtem T,Thongtem S.Photocatalysis of WO3 nanoplates synthesized by conventional-hydrothermal and microwave-hydrothermal methods and of commercial WO3 nanorods[J].Journal of Nanomaterials,2014,2014:131.
[19]Zhou L,Zou J,Yu M M,et al.Green synthesis of hexagonal-shaped WO3·0.33H2O nanodiscs composed of nanosheets[J].Crystal Growth&Design,2008,8(11):3993-3998.
[20]Guéry C,Choquet C,Dujeancourt F,et al.Infrared and X-ray studies of hydrogen intercalation in different tungsten trioxides and tungsten trioxide hydrates[J].Journal of Solid State Electrochemistry,1997,1(3):199-207.
[21]Xie Y P,Liu G,Yin L,et al.Crystal facet-dependent photocatalytic oxidation and reduction reactivity of monoclinic WO3for solar energy conversion[J].Journal of Materials Chemistry,2012,22(14):6746-6751.
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