磷酸盐热防护陶瓷瓦修复剂及耐高温性能分析
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摘要
针对热防护陶瓷瓦的损伤修复,研制了一种磷酸盐修复剂,通过扫描电镜(SEM)、差式扫描量热(DSC)以及X射线衍射分析(XRD)等方法,对磷酸盐修复剂的微观形貌、物相结构与耐高温性能进行研究,最后通过拉伸剪切实验对其高温机械性能进行测试和分析。结果表明:10%纳米Al N的加入可以促进树脂与固化剂的反应,降低固化温度,并提高其与碳化硅陶瓷的粘附强度;过量的纳米Al N会使固化反应剧烈,导致修复剂表面疏松,从而降低剪切强度。磷酸盐(Al PO4(10-0423))在高温时(1 000℃)转变成更稳定的磷酸盐晶体(Al PO4(11-0500)),增强了其高温环境下的稳定性。该研究可为重复使用飞行器热防护系统(TPS)的设计与修复提供参考。
In this study,we developed a nano-modified inorganic phosphate repair agent to repair damage to ceramic insulation tiles. The microstructure,phase structure and high temperature resistance were researched through scanning electron microscope( SEM),differential scanning calorimeter( DSC) and X-ray diffraction( XRD). Finally,the mechanical properties at high temperature were tested and analyzed by tensile shear test. The results show that10% nano-aluminum nitride( Al N) can promote the behavior of the resin as a curing agent,then reduce the curing temperature and increase the adhesion strength. An excessive amount of nano-AlN causes a severe curing reaction,which results in the loosening of the repair agent surface,thereby reducing the shear strength. Phosphate Al PO4( 10-0423) is converted to more stable phosphate crystals Al PO4( 11-0500) at high temperature( 1 000 ℃),which enhances the heat-resistant stability of the repair agent. This study can provide a reference for the design and repair of Thermal protection system( TPS) for reusable launch vehicle.
In this study,we developed a nano-modified inorganic phosphate repair agent to repair damage to ceramic insulation tiles. The microstructure,phase structure and high temperature resistance were researched through scanning electron microscope( SEM),differential scanning calorimeter( DSC) and X-ray diffraction( XRD). Finally,the mechanical properties at high temperature were tested and analyzed by tensile shear test. The results show that10% nano-aluminum nitride( Al N) can promote the behavior of the resin as a curing agent,then reduce the curing temperature and increase the adhesion strength. An excessive amount of nano-AlN causes a severe curing reaction,which results in the loosening of the repair agent surface,thereby reducing the shear strength. Phosphate Al PO4( 10-0423) is converted to more stable phosphate crystals Al PO4( 11-0500) at high temperature( 1 000 ℃),which enhances the heat-resistant stability of the repair agent. This study can provide a reference for the design and repair of Thermal protection system( TPS) for reusable launch vehicle.
引文
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[12]CHASSEAUD P T. Adhesives,syntactics and laminating resins for aerospace repair and maintenance applications from Ciba specialty chemicals[J]. International journal of adhesion and adhesives,1999,19(2/3):217-229.
[13]HIGGINS A. Adhesive bonding of aircraft structures[J].International journal of adhesion and adhesives,2000,20(5):367-376.
[14]HAN H J,KIM D P. Studies on curing chemistry of aluminum-chromium-phosphates as low temperature curable binders[J]. Journal of sol-gel science and technology,2003,26(1/2/3):223-228.
[15]WANG C,HUANG Y D,WANG B. Study on heat-resistant property of adhesive/carbon-carbon composites joints[J]. International journal of adhesion and adhesives,2006,26(4):206-211.
[16]WANG Xiaozhou,WANG Jun,WANG Hao. A heat-resistant organic adhesive for joining Al2O3ceramics in air and argon atmosphere[J]. Journal of manufacturing processes,2017,26:67-73.
[17]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会. GB/T 7124-2008,胶粘剂拉伸剪切强度的测定(刚性材料对刚性材料)[S].北京:中国标准出版社,2008.General Administration of Quality Supervision,Inspection and Quarantine of the People's Republic of China,Standardization Administration of China. GB/T 7124-2008,Adhesives-determination of tensile lap-shear strength of rigid-to-rigid bonded assemblies[S]. Beijing:Standards Press of China,2008.
[2]杨亚政,杨嘉陵,方岱宁.高超声速飞行器热防护材料与结构的研究进展[J].应用数学和力学,2008,29(1):47-56.YANG Yazheng,YANG Jialing,FANG Daining. Research progress on the thermal protection materials and structures in hypersonic vehicles[J]. Applied mathematics and mechanics,2008,29(1):47-56.
[3]王康太,冯坚,姜永刚,等.陶瓷纤维刚性隔热瓦研究进展[J].材料导报,2011,25(12):35-39.WANG Kangtai,FENG Jian,JIANG Yonggang,et al. Development of ceramic fiber rigid insulation tiles[J]. Materials review,2011,25(12):35-39.
[4]鲁芹,胡龙飞,罗晓光,等.高超声速飞行器陶瓷复合材料与热结构技术研究进展[J].硅酸盐学报,2013,41(2):251-260.LU Qin,HU Longfei,LUO Xiaoguang,et al. Development of ceramic composite and hot structures for hypersonic vehicles[J]. Journal of the Chinese ceramic society,2013,41(2):251-260.
[5]PAUL A,BINNER J,VAIDHYANATHAN B,et al. UHTC composites for hypersonic applications[J]. American ceramic society bulletin,2012,91(1):22-28.
[6]FAHRENHOLTZ W G,HILMAS G E. Ultra-high temperature ceramics:materials for extreme environments[J].Scripta materialia,2017,129:94-99.
[7]袁庆智,孙越强,王世金,等.天基微小空间碎片探测研究[J].空间科学学报,2005,25(3):212-217.YUAN Qingzhi,SUN Yueqiang,WANG Shijin,et al. Research of micro-space-debris detection[J]. Chinese journal of space science,2005,25(3):212-217.
[8]WALKER J D. The trail to the leading edge:detective work in san Antonio led to understanding the loss of Columbia[J]. Mechanical engineering,2004,126(3):28-31.
[9]CLARK S,LARIN M,ROCHELLE B. NASA shuttle orbiter reinforced carbon Carbon(RCC)crack repair arc-jet testing[C]//Proceedings of ASME District E Student Professional Development. Edinburg:American Society of Mechanical Engineers,2007.
[10]SINGH M. In-space repair of reinforced carbon-carbon thermal protection system structures[C]//Proceedings of the 29th International Conference on Advanced Ceramics and Composites. Cocoa Beach,Florida,2005:3-9.
[11]李阳,汪涛.高超声速飞行器TPS破损修复涂料[J].宇航材料工艺,2011,41(4):32-35.LI Yang,WANG Tao. Repair coating for TPS of hypersonic vehicles[J]. Aerospace materials&technology,2011,41(4):32-35.
[12]CHASSEAUD P T. Adhesives,syntactics and laminating resins for aerospace repair and maintenance applications from Ciba specialty chemicals[J]. International journal of adhesion and adhesives,1999,19(2/3):217-229.
[13]HIGGINS A. Adhesive bonding of aircraft structures[J].International journal of adhesion and adhesives,2000,20(5):367-376.
[14]HAN H J,KIM D P. Studies on curing chemistry of aluminum-chromium-phosphates as low temperature curable binders[J]. Journal of sol-gel science and technology,2003,26(1/2/3):223-228.
[15]WANG C,HUANG Y D,WANG B. Study on heat-resistant property of adhesive/carbon-carbon composites joints[J]. International journal of adhesion and adhesives,2006,26(4):206-211.
[16]WANG Xiaozhou,WANG Jun,WANG Hao. A heat-resistant organic adhesive for joining Al2O3ceramics in air and argon atmosphere[J]. Journal of manufacturing processes,2017,26:67-73.
[17]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会. GB/T 7124-2008,胶粘剂拉伸剪切强度的测定(刚性材料对刚性材料)[S].北京:中国标准出版社,2008.General Administration of Quality Supervision,Inspection and Quarantine of the People's Republic of China,Standardization Administration of China. GB/T 7124-2008,Adhesives-determination of tensile lap-shear strength of rigid-to-rigid bonded assemblies[S]. Beijing:Standards Press of China,2008.