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反应温度、反应时间和搅拌速率对纳米铜粉尺寸和分散性的影响

Effects of reaction temperature, reaction time, and stirring rate on particle size and dispersion of nano-copper powders

  • 摘要: 为解决液相还原法纳米铜粉粒径控制难、易团聚等问题,通过对比直接还原法、络合还原法与醇溶剂还原法三种方法,系统研究了反应温度、反应时间及搅拌速率对铜粉形貌、粒径及分散性的影响。结果表明:醇溶剂法与络合法在调控粒径分布和改善分散性方面显著优于直接还原法。特别是醇溶剂法,利用丙三醇同时作为溶剂与还原剂,凭借缓慢的还原速率和优异的表面修饰作用,成功制备出平均粒径约为200 nm、分散性良好的球形纳米铜粉。明确了三种方法的最佳工艺参数(反应温度、反应时间和搅拌速率),直接还原法为80 ℃、90 min、400 r·min−1,能够制备出粒径在300 nm左右的铜粉;络合还原法为90 ℃、90 min、300 r·min−1,能够制备出粒径在250 nm左右的铜粉;醇溶剂还原法为160 ℃、120 min、300 r·min−1,能够制备出粒径在200 nm左右的铜粉。

     

    Abstract: To solve the problems of difficult particle size control and easy agglomeration for the nano-copper powders prepared by liquid-phase reduction, the normal method (NMM), complex reduction method (CRM), and alcohol solvent reduction method (ARM) were compared, and the effects of reaction temperature, reaction time, and stirring rate on the morphology, particle size, and dispersion of copper powders were systematically investigated. The results show that the alcohol solvent method and complex method are significantly superior to the normal method in regulating particle size distribution and improving dispersion. Especially, the alcohol solvent method, using glycerol as both the solvent and the reducing agent, successfully prepares the spherical nano-copper powders with average particle size of about 200 nm with good dispersion, due to a slow rate of restoration and excellent surface modification capabilities. The optimal process parameters (reaction temperature, reaction time, and stirring rate) were clarified for the three methods, which is 80 ℃, 90 min, and 400 r·min−1 for NMM (the prepared copper powders with particle size of about 300 nm), 90 ℃, 90 min, and 300 r·min−1 for CRM (the prepared copper powders with particle size of about 250 nm), and 160 ℃, 120 min, and 300 r·min−1 for ARM (the prepared copper powders with particle size of about 200 nm).

     

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