發(fā)布時間：2018-03-04 02:11

  本文選題：復合納米粒子　切入點：有機硅樹脂　出處：《哈爾濱工業(yè)大學》2015年碩士論文　論文類型：學位論文

【摘要】：隨著科學技術的快速發(fā)展,有機硅樹脂作為一種新型材料廣泛用于航空航天及電子等高端領域。大多數情況下有機硅樹脂都采用高溫固化,為了使有機硅樹脂的機械性能和耐高溫性能得到一定程度上的提升,一般采用提高有機硅樹脂交聯度和添加填料等手段。近年來紫外光固化由于其獨特的優(yōu)勢得到了越來越廣泛的關注,在體系中加入一定含量高分散性的納米粒子更可以有效結合納米粒子的性能以及紫外光快速固化和無溶劑的特點,從而得到性能優(yōu)異的無機-有機納米復合材料體系。本文主要研究的是不同的復合納米粒子改性有機硅樹脂在高溫固化和UV光固化行為的研究,分析不同固化方式對有機硅樹脂的熱穩(wěn)定性能的影響。首先采用兩步法,在高溫水熱條件下合成Co3O4/rm GO,用X射線光電子能譜(XPS)、透射電鏡(TEM)等表征手段對其結構和負載原理進行分析,發(fā)現在合成過程中加入氨水可以調節(jié)鈷離子的水解和氧化以及對石墨烯的結構產生變化,得到N摻雜氧化石墨烯負載納米粒子復合材料Co3O4/N-rm GO。對Co3O4/N-rm GO改性的甲基硅樹脂進行熱分解動力學研究,發(fā)現初始分解溫度由原來的185℃提高到235℃,熱分解活化能E1為87.95247 k J/mol,E2為248.7991 k J/mol,并求出在“回咬”和“重排”過程中甲基硅樹脂的降解速率方程。為了使有機硅樹脂可以在UV下進行固化,在合成甲基硅樹脂的原料中加入γ-甲基丙烯酰氧基硅基丙基三甲氧基硅烷,在p H=4~5,60℃條件下水解縮聚得到帶有雙鍵的丙烯酰氧基有機硅樹脂。通過核磁(NMR),氣相凝膠色譜(GPC)等手段證實所合成樹脂的結構端基為羥基,側鏈帶有酰氧官能團。之后在20 m W/cm2功率下,樣品厚度也為10μm,紫外光引發(fā)劑量為1wt%條件下,得到丙烯酰氧基有機硅樹脂每個自由基所連接的單元數為1153。無機-有機雜化材料在一定程度上結合了納米粒子的高性能以及有機聚合物易加工和改性的特點。因為Ti O2/rm GO對紫外光有一定的吸收能力及催化能力,所以首先我們在水熱條件下通過調節(jié)C2H5O H/H2O的比例得到不同粒徑的Ti O2納米粒子,發(fā)現10nm Ti O2/rm GO納米粒子固化時間和最終轉化率最高,復合納米粒子的的加入量為5%時,轉化率為85%,固化時間為15s。
[Abstract]:With the rapid development of science and technology, silicone resin as a new material widely used in aerospace and other high-end electronic fields. Most cases are silicone resin with high temperature curing, in order to make the mechanical properties of silicone resin and high temperature resistant performance has been improved to a certain extent, improve the use of general silicone resin crosslinking agent and adding filler etc. in recent years, the UV curing method. Because of its unique advantage has been more and more attention, adding some content in the system of nanoparticles with high dispersion can more effectively with nano particle properties and UV curing and non solvent characteristics, so as to obtain excellent properties of organic inorganic nanocomposite materials. This paper mainly studies the system the study of different composite nanoparticles modified silicone resin in high temperature curing and UV curing behavior, divided Effect of thermal stability analysis of different curing methods on silicone resin. The first two steps in high temperature hydrothermal synthesis conditions of Co3O4/rm GO, by X ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM) were characterized by means of the analysis of its structure and load principle, adding hydrolysis and oxidation of ammonia can regulate cobalt now the ions in the process of synthesis and structure on graphene changes, Co3O4/N-rm GO. composite nanoparticles were obtained on Co3O4/N-rm GO modified methyl silicone resin by thermal decomposition kinetics research supported N doped graphene oxide, it is found that the initial decomposition temperature increased from 185 C to 235 C, the activation energy of thermal decomposition of E1 87.95247 K J/mol E2 248.7991 K J/mol, and calculated in the degradation rate equation of methyl silicone resin bite back "and" rearrangement "in the process. In order to make the silicone resin can be cured under UV, Join gamma methacryloxy propyl trimethoxysilane silicon in the synthesis of methyl silicone resin raw materials, with double bond acryloxyl silicone resin in P H=4~5,60 C under the conditions of hydrolysis and condensation by NMR (NMR), gas chromatography gel (GPC) means that the terminal structure of synthetic resin the hydroxyl groups with acyl side chain oxygen functional groups. After 20 m W/cm2 power, the thickness of the sample is 10 m, the UV dose of 1wt% under the condition of the number of units are acryloxyl silicone resin each free radical connected 1153. inorganic organic hybrid materials to a certain extent with nanoparticles high performance organic polymer and easy processing and modification of Ti O2/rm GO. Because of absorptive capacity and catalytic ability of ultraviolet light, so first we under hydrothermal conditions were obtained by adjusting the C2H5O ratio of H/H2O Ti O2 nanoparticles with different particle sizes showed that the curing time and final conversion rate of 10nm Ti O2/rm GO nanoparticles were the highest. When the amount of composite nanoparticles was 5%, the conversion rate was 85%, and the curing time was 15s..

【學位授予單位】：哈爾濱工業(yè)大學
【學位級別】：碩士
【學位授予年份】：2015
【分類號】：TB33

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本文編號：1563677