| 引用本文: | 张涛,刘洋,赵凯,孙凤莲.液相还原法制备纳米镍粉[J].材料科学与工艺,2018,26(6):51-56.DOI:10.11951/j.issn.1005-0299.20170145. |
| ZHANG Tao,LIU Yang,ZHAO Kai,SUN Fenglian.Preparation of nano nickel powder by liquid phase reduction method[J].Materials Science and Technology,2018,26(6):51-56.DOI:10.11951/j.issn.1005-0299.20170145. |
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| 摘要: |
| 为优化纳米镍粉的液相还原法制备工艺，本文以硫酸镍为主盐，水合肼为还原剂，水浴75 ℃条件下，选取产物纯度、产物粒径、反应速率等关键指标开展工艺优化试验，分别研究了NaOH加入量、溶剂种类、有无分散剂，反应物摩尔比，加料顺序五个变量对于镍粉制备的影响.采用XRD和TEM对产物镍粉进行了表征.结果表明，NaOH的加入量影响产物组成，溶剂种类影响产物粒径大小，分散剂对产物的团聚状态有影响，反应物摩尔比以及加料顺序影响体系的反应速率.最终获得如下的优化工艺：NaOH的加入量在0.015~0.02 mol，乙醇和乙二醇做反应溶剂，加入分散剂PVP，反应物摩尔比为4: 1以及采用氢氧化钠与水合肼混合后再向混合溶液中加入硫酸镍溶液的顺序可以获得较为纯净、粒径较小、分散性好的球形纳米镍粉，并且有较快的反应速率.
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| 关键词: 液相还原法 纳米镍粉 粒径 对比试验 |
| DOI：10.11951/j.issn.1005-0299.20170145 |
| 分类号:TM241 |
| 文献标识码:A |
| 基金项目: |
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| Preparation of nano nickel powder by liquid phase reduction method |
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ZHANG Tao,LIU Yang, ZHAO Kai,SUN Fenglian
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(School of Material Science and Engineering, Harbin University of Science and Technology, Harbin 150001,China)
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| Abstract: |
| In order to optimize the preparation process of nano-nickel powder by liquid phase reduction method, reaction rate, product purity, and product particle diameter were selected as key research aspects when using nickel sulfate as main salt and hydrazine hydrate as reducing agent in water bath at 75 ℃.Effects of the addition of NaOH, solvent types, presence or absence of dispersant, molar ratio of reactants, and feed sequences of reactants on the preparation of nickel powder were studied. The product nickel powder was characterized by XRD and TEM methods. The results showed that the addition of NaOH could affect the composition of the product, the solvent type could affect the particle diameter of the product, dispersant could affect the agglomeration of product particles, the molar ratio of the reactants and feed sequences of the reactants determined the reaction time. In order to prepare relatively pure, small, and well dispersed nickel nanosphere powder at a higher reaction rate, PVP, NaOH, N2H4 · H2O, NiSO4 · 6H2O were added in sequence into the solvent of C2H5OH and C2H6O2. The amount of NaOH addition should be controlled precisely (0.015 mol to 0.02 mol), which can produce intermediate product and provide alkaline condition for follow-up reactions. Relatively high reaction rate was obtained with the molar ratio of main salt and reducing agent (N2H4: Ni2+) of 4: 1.
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| Key words: liquid phase reduction method nano-nickel powder partical diameter contrast test |
