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不同類型核殼結(jié)構(gòu)二氧化硅的制備與表征

發(fā)布時(shí)間:2018-03-12 19:07

  本文選題:核殼結(jié)構(gòu) 切入點(diǎn):光譜分析 出處:《山東師范大學(xué)》2015年碩士論文 論文類型:學(xué)位論文


【摘要】:近年來(lái),“納米熱”已經(jīng)是越來(lái)越讓人們所熟悉,與納米材料有關(guān)的研究與應(yīng)用的成果也源源不斷的出現(xiàn)在我們世人的眼前[1]。其中的有關(guān)納米級(jí)的半導(dǎo)體材料的研究與應(yīng)用也開(kāi)始越來(lái)越受到人們的重視!Si作為第一代的半導(dǎo)體材料,它的地位與重要性是無(wú)法被取代的[2-3]。自核殼介孔SiO2納米材料的出現(xiàn)開(kāi)始,各國(guó)的科學(xué)家制備出了許多種不同形貌的核殼SiO2納米材料(例如球狀、棒狀、片狀等)[4-9]。 美國(guó)加利福尼亞大學(xué)的Sang Hoon Joo[10]等人采用溶膠-凝膠法,充分水解了正硅酸四乙酯,然后采用了十四烷基三甲基溴化銨(TTAB)制備出了高性能的Pt/SiO2。許多科學(xué)家采用這種方法合成出來(lái)的核殼介孔SiO2的外貌和尺寸等,我們都可以通過(guò)對(duì)表面活性劑的調(diào)整來(lái)調(diào)節(jié)它們的尺寸大小[11-15]。Zhang[16]等人將正硅酸四乙酯水解,合成了有序介孔的SiO2磁性核殼納米材料,這種核殼的優(yōu)點(diǎn)有很多,例如:核殼的大小、厚度以及磁性粒子的包裹量都是可以進(jìn)行調(diào)整的,并且這種核殼納米材料的密度很低,殼層的比表面積較高,介孔的孔徑大。趙東元等[17]用Stober法制備出了一種形態(tài)較為完整的核殼-結(jié)構(gòu)介孔SiO2微球,這種方法制備的微球的直徑大約在400nm,球形狀態(tài)較為完整,并且介孔的孔徑為3nm左右。Hyeon[18-22]課題組采用了一種新的方法,他們制備出了一種單分散性較好的Fe3O4/SiO2微球,采用這種方法制備的磁性SiO2微球的順磁性很強(qiáng),微球粒子的尺寸非常的均一,但是它存在的缺點(diǎn)就是:這種SiO2微球磁強(qiáng)度較低、而且關(guān)鍵的是它的表面結(jié)構(gòu)沒(méi)有一定的順序性,這些缺點(diǎn)導(dǎo)致了它其在領(lǐng)域的應(yīng)用與研究相對(duì)的匱乏。 本文主要講述了兩種不同核殼結(jié)構(gòu)納米SiO2材料的制備與表征。: 第一種核殼介孔二氧化硅的方法:第一步,,采用水解TEOS的方法制備SiO2微球,第二步:采用溶膠-凝膠法,在二氧化硅微球的表面包裹上一層有序介孔的SiO2核殼。第二種就是PS/SiO2核殼及二氧化硅空心球。第一步,制備聚苯乙烯微球,第二步,在聚苯乙烯微球的表面采用特殊的表面活性劑,制備上一種二氧化硅殼層;此時(shí)就已經(jīng)制備好了PS/SiO2核殼,并對(duì)其進(jìn)行各種表征。但是我們想到PS微球在高溫中能夠揮發(fā)的特點(diǎn),利用此特性,對(duì)樣品進(jìn)行高溫煅燒,除去聚苯乙烯球體,得到核殼二氧化硅空心微球。采用溶膠-凝膠法在特定條件下制備了核-殼二氧化硅微球,利用TEM和Raman光譜分別對(duì)核殼SiO2的微觀結(jié)構(gòu)進(jìn)行了觀察和光譜分析。分析結(jié)果表明:制備的核殼孔SiO2樣品,是由外表面為孔徑7nm,厚度30nm的SiO2殼層,包裹著核為直徑為200nm的實(shí)心SiO2微球所組成,核殼的介孔殼層的比表面積較大,同時(shí)還具備著良好的光譜性質(zhì)。
[Abstract]:In recent years, the "nano heat" is more and more people are familiar with the research and application of nano materials related to the results of Everfount also appeared in the research and application of nano semiconductor materials we the eyes of the world of the [1]. which also began to more and more people pay more attention to Si as the first generation of semiconductor materials! The position and importance of it is cannot be replaced from the [2-3]. core-shell mesoporous SiO2 nano materials, preparation of scientists prepared many different morphologies of SiO2 core-shell nano materials (such as spherical, rod, sheet etc.) [4-9].
The University of California Sang Hoon Joo[10] et al by using sol-gel method, the hydrolysis of TEOS four fully acetate, and then using the fourteen alkyl three methyl bromide (TTAB) was prepared by core-shell mesoporous SiO2 high performance Pt/SiO2. many scientists using this method, the synthesis of appearance and size, we can the surfactant adjustment to adjust the size of [11-15].Zhang[16], they will four ethyl orthosilicate hydrolysis, SiO2 magnetic core-shell nano ordered mesoporous materials were synthesized, there are a lot of advantages, such as: the core-shell core-shell magnetic particle size, thickness and the amount of all can be adjusted. And this kind of core-shell nano material density is very low, the shell of high specific surface area, pore diameters. Zhao Dongyuan [17] Stober was prepared by core-shell morphology is a complete - The structure of mesoporous SiO2 microspheres, microspheres prepared by this method is about 400nm diameter, spherical state is complete, and the pore size of mesoporous 3nm.Hyeon[18-22] research group has adopted a new method, they prepared a good monodisperse Fe3O4/SiO2 microspheres, magnetic SiO2 microspheres using this method the preparation of CIS strong magnetic microspheres, uniform particle size is very, but it has the drawback is: the SiO2 magnetic microspheres with low strength, but the key is the surface structure of it without certain order, these shortcomings led to it in the field of research and application of relative scarcity.
In this paper, the preparation and characterization of two nano SiO2 materials with different nuclear shell structures are described.
The first method of core-shell mesoporous silica by hydrolysis method: the first step, the preparation of TEOS SiO2 microspheres, the second step by a sol-gel method on the surface of silica microspheres coated with a layer of ordered mesoporous SiO2 core shell. The second is the PS/SiO2 core-shell and hollow silica spheres. The first step. Preparation of polystyrene microspheres, the second step, using special surfactant on the surface of polystyrene microspheres, preparation of a silica shell; this has prepared PS/SiO2 core-shell, and characterized by many. But we have the characteristics of PS microspheres in high temperature volatilization, using this characteristic of high temperature calcination of samples, removal of the polystyrene spheres, core-shell silica hollow microspheres were obtained by sol-gel method. Under certain conditions the preparation of core-shell silica microspheres, using TEM and Raman spectra respectively of core shell SiO The microstructure of 2 were analyzed and observed spectra. Analysis results show that the core-shell hole SiO2 sample preparation, is composed of outer surface diameter 7Nm, thickness 30nm SiO2 shell, which is wrapped around the nuclear 200nm diameter SiO2 solid microspheres, core-shell mesoporous shell of the specific surface area is large at the same time, also has a good spectral properties.

【學(xué)位授予單位】:山東師范大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2015
【分類號(hào)】:TB383.1;O613.72

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