溶胶—凝胶法制备钛酸铝薄膜的工艺研究
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摘要
本文首先创新性地用硝酸铝(Al(NO_3)_3·9H_2O)替代铝醇盐作为铝源,钛酸丁酯作为钛源,采用水解溶胶-凝胶法(HSG)制备钛酸铝薄膜。在此基础上,以无水三氯化铝和四氯化钛为前驱体原料,乙醇为氧供体,在国际上首次采用非水解溶胶-凝胶法(NHSG)制备钛酸铝薄膜。同时本文还首次对NHSG法制备的钛酸铝进行了稳定化掺杂改性。运用偏光显微镜、DTA-TG、XRD、Zeta电位计、FE-SEM等测试手段优化了HSG法和NHSG法制备钛酸铝镀膜溶胶的工艺、不同基片的镀膜工艺以及薄膜的热处理工艺,并对两种方法所制钛酸铝薄膜的性能进行了初步研究;借助FT-IR对比研究了HSG法和NHSG法制备钛酸铝的溶胶-凝胶转变过程。结果表明:
HSG法制备钛酸铝薄膜时,制备镀膜溶胶的最优工艺参数如下:前驱体浓度为0.6mol/L、乙酰丙酮与钛酸丁酯的摩尔比为1:1、pH值为1、陈化时间为72h;优化的镀膜工艺为:浸渍提拉速度为1mm/s、3次镀膜、对多孔的莫来石基片和表面粗糙的碳化硅基片每次浸渍时间分别为30s和10s;在HSG法制得的钛酸铝凝胶中,铝多以Al~(3+)的形式富集于Ti-O-Ti凝胶网络之间,钛酸铝薄膜的合成温度为1350℃;制得的薄膜具有较好的抗铝熔体侵蚀性能和良好的抗硝酸钠熔体腐蚀性能。
NHSG法制备钛酸铝薄膜时,优选AGSE作为溶剂,制备镀膜溶胶的最优工艺参数如下:前驱体浓度为0.6mol/L、四丁基溴化铵用量为0.5g/100ml溶胶、陈化温度为110℃、陈化时间为8h;在NHSG法制得的钛酸铝凝胶中形成了Al-O-Ti键合,钛酸铝薄膜的合成温度为750℃;所制的薄膜具有较好的抗硝酸钠熔体腐蚀性能,热处理温度升至1350℃后,薄膜的抗硝酸钠熔体腐蚀性能较750℃时有明显提高。
此外本文还运用XRD、FT-IR及热膨胀仪等测试手段对NHSG法制备的钛酸铝进行了稳定化掺杂改性的初步研究,结果表明:以乙醇铁、乙醇镁或醋酸镁为稳定掺杂剂时,铁、镁离子能在1050℃低温下进入钛酸铝的晶格:镁掺杂时,镁稳定剂须在铝、钛前驱体发生缩聚反应之后引入;乙醇铁、乙醇镁和两者复合掺杂后样品平均热膨胀系数(20～1000℃)由掺杂前的8.779×10~(-6)/℃分别降至0.578×10~(-6)/℃、0.502×10~(-6)/℃和-0.140×10~(-6)/℃,为NHSG法所制钛酸铝薄膜的改性打下了坚实的基础。
Aluminum titanate film has been prepared by hydrolytic sol-gel method (HSG) creatively using aluminum nitrate to substitute for aluminium alkoxide as aluminum source, tetrabutyl titanate as titanium source. Based on this, aluminum titanate film has also been prepared by nonhydrolytic sol-gel method (NHSG) for the first time internationally using anhydrous aluminum chloride and titanium tetrachloride as precursors, ethanol as oxygen donor. Meanwhile, the aluminum titanate prepared via nonhydrolytic sol-gel route has firstly been stabilized by doping modification. The preparation process of aluminum titanate coating sol, coating technology of different substrates and heat treatment process of film has been optimized by polarizing microscope, DTA-TG, XRD, Zeta potentiometer, FE-SEM and so on. The performance of aluminum titanate film prepared by above two methods has been preliminarily studied. The sol-gel transition process of aluminum titanate prepared by the two methods has also been comparatively researched by FT-IR. The study shows the following results.
When aluminum titanate film is prepared by HSG method, the optimum procedure parameters are as follows: the precursors concentration is 0.6mol/L, the molar ratio of acetylacetone to butyl titanate equals to 1 : 1, the pH value and aging time are 1 and 72h, respectively. The optimal coating parameters are as follows: vertical sliding velocity is 1mm/s, coating for three times, the dipping time for porous mullite substrate and coarse silicon carbide substrate are 30s and 10s separately. In the aluminum titanate gel prepared by HSG method, the aluminum is located among the Ti-O-Ti gel net in the form of Al~(3+), which leads to the synthesis temperature of aluminum titanate is as high as 1350℃. The film has a good performance of antierosion to aluminum melt and sodium nitrate melt.
AGSE is the optimal solvent when the aluminum titanate film is prepared by NHSG method. The optimum procedure parameters are as follows: the precursors concentration equals to 0.6mol/L, the dosage of tetrabutyl ammonium bromide is 0.5g/100ml sol, the aging temperature and the aging time are 110℃and 8h, respectively. The Al-O-Ti bond is formed in the aluminum titanate gel prepared by NHSG method which results in the synthesis temperature of aluminum titanate film decrease to 750℃. The film has a good performance of anticorrosion to sodium nitrate melt and the performance is improved obviously when the heat treat temperature rise to 1350℃.
In addition, the stabilization doping modification to aluminum titanate prepared by NHSG method has also been preliminarily studied by XRD, FT-IR and thermal expansion instrument. The results show that magnesian ion and iron ion can be dopped into the lattice of aluminum titanate at a low temperature of 1050℃when magnesium ethoxide, iron ethoxide or magnesium acetate was used as dopant. Magnesium dopants should be added after the polycondensation of aluminum and titanium precursors. The average thermal expansion coefficients of samples(20℃to 1000℃) decrease from 8.779×10~(-6)/℃before modification to 0.578×10~(-6)/℃, 0.502×10~(-6)/℃and -0.140×10~(-6)/℃separately when using iron ethoxide, magnesium ethoxide and their compound as dopants.
HSG法制备钛酸铝薄膜时,制备镀膜溶胶的最优工艺参数如下:前驱体浓度为0.6mol/L、乙酰丙酮与钛酸丁酯的摩尔比为1:1、pH值为1、陈化时间为72h;优化的镀膜工艺为:浸渍提拉速度为1mm/s、3次镀膜、对多孔的莫来石基片和表面粗糙的碳化硅基片每次浸渍时间分别为30s和10s;在HSG法制得的钛酸铝凝胶中,铝多以Al~(3+)的形式富集于Ti-O-Ti凝胶网络之间,钛酸铝薄膜的合成温度为1350℃;制得的薄膜具有较好的抗铝熔体侵蚀性能和良好的抗硝酸钠熔体腐蚀性能。
NHSG法制备钛酸铝薄膜时,优选AGSE作为溶剂,制备镀膜溶胶的最优工艺参数如下:前驱体浓度为0.6mol/L、四丁基溴化铵用量为0.5g/100ml溶胶、陈化温度为110℃、陈化时间为8h;在NHSG法制得的钛酸铝凝胶中形成了Al-O-Ti键合,钛酸铝薄膜的合成温度为750℃;所制的薄膜具有较好的抗硝酸钠熔体腐蚀性能,热处理温度升至1350℃后,薄膜的抗硝酸钠熔体腐蚀性能较750℃时有明显提高。
此外本文还运用XRD、FT-IR及热膨胀仪等测试手段对NHSG法制备的钛酸铝进行了稳定化掺杂改性的初步研究,结果表明:以乙醇铁、乙醇镁或醋酸镁为稳定掺杂剂时,铁、镁离子能在1050℃低温下进入钛酸铝的晶格:镁掺杂时,镁稳定剂须在铝、钛前驱体发生缩聚反应之后引入;乙醇铁、乙醇镁和两者复合掺杂后样品平均热膨胀系数(20～1000℃)由掺杂前的8.779×10~(-6)/℃分别降至0.578×10~(-6)/℃、0.502×10~(-6)/℃和-0.140×10~(-6)/℃,为NHSG法所制钛酸铝薄膜的改性打下了坚实的基础。
Aluminum titanate film has been prepared by hydrolytic sol-gel method (HSG) creatively using aluminum nitrate to substitute for aluminium alkoxide as aluminum source, tetrabutyl titanate as titanium source. Based on this, aluminum titanate film has also been prepared by nonhydrolytic sol-gel method (NHSG) for the first time internationally using anhydrous aluminum chloride and titanium tetrachloride as precursors, ethanol as oxygen donor. Meanwhile, the aluminum titanate prepared via nonhydrolytic sol-gel route has firstly been stabilized by doping modification. The preparation process of aluminum titanate coating sol, coating technology of different substrates and heat treatment process of film has been optimized by polarizing microscope, DTA-TG, XRD, Zeta potentiometer, FE-SEM and so on. The performance of aluminum titanate film prepared by above two methods has been preliminarily studied. The sol-gel transition process of aluminum titanate prepared by the two methods has also been comparatively researched by FT-IR. The study shows the following results.
When aluminum titanate film is prepared by HSG method, the optimum procedure parameters are as follows: the precursors concentration is 0.6mol/L, the molar ratio of acetylacetone to butyl titanate equals to 1 : 1, the pH value and aging time are 1 and 72h, respectively. The optimal coating parameters are as follows: vertical sliding velocity is 1mm/s, coating for three times, the dipping time for porous mullite substrate and coarse silicon carbide substrate are 30s and 10s separately. In the aluminum titanate gel prepared by HSG method, the aluminum is located among the Ti-O-Ti gel net in the form of Al~(3+), which leads to the synthesis temperature of aluminum titanate is as high as 1350℃. The film has a good performance of antierosion to aluminum melt and sodium nitrate melt.
AGSE is the optimal solvent when the aluminum titanate film is prepared by NHSG method. The optimum procedure parameters are as follows: the precursors concentration equals to 0.6mol/L, the dosage of tetrabutyl ammonium bromide is 0.5g/100ml sol, the aging temperature and the aging time are 110℃and 8h, respectively. The Al-O-Ti bond is formed in the aluminum titanate gel prepared by NHSG method which results in the synthesis temperature of aluminum titanate film decrease to 750℃. The film has a good performance of anticorrosion to sodium nitrate melt and the performance is improved obviously when the heat treat temperature rise to 1350℃.
In addition, the stabilization doping modification to aluminum titanate prepared by NHSG method has also been preliminarily studied by XRD, FT-IR and thermal expansion instrument. The results show that magnesian ion and iron ion can be dopped into the lattice of aluminum titanate at a low temperature of 1050℃when magnesium ethoxide, iron ethoxide or magnesium acetate was used as dopant. Magnesium dopants should be added after the polycondensation of aluminum and titanium precursors. The average thermal expansion coefficients of samples(20℃to 1000℃) decrease from 8.779×10~(-6)/℃before modification to 0.578×10~(-6)/℃, 0.502×10~(-6)/℃and -0.140×10~(-6)/℃separately when using iron ethoxide, magnesium ethoxide and their compound as dopants.
引文
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