电化学方法制备纳米NiO及反应机理初探

电化学（中英文） ›› 2002, Vol. 8 ›› Issue (4): 427-432.

电化学方法制备纳米NiO及反应机理初探

顾家山,韩爱杰,周幸福,褚道葆,林昌健

安徽师范大学化学与材料科学学院有机化学研究所,安徽师范大学化学与材料科学学院有机化学研究所,安徽师范大学化学与材料科学学院有机化学研究所,安徽师范大学化学与材料科学学院有机化学研究所,厦门大学固体表面物理化学国家重点实验室安徽芜湖241000 ,安徽芜湖241000 ,安徽芜湖241000 ,安徽芜湖241000 ,福建厦门361005

收稿日期:2002-11-28 修回日期:2002-11-28 出版日期:2002-11-28 发布日期:2002-11-28

Electrochemical Preparation and Reaction Mechanism of Nanocrystalline NiO

GU Jia-shan 1, HAN Ai-jie 1, ZHOU Xing-fu 1 , CHU Dao-bao 1* , LIN Chang-jian 2

(1.College of Chemistry and Materials Science, Anhui Normal University, Wuhu 241000, 2.State Key Laboratory for Physics Chemistry of Solid Surfaces, Xiamen University, Xiamen 361005, China

Received:2002-11-28 Revised:2002-11-28 Published:2002-11-28 Online:2002-11-28

摘要/Abstract

摘要： 采用电化学法一步制备了镍醇盐配合物Ni(OEt) 2 (acac) 2 (acac为乙酰丙酮基 ) ,并以其作为前驱体 ,控制一定水解条件制得胶体 ,分别在 4 5 0℃ ,60 0℃煅烧均得到具有立方晶型的纳米NiO粉体 .通过红外光谱 (FT_IR)、核磁共振 (1HNMR)、拉曼光谱 (Ramanspectrum)、X_射线粉末衍射 (XRD)、透射电子显微镜 (TEM)等手段对前驱体和NiO粉体进行了表征 .结果表明 ,电解合成的最佳温度为 30～ 4 0℃ ,不溶性镍醇盐配合物升温到 4 0～ 5 0℃即可溶解 .电解法制备得到的纳米NiO层呈球形单分散结构 ,粒径在 10～ 15nm左右 .本文同时讨论了电合成纳米NiO的反应机理

关键词: 电化学, 溶胶-凝胶, 纳米NiO

Abstract: Metallic nickel was electrochemically dissolved in absolute ethanol and acetylacetone mixed solutions and in the presence of Bu 4NBr (as an electron-conductive additive). The electrolyte solution containing the precursor was then directly hydrolyzed to obtain nanocrystalline NiO. The precursor was characterized by FTIR?HNMR?Raman spectra and the nano-powder was characterized by XRD and TEM. The results showed that the NiO powder after calcined at 450 ℃ had formed the cubic NaCl structure and the nanocrystalline NiO prepared by this method had narrow size distribution of 10～15 nm. Moreover, the product yield could be improved by controlling temperature below 30～40 ℃. The reaction mechanism was also discussed in this paper.

Key words: Electrochemistry, Sol-gel, Nano-sized NiO

中图分类号:

O646

顾家山,韩爱杰,周幸福,褚道葆,林昌健. 电化学方法制备纳米NiO及反应机理初探[J]. 电化学（中英文）, 2002, 8(4): 427-432.

GU Jia-shan 1, HAN Ai-jie 1, ZHOU Xing-fu 1 , CHU Dao-bao 1* , LIN Chang-jian 2 . Electrochemical Preparation and Reaction Mechanism of Nanocrystalline NiO[J]. Journal of Electrochemistry, 2002, 8(4): 427-432.

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链接本文: https://electrochem.xmu.edu.cn/CN/

https://electrochem.xmu.edu.cn/CN/Y2002/V8/I4/427

参考文献

[1]　GabrRM ,El_NaimiAN ,Al_ThaniM .G .Effectofthermaltreatmentonthekineticsandsinteringcharac teristicsofnickelhydroxideasaprecursorforthethermalgenesisofnickeloxidecatalyst[J].ThermochimicaActa,1992,197:307～318. [2]　ChristrosfovaStG ,DanovaN ,GeorgievaM ,etal.Investigationofanickeloxidesystemforheterogeneousoxidationoforganiccompounds[J].AppliedCatalysisA :General,1995,128:219～229. [3]　Ken_ichiroOta,ShigenoriMitsushima,ShigemiKato,etal.Solubilitiesofnickeloxideinmoltencarbonate[J].J.Electrochem.Soc.,1992,139(3):667～671. [4]　VarkeyAJ ,FortAF .Solutiongrowthtechniquefordepositionofnickeloxidethinfilims[J].ThinSolidFlims,1993,235:47～50. [5]　MasayaChigane,Masamllshikawa.Characterizationofelectrochromicnickeloxidethinfilmpreparedbyan odicdeposition[J].J.Chem.Soc.Faradaytrans.,1992,88(15):2203～2205. [6]　XiaofengChen,XingfangHu,JingweiFeng.Nanostructurednickeloxidefilmsandtheirelectrochromicproperities[J].Nanostructuredmaterials,1995,6:309～312. [7]　YoshiyukiSato,ShigeharuTamura,KensukeMurai.Electrochromicpropertiesofnickeloxidefilmspreparedbytheoxidationofnickel_carboncompositefilms[J].J .Appl.Phys.,1996,35(12A):6275～6279. [8]　Kuo_ChuanLiu,MarcA .AndersonPorousnickeloxide/nickelfilmsforelectrochemicalcapacitors[J].J .Elec trochem.Soc.,1996,143(1):124～130. [9]　VenkatSrinivasan,JohnW .WeidnerAnelectrochemicalrouteformakingporousnickeloxideelectrochemicalcapacitors[J].J.Electrochem.Soc.,1997,144(8):L210～L213. [10]　WangZC ,ZhangLH ,LiX ,etal.PreparationofNanocrystallineNiObysol- gelprocess[J].ChemicalJournalofChineseUniversities,1992,13(10):1287～1290(inChinese). [11]　WangSW ,ChenXL ,ChenX ,etal.Preparingfinepowderbymethodoflaserchemistry_preparationofnickelseriespowder[J].ChineseLaser,1989,16(12):741～742. [12]　ZhuCY ,LiuZH ,ChenW ,etal.AdvancesinpreparationandapplicationofNiOultra_finepowder[J].FunctionMaterials,1999,30(4):345～349. [13]　SunG ,YanS ,ZhangZD ,Novelroutetoprepareglass_sol_gelprocess[J].ChemistryBulletin,1990,11:45～51. [14]　BaranwalBP ,RamC ,Mehrotra.Chemistryofalkoxocomplexes,partⅡ.Synthesisandcharacterizationofsomemono(chelato)mono(alkoxo)nickel(Ⅱ)complexes[J].TransitionMet.Chem.,1978,3:220～224. [15]　JohnErringtonR ,JohnRidland,WilliamClegg.β_diketonatederivativesoftitaniumalkoxides:X_raycrystalstructuresandsolutiondynamicsofthebinuclearcomplexesTi(OR)3(dik)2[J].Polyhedron,1998,17(5_6):659～674. [16]　JohannDesilvestro,DennisA .Corrigan,MichaelJ .Weaver.Characterizationofredoxstatesofnickelhydrox idefilmelectrodesbyinsitusurfaceRamanspectroscopy[J].J.Electrochem.Soc.,1988,135(14):885～891. [17]　LiD .ElectrochemicalTheory[M ].Beijing:Beijing-Univ.ofAeronauticandAstronauticsPress,1998. [18]　J .Livage,C .Sanchez.Sol_gelChemistry[J].JournalofNon_CrystallineSolids,1992,145:11～19. [19]　YanYL ,LinGL ,LinBL .Agglomerationpreventionofparticlesofnanometerpowderspreparebyliquid_phasemethod[J].CaiLiaoDaoBao,1998,12(2):11～13.