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研究生:陳信宏
論文名稱:奈米銀微粒之化學合成與應用研究
論文名稱(外文):Study on Chemical Synthesis and Application of Nanosized Silver Particles
指導教授:周更生周更生引用關係
學位類別:碩士
校院名稱:國立清華大學
系所名稱:化學工程學系
學門:工程學門
學類:化學工程學類
論文種類:學術論文
論文出版年:2002
畢業學年度:90
語文別:中文
中文關鍵詞:奈米銀微粒奈米複合材料乙二醇還原法
相關次數:
  • 被引用被引用:14
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本研究以硝酸銀作為前驅物,利用化學還原方式在乙二醇相中合成奈米金屬銀微粒,並加入高分子PVP做為保護劑,避免已還原的銀微粒繼續再次凝聚。隨著PVP量的增加和持溫溫度的下降奈米銀微粒呈現縮小的趨勢,粒徑範圍可控制在30-50nm之間。進一步克服熱傳阻力後,乙二醇還原法具有可系統放大之優勢。
為了避免大量PVP的存在影響粒子間無法彼此接觸,合成出之奈米銀微粒需經過分離與純化之程序。本研究藉由加入五倍體積的丙酮,配合高速離心使得PVP膠體沈澱,隨後利用1:3水丙酮系統洗滌離心沈澱物兩次,可得無PVP保裹之奈米顆粒,清洗步驟損失約21wt.%之奈米銀微粒。將奈米銀微粒再分散於四氫喃(THF)溶劑中,並在溶液中加入高分子基材(環氧樹脂),利用揮發方式去除四氫喃溶劑,以完成高分子複合材料之製備。
在奈米高分子複合材料電性研究方面,當填充物奈米銀微粒粒徑縮小至40nm時,其臨界體積分率(Vc)可大幅降至1.13vol.%以下。此外,經過三滾筒混鍊再加工步驟,利用滾輪間剪切作用力使得凝聚粒子再分散,可大幅改善奈米粒子的凝聚現象,使得膠體電性更佳均一。
Nanosized silver particles were produced by chemical reduction method using silver nitrate as precursor. PVP was added as a protective agent to avoid agglomeration of these nanosized Ag colloids. Increasing PVP concentration and decreasing aging temperature for a given mass of precursor were found to yield smaller nanosized silver particles. By varying the initial conditions, the colloidal size can be controlled within the range of 30-50nm. Results indicated that this polyol process can be easily scaled up if we can overcome the problem of heat transfer to assume uniform temperature distribution within the reactor.
In order to reduce the influence of PVP in future applications, the synthesized particles must be separated and purified. The suspension was first washed by acetone, followed by centrifugation to separate PVP-Ag colloids. Then the colloids were washed two times by water/acetone(1:3) solution. After these steps, we could then obtain pure silver nanoparticles without PVP. The silver loss however was about 21wt.%. These agglomerated silver nanoparticles were then dissolved in tetrahydrofuran and mixed with epoxy resin. Tetrahydrofuran was later removed by evaporation to obtain Ag-resin nanocomposite.
With regards to the electric properties of nanocomposite, the apparent critical volume fraction decreased to about 1.13vol.% when we used 40nm nanosized silver particles as conductive fillers. In addition, we found that the three-roll-mill process could help to disperse well Ag nanoparticles in the composite and to obtain uniform electric properties.
摘要
Abstract
第一章 前言 1
第二章 文獻回顧 3
2.1概要 3
2.2導電機制 3
2.3填充物 4
2.3.1導電性填充物 5
2.3.2填充物形狀因子 7
2.3.3填充物大小因素 8
2.4奈米高分子複合材料製造法 10
2.4.1奈米金屬微粒的合成 11
2.4.1.1還原劑還原法 12
2.4.1.2光還原法 14
2.5微粒於高分子中分散性 17
2.6未來展望 19
第三章 實驗方法 21
3.1實驗藥品 21
3.2實驗儀器 22
3.3實驗步驟 25
3.3.1奈米銀微粒之製備 25
3.3.2轉化率之研究 27
3.3.3奈米高分子複合材料之製作 28
第四章 結果與討論 31
4.1製備奈米銀微粒 31
4.1.1光還原法 31
4.1.1.1水相中合成奈米銀微粒 31
4.1.1.2光還原率之探討 35
4.1.2乙二醇還原法 36
4.1.2.1還原率分析 37
4.1.2.2 PVP添加量對銀微粒粒徑之影響 39
4.1.2.3持溫溫度對銀微粒粒徑之影響 47
4.1.2.4Scale-up之影響 48
4.1.2.5乙二醇還原法定性機制探討 50
4.1.2.6奈米金屬微粒生成機制探討 51
4.2奈米銀微粒處理與高分子複合材料製作方法之研究 55
4.2.1奈米銀微粒分離、純化與再分散 55
4.2.2再分散液 59
4.2.3奈米銀微粒與高分子混合方法及電性分析 61
第五章 結論 67
第六章 參考文獻 68
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