本文選題：溶液燃燒法 + 凝膠反應(yīng)　； 參考：《蘭州大學(xué)》2015年碩士論文

【摘要】：溶液燃燒法是燃燒法的一種,溶液的成分主要由金屬離子的鹽類(lèi)作為的氧化劑,有機(jī)化合物作為的燃料組成,溶液在不同的環(huán)境下經(jīng)過(guò)燃燒后形成相應(yīng)的化合物。溶液燃燒法主要運(yùn)用于制備金屬氧化物、碳化物、氮化物、硼化物、鋁化合物等納米材料。溶液燃燒法中不需要提供能夠讓金屬化合物結(jié)晶所需的所有熱量,只需要用達(dá)到燃料燃點(diǎn)的溫度來(lái)引起燃料燃燒,通過(guò)燃燒釋放出的熱量使化合物結(jié)晶形成不同的結(jié)構(gòu)得到產(chǎn)物。常用的溶液燃燒法有兩個(gè)步驟：(1)大多數(shù)的溶液配置過(guò)程包含溶液向膠體轉(zhuǎn)換并最終形成凝膠的過(guò)程；(2)燃燒過(guò)程。因此最終溶液燃燒會(huì)成為凝膠燃燒。通常實(shí)驗(yàn)中的前驅(qū)體溶液經(jīng)過(guò)凝膠反應(yīng)形成由金屬鹽與醇類(lèi)組成的螯合物。目前關(guān)于溶液燃燒法的研究報(bào)告很多,但由于溶液燃燒法的反應(yīng)速率非�？�,很難控制產(chǎn)物的形貌、尺寸、結(jié)構(gòu)、分散性等,而在納米材料中上述參數(shù)通常對(duì)性能有著決定性的影響,因此針對(duì)這些問(wèn)題提出改進(jìn)方法也是現(xiàn)在溶液燃燒法的主要研究課題。納米ZnO具有非常優(yōu)良的物理和化學(xué)性能,并且根據(jù)文獻(xiàn)記載納米ZnO的形貌非常多,隨著實(shí)驗(yàn)條件的輕微改變就能體現(xiàn)在形成的ZnO納米結(jié)構(gòu)上。因此本工作的設(shè)計(jì)是通過(guò)溶液燃燒法制備納米ZnO,通過(guò)改變實(shí)驗(yàn)條件達(dá)到控制ZnO的納米結(jié)構(gòu)的目的,并通過(guò)光催化輔助了解每種ZnO納米結(jié)構(gòu)的光催化性能。(一)傳統(tǒng)的溶液燃燒法制備ZnO納米結(jié)構(gòu)傳統(tǒng)的溶液燃燒法主要是指在反應(yīng)過(guò)程中形成凝膠,本文中的凝膠方法為Pechini法。前驅(qū)體的成分為硝酸鋅、檸檬酸、去離子水和乙二醇。前驅(qū)體通過(guò)金屬硝酸鹽與檸檬酸的醇溶液形成螯合物的方式將溶液轉(zhuǎn)變成凝膠,之后對(duì)凝膠進(jìn)行燃燒制備ZnO納米結(jié)構(gòu)。在實(shí)驗(yàn)設(shè)計(jì)中,分別對(duì)硝酸鋅與檸檬酸的質(zhì)量比、去離子水與乙二醇的體積比及凝膠反應(yīng)時(shí)間對(duì)ZnO納米結(jié)構(gòu)的影響等幾方面進(jìn)行了討論,并對(duì)所形成的ZnO納米結(jié)構(gòu)的光催化性能進(jìn)行了測(cè)試。(二) 以PVP為燃料的溶液燃燒法制備ZnO納米結(jié)構(gòu)以PVP為燃料的溶液燃燒法主要是指反應(yīng)中沒(méi)有溶液向凝膠轉(zhuǎn)變的過(guò)程,實(shí)驗(yàn)主要是通過(guò)PVP模板的作用來(lái)形成ZnO納米結(jié)構(gòu)。前驅(qū)體溶液中的成分是乙酸鋅、PVP、酒精與去離子水。將溶液攪拌成透明淡綠色時(shí)進(jìn)行燃燒反應(yīng),前驅(qū)體溶液依舊呈膠狀,但并不是形成凝膠,主要原因是由于PVP是一種大分子聚合物,溶解在溶液中呈現(xiàn)出一種粘稠的狀態(tài),沒(méi)有凝膠形成是與傳統(tǒng)溶液燃燒法的本質(zhì)區(qū)別。在實(shí)驗(yàn)設(shè)計(jì)中,分別從反應(yīng)溫度、升溫速率、乙酸鋅加入量、酒精與去離子水的體積比對(duì)ZnO納米結(jié)構(gòu)的影響等幾個(gè)方面進(jìn)行了討論,并對(duì)其不同ZnO納米結(jié)構(gòu)的光催化性能進(jìn)行了研究。
[Abstract]:Solution combustion is a kind of combustion method. The composition of solution is mainly composed of salts of metal ions as oxidant and organic compounds as fuel. The solution is burned in different environments to form corresponding compounds. Solution combustion method is mainly used in the preparation of metal oxides, carbides, nitrides, boride, aluminum compounds and other nanomaterials. The solution combustion process does not need to provide all the heat needed to allow the metal compounds to crystallize; it only requires a temperature that reaches the fuel ignition point to cause the fuel to burn. The compounds are crystallized into different structures by the heat released by combustion. The common solution combustion method has two steps: 1) most of the solution configuration processes include the process of solution to colloid conversion and finally the formation of gel. Therefore, the final solution combustion will become gel combustion. The precursor solution in the experiment usually reacts with gel to form a chelate composed of metal salts and alcohols. At present, there are many reports on solution combustion method, but because the reaction rate of solution combustion method is very fast, it is difficult to control the morphology, size, structure, dispersity of the product, etc. The above parameters usually have a decisive effect on the properties of nanomaterials, so it is also the main research topic of solution combustion method to propose an improved method to solve these problems. Nanocrystalline ZnO has excellent physical and chemical properties, and the morphology of nanocrystalline ZnO is very numerous according to the literature. With the slight change of experimental conditions, it can be reflected in the formed ZnO nanostructures. Therefore, the design of this work is to prepare nanocrystalline ZnOs by solution combustion method, to control the nanostructures of ZnO by changing the experimental conditions, and to understand the photocatalytic properties of each ZnO nanostructure by photocatalytic assistance. (1) the traditional solution combustion method for the preparation of ZnO nanostructure mainly refers to the formation of gel in the reaction process. The gel method in this paper is Pechini method. The precursors are zinc nitrate, citric acid, deionized water and ethylene glycol. The precursor transformed the solution into a gel by chelating the metal nitrate with the citric acid alcohol solution, and then burned the gel to prepare the ZnO nanostructure. The effects of the mass ratio of zinc nitrate and citric acid, the volume ratio of deionized water to ethylene glycol and the gel reaction time on the ZnO nanostructures were discussed. The photocatalytic properties of the ZnO nanostructures were tested. (2) ZnO nanostructures were prepared by solution combustion method using PVP as fuel. Solution combustion method with PVP as fuel mainly refers to the process of transition from solution to gel in the reaction. The experiment mainly involves the formation of ZnO nanostructures by the action of PVP template. The precursors are zinc acetate PVP, alcohol and deionized water. When the solution is stirred to a translucent greenish green, the precursor solution is still colloidal, but not a gel. The main reason is that PVP is a macromolecular polymer that dissolves in the solution and presents a viscous state. No gel formation is essentially different from conventional solution combustion. In the experimental design, the effects of reaction temperature, heating rate, the amount of zinc acetate added, the volume ratio of alcohol to deionized water on the ZnO nanostructures were discussed. The photocatalytic properties of different ZnO nanostructures were studied.
【學(xué)位授予單位】：蘭州大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類(lèi)號(hào)】：TB383.1;O614.241

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