纳米结构V2O5空心微球的制备与表征

doi:10.3724/SP.J.1077.2008.00043

无机材料学报

纳米结构V₂O₅空心微球的制备与表征

朱丁, 刘恒, 姚亚东, 李大成

四川大学材料科学与工程学院, 成都 610064

收稿日期:2007-01-12 修回日期:2007-07-30 出版日期:2008-01-20 网络出版日期:2008-01-20

Fabrication and Characterization of Nanostructural Vanadium Pentoxide Hollow Microspheres

ZHU Ding, LIU Heng, YAO Ya-Dong, LI Da-Cheng

College of Materials Science and Engineering, SiChuan University, Chengdu 610064, China

Received:2007-01-12 Revised:2007-07-30 Published:2008-01-20 Online:2008-01-20

摘要/Abstract

摘要： 以自制的二乙酰丙酮氧钒(VO(aca)₂)为原料, 通过软模板法组装出聚乙烯吡咯烷酮(PVP)/钒前驱体核壳结构的复合微球. 对复合微球进行热处理后制备得φ(0.5～1.0)μm五氧化二钒(V₂O₅) 中空微球. 分别采用扫描电镜(SEM)、透射电镜(TEM)和X射线衍射仪(XRD)对最终产物的球形外观、中空结构和物相组成进行了表征, 结合VO(acac)₂、溶解于乙二醇的PVP、溶解于乙二醇的VO(acac)₂与复合微球的红外光谱(FTIR)和复合微球的差热曲线(DTA), 探讨了V₂O₅中空微球形成的机理. 对影响实验的因素如PVP和VO(acac)₂的浓度、保温时间等进行了研究. 结果表明: 通过严格控制PVP和VO(acac)₂的浓度能够确保V₂O₅球壳结构的形成; 当总反应时间在75～90min范围内时, 所得空心球的几何外形和表面形貌均较为理想.

关键词: 模板自组装, PVP/钒前驱体复合微球, V₂O₅, 空心微球

Abstract: Polyvinylpyrrolidone(PVP)/vanadyl glycolate (VO(OCH2-CH2O)) core-shell microspheres were assembled by soft-templating method using vanadyl acetylacetone (VO(acac₂) as raw materials. And then vanadium pentoxide (V₂O₅) hollow spheres with particle size from 0.5 to 1μm were obtained by the calcination of composite microspheres. SEM, TEM and XRD were adopted to characterize the spherical morphology, hollow structure and phase composition of the final product, respectively. The mechanism of the formation of V₂O₅ hollow spheres was discussed based on the FTIR of VO(acac)₂, PVP dissolved in EG, VO(acac)2 dissolved in EG, VO(OCH₂-CH₂O)/PVP microspheres and the DTA curve of composite microspheres. Effects of concentration of reagents, the time of reaction on the experiment were studied. The results indicate that the core-shell composite microspheres can be prepared through the precise control of the concentration of PVP and VO(acac)₂, and the microspheres will be formed with ideal shape and surface morphology with reaction time ranging from 75min to 90min.

Key words: templating self-assembly, PVP/vanadium precursor composite microspheres, V₂O₅, hollow microspheres

中图分类号:

TB321

朱丁,刘恒,姚亚东,李大成. 纳米结构V₂O₅空心微球的制备与表征[J]. 无机材料学报, DOI: 10.3724/SP.J.1077.2008.00043.

ZHU Ding,LIU Heng,YAO Ya-Dong,LI Da-Cheng. Fabrication and Characterization of Nanostructural Vanadium Pentoxide Hollow Microspheres[J]. Journal of Inorganic Materials, DOI: 10.3724/SP.J.1077.2008.00043.

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纳米结构V₂O₅空心微球的制备与表征

Fabrication and Characterization of Nanostructural Vanadium Pentoxide Hollow Microspheres

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