發(fā)布時(shí)間：2018-03-04 02:11

  本文選題：復(fù)合納米粒子　切入點(diǎn)：有機(jī)硅樹(shù)脂　出處：《哈爾濱工業(yè)大學(xué)》2015年碩士論文　論文類(lèi)型：學(xué)位論文

【摘要】：隨著科學(xué)技術(shù)的快速發(fā)展,有機(jī)硅樹(shù)脂作為一種新型材料廣泛用于航空航天及電子等高端領(lǐng)域。大多數(shù)情況下有機(jī)硅樹(shù)脂都采用高溫固化,為了使有機(jī)硅樹(shù)脂的機(jī)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(jī)硅樹(shù)脂交聯(lián)度和添加填料等手段。近年來(lái)紫外光固化由于其獨(dú)特的優(yōu)勢(shì)得到了越來(lái)越廣泛的關(guān)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(jié)合納米粒子的性能以及紫外光快速固化和無(wú)溶劑的特點(diǎn),從而得到性能優(yōu)異的無(wú)機(jī)-有機(jī)納米復(fù)合材料體系。本文主要研究的是不同的復(fù)合納米粒子改性有機(jī)硅樹(shù)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(duì)有機(jī)硅樹(shù)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(xiàn)光電子能譜(XPS)、透射電鏡(TEM)等表征手段對(duì)其結(jié)構(gòu)和負(fù)載原理進(jìn)行分析,發(fā)現(xiàn)在合成過(guò)程中加入氨水可以調(diào)節(jié)鈷離子的水解和氧化以及對(duì)石墨烯的結(jié)構(gòu)產(chǎn)生變化,得到N摻雜氧化石墨烯負(fù)載納米粒子復(fù)合材料Co3O4/N-rm GO。對(duì)Co3O4/N-rm GO改性的甲基硅樹(shù)脂進(jìn)行熱分解動(dòng)力學(xué)研究,發(fā)現(xiàn)初始分解溫度由原來(lái)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(guò)程中甲基硅樹(shù)脂的降解速率方程。為了使有機(jī)硅樹(shù)脂可以在UV下進(jìn)行固化,在合成甲基硅樹(shù)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(jī)硅樹(shù)脂。通過(guò)核磁(NMR),氣相凝膠色譜(GPC)等手段證實(shí)所合成樹(shù)脂的結(jié)構(gòu)端基為羥基,側(cè)鏈帶有酰氧官能團(tuán)。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(jī)硅樹(shù)脂每個(gè)自由基所連接的單元數(shù)為1153。無(wú)機(jī)-有機(jī)雜化材料在一定程度上結(jié)合了納米粒子的高性能以及有機(jī)聚合物易加工和改性的特點(diǎn)。因?yàn)門(mén)i O2/rm GO對(duì)紫外光有一定的吸收能力及催化能力,所以首先我們?cè)谒疅釛l件下通過(guò)調(diào)節(jié)C2H5O H/H2O的比例得到不同粒徑的Ti O2納米粒子,發(fā)現(xiàn)10nm Ti O2/rm GO納米粒子固化時(shí)間和最終轉(zhuǎn)化率最高,復(fù)合納米粒子的的加入量為5%時(shí),轉(zhuǎn)化率為85%,固化時(shí)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(xué)位授予單位】：哈爾濱工業(yè)大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類(lèi)號(hào)】：TB33

【參考文獻(xiàn)】

相關(guān)期刊論文 前1條

1 馬悅欣;劉坤;周楠;;甲基苯基硅樹(shù)脂及其復(fù)合材料的性能研究[J];化學(xué)與粘合;2007年06期

相關(guān)博士學(xué)位論文 前1條

1 聶仁峰;石墨烯基材料的制備及其在多相催化中的應(yīng)用[D];浙江大學(xué);2014年

相關(guān)碩士學(xué)位論文 前2條

1 白惠文;氧化石墨烯改性有機(jī)硅樹(shù)脂耐熱性的研究[D];哈爾濱工業(yè)大學(xué);2012年

2 劉艷;有機(jī)硅樹(shù)脂基透波材料的制備及性能研究[D];濟(jì)南大學(xué);2014年

，

本文編號(hào)：1563677