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材料研究学报  2017, Vol. 31 Issue (12): 947-954    DOI: 10.11901/1005.3093.2017.161
  研究论文 本期目录 | 过刊浏览 |
脉冲电磁场对用湿法制备的草酸镍盐形貌和粒度的影响
彭淑静, 唐立丹, 王冰, 王建中(), 林静
辽宁工业大学化学与环境工程学院 锦州 121001
Effects of Pulsed Electromagnetic Field on the Morphology and Powder Size during Nickel Oxalate Salt Produced by Wet Chemical Method
Shujing PENG, Lidan TANG, Bing WANG, Jianzhong WANG(), Jing LIN
School of Chemical and Environmental Engineering, Liaoning University of Technology, Jinzhou 121001, China
引用本文:

彭淑静, 唐立丹, 王冰, 王建中, 林静. 脉冲电磁场对用湿法制备的草酸镍盐形貌和粒度的影响[J]. 材料研究学报, 2017, 31(12): 947-954.
Shujing PENG, Lidan TANG, Bing WANG, Jianzhong WANG, Jing LIN. Effects of Pulsed Electromagnetic Field on the Morphology and Powder Size during Nickel Oxalate Salt Produced by Wet Chemical Method[J]. Chinese Journal of Materials Research, 2017, 31(12): 947-954.

全文: PDF(5177 KB)   HTML
摘要: 

以氯化镍为母液、草酸铵为沉淀剂,用脉冲电磁场(PEMF)辅助草酸盐沉淀法制备了纤维状草酸镍盐。使用XRD、FT-IR、SEM以及激光粒度仪等手段分别表征了产物的物相、形貌和粒度,研究了脉冲电压、脉冲频率和脉冲处理时间等因素对草酸镍盐形貌和粒度的影响,并初步探讨了PEMF的作用机理。与未用PEMF处理的常规制备方法相比,该方法的加料速度由2 mL/min提高到5 mL/min;当脉冲电压为600 V、脉冲频率为4 Hz、脉冲处理时间为3 min时粉体的长径比由原来的7:1增加到25:1,且没有出现明显的团聚。适当的PEMF处理可使草酸镍盐的氨镍比为0.5~2.5,制备出较理想的纤维状形貌的草酸镍盐。

关键词 无机非金属材料草酸镍盐湿法制备脉冲电磁场形貌粒度    
Abstract

Fibrous particles of nickel oxalate salt were prepared by wet chemical method under the action of pulsed electromagnetic field (PEMF) using NiCl2 solution as original liquid and (NH4)2C2O4 solution as precipitant reagents, and which then were characterized by means of X-ray diffractometer (XRD), Fourier transform infrared spectrum (FT-IR), scanning electron microscopy (SEM) and laser granularity analyzer. The effect of PEMF parameters on the morphology and powder size of nickel oxalate salt was examined and the relevant mechanism model of interaction between PEMF and reaction system was preliminarily disccussed. Results show that in comparison to the conventional precipitation method, the feeding speed for the present process can be enhanced from 2 mL/min to 5 mL/min, and the aspect ratio of fibrous particles of nickel oxalate salt increased from 7:1 to 25:1 for the produced fibrous particles under PEMF with voltage 600 V, frequency 4 Hz and treatment time 3 min. Besides, not obvious agglomeration could be seen for the products. Finally, the desired fibrous particles of nickel oxalate salt could be prepared by a process in solutions with ammonia to nickel within a range of 0.5 to 2.5 and with appropriate PEMF parameters.

Key wordsinorganic non-metallic matericals    nickel oxalate salt    wet chemical method    pulsed electromagnetic field    morphology    powder size
收稿日期: 2017-03-02     
ZTFLH:  TF76  
基金资助:辽宁省自然科学基金(201202096), 辽宁省教育厅团队项目(LT2013014), 辽宁省教育厅一般研究项目(L2015236)
作者简介:

作者简介 彭淑静,女,1982年生,讲师

图1  PEMF辅助反应装置的示意图
图2  脉冲电压不同的草酸镍盐的SEM照片
图3  脉冲频率不同的草酸镍盐的SEM照片
图4  脉冲处理时间不同的草酸镍盐的SEM照片
图5  脉冲电压不同的草酸镍盐的XRD图谱
图6  脉冲电压不同的草酸镍盐的粒度分布
图7  脉冲电压不同的草酸镍盐的IR图谱
图8  脉冲电压不同的草酸镍盐的电导率
图9  脉冲电磁场与草酸镍盐反应体系间的交互作用机制示意图
[1] Wang S Q, Liu F C, Chen J J, et al.Influence of flaky nickel powder on permeation resistance of fluorocarbon coatings[J]. Chin. J. Meter. Ras., 2015, 29(4): 255(王思齐, 刘福春, 陈军君等. 片状镍粉对氟碳涂层抗渗透性的影响[J]. 材料研究学报, 2015, 29(4): 255)
[2] Zhang C F, Wu L L, Li C J, et al.Peparation of fiber precursor of Ni-Co alloy powder[J]. Chine. J. Nonferrous Met., 2002, 12(1): 183(张传福, 吴琳琳, 黎昌俊等. 纤维状镍钴合金粉的制备[J]. 中国有色金属学报. 2002, 12(1): 183)
[3] Lian J B, Lei M X, Gao Y X, et al.Synthesis of ultrafine nickel powder by chemical precipitation-reduction method[J]. Powder Metall. Ind., 2013, 23(6): 24(连景宝, 雷明霞, 高云侠等. 化学沉淀-还原法合成超细镍粉的研究[J]. 粉末冶金工业, 2013, 23(6): 24)
[4] Okamoto T, Ichino R, Okido M, et al.Effect of ammonia on the crystal morphology of nickel oxalate precipitates and their thermal decomposition into metallic nickel[J]. Mater. Trans., 2005, 46(2): 171
[5] Niu H L, Chen Q W, Zhu H F, et al.Magnetic field-induced growth and self-assembly of cobalt nanocrystallites[J]. J. Mater. Chem., 2003, 13: 1803
[6] Wang F, Gu H Z, Zhang Z C.Preparation of cobalt nanocrystals in the homogenous solution with the presence of a static magnetic field[J]. Mater. Res. Bull., 2003, 38(2): 347
[7] Chen F, Peng S J, Fang W B, et al.Preparation of fibrous nickel oxalate by nickel ammonia complexinig precipitation[J]. Powder Metall. Technol., 2015, 33(6): 449(陈飞, 彭淑静, 方文博等. 镍氨络合沉淀法制备纤维状草酸镍氨复盐粉体[J]. 粉末冶金技术, 2015, 33(6): 449)
[8] Mesina M B, Jong T P R, Dalmjin W L. Scrap stainless steel detection using a pulsed electromagnetic field[J]. Int. J. Miner. Process., 2005, 76(1-2): 21
[9] Liu Z H.Morphology and size control of nickel and cobalt oxalate particles [D]. Changsha: Central South University, 2007(刘志宏, 镍钴草酸盐制备中的形貌与粒度控制 [D]. 长沙: 中南大学, 2007)
[10] Du H L, Wang J Z, Qi J G, et al.Effects of pulsed electromagnetic field on CoC2O42H2Opowder size[J]. Acta Metall. Sin., 2009, 45(8): 1019(杜慧玲, 王建中, 齐锦刚等. 脉冲电磁场对CoC2O42H2O粒度的影响[J]. 金属学报, 2009, 45(8): 1019)
[11] Zhang C F, Wu J H, Zhan J, et al.Precuisor synthesis of fibrillar nanocrystalline nickel powder[J]. Nonferrous Metals, 55(3), 25(2003)(张传福, 邬建辉, 湛菁等. 纤维状纳米镍粉前驱体的合成[J]. 有色金属, 2003, 55(3): 25)
[12] Yau S T, Bekilov P G.Quasi-planar nucleus structure in apoferritin crystallization[J]. Nature, 2000, 406: 494
[13] Du H L, Wang J Z, He L J, et al.Size control of cobalt oxalate powders by means of pulsed electromagnetic field[J]. J. Funct. Mater., 2009, 40(7): 1097(杜慧玲, 王建中, 何力佳等. 脉冲电磁场对草酸钴粒度的控制[J]. 功能材料, 2009, 40(7): 1097)
[14] Xu Y.Electromagnetism(the second edition) [M]. Beijing: Science Press, 2004(徐游. 电磁学(第二版) [M]. 北京: 科学出版社, 2004)
[15] Shi E W, Chen Z Z, Yuan R L, et al.Hydrothermal Crystallography [M]. Beijing: Science Press, 2004(施尔畏, 陈之战, 元如林等. 水热结晶学 [M]. 北京: 科学出版社, 2004)
[16] Ma Z C, Wei Y, Zheng X Z, et al.Study on synthesizing spindle-shaped α-Fe203 powder by air oxidation of ferrous salt[J]. J. Funct. Mater., 1998, 29(5): 465(马子川, 魏雨, 郑学忠等. 亚铁盐氧化法合成纺锤形α-Fe203微粒条件的研究[J]. 功能材料, 1998, 29(5): 465)
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