本文關(guān)鍵詞： Stober法 二氧化硅微球 電子封裝 一步法 連續(xù)滴加法　出處：《西安電子科技大學(xué)》2015年碩士論文　論文類型：學(xué)位論文

【摘要】：本文致力于通過Stober法合成用于電子封裝中的二氧化硅微球。我們首先探討了二氧化硅的廣闊應(yīng)用前景,以尋求它的潛在應(yīng)用價(jià)值。文中綜述了Stober法的來源及相關(guān)的研究工作進(jìn)展,以及Stober法中二氧化硅微球的合成機(jī)理及基于亞顆粒團(tuán)聚和單體添加的生長(zhǎng)模型。在一步添加法中,研究了反應(yīng)時(shí)間、溫度、正硅酸乙酯濃度、水濃度及氨濃度對(duì)微球形貌、粒徑和分布的影響。其中隨著反應(yīng)時(shí)間的延長(zhǎng),顆粒粒徑隨之增大,但反應(yīng)較為迅速,在一到兩小時(shí),反應(yīng)已基本完成。反應(yīng)溫度越高,顆粒粒徑越小,同時(shí)單分散性也變差。隨著水濃度的提高,顆粒的均勻性變好,同時(shí)顆粒的粒徑先增加后減小,在12mol/L附近時(shí)達(dá)到最大值。正硅酸乙酯的濃度越高,顆粒粒徑越大。當(dāng)氨濃度從0.5mol/L增加到3mol/L時(shí),顆粒的粒徑隨之增大,但粒徑分布傾向于變寬。為了擴(kuò)大微球的粒徑,減少初期成核的微晶核的數(shù)目,采用連續(xù)滴加法,在水解液中滴加硅源溶液,以獲得更少的晶核。試樣的掃描電子顯微鏡圖片表明:攪拌速率越低,最終獲得的微球越均一,在高的攪拌速率下,微球呈現(xiàn)多尺度的分布。使用激光粒度散射儀測(cè)量了顆粒的粒度分布,發(fā)現(xiàn)顆粒呈單分散分布。為了進(jìn)一步減少初期的成核數(shù)目,通過在水解液中添加電解質(zhì)氯化鉀,降低亞顆粒的表面電位,加速顆粒的團(tuán)聚作用。在滴加速率為0.834ml/min時(shí),當(dāng)氯化鉀濃度從0mM到6mM時(shí),顆粒的粒徑增加,分布更均勻。隨著滴加速率的降低,顆粒自由生長(zhǎng)過程的延長(zhǎng),顆粒的粒徑增加,均勻性增強(qiáng)。共溶劑中水的濃度越低,顆粒的均勻性越好。
[Abstract]:This paper is devoted to the synthesis of silica microspheres for electronic packaging by Stober method. In order to seek its potential application value, this paper reviews the source and related research progress of Stober method, the synthesis mechanism of silica microspheres in Stober method and the growth model based on sub-particle agglomeration and monomer addition. The effects of reaction time, temperature, ethyl orthosilicate concentration, water concentration and ammonia concentration on the morphology, particle size and distribution of microspheres were studied. The reaction was basically completed. The higher the reaction temperature, the smaller the particle size and the worse the monodispersity. With the increase of water concentration, the uniformity of the particle became better, and the particle size first increased and then decreased. The higher the concentration of ethyl orthosilicate, the larger the particle size. When ammonia concentration increased from 0.5 mol / L to 3 mol / L, the particle size increased, but the particle size distribution tended to widen. The number of micrystalline nuclei in the initial nucleation was reduced, and the silicon source solution was added in the hydrolysate by a continuous drop addition method to obtain fewer crystal nuclei. The SEM images of the samples showed that the lower the stirring rate, the more uniform the final microspheres were obtained. At high stirring rate, the microspheres show a multi-scale distribution. The particle size distribution is measured by laser particle size scattering instrument, and the particle size distribution is found to be monodisperse. In order to further reduce the nucleation number in the initial stage, the particle size distribution is found to be monodisperse. By adding electrolyte potassium chloride to the hydrolysate, the surface potential of the sub-particles was decreased and the agglomeration of the particles was accelerated. When the dropping rate was 0.834 ml / min, the particle size increased when the concentration of potassium chloride was from 0 mm to 6 mm. With the decrease of dropping rate and the prolongation of the free growth process, the particle size increases and the uniformity increases. The lower the concentration of water in the co-solvent, the better the uniformity of the particles.
【學(xué)位授予單位】：西安電子科技大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：TQ127.2

【參考文獻(xiàn)】

相關(guān)期刊論文 前10條

1 邢彥君;趙小磊;王建莉;侯翠霞;;微球材料研究進(jìn)展[J];廣州化工;2015年11期

2 賈寧寧;高延敏;周超;宋東坡;;工藝因素對(duì)溶膠-凝膠法制備SiO_2微球粒徑的影響[J];武漢科技大學(xué)學(xué)報(bào);2013年01期

3 孫立國(guó);趙冬梅;玄立春;張貞浴;欒羽佳;李佰林;;二氧化硅微球的制備及自組裝[J];黑龍江大學(xué)自然科學(xué)學(xué)報(bào);2012年01期

4 姜小陽(yáng);李霞;;納米二氧化硅微球的應(yīng)用及制備進(jìn)展[J];硅酸鹽通報(bào);2011年03期

5 ;Size control of monodisperse nonporous silica particles by seed particle growth[J];Particuology;2011年03期

6 楊水金;王敏;楊小三;;二氧化硅負(fù)載磷鎢雜多酸催化合成環(huán)己酮乙二醇縮酮[J];稀有金屬;2007年04期

7 毛丹;姚建曦;王丹;;有機(jī)溶劑對(duì)正硅酸乙酯水解制備二氧化硅微球的影響[J];稀有金屬材料與工程;2007年S1期

8 李曦;劉連利;王莉莉;;納米二氧化硅的研究現(xiàn)狀與進(jìn)展[J];渤海大學(xué)學(xué)報(bào)(自然科學(xué)版);2006年04期

9 何清玉,郭鍇,王琳;超重力反應(yīng)沉淀法制備超細(xì)二氧化硅[J];無(wú)機(jī)鹽工業(yè);2005年09期

10 霍玉秋,閆玉濤,劉曉霞,丁津原,翟玉春,田彥文;單分散納米SiO_2的制備及其作為潤(rùn)滑油添加劑的摩擦學(xué)性能研究[J];摩擦學(xué)學(xué)報(bào);2005年01期

，

本文編號(hào)：1517892