基于化学还原法的纳米锡颗粒制备方法研究

发布时间：2018-05-20 23:36

  本文选题：化学还原法 + 纳米锡　； 参考：《哈尔滨工业大学》2016年硕士论文

【摘要】：在纳米尺度下锡颗粒具有较低的熔点以及较高的储锂容量,这使得纳米锡颗粒在喷墨印刷、纳米无铅焊料以及锂离子电池电极等领域有着巨大的应用前景。目前纳米锡颗粒最常用的制备方法是基于表面活性剂为PVP体系和Phen体系的液相化学还原法,其应用方面主要集中于锂离子电池电极领域,然而对于纳米颗粒一个非常重要的领域(低温烧结),国内外关于纳米锡的研究还十分缺乏。本课题以这两个反应体系为基础,制备出了一系列不同尺寸的纳米锡颗粒,通过对其烧结性能的研究,明确了烧结工艺对纳米锡颗粒烧结组织和导电性能的影响。基于PVP体系,本课题主要研究了PVP含量和PVP分子量对纳米锡颗粒尺寸的影响。实验结果表明随着PVP含量的增加以及PVP分子量的减小,纳米锡颗粒尺寸呈现减小的趋势,当PVP含量为1.0 g、PVP分子量为24000时,可以得到平均尺寸约为23 nm的纳米锡颗粒。基于Phen体系,本课题主要研究了溶剂、还原剂加入方式、邻菲罗啉含量以及反应物浓度对纳米锡颗粒的影响。实验结果表明随着邻菲罗啉含量的增加以及反应物浓度的降低,纳米锡颗粒的尺寸降低。当邻菲罗啉含量为4.5 g、反应物浓度为0.01 g/ml时,可以获得最小平均尺寸为30.4 nm的纳米锡颗粒。本课题还研究了烧结工艺对纳米锡颗粒烧结体的导电性的影响。实验结果表明随着烧结时间以及烧结温度的增加,纳米锡的电阻率降低。这种下降趋势在较低的烧结温度时更为明显。在150℃下烧结20 min,纳米锡颗粒烧结体的电阻率为141.09μΩ·cm,是块状锡(11μΩ·cm)的14倍;当烧结温度和烧结时间上升到200℃和60 min时,烧结体的电阻率可以降低到21.5μΩ·cm,仅为块状锡的2倍。
[Abstract]:Tin particles have low melting point and high lithium storage capacity at nanometer scale, which makes tin nanoparticles have great application prospects in inkjet printing, nano-lead-free solder and lithium ion battery electrode. At present, the most commonly used preparation method of nano-tin particles is the liquid-phase chemical reduction method based on surfactant PVP system and Phen system. Its application is mainly concentrated in the field of lithium ion battery electrode. However, a very important field for nanocrystalline particles (low-temperature sintering), domestic and foreign research on nano-tin is still very scarce. On the basis of these two reaction systems, a series of tin nanoparticles of different sizes were prepared in this paper. The effect of sintering process on the sintering microstructure and electrical conductivity of nano-tin particles was determined by the study of their sintering properties. Based on PVP system, the effects of PVP content and PVP molecular weight on the size of tin nanoparticles were studied. The experimental results show that the size of tin nanoparticles decreases with the increase of PVP content and the decrease of PVP molecular weight. When the PVP content is 1. 0 g PVP molecular weight is 24 000, the average size of tin nanoparticles is about 23 nm. Based on Phen system, the effects of solvent, reducing agent addition, o-phenanthroline content and reactant concentration on tin nanoparticles were studied. The results show that the size of tin nanoparticles decreases with the increase of o-phenanthroline content and the decrease of reactant concentration. When the content of o-phenanthroline is 4.5 g and the concentration of reactant is 0.01 g/ml, the smallest average size of tin nanoparticles is 30.4 nm. The effect of sintering process on the electrical conductivity of tin nanoparticles was also studied. The experimental results show that the resistivity of nanocrystalline tin decreases with the increase of sintering time and sintering temperature. This downward trend is more obvious at lower sintering temperature. When sintered at 150 鈩，

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