發(fā)布時間：2018-08-26 07:22

【摘要】：TiO2作為一種光催化劑具有廉價、無毒,在水溶液中穩(wěn)定等優(yōu)點,成為最有開發(fā)前途的綠色環(huán)保型催化劑之一。納米TiO2具備良好的耐侯性、耐化學腐蝕性、抗紫外線能力強、透明性優(yōu)異等特點,用途廣泛。將納米TiO2制備成薄膜既可解決催化劑分離和難回收的問題,還可克服懸浮相催化劑穩(wěn)定性差和易中毒等缺點,具有重要的理論研究和實際應用價值。 本文以鈦酸丁酯、無水乙醇、冰醋酸、高純水為原料,采用溶膠-凝膠(sol-gel)法進行了TiO2粉體和薄膜的制備研究,考察了工藝條件對溶膠、粉體及薄膜性質的影響。通過X射線分析(XRD)、差示掃描量熱(DSC)、光學顯微鏡等測試技術對溶膠、粉體和薄膜進行了表征,主要研究內容及相關結論如下： (1)采用溶膠-凝膠法,研究了不同原料配比及反應溫度對形成凝膠時間的影響,結果表明：溶膠凝膠形成時間隨加水量的增加而縮短；隨無水乙醇用量的增加而延長；隨冰醋酸用量的增加而延長,但達到一定量后再增加冰醋酸用量就會縮短溶膠凝膠形成時間；反應溫度升高溶膠凝膠形成時間縮短。 (2)重點研究了制備TiO2粉體的工藝條件及TiO2粉體晶型轉變的影響因素。優(yōu)化出制備TiO2粉體的合適工藝條件： 鈦酸丁酯、水、無水乙醇、冰醋酸的物質的量之比為1:4:25:1,反應溫度為25℃。 (3)TiO2粉體的晶型轉變過程是一種依賴于升溫速率的動力學過程。TiO2粉體晶型轉變體積分數的增大,其晶型轉變激活能隨之增大； (4)焙燒溫度和焙燒時間是影響TiO2晶體結構轉變的主要因素,隨著焙燒溫度的升高,TiO2晶型結構逐步由無定形態(tài)向銳鈦礦→銳鈦礦和金紅石混合晶型→金紅石轉變；隨焙燒時間的延長,金紅石晶型含量逐漸增大,銳鈦礦相含量逐漸減少； (5)升溫速率、原料配比、強磁場等對TiO2晶體結構沒有太大的影響,影響的只是銳鈦礦型和金紅石型結構TiO2粉體的相對含量； (6)焙燒溫度對TiO2粉體粒度有一定的影響,焙燒溫度的升高,粉體粒度增大；但TiO2粉體的粒度分布變窄； (7)升溫速率對粉體粒度有一定的影響。最高焙燒溫度相同,升溫速率快,所得粉體粒度較��； (8)不同原料配比對粉體粒度有一定的影響。相同焙燒條件下,水量較大時的原料,所制得的粉體粒度較小。 (9)利用正交實驗獲得了旋轉涂膜法制備TiO2薄膜的合適工藝條件： 鈦酸丁酯、水、無水乙醇、冰醋酸的物質的量之比為1:3:25:1、反應溫度為25℃、涂膜次數為2次。
[Abstract]:As a kind of photocatalyst, TiO2 has many advantages, such as low cost, non-toxicity, stability in aqueous solution, etc. It has become one of the most promising green environmental protection catalysts. The problems of separation and hard recovery of the catalyst can also overcome the disadvantages of poor stability and poisoning of the suspended phase catalyst, which has important theoretical research and practical application value.
In this paper, titanium dioxide powder and thin film were prepared by sol-gel method with butyl titanate, anhydrous ethanol, glacial acetic acid and high purity water as raw materials, and the effects of processing conditions on the properties of sol, powder and thin film were investigated. The films were characterized, and the main research contents and conclusions were as follows:
(1) The effects of the ratio of raw materials and reaction temperature on the gelation time were studied by sol-gel method. The results showed that the gelation time was shortened with the increase of the amount of water, prolonged with the increase of the amount of absolute ethanol, and prolonged with the increase of the amount of glacial acetic acid. The sol-gel formation time will be shortened and the formation time of sol-gel will be shortened.
(2) The technological conditions of preparing titanium dioxide powder and the influencing factors of crystal transformation of titanium dioxide powder were studied.
The ratio of butyl titanate, water, absolute alcohol and glacial acetic acid is 1:4:25:1, and the reaction temperature is 25 C.
(3) The crystalline transformation of TiO2 powder is a kinetic process depending on the heating rate, and the activation energy of crystalline transformation increases with the increase of the volume fraction of crystalline transformation.
(4) The calcination temperature and time are the main factors affecting the crystal structure transformation of titanium dioxide. With the increase of calcination temperature, the crystal structure of titanium dioxide gradually transforms from amorphous to anatase-anatase-rutile mixed crystal to rutile. With the increase of calcination time, the rutile content increases gradually and the anatase phase content decreases gradually. Less;
(5) The heating rate, the ratio of raw materials and the strong magnetic field have little effect on the crystal structure of titanium dioxide, but only the relative content of anatase and rutile titanium dioxide powders.
(6) The calcination temperature has certain influence on the particle size of TiO2 powder, the particle size increases with the increase of calcination temperature, but the particle size distribution becomes narrow.
(7) The heating rate has a certain effect on the particle size of the powders.
(8) Different raw material ratios have certain influence on the particle size of the powders. Under the same roasting conditions, the powders prepared with higher water content have smaller particle size.
(9) the suitable technological conditions for preparing TiO2 thin films by rotating coating method were obtained by orthogonal experiment.
The mass ratio of butyl titanate, water, ethanol and glacial acetic acid is 1:3:25:1, the reaction temperature is 25 C and the coating times are 2 times.
【學位授予單位】：東北大學
【學位級別】：碩士
【學位授予年份】：2011
【分類號】：TB383.2;TB383.3

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