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基于化學(xué)還原法的納米錫顆粒制備方法研究

發(fā)布時(shí)間:2018-05-20 23:36

  本文選題:化學(xué)還原法 + 納米錫。 參考:《哈爾濱工業(yè)大學(xué)》2016年碩士論文


【摘要】:在納米尺度下錫顆粒具有較低的熔點(diǎn)以及較高的儲(chǔ)鋰容量,這使得納米錫顆粒在噴墨印刷、納米無鉛焊料以及鋰離子電池電極等領(lǐng)域有著巨大的應(yīng)用前景。目前納米錫顆粒最常用的制備方法是基于表面活性劑為PVP體系和Phen體系的液相化學(xué)還原法,其應(yīng)用方面主要集中于鋰離子電池電極領(lǐng)域,然而對(duì)于納米顆粒一個(gè)非常重要的領(lǐng)域(低溫?zé)Y(jié)),國(guó)內(nèi)外關(guān)于納米錫的研究還十分缺乏。本課題以這兩個(gè)反應(yīng)體系為基礎(chǔ),制備出了一系列不同尺寸的納米錫顆粒,通過對(duì)其燒結(jié)性能的研究,明確了燒結(jié)工藝對(duì)納米錫顆粒燒結(jié)組織和導(dǎo)電性能的影響;赑VP體系,本課題主要研究了PVP含量和PVP分子量對(duì)納米錫顆粒尺寸的影響。實(shí)驗(yàn)結(jié)果表明隨著PVP含量的增加以及PVP分子量的減小,納米錫顆粒尺寸呈現(xiàn)減小的趨勢(shì),當(dāng)PVP含量為1.0 g、PVP分子量為24000時(shí),可以得到平均尺寸約為23 nm的納米錫顆粒;赑hen體系,本課題主要研究了溶劑、還原劑加入方式、鄰菲羅啉含量以及反應(yīng)物濃度對(duì)納米錫顆粒的影響。實(shí)驗(yàn)結(jié)果表明隨著鄰菲羅啉含量的增加以及反應(yīng)物濃度的降低,納米錫顆粒的尺寸降低。當(dāng)鄰菲羅啉含量為4.5 g、反應(yīng)物濃度為0.01 g/ml時(shí),可以獲得最小平均尺寸為30.4 nm的納米錫顆粒。本課題還研究了燒結(jié)工藝對(duì)納米錫顆粒燒結(jié)體的導(dǎo)電性的影響。實(shí)驗(yàn)結(jié)果表明隨著燒結(jié)時(shí)間以及燒結(jié)溫度的增加,納米錫的電阻率降低。這種下降趨勢(shì)在較低的燒結(jié)溫度時(shí)更為明顯。在150℃下燒結(jié)20 min,納米錫顆粒燒結(jié)體的電阻率為141.09μΩ·cm,是塊狀錫(11μΩ·cm)的14倍;當(dāng)燒結(jié)溫度和燒結(jié)時(shí)間上升到200℃和60 min時(shí),燒結(jié)體的電阻率可以降低到21.5μΩ·cm,僅為塊狀錫的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,

本文編號(hào):1916757

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