室温下肼还原法制备纳米镍的研究
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摘要
以氯化镍为原料,水合肼为还原剂,不采取任何保护措施不加修饰剂的情况下,在室温通过化学还原法制备了球形金属镍纳米粒子.通过X射线衍射(XRD)和能量散射光谱(EDS)对产物的晶相结构和成分进行了分析;使用扫描电镜(SEM)对制备镍纳米粒子的形貌进行了观察;并对产物的磁学性能进行了测量分析.对制备过程中的反应机理也进行了探讨.研究结果表明,在乙醇介质中,以水合肼为还原剂,控制好各种反应参数,在室温下可以制备粒径为50 nm左右球形金属镍纳米粒子.镍纳米粒子的饱和磁化强度(Ms)为35.3 emu/g,矫顽力(Hc)为114.2 Oe.
Spherical pure metallic nickel nanoparticles were successfully synthesized by the chemical reduction of nickel chloride with hydrazine hydrate at room temperature without any protective agent and inert gas protection. The crystal structure and composition of the products were analyzed by X-ray diffraction(XRD) and energy dispersive spectroscopy( EDS). The morphology of the nickel nanoparticles was observed by scanning electron microscopy(SEM). The magnetic properties were also measured. And at last,the reaction mechanism was discussed. The experimental results show that the sample with average size about 50 nm can be synthesized in alcohol medium at room temperature under the good control of various reaction parameters and hydrazine hydrate is the reducing agent. The saturation magnetization(Ms) is 35.3 emu/g and the coercivity(Hc) is 114.2 Oe.
Spherical pure metallic nickel nanoparticles were successfully synthesized by the chemical reduction of nickel chloride with hydrazine hydrate at room temperature without any protective agent and inert gas protection. The crystal structure and composition of the products were analyzed by X-ray diffraction(XRD) and energy dispersive spectroscopy( EDS). The morphology of the nickel nanoparticles was observed by scanning electron microscopy(SEM). The magnetic properties were also measured. And at last,the reaction mechanism was discussed. The experimental results show that the sample with average size about 50 nm can be synthesized in alcohol medium at room temperature under the good control of various reaction parameters and hydrazine hydrate is the reducing agent. The saturation magnetization(Ms) is 35.3 emu/g and the coercivity(Hc) is 114.2 Oe.
引文
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[13]Hwang J H,Dravid V P,Teng M H,et al.Magnetic properties of graphitically encapsulated nickel nanocrystals[J].J.Mater.Res.,1997(12):1076-1082.
[2]Lewis L N.Chemical catalysis by colloids and clusters[J].Chemical Reviews,1993,93(8):2693-2370.
[3]黄园英,刘菲,汤鸣臬,等.纳米镍/铁和铜/铁双金属对四氯乙烯脱氯研究[J],环境科学学报,2007,27(1):80-85.Huang Yuanying,Liu Fei,Tang Minggao,et al.Dechlorination of tetrachloroethene with nanoscale Ni/Fe and Cu/Fe bimetallic particles[J].Acta Scientiae Circumstantiae,2007,27(1):80-85.(in Chinese)
[4]冯丽,葛小鹏,李一,等.酸性体系中纳米镍对2,4-二氯苯酚降解性能的研究[J].科学通报,2011,56(16):1308-1316.
[5]姚开胜,芦雷鸣,吴云骥,等.新法合成纳米镍催化剂及其催化还原对硝基甲苯[J].现代化工,2008,28(2):56-57.Yao Kaisheng,Lu Leiming,Wu Yunji,et al.Synthesis of nanosized nickel catalysts and catalysis of p-nitrotoluene reduction by it[J].Modern Chemical Industry,2008,28(2):56-57.(in Chinese)
[6]Jordan A,Scholz R,Wust P,et al.Magnetic fluid hyperthermia(MFH):cancer treatment with AC magnetic field induced excitation of biocompatible superparamagnetic nanoparticles[J].J.Magn.Magn.Mater.,1999,201(1/3):413-419.
[7]Huang Guoyong,Xu Shengming,Xu Gang,et al.Preparation of fine nickel powders via reduction of nickel hydrazine complex precursors[J].Trans.Nonferrous.Met.Soc.China,2009(19):389-393.
[8]Nouneha K,Oyamab M,Diazc R,et al.Nanoscale synthesis and optical features of metallic nickel nanoparticles by wet chemical approaches[J].J.Alloys.Compd.,2011(509):5882-5886.
[9]Knecht M R,Garcia-Martinez J C,Crooks R M.Synthesis,characterization and magnetic properties of dendrimer-encapsulated nickel nanoparticles containing<150 atoms[J].Chem.Mater.,2006,18(21):5039-5044.
[10]Park JW,Chae E H,Kim S H,et al.Preparation of fine Ni powders from nickel hydrazine complex[J].Mater.Chem.Phys.,2006(97):371-378.
[11]晋传贵,檀杰.化学还原法制备金属镍纳米颗粒[J].安徽工业大学学报,2007,24(1):36-38.Jin Chuangui,Tan Jie.Preparation of nickle nanoparticles by chemical reduction method[J].J.of Anhui University of Technology,2007,24(1):36-38.(in Chinese)
[12]马玉亮,王洁炜,周琼.两种还原剂体系制备纳米镍粒子结构与磁性的对比[J].稀有金属,2006,30(4):436-439.Ma Yuliang,Wang Jiewei,Zhou Qiong.Structure and characterization of magnetic nickel nanoparticle by different reducing agents[J].Chinese Journal of Rare Metals,2006,30(4):436-439.(in Chinese)
[13]Hwang J H,Dravid V P,Teng M H,et al.Magnetic properties of graphitically encapsulated nickel nanocrystals[J].J.Mater.Res.,1997(12):1076-1082.