以六水合氯化铝(AlCl3·6H2O)、正硅酸乙酯(TEOS)和八水合氧氯化锆(ZrOCl2·8H2O)为混合前驱体,以环氧丙烷(PO)作为凝胶网络诱导剂,乙醇和水作为溶剂,采用溶胶-凝胶工艺和二氧化碳超临界干燥技术制备出了Al2O3-SiO2-ZrO2三元复合气凝胶。研究了不同PO添加量、醇水体积比和Al/Si/Zr摩尔比对其性能和结构的影响,采用扫描电镜、比表面积分析仪和多功能粉体物理特性测试仪对气凝胶的凝胶形态、微观形貌及孔结构进行表征。结果表明:当PO添加量为88mL,醇水体积比为8∶9,Al/Si/Zr摩尔比为12∶3∶1和12∶4∶1时制备出的气凝胶结构性能良好,且凝胶时间在较合适的范围内,具有较低的密度为0.125g/cm3和0.143g/cm3,较高的比表面积为683.14m2/g和684.56m2/g。
Al2O3-SiO2-ZrO2 ternary composite aerogels were prepared by sol-gel process and carbon dioxide supercritical drying technology using aluminum chloride hexahydrate (AlCl3·6H2O),ethyl orthosilicate (TEOS),and zirconium oxychloride octahydrate (ZrOCl2·8H2O) as the mixed precursors,propylene oxide (PO) as the inducer of the gel network,and ethanol and water as the solvents.The effects of different PO additions,alcohol/water volume ratios and Al/Si/Zr molar ratios on the properties and structures of the aerogels were investigated.The gel morphology,microscopic morphology and pore structure of the aerogels were characterized by SEM,surface area analyzer and multi-functional powder physical property tester.The results showed that when the PO addition was 88mL,the alcohol-water volume ratio was 8∶9,and the Al/Si/Zr molar ratios were 12∶3∶1 and 12∶4∶1,the prepared aerogels had good structural properties,and the gelation time was in a more suitable range,with lower densities of 0.125g/cm3 and 0.143g/cm3,and higher specific surface areas of 683.14m2/g and 684.56m2/g.
[1] Uyanna O,Najafi H.Thermal protection systems for space vehicles:a review on technology development,current challenges and future prospects-ScienceDirect[J].Acta Astronautica,2020,176:341-356.
[2] 彭飞,姜勇刚,冯坚,等.耐高温氧化铝气凝胶隔热复合材料研究进展[J].无机材料学报,2021,36(7):673-684.
[3] Fidalgo A,Farinha J P S,Martinho J M G,et al.Nanohybrid silica/polymer aerogels:the combined influence of polymer nanoparticle size and content[J].Materials and Design,2020,189:108521.
[4] Zeng Q,Mao T,Li H D,et al.Thermally insulating lightweight cement-based composites incorporating glass beads and nano-silica aerogels for sustainably energy-saving buildings[J].Energy and Buildings,2018,174:97-110.
[5] 罗丹,龙丽娟,秦舒浩,等.玻璃纤维和碳纤维增强二氧化硅气凝胶复合材料的制备及性能研究[J].化工新型材料,2022,50(4):161-165.
[6] Dai S,Ju Y H,Gao H J,et al.Preparation of silica aerogel using ionic liquids as solvents[J].Chemical Communication,2000,200:243-244.
[7] Poco J F,Satcher Jr J H,Hrubesh L W.Synthesis of high porosity,monolithic alumina aerogels[J].Journal of Non-crystallinc Solids,2001,285:57-63.
[8] 沈军,汪国庆,王珏,等.SiO2气凝胶的常压制备及其热传输特性[J].同济大学学报(自然科学版),2004,32(8):1106-1110.
[9] 王义,张翱,盛兵,等.铝硅酸盐纤维增强Al2O3-SiO2复合材料的制备与性能研究[J].材料研究与应用,2019,13(3):180-186.
[10] Zu G,Shen J,Zou L,et al.Nano engineering super heat-resistant,strong alumina aeroegels[J].Chemistry of Materials,2013,25:4757-4764.
[11] 李智鹏.氧化铝-氧化硅-氧化锆三元复合气凝胶的制备和表征[D].北京:北京化工大学,2014.
[12] 刘旭华.Al2O3-SiO2气凝胶及其高温隔热复合材料的制备与性能研究[D].上海:华东理工大学.
[13] 刘铸汉.SiO2/Al2O3/MgO/ZrO2四元复合气凝胶的制备和表征[D].北京:北京化工大学,2020.
[14] 张冯.Al2O3-SiO2气凝胶的制备及其性能研究[D].北京:北京化工大学,2014.
[15] 陈恒.Al2O3和Al2O3-SiO2气凝胶及其复合材料的制备和性能研究[D].济南:济南大学,2016.
