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納米二氧化鈦粉體制備工藝及其性能研究_畢業(yè)論文初稿-閱讀頁

2024-09-15 21:48本頁面
  

【正文】 1 1 2 7 2 A n a t a s e T i O 2 圖 43 煅燒溫度為 600℃條件下制備樣品 TO12 的 XRD 衍射圖譜 從以上圖中可以看出 ,不同煅燒溫度條件下制備的納米二氧化鈦微粉試樣的主要的強(qiáng)峰均為 Anatase-銳鈦礦( 101) ,證明在溶液 PH 值為 , 400~600℃煅 燒時(shí)的產(chǎn)物晶體結(jié)構(gòu)為純銳鈦型,此溫度段制備的銳鈦礦型純度非常高。 20 30 40 50 60 702 T h e t a ( 176。 圖 34 是不同煅燒溫度條件下制備的二氧化鈦樣品的 XRD 圖譜。(如圖35 為樣品 TO12 的 XRD 衍射圖譜的擬合報(bào)告可知:銳鈦礦相的特征峰出現(xiàn)在2θ 176。、 176。、 176。、 176。、 176。、 176。附近對(duì)應(yīng)的晶面指數(shù)如圖 33 分別為( 101)、( 103)、( 004)、( 112)、( 200)、( 105)、( 211)、( 213)、( 20( 116)、( 220)、( 107)、( 215)、( 301)。 大約在 600 攝氏度時(shí),衍射峰變得尖銳,此時(shí)樣品的晶化已經(jīng)相當(dāng)完全,晶型轉(zhuǎn)變基本完成。因此煅燒溫度在 400℃ ~600℃之間生成的 TiO2易于轉(zhuǎn)變?yōu)榻Y(jié)晶度高的銳鈦礦晶體。用 德國布魯克 D8 系列 X 射線(粉末)衍射儀 , 用一步為 176。 范圍獲得 XRD 圖譜。 Anatase(101)Anatase(103) Anatase(004)Anatase(112)Anatase(200)Anatase(105)Anatase(211)Anatase(213)Anatase(204)Anatase(116)Anatase(220)Anatase(215)Anatase(301)10 20 30 40 50 60 70 802 T h e t a ( 176。05010 015 020 025 030 035 040 045 0Intensity(Counts)[ z hao x unn aT O 6. ra w ] 1 2038 6 1 1 5 7 A n a t a s e T i 0 . 7 2 O 2 圖 37 溶液 PH 值為 條件下制備樣品 TO6 的 XRD 衍射圖譜 從以上圖中可以看出 ,不 同 PH 值條件下制備的納米二氧化鈦微粉試樣的主要的強(qiáng)峰均為 Anatase- 銳鈦礦( 101) ,證明在溶液 PH 值為 ~, 500℃煅燒時(shí)的產(chǎn)物晶體結(jié)構(gòu)為純銳鈦型,制備的銳鈦礦型純度非常高。010 020 030 040 050 0Intensity(Counts)[ z hao x unn aT O 4. ra w ] 4 7[ z hao x unn aT O 5. ra w ] 4 7[ z hao x unn aT O 6. ra w ] 1 2038 6 1 1 5 7 A n a t a s e T i 0 . 7 2 O 2( d )( e )( f ) 圖 38 不同 PH 值溶液制備樣品的 XRD 衍射圖譜 ( d) 、( e) 、( f) 圖 38 是不同 PH 值溶液制備的二氧化鈦樣品的 XRD 圖譜。比較發(fā)現(xiàn) ,在酸性條件下,隨著溶液 PH 值增大 ,衍射峰半高寬減小,峰強(qiáng)度增加 ,晶化特征逐漸明顯 。 說明隨煅燒溫度的升高 ,晶體發(fā)育趨于完好 ,結(jié)晶度提高。由于納米二氧化鈦具有很強(qiáng)的吸收紫外線能力、奇特的顏色效應(yīng)、較好的熱穩(wěn)定性、化學(xué)穩(wěn)定性和優(yōu)良的光學(xué)、電學(xué)及力學(xué)等方面的特性,其中銳鈦礦型具有較高的催化效率,金紅石型結(jié)構(gòu)比較穩(wěn)定具有較強(qiáng)的覆蓋力、著色力和紫外線吸收能力。 致謝 本 論 文 的工作 是在朱協(xié)彬 院長 的悉心指導(dǎo)下完成的。在做畢業(yè)設(shè)計(jì)期間,從 選擇課題 、搜索資料、確定實(shí)驗(yàn)方案、購買實(shí)驗(yàn)材料、配置實(shí)驗(yàn)設(shè)備、進(jìn)行探索實(shí)驗(yàn)、到最后進(jìn)行論文寫作的過程中遇到了不少的困難,但都在朱院長的悉心指導(dǎo)及不斷地鼓勵(lì)下克服了。當(dāng)時(shí)朱院長的認(rèn)真、負(fù)責(zé)、孜孜不倦的科研及教學(xué)精神給予了我極大的精神支持及工作動(dòng)力。 朱院長在教學(xué)及科研過程中比較嚴(yán)謹(jǐn)、嚴(yán)肅,但在與學(xué)生交流的過程中卻非常平易近人、和藹。 同時(shí)還要感謝實(shí)驗(yàn)過程中陶峰博士、陳志浩博士、劉明朗老師及陳偉、張孟、陳靜等幾位研究生的幫助和指導(dǎo)!并且感謝銀橋科貿(mào)有限公司對(duì)我們?cè)囼?yàn)原材料的支持!謝謝你們! 附錄 A 外文文獻(xiàn)及翻譯 Effect of pH on TiO2 nanoparticles via sol gel method Siti Aida Ibrahim, and Srimala Sreekantan Abstract― A series of titania nanoparticles was successfully synthesized via sol gel method using titanium tetraisopropoxide as a precursor. In this paper, data concerning the effect of pH towards the development of TiO2 nanoparticles is reported. The samples were characterised by xray diffraction (XRD) and Scanning Electron Microscopy (SEM). XRD results showed the existence of nanocrystalline anatase phases with crystallite size ranging from 714 nm. Surface morphological studies obtain from SEM micrograph showed the particles with rodlike shape are rutile while the spherical shapes are anatase in nature. It was also found the pH of the solution affect the agglomeration of the particles. Results of photocatalytic studies exhibits that titania powder prepared at pH 9 has an excellent photocatalytic activity with degradation % within 60 minutes. Keywords: TiO2 nanoparticles, sol gel, photocatalytic Ⅰ INTRODUCTION ITANIA ( TiO2) nanoparticles is a promising materials and widely used in many applications due to its high photocatalytic activity [1,2] , excellent gassensitive properties [3] and dielectric properties [4]. Crystalline titania has three modification phases which are rutile (tetragonal, P42 /mnm), anatase (tetragonal, I41/amd) and brookite (orthorhombic, Pcab). Anatasetype TiO2 has excellent photocatalytic activity and widely used as catalysts for deposition of a wide variety of anic and inanic pollutants. Many methods have been established for titania synthesis such as solgel technique [58], hydrothermal method [5,9], chemical vapor deposition [10] , direct oxidation and others. Among them, the solgel technique is one of the most used methods due to its possibility of deriving unique metastable structure at low reaction temperatures and excellent chemical homogeinity. In sol gel processes, TiO2 is usually prepared by the reactions of hydrolysis and polycondensation of titanium alkoxide, (TiOR)n to form oxopolymers, which are transformed into anoxide work. These reactions can be schematically represented as follows: Hydrolysis: M(OR)n+H2O→M(OR) n1(OH)+ROH (1) Condensation Dehydration: M(OR)n+M(OR)n1→M 2O(OR)2n2+ROH (2) Dealcoholation: 2M(OR)n1(OH) →M 2O(OR)2n2+H2O (3) the overall reaction is M(OR)n+H2O→MO n/2+nROH (4) where M= Si, Ti, Zr, etc and R = alkyl group. The relative rates of hydrolysis and polycondensation strongly affected the structure and properties of metal oxides. Factors that crucial in the formation of metal oxides includes reactivity of metal alkoxides, water to alkoxides ratio, pH of reaction medium, nature of solvent and additives and reaction temperature. By varying these process parameters, materials with different surface chemistry and microstructure can be obtained. Typically, in sol gel method, the solgel derived precipitates are amorphous in nature. Therefore, it is require for further heat treatment to induce crystallization. To induce transition from amorphous to anatase phase, generally an annealing temperature higher than 300 176。C. Characterization. The titania samples were characterized by powder Xray diffraction (XRD) with Bruker D8 powder diffractometer (40 kV, 30mA) using CuKα radiation (λ= 197。 by step scanning mode with the step size of 176。. It is also noticed that pH affects particles size and degree of crystallinity. A trace of rutile was found in sample prepared at pH 1 at
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