本文選題：球磨化學(xué)反應(yīng)法　切入點：3Y-ZrO_2　出處：《廣東工業(yè)大學(xué)》2011年碩士論文

【摘要】：氧化鋯陶瓷具有十分優(yōu)異的物理、化學(xué)性能,不僅在科研領(lǐng)域已經(jīng)成為研究熱點,而且在工業(yè)生產(chǎn)中也得到了廣泛的應(yīng)用,是結(jié)構(gòu)材料、耐火材料和電子材料的重要原料。其主要應(yīng)用在：四方氧化鋯多晶體陶瓷、氧化鋯超塑性陶瓷、部分穩(wěn)定氧化鋯陶瓷、氧化鋯生物陶瓷等方面。而3Y-ZrO2(摩爾分數(shù)為3%Y2O3(?)急定的四方相ZrO2陶瓷)作為四方氧化鋯多晶體(TZP)陶瓷的一種,其硬度高,耐磨性、耐腐蝕性能好,常用于嚴酷環(huán)境和苛刻負載條件。因此,3Y-ZrO2的研究一直方興未艾。制備氧化鋯陶瓷粉體的傳統(tǒng)方法有物理法和化學(xué)法兩大類,包括噴霧熱解法、液相法、氣相法、固相法等。 本研究借助固相法固有的優(yōu)勢及特點,利用球磨化學(xué)反應(yīng)法法制備3Y-ZrO2陶瓷粉體。借助TG-DTA分析前驅(qū)體的熱分解過程,通過XRD、TEM、DLS、BET對所得產(chǎn)物進行了表征,并系統(tǒng)地探討了工藝條件對最終產(chǎn)物的平均晶粒粒徑、晶相含量、粒度分布及粉體形貌的影響,研究內(nèi)容如下：(1)通過單因素實驗,考察前驅(qū)體制備過程中各因素(如金屬離子與草酸的摩爾比、球料質(zhì)量比、球磨轉(zhuǎn)速、球磨時間)對最終產(chǎn)物的影響(如平均晶粒粒度、晶相含量、晶體形貌等)；并采用正交試驗對單因素結(jié)果進行優(yōu)化,優(yōu)化結(jié)果顯示各因素對粉體的平均晶粒大小影響順序為：金屬離子與草酸的摩爾比球料質(zhì)量比球磨速度。從節(jié)約原料和提高效率考慮,最佳工藝條件為：金屬離子與草酸的摩爾比1：1.5,球料質(zhì)量比為10：1,球磨時間為1h,球磨速度為200rpm。該工藝條件下所得3Y-ZrO2陶瓷粉體的平均晶粒粒徑為14.0nm,形狀比較規(guī)整,近似球型結(jié)構(gòu),粒度分布均勻,分散性較好。通過對前驅(qū)體進行TG-DTA分析,確定最佳煅燒工藝為：煅燒溫度為650℃,煅燒時間為2h。隨著煅燒溫度的升高,煅燒時間的延長,所得產(chǎn)物的平均晶粒粒徑增大,四方相氧化鋯的含量逐漸減少。(2)在行星球磨制備3Y-ZrO2超細粉體的工藝基礎(chǔ)上,利用攪拌球磨反應(yīng)法進行放大實驗,本次研究放大實驗所制備的3Y-ZrO2超細粉體的表征結(jié)果顯示該粉體粒度分布均勻、分散性良好,其平均晶粒粒徑約為24.9nm,比表面積為32.4608 m2/g。粉體經(jīng)配料球磨24小時后噴霧造粒,粉料成型性能好,表面手感光滑,松裝密度小。燒結(jié)溫度1530度,成瓷后顏色死白,無透感,不吸紅,收縮偏大。分析原因在于原料中鐵雜質(zhì)的含量較高,前驅(qū)體的煅燒過程中,其煅燒工藝未嚴格控制。 (3)選擇放大實驗所得前驅(qū)體進行煅燒試驗,結(jié)果表明,隨著煅燒溫度的升高,煅燒時間的延長,樣品中的平均粒徑增大,四方氧化鋯的體積含量逐漸減少,單斜相氧化鋯的體積含量逐漸增大。在前人的研究結(jié)果上,我們認為本研究理論解釋更接近Garvie的觀點,單斜氧化鋯具有比四方氧化鋯大的表面能。而在一定的溫度和壓力下,隨著氧化鋯粒徑的長大,單斜相與四方相結(jié)構(gòu)之間的表面能差別逐漸減少。
[Abstract]:Zirconia ceramics have excellent physical and chemical properties, not only in the research field has become a research hotspot, but also in industrial production has been widely used as structural materials, Important materials for refractories and electronic materials. Their main applications are: tetragonal zirconia polycrystalline ceramics, zirconia superplastic ceramics, partially stabilized zirconia ceramics, zirconia bioceramics, etc. ) as a kind of tetragonal zirconia polycrystalline ZrO2 ceramics, it has high hardness, wear resistance and corrosion resistance. The traditional methods of preparing zirconia ceramic powders include physical and chemical methods, including spray pyrolysis, liquid phase method, gas phase method, solid phase method and so on. In this study, 3Y-ZrO2 ceramic powders were prepared by ball milling chemical reaction method with the help of the inherent advantages and characteristics of solid state method. The thermal decomposition process of the precursor was analyzed by TG-DTA, and the obtained products were characterized by XRDX Tem Tem DLSX BET. The effects of processing conditions on the average grain size, crystal phase content, particle size distribution and powder morphology of the final product were systematically discussed. The effects of various factors (such as molar ratio of metal ions to oxalic acid, mass ratio of ball to material, ball milling speed, milling time) on the final product (such as average grain size, crystal phase content) were investigated. The single factor results were optimized by orthogonal test. The optimized results show that the order of the influence of various factors on the average grain size of the powder is as follows: the molar ratio of metal ions to oxalic acid is the rate of ball milling. The optimum technological conditions are as follows: the molar ratio of metal ion to oxalic acid is 1: 1.5, the mass ratio of ball to material is 10: 1, the milling time is 1 h, and the milling speed is 200rpm.The average grain size of 3Y-ZrO2 ceramic powder is 14.0 nm, the shape is relatively regular, and the shape is similar to the spherical structure. The particle size distribution is uniform and the dispersity is good. Through the TG-DTA analysis of the precursor, the optimum calcination process is determined as follows: the calcination temperature is 650 鈩，

本文編號：1690187