不同气氛中热分解碳酸镍制备纳米氧化镍
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摘要
以碳酸镍(NiCO3)在空气和氩气中的热重-差热(TG-DSC)分析为理论依据,利用X射线衍射仪(XRD)、热场发射扫描电子显微镜(SEM)和高分辨透射电子显微镜(TEM)对NiCO3在空气或氩气中热分解最终产物进行表征。研究结果表明:Ni CO3在氩气中的热分解温度总的趋势是小于其在空气中的热分解温度。前者的热分解过程只有两步,而后者的热分解过程却需要三步。NiCO3在空气和氩气中热分解的最终产物均为NiO。以6℃/min升温速率升至450℃并在450℃保温20 min热分解NiCO3时,在空气中热分解NiCO3能获得约10nm的NiO,而在氩气中热分解NiCO3能获得约5 nm的NiO。这两者NiO的粒径分布都较均匀。
The thermal decomposition of NiCO3 is based on its TG-DSC in the air and the argon. The thermal decomposition products of NiCO3 in the air and the argon are characterized with X-ray diffraction( XRD),scanning electron microscope( SEM) and transmission electron microscope( TEM). The results show that the thermal decomposition temperature of NiCO3 in the argon is much less than that of NiCO3 in the air. And the thermal decomposition processes of the former have two steps; those of the latter have three steps. The phase of the thermal decomposition products of NiCO3 in the air or the argon is NiO. NiCO3 is pyrolyzed from the room temperature to 450℃ at the rate of 6 ℃ / min and for 20 min at 450 ℃. The particle size of Ni O of thermal decomposition of NiCO3 in the air is about 10 nm,and that of NiCO3 in the argon is about 5 nm. Their particle size distribution is homogeneous.
The thermal decomposition of NiCO3 is based on its TG-DSC in the air and the argon. The thermal decomposition products of NiCO3 in the air and the argon are characterized with X-ray diffraction( XRD),scanning electron microscope( SEM) and transmission electron microscope( TEM). The results show that the thermal decomposition temperature of NiCO3 in the argon is much less than that of NiCO3 in the air. And the thermal decomposition processes of the former have two steps; those of the latter have three steps. The phase of the thermal decomposition products of NiCO3 in the air or the argon is NiO. NiCO3 is pyrolyzed from the room temperature to 450℃ at the rate of 6 ℃ / min and for 20 min at 450 ℃. The particle size of Ni O of thermal decomposition of NiCO3 in the air is about 10 nm,and that of NiCO3 in the argon is about 5 nm. Their particle size distribution is homogeneous.
引文
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2 EstelléJ,Salagre P,Cesteros Y,et al.Comparative study of the morphology and surface properties of nickel oxide prepared from different precursors.Solid State Ionics,2003;156:233—243
3 张煜,邱运仁.纳米氧化镍的制备及性能表征.化工进展,2010;29(5):918—921Zhang Yu,Qiu Yunren.Preparation and characterization of Ni O nanoparticles.Chemical Industry and Engineering Progress,2010;29(5):918—921
4 王红涛,张乐观,贺茂云.纳米氧化镍制备及表征.无机盐工业,2012;44(3):60—62Wang Hongtao,Zhang Leguan,He Maoyun.Preparation and characterization of nano-sized nickel oxide.Inorganic Chemicals Industry,2012;44(3):60—62
5 耿树东,张钰,陈连发,等.化学沉淀法制备纳米氧化镍粉体.吉林化工学院学报,2012;29(5):8—10Geng Shudong,Zhang Yu,Chen Lianfa,et al.Nanometer-sized Ni O power prepared by chemical sendimentation method.Journal of Jilin Institute of Chemical Technology,2012;29(5):8—10
6 刘焕彬,陈小泉.纳米科学与技术导论.北京:化学工业出版社,2006Liu Huanbin,Chen Xiaoquan.Introduction to nano science and technology.Beijing:Chemical Industry Press,2006
7 邓建成,邓晶晶,刘博,等.不同形貌纳米氧化镍的制备及其电容特性研究.湘潭大学自然科学学报,2009;31(1):47—52Deng Jiancheng,Deng Jingjing,Liu Bo,et al.Preparation and electrochemical capacitance characterization of nano-scale Ni O with different shapes.Natural Science Journal of Xiangtan University,2009;31(1):47—52
8 罗元庆,韩永朝,魏娜,等.超声法制备纳米氧化镍其性能研究.西北民族大学学报(自然科学版),2014;35(93):27—31Luo Yuanqing,Han Yongchao,Wei Na,et al.Synthesis and characterization of Ni O nanospheres with ultrasonic method.Journal of Northwest University for Nationalities(Natural Science),2014;35(93):27—31
9 Ansar A,Soysal D,Schiller G.Nanostructured functional layers for solid oxide fuel cells.International Journal of Energy Research,2009;33:1191—1202
10 Karthik K,Kalai S G,Kanagaraj M,et al.Particle size effect on the magnetic properties of Ni O nanoparticles prepared by a precipitation method.Journal of Alloys and Compounds,2011;509:181—184
11 傅小明,谢晨晨,周良谊.空气中热分解二水草酸镍制备纳米氧化镍.中国有色冶金,2011;5:67—69Fu Xiaoming,Xie Chenchen,Zhou Liangyi.Preparation of nano Ni O by the pyrolytic decomposition Ni C2O4·2H2O in the air.China Nonferrous Metallurgy,2011;5:67—69
12 陈爱良,杜作娟,贾喜君,等.对制备超细Ni O粉末热分解动力学过程的探讨.湖南冶金,2002;6:17—20Chen Ailiang,Du Zuojuan,Jia Xijun,et al.Research of the kinetics of thermal decomposition of making Ni O powders.Hunan Metallurgy,2002;6:17—20
13 周公度,段连运.结构化学基础.北京:北京大学出版社,1995Zhou Gongdu,Duan Lianyun.The basis of structural chemistry.Beijing:Beijing University Press,1995