不同摩尔比Al_2O_3-ZrO_2复合薄膜的性能探究
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摘要
以不同摩尔比(r)的氧化铝(Al_2O_3)溶胶和氧化锆(ZrO_2)溶胶,通过溶胶-凝胶法制备Al_2O_3-ZrO_2复合薄膜,用乌氏黏度计、热重分析仪(TG-DTG)、红外光谱仪(FTIR)、X射线衍射仪(XRD)、扫描电镜(SEM)、比表面积和孔结构分析仪及激光粒度仪对复合膜的黏度、热稳定性、晶相组成、表面形貌、比表面积和孔结构及粒度大小进行表征分析.结果表明,复合溶胶的摩尔比是影响Al_2O_3-ZrO_2复合溶胶黏度和薄膜开裂的重要因素.随着r值的增大,复合膜的黏度减小,开裂度逐渐减缓;r=1的复合溶胶澄清透明,且在干燥后几乎无开裂,黏度为2.64mPa·s;800℃热处理后,r=1的Al_2O_3-ZrO_2复合膜热稳定性良好,结构致密,孔径分布窄,晶粒尺寸为31.30nm,其比表面积、平均孔径分别为84.98m~2/g、9.75nm.
Al_2O_3-ZrO_2 composite membranes have been prepared by sol-gel method using Al_2O_3 and ZrO_2 sols with different molar ratios(r).Ubbelohde viscosity measurements,thermogravimetry(TG-DTG),Fourier transform infrared(FTIR)spectroscopy,X-ray diffraction(XRD),scanning electron microscopy(SEM),and nitrogen adsorption-desorption measurements were employed to analyze the thermal stability,crystal phases,surface morphology,specific surface area and pore structures of the resulting Al_2O_3-ZrO_2 composite membranes.The results showed that varying the Al_2O_3∶ZrO_2 molar ratio in the composite sol had a significant effect on its viscosity,and the viscosity of the composite sol decreased,and the cracking degree after drying decreased more gradually,with increasing r.After thermal treatment at 800°C,the main crystal phase was t-ZrO_2 and the Al_2O_3 in the composite membranes inhibited the crystallization and transparency of ZrO_2 grains.The Al_2O_3-ZrO_2 composite sol with r=1 was clear and transparent and showed no cracking after drying;its viscosity was 2.64 mPa·s.This corresponding Al_2O_3-ZrO_2 composite membrane had good thermal stability,a compact structure,narrow pore size distribution,and a grain size of 31.3 nm.The specific surface area and average pore diameter were 85 m~2/g and 9.8 nm respectively.
Al_2O_3-ZrO_2 composite membranes have been prepared by sol-gel method using Al_2O_3 and ZrO_2 sols with different molar ratios(r).Ubbelohde viscosity measurements,thermogravimetry(TG-DTG),Fourier transform infrared(FTIR)spectroscopy,X-ray diffraction(XRD),scanning electron microscopy(SEM),and nitrogen adsorption-desorption measurements were employed to analyze the thermal stability,crystal phases,surface morphology,specific surface area and pore structures of the resulting Al_2O_3-ZrO_2 composite membranes.The results showed that varying the Al_2O_3∶ZrO_2 molar ratio in the composite sol had a significant effect on its viscosity,and the viscosity of the composite sol decreased,and the cracking degree after drying decreased more gradually,with increasing r.After thermal treatment at 800°C,the main crystal phase was t-ZrO_2 and the Al_2O_3 in the composite membranes inhibited the crystallization and transparency of ZrO_2 grains.The Al_2O_3-ZrO_2 composite sol with r=1 was clear and transparent and showed no cracking after drying;its viscosity was 2.64 mPa·s.This corresponding Al_2O_3-ZrO_2 composite membrane had good thermal stability,a compact structure,narrow pore size distribution,and a grain size of 31.3 nm.The specific surface area and average pore diameter were 85 m~2/g and 9.8 nm respectively.
引文
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[14]郭金玲,沈岳年.用Scherrer公式计算晶粒度应注意的几个问题[J].内蒙古师范大学学报:自然科学版,2009,38(3):357-358.
[15]白周喜,高如琴,周宁生,等.ZrO2含量对Al2O3/ZrO2复相陶瓷微观结构和力学性能的影响[J].硅酸盐通报,2013,32(8):1640-1644.
[16]同帜,霍乐乐,董旭娟,等.溶胶-凝胶法制备氧化锆薄膜的工艺与表征[J].粉末冶金材料科学与工程,2016,21(1):174-179.
[17]同帜,行静,樊璐,等.以硝酸铝为前驱体制备Al2O3薄膜及其表征[J].膜科学与技术,2017,37(5):56-60.
[2]刘志刚.Al2O3-ZrO2陶瓷复合材料的制备和强韧化机理研究[D].青岛:中国海洋大学,2009.
[3]杜红菊.多孔Al2O3-ZrO2陶瓷的微观结构[J].现代技术陶瓷,2015,36(4):50-53.
[4]Gandhi A S,Jayaram V,Chokshi A H.Dense amorphous zirconia-alumina by low-temperature consolidation of spray-pyrolyzed powders[J].J Am Ceram Soc,2010,82(10):2613-2618.
[5]Gandhi A S,Jayaram V,Chokshi A H.Low temperature densificaton behaviour of metastable phases in ZrO2-Al2O3 powders produced by spray pyrolysis[J].Mater Sci Eng A,2001,S304/306(1):785-789.
[6]Gandhi A S,Jayaram V.Pressure consolidation of amorphous ZrO2-Al2O3by plastic deformation of powder particles[J].Acta Mater,2002,50(8):2137-2149.
[7]Gandhi A S,Jayaram V.Plastically deforming amorphous ZrO2-Al2O3[J].Acta Mater,2003,51(6):1641-1649.
[8]李强伟,华小红.Al2O3/ZrO2复合金属陶瓷模具材料的研究[J].中国陶瓷,2014,(11):70-73.
[9]刘国玺,李克智,李国斌.ZrO2添加量对Al2O3-ZrO2复相陶瓷性能的影响[J].兵器材料科学与工程,2015,(4):37-40.
[10]李健生,郝艳霞,张烨,等.以无机盐前驱体制备中空纤维担载Al2O3/ZrO2复合膜[J].稀有金属材料与工程,2006,35(9):1449-1452.
[11]同帜,胡敏盾,董旭娟,等.SiO2-ZrO2复合膜的制备及其工艺参数的研究[J].膜科学与技术,2014,34(6):35-38.
[12]周锋,傅迎庆,梁开明,等.工艺参数对TiO2溶胶黏度及胶凝时间的影响[J].大连海事大学学报,2008,34(4):87-90.
[13]吴东兵,刘羽,牛志睿,等.溶胶-凝胶法制备SiO2的溶胶黏度性能研究[J].陕西科技大学学报,2008,26(2):53-56.
[14]郭金玲,沈岳年.用Scherrer公式计算晶粒度应注意的几个问题[J].内蒙古师范大学学报:自然科学版,2009,38(3):357-358.
[15]白周喜,高如琴,周宁生,等.ZrO2含量对Al2O3/ZrO2复相陶瓷微观结构和力学性能的影响[J].硅酸盐通报,2013,32(8):1640-1644.
[16]同帜,霍乐乐,董旭娟,等.溶胶-凝胶法制备氧化锆薄膜的工艺与表征[J].粉末冶金材料科学与工程,2016,21(1):174-179.
[17]同帜,行静,樊璐,等.以硝酸铝为前驱体制备Al2O3薄膜及其表征[J].膜科学与技术,2017,37(5):56-60.