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  • 學位論文

聚(鄰-(胺基苯甲基醚-十二烷基苯磺酸))-蒙脫土奈米複合材料及壓克力共聚物-銀粒子奈米複合材料之製備與性質研究

Preparation and Property Studies of Poly(o-methoxyaniline-DBSA)/Clay Nanocomposites and Copolyacrylate-Ag Particle Nanocomposites

指導教授 : 葉瑞銘
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摘要


摘要 本研究主要分為兩部份,ㄧ是以乳化聚合(Emulsion polymerization)方式製備聚(鄰-(胺基苯甲基醚-十二烷基苯磺酸)),將(鄰-胺基苯甲基醚)單體與界面活性劑十二烷基苯磺酸形成一錯合物,將此錯合物溶液加入到已膨潤一天的蒙脫土中,進一步加入過硫酸銨(APS)作為鏈起始劑進行聚合反應,再藉由過濾以及烘乾得到聚(鄰-(胺基苯甲基醚-十二烷基苯磺酸))-蒙脫土奈米複合材料,並利用傅立葉紅外光譜(FTIR)鑑定其複材之結構。 在本研究中將進一步探討奈米複合材料在防腐蝕性質、熱性質及導電度之變化。並利用廣角X-ray繞射儀(WAXRD)觀察黏土之層間距變化;利用穿透式電子顯微鏡(TEM)觀察黏土分散於高分子基材中的分散情形;使用循環伏特電位儀(CV)量測防腐蝕性質之相關數據,同時以阻抗 (Impedance)做一輔助性之證據;另外,以掃描式電子顯微鏡(SEM)看表面型態變化,與利用表面接觸角分析儀(contanct angle)測量其複合材料親、疏水性之變化,並用凝膠滲透層析儀(GPC)觀察複材之分子量變化,同時利用UV-Vis分光光譜儀(UV-vis)觀察其結構的變化,以及利用四點探針偵測其導電度的變化,最後以熱重分析儀(TGA)觀察奈米複合材料之熱性質變化。 第二部分則是利用2-丙烯酸羥乙酯(HEA)與縮水甘油甲基丙烯酸酯(GMA)行自由基聚合反應(Free radaical polymerization) ,以AIBN為起始劑,進行聚合反應形成共聚高分子;另外,將硝酸銀溶於DMAc中,並加入3~5滴醋酸水溶液,製備硝酸銀的前驅液,再將2-丙烯酸羥乙酯(HEA)與縮水甘油甲基丙烯酸酯(GMA)加入,並加入AIBN起始反應,形成 (GMA-HEA)-Ag particle 奈米複合材料,對於結構部份使用傅立葉紅外光譜(FTIR)來鑑定其複合材料之結構。 另外,因為熱導材料在文獻上較少被探討,因此,在本研究中針對(GMA-HEA)-Ag particle 奈米複合材料之熱傳導性做一個研究;利用UV-vis分光光譜儀(UV-vis)、廣角X-ray繞射儀(WAXRD)偵測銀的變化,並提出機制推論銀離子被還原為銀粒子,而UV-vis部份因為有較寬的吸收帶,推論其粒子大小不均一,此由穿透式電子顯微鏡(TEM)可以直接證實。再者,利用TEM與元素分佈地圖(SEM mapping)也可以觀察銀粒子之分散,同時由TEM發現銀粒子與共聚高分子是以核-殼(core-shell)的形式存在的;另外,也藉由掃描式電子顯微鏡(SEM)觀察其結構型態,且用原子力顯微鏡(AFM)觀察複材之表面粗糙度,並利用表面接觸角分析儀(contact angle) 測量表面之親、疏水性之變化;也藉由熱失重分析儀(TGA)、微差掃瞄式熱分析儀(DSC)觀察複材之熱性質變化,以及利用動態機械分析儀(DMA)測試(GMA-HEA)-Ag particle 奈米複合材料之機械性質。

並列摘要


Abstract This thesis involed two parts : First, emulsion polymerization has been empolyed for the synthesis of polymer–clay nanocomposite(PCN) , which can be dissolved in common organic solvents such as NMP. Ammonium Peroxodisulfate is regarded as the oxidizing agent. Dodecylbenzenesulfonic acid (DBSA) has been selected as the dopant since it also functioned as the surfactant. Firstly, o-methoxyaniline monomer and DBSA were formed (o-methoxyaniline-DBSA) complex. Furthermore, the complex permeated in layers of montmorillonite and starts process of polymerization after adding the initiator APS at room temperature. Structures and dispersed behaviors of Clay of (PMA-DBSA) and as-synthesized PCN materials were subsequently characterized by FTIR spectroscopy, wide-angle powder X-ray diffraction(WXRD), and transmission electron microscopy(TEM). (PMA-DBSA)/Clay nanocomposite materials in the form of coatings with low loading of Na+-MMT clay (e.g.,5 wt%, PMA5) on cold rolled steel (CRS) were showed better property of corrosion protection based on a series of electrochemical measurements of corrosion potential, polarization resistance. The molecular weights of (PMA-DBSA) extracted from PCN materials and neat (PMA-DBSA) were determined by gel permeation chromatography (GPC) with NMP as eluant. Effects of material composition on the morphology, electrical conductivity and thermal properties of uniform (PMA-DBSA) and a series of (PMA-DBSA)/Clay nanocomposites, were also observed by scanning electron micrograph (SEM), four-point probe technique, ultraviolet-visible spectra, contact angle, and Thermal gravimetric analyzer( TGA ), respectively. Second, (GMA-HEA) copolymer were prepared by free radical process. We use 2,2’-Azobis-isobutyronitrile (AIBN) as initiator. For systhesis of (GMA-HEA)-Ag particle nanocomposite , firstly , we can use AgNO3 to dissolve in DMAc, and add 3~5 drops CH3COOH(aq) to the solution, which can formed a Ag precursor solution. In addition, add Glycidyl methacrylate (GMA) and 2-Hydroxyethyl acrylate (HEA) to Ag precursor solution, and get in on 2,2’-Azobis-isobutyronitrile (AIBN) in the solution. Finally, (GMA-HEA)-Ag particle nanocomposite were produced. Structures and dispersed behaviors of Ag particle of (GMA-HEA) and as-synthesized (GMA-HEA)-Ag particle nanocomposite were subsequently characterized by FTIR spectroscopy, wide-angle powder X-ray diffraction (WXRD), transmission electron microscopy (TEM), ultraviolet-visible spectra (UV-vis) and SEM-Mapping. Results of UV-vis and TEM, we can understand relation betweecn size and sharp of Ag particle, and we address the machism of Ag ion reduced Ag particle. Effects of material composition on the morphology, thermal conductivity, thermal properties, and mechanical properties of uniform (GMA-HEA) and a series of (GMA-HEA)-Ag particle nanocomposite materials, were also observed by scanning electron micrograph (SEM), hot disk, atomic force microscopy (AFM), contact angle, thermal gravimetric analyzer (TGA), differential scanning calorimeter (DSC) and dynamic mechanical analyzer(DMA), respectively.

並列關鍵字

Ag Particle DBSA Clay o-methoxyaniline

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