本文選題：非水解溶膠-凝膠法　切入點(diǎn)：鈦酸鋁　出處：《景德鎮(zhèn)陶瓷學(xué)院》2010年碩士論文

【摘要】： 本研究以無水三氯化鋁和四氯化鈦為前驅(qū)體,正丁醇為氧供體,采用非水解溶膠-凝膠法,創(chuàng)新性地運(yùn)用回流結(jié)合容彈凝膠化工藝合成鈦酸鋁納米粉體。借助XRD、SEM、TEM、FT-IR、DTA-TG等測(cè)試手段研究了不同凝膠化工藝、前驅(qū)體濃度、PEG的分子量(用量)及添加時(shí)機(jī)等工藝參數(shù)對(duì)鈦酸鋁的低溫合成及其分散效果的影響;此外,對(duì)比分析了不同合成方法對(duì)鈦酸鋁陶瓷燒結(jié)性能的影響。 同時(shí),還系統(tǒng)地對(duì)非水解溶膠-凝膠法制備的鈦酸鋁粉體進(jìn)行了穩(wěn)定化研究,借助FT-IR、XRD、DTA-TG、熱膨脹儀等測(cè)試手段研究了鐵、鎂源種類及用量和鎂源的加入時(shí)機(jī)等對(duì)低溫穩(wěn)定鈦酸鋁效果的影響,并對(duì)穩(wěn)定鈦酸鋁的熱膨脹特性及燒結(jié)性能進(jìn)行了研究。 研究表明:回流及容彈凝膠化工藝條件下,較優(yōu)的溶劑分別為三氯甲烷和二氯甲烷, PEG的引入會(huì)大大影響鈦酸鋁的低溫合成效果;在回流結(jié)合容彈凝膠化的工藝條件下,前驅(qū)體濃度為2.25mol/L,在回流工藝之后容彈工藝之前引入占前驅(qū)體總質(zhì)量3wt%的PEG1000,可合成出平均粒徑為20-30nm的鈦酸鋁納米粉體。鈦酸鋁凝膠中Al-O-Ti鍵的形成是非水解溶膠凝膠法能在750℃低溫合成鈦酸鋁的關(guān)鍵;采用非水解溶膠-凝膠法回流結(jié)合容彈的凝膠化工藝制備的鈦酸鋁粉體燒結(jié)體的抗折強(qiáng)度高達(dá)18.3MPa,是固相法的6.3倍,水解法的2.5倍。 鎂、鐵的醇鹽和其無水有機(jī)酸鹽能在750℃低溫下使鐵、鎂離子進(jìn)入鈦酸鋁晶格,起到穩(wěn)定鈦酸鋁的作用。鎂鐵復(fù)合摻雜穩(wěn)定鈦酸鋁效果明顯優(yōu)于單一鐵、鎂摻雜,且固定摻雜量為20mol%(鐵、鎂摻雜量比例為1:1)時(shí),穩(wěn)定化效果最優(yōu),合成的鈦酸鋁粉體在1100℃保溫80h不分解,熱膨脹系數(shù)僅為-0.039×10-6/℃。鎂源改性劑引入時(shí)機(jī)在鋁、鈦前驅(qū)體發(fā)生縮聚反應(yīng)之后加入的穩(wěn)定效果較優(yōu)。
[Abstract]:In this study, anhydrous aluminum trichloride and titanium tetrachloride were used as precursors and n-butanol as oxygen donor. Aluminum titanate nanocrystalline powders were synthesized by refluxing and capacitive gelation process. Different gelation processes were studied by means of XRDX SEMX TEMT FT-IRT DTA-TG and so on. The effects of molecular weight (dosage) of precursor concentration of PEG and adding time on the low temperature synthesis and dispersion effect of aluminum titanate were studied, and the effects of different synthesis methods on sintering properties of aluminum titanate ceramics were compared and analyzed. At the same time, the stabilization of aluminum titanate powder prepared by non-hydrolytic sol-gel method was studied systematically. Iron was studied by means of FT-IRX XRDX DTA-TG, thermal expansion instrument, etc. The effects of the type and amount of magnesium source and the addition time of magnesium source on the effect of stabilizing aluminum titanate at low temperature were studied. The thermal expansion characteristics and sintering properties of stabilized aluminum titanate were also studied. The results show that the optimal solvents are trichloromethane and dichloromethane under the conditions of reflux and elastomeric gelation, and the introduction of PEG will greatly affect the low temperature synthesis of aluminum titanate, The concentration of precursor is 2.25mol / L, and PEG1000, which accounts for 3wt% of the total mass of precursor, is introduced before the reflux process. The formation of Al-O-Ti bond in aluminum titanate gel is unhydrolyzed sol-gel with the average particle size of 20-30nm. The key to the synthesis of aluminum titanate at 750 鈩，

本文編號(hào)：1661989