本文選題：溶膠-凝膠 + 相分離　； 參考：《浙江大學(xué)》2016年碩士論文

【摘要】：氧化鋯基多孔材料兼具有氧化鋯基材料低熱導(dǎo)率、高熱穩(wěn)定性以及多孔材料比表面積高、隔熱性好和吸附性好等特點(diǎn),可廣泛用于催化、分離、隔熱等領(lǐng)域。本文綜合論述了氧化釔穩(wěn)定氧化鋯、鋯酸鑭和鋯酸鋇三種氧化鋯基材料的研究現(xiàn)狀,采用溶膠-凝膠伴隨相分離法制備了氧化釔穩(wěn)定氧化鋯、鋯酸鑭以及錯(cuò)酸鋇多孔塊體材料,重點(diǎn)分析了相分離誘導(dǎo)劑、凝膠促進(jìn)劑、溶劑組成以及熱處理溫度對(duì)樣品微觀形貌和多孔結(jié)構(gòu)的影響。制備出的具有共連續(xù)骨架、貫通大孔結(jié)構(gòu)氧化鋯基多孔材料,為氧化鋯基多孔材料的應(yīng)用奠定了重要基礎(chǔ)。主要研究內(nèi)容和結(jié)果如下：(1)以廉價(jià)的氯化物無機(jī)鹽氧氯化鋯、氯化釔為前驅(qū)體,乙醇和去離子水的混合溶液為溶劑,聚氧化乙烯為相分離誘導(dǎo)劑,乙二醇為絡(luò)合劑,甲酰胺為干燥控制化學(xué)添加劑,環(huán)氧丙烷為凝膠促進(jìn)劑,采用溶膠-凝膠伴隨相分離法制備氧化釔穩(wěn)定氧化鋯多孔塊體材料。40℃條件下凝膠反應(yīng)得到的濕凝膠經(jīng)過常壓干燥后可以得到具有共連續(xù)骨架的氧化釔穩(wěn)定氧化鋯多孔塊體。相分離后,相分離誘導(dǎo)劑主要分布在液相中,體系熵的減小是相分離的主要驅(qū)動(dòng)力。釔的摻雜量對(duì)于凝膠微觀形貌影響不大,摻雜0.094～0.337g氯化釔得到的樣品都擁有理想的共連續(xù)骨架,樣品的平均大孔孔徑為1.7μm左右,且孔隙率均超過60%。熱處理后,釔摻雜的氧化鋯多孔塊體沒有出現(xiàn)單斜相氧化鋯晶型,釔的摻雜能夠?qū)ρ趸喌木w結(jié)構(gòu)起到穩(wěn)定化作用；摻雜0.264 g氯化釔得到的樣品經(jīng)800℃熱處理后,平均大孔孔徑因?yàn)闊Y(jié)作用減小至0.7μm,樣品的比表面積也由287m2·g-1降低至34 m2·g-1。(2)以氧氯化鋯、氯化鑭為前驅(qū)體,乙醇和去離子水的混合溶液為溶劑,聚氧化乙烯為相分離誘導(dǎo)劑,乙二醇為絡(luò)合劑,甲酰胺為干燥控制化學(xué)添加劑,環(huán)氧丙烷為凝膠促進(jìn)劑,采用溶膠-凝膠伴隨相分離法制備鋯酸鑭多孔塊體材料。通過優(yōu)化原料比例得到的濕凝膠,在進(jìn)行溶劑置換后常壓干燥,可以得到具有共連續(xù)骨架的鋯酸鑭多孔塊體。樣品干凝膠1100℃熱處理后能夠得到F-結(jié)構(gòu)的鋯酸鑭,提高熱處理溫度F-結(jié)構(gòu)鋯酸鑭向P-結(jié)構(gòu)鋯酸鑭轉(zhuǎn)變；熱處理后得到的樣品中仍含有少量氧化鋯。采用該方法得到的鋯酸鑭塊體熱處理前孔隙率為55%,1100℃熱處理后樣品孔隙率上升至69%,但熱處理前后的樣品比表面積都相對(duì)較低。(3)以氧氯化鋯、氯化鋇為前驅(qū)體,乙醇和去離子水的混合溶液為溶劑,聚氧化乙烯為相分離誘導(dǎo)劑,甲酰胺為干燥控制化學(xué)添加劑,環(huán)氧丙烷為凝膠促進(jìn)劑,乙二醇為絡(luò)合劑,采用溶膠-凝膠伴隨相分離法制備鋯酸鋇多孔塊體材料。通過調(diào)整相分離誘導(dǎo)劑和凝膠促進(jìn)劑的用量,可以制備出具有理想共連續(xù)骨架、平均大孔孔徑為1.8μm、孔隙率高達(dá)63%的鋯酸鋇多孔塊體材料。1100℃熱處理后,樣品中出現(xiàn)通過固相反應(yīng)生成的鋯酸鋇晶型；熱處理后樣品大孔結(jié)構(gòu)變化不大,樣品平均孔徑為1.5μm,孔隙率為65%,但樣品比表面積由熱處理前188m2·g-1降低至0.8 m2·g-1。
[Abstract]:Zirconia based porous materials have the characteristics of low thermal conductivity, high thermal stability, high thermal stability, high surface area, good heat insulation and good adsorbability, and can be widely used in catalysis, separation and heat insulation. This paper deals with the research of three zirconia based zirconia, lanthanum zirconate and barium zirconate. Yttrium oxide stabilized zirconium oxide, lanthanum zirconate and barium silicate porous block materials were prepared by sol-gel adjoint phase separation method. The phase separation inducer, gel promoter, solvent composition and the effect of heat treatment temperature on the micromorphology and porous structure of the sample were emphatically analyzed. The co continuous skeleton and through macroporous structure were prepared. The zirconia based porous material has laid an important foundation for the application of zirconia based porous materials. The main research contents and results are as follows: (1) using the cheap chloride inorganic salt and oxygen zirconium chloride, yttrium chloride as the precursor, the mixed solution of ethanol and deionized water as the solvent, the polyethylene oxide as the phase separation inducer, the ethylene glycol as complexing agent, formyl Amine is a chemical additive for drying control, and the epoxy propane is a gel promoter. The porous yttrium oxide stabilized zirconia porous block material is prepared by the sol-gel accompanying phase separation method. The gel reaction obtained by the gel reaction under the condition of the gel reaction can get the porous yttrium stabilized zirconia porous block with CO continuous skeleton after the gel reaction. Phase separation can be obtained. The phase separation inducer is mainly distributed in the liquid phase. The decrease of the system entropy is the main driving force of the phase separation. The doping amount of yttrium has little effect on the micromorphology of the gel. The samples doped with 0.094 ~ 0.337g yttrium chloride have an ideal co continuous skeleton, the average pore size of the sample is about 1.7 mu, and the porosity is more than 60%. heat. After treatment, the yttrium doped zirconia porous block has no monoclinic zirconia crystal. The doping of yttrium can stabilize the crystal structure of zirconia; the average pore size of the sample doped with 0.264 g yttrium chloride is reduced to 0.7 m after the heat treatment at 800 C, and the specific surface area of the sample is also 287m2. G-1 It is reduced to 34 m2. G-1. (2) with zirconium oxychloride, lanthanum chloride as precursor, mixed solution of ethanol and deionized water as solvent, polyethylene oxide as phase separation inducer, ethylene glycol as complexing agent, formamide as the chemical additive for drying control, epoxy propane as gel promoter, and preparation of lanthanum zirconate porous block by sol-gel adjoint phase separation method The porous lanthanum zirconate block with CO continuous skeleton can be obtained by drying the wet gel obtained by optimizing the proportion of raw materials. The sample dry gel can get F- structure lanthanum zirconate after heat treatment at 1100 C, and improve the heat treatment temperature F- structure lanthanum zirconate to P- structure lanthanum zirconate. After heat treatment, the heat treatment can be obtained. A small amount of zirconium oxide was still contained in the sample. The porosity of the lanthanum zirconate block before heat treatment was 55%, the porosity of the sample increased to 69% after heat treatment at 1100 C, but the surface area of the sample before and after heat treatment was relatively low. (3) zirconium chloride, barium chloride were used as the precursor, and the mixed solution of ethanol and deionized water was used as solvent. Ethylene oxide is a phase separation inducer. Formamide is a chemical additive for drying control. Epoxy propane is a gel promoter and ethylene glycol is the complexing agent. Barium zirconate porous block material is prepared by sol-gel adjoint phase separation method. The ideal co continuous skeleton can be prepared by adjusting the dosage of phase separation inducer and gel promoter. After heat treatment at.1100 C, the average pore size is 1.8 u m and the porosity is up to 63%. The sample appears barium zirconate crystal formed by solid state reaction. The macropore structure changes little after heat treatment, the average pore size is 1.5 mu m and the porosity is 65%, but the surface area of the sample is reduced to 188m2. G-1 before heat treatment. 0.8 m2. G-1.
【學(xué)位授予單位】：浙江大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2016
【分類號(hào)】：TQ174.1

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