Fe基高温合金涂层封填C/C-ZrC-SiC复合材料的制备及抗烧蚀机制
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摘要
为了改善C/C-ZrC-SiC复合材料在高超声速飞行器热防护领域的使用性能,采用低压悬浮浸渗法制备出Fe基高温合金涂层封填C/C-ZrC-SiC复合材料。利用XRD、SEM、EDS等手段研究氧乙炔焰烧蚀前后Fe基高温合金涂层封填C/C-ZrC-SiC复合材料表层微观结构演变规律,阐明了Fe基高温合金涂层对C/C-ZrC-SiC复合材料烧蚀行为的影响。结果表明:C/C-ZrC-SiC复合材料在1 650℃的大气环境下并通过低压悬浮浸渗法浸渗2h后,其表层形成一层均匀、致密、且结合紧密的Fe基高温合金涂层。在2 500℃下烧蚀180s后,改性后的C/CZrC-SiC复合材料表面出现较小的烧蚀坑,质量烧蚀率相比未表面改性的试样降低了8%,线烧蚀率降低了35%。且表面生成一层均匀致密的Fe2O3-ZrO2复合氧化物保护层,大大降低了表面裂纹、孔洞等缺陷的产生,从而降低了氧的扩散速率及缺陷带来的应力集中。最终Fe基高温合金覆盖层提高了C/C-ZrC-SiC复合材料的高温抗氧化性和抗机械剥蚀性能。
The C/C-ZrC-SiC composites filled with Fe-based superalloy coating were prepared by low pressure suspension impregnation to improve the C/C-ZrC-SiC composites used in the field of hypersonic flight vehicle's thermal protective performance.The evolution rule of the surface microstructure of the C/C-ZrC-SiC composites filled with Fe-based superalloy before and after oxy-acetylene flame ablation was studied by means of XRD,SEM and EDS.And the effect of the Fe-based superalloy coating on the ablation behavior of the C/C-ZrC-SiC composites was clarified.The results show that the C/C-ZrC-SiC composites are infiltrated by low pressure suspension infiltration at1 650℃for 2 h,and a uniform,dense and tightly bonded Fe-based superalloy coating is formed on the surface.After the ablation at 2 500℃for 180 s,the surface of the modified the C/C-ZrC-SiC composites generates a smaller ablation pit,and the mass and linear ablation rate are reduced by 8%and 35%respectively than the unmodified sample.And a uniform and dense protective layer of the Fe2 O3-ZrO2 composite oxides is formed on the surface,which greatly reduces the occurrence of surface cracks,holes and other defects,thereby reducing the diffusion rate of oxygen and the stress concentration caused by defects.The Fe-based superalloy coating improves the high temperature oxidation resistance and mechanical corrosion resistance of the C/C-ZrC-SiC composites.
The C/C-ZrC-SiC composites filled with Fe-based superalloy coating were prepared by low pressure suspension impregnation to improve the C/C-ZrC-SiC composites used in the field of hypersonic flight vehicle's thermal protective performance.The evolution rule of the surface microstructure of the C/C-ZrC-SiC composites filled with Fe-based superalloy before and after oxy-acetylene flame ablation was studied by means of XRD,SEM and EDS.And the effect of the Fe-based superalloy coating on the ablation behavior of the C/C-ZrC-SiC composites was clarified.The results show that the C/C-ZrC-SiC composites are infiltrated by low pressure suspension infiltration at1 650℃for 2 h,and a uniform,dense and tightly bonded Fe-based superalloy coating is formed on the surface.After the ablation at 2 500℃for 180 s,the surface of the modified the C/C-ZrC-SiC composites generates a smaller ablation pit,and the mass and linear ablation rate are reduced by 8%and 35%respectively than the unmodified sample.And a uniform and dense protective layer of the Fe2 O3-ZrO2 composite oxides is formed on the surface,which greatly reduces the occurrence of surface cracks,holes and other defects,thereby reducing the diffusion rate of oxygen and the stress concentration caused by defects.The Fe-based superalloy coating improves the high temperature oxidation resistance and mechanical corrosion resistance of the C/C-ZrC-SiC composites.
引文
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[16]王玲玲,嵇阿琳,崔红,等.ZrC改性C/C-SiC复合材料的力学性能和抗烧蚀性能[J].复合材料学报,2016,33(2):373-378.WANF L L,JI A L,CUI H,et al.Mechanical and anti-ablative performance of C/C-SiC composites modified by ZrC[J].Acta Materiae Compositae Sinica,2016,33(2):373-378(in Chinese).
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[19]WU G X,YAZHENSKIKH E,HACK K,et al.Viscosity model for oxide melts relevant to fuel slags Part 1:Pure oxides and binary systems in the system SiO2-Al2O3-CaO-MgO-Na2O-K2O[J].Fuel Processing Technology,2015,137:93-103.
[20]武高辉,康鹏超,张强.基于新型防热机理的防热材料的设计与试验验证[J].中国材料进展,2012,31(1):56-61.WU G H,KANG P C,ZHANG Q.The design and test verification of thermal protection materials based on new thermal mechanism[J].Materials China,2012,31(1):56-61(in Chinese).
[21]王梦得.Gr/Al-Si耗散防热材料的设计制备及性能研究[D].哈尔滨:哈尔滨工业大学,2016.WANG M D.Research design fabrication and an properties of Gr/Al-Si dissipative thermal protective materials[D].Harbin:Harbin Institute of Technology,2016(in Chinese).
[22]李冰清.Al20Si/Gr耗散防热材料氧-乙炔和发动机燃烧室烧蚀性能研究[D].哈尔滨:哈尔滨工业大学,2011.LI B Q.Research on the O2-C2H2and ramjet combustor ablation resistance of Al20Si/G transpiring coolant materials[D].Harbin:Harbin Institute of Technology,2011(in Chinese).
[23]姜鹤.Gr/Al-Mg复合材料抗热震性抗烧蚀性能研究[D].哈尔滨:哈尔滨工业大学,2008.JIANG H.Study on properties of thermal shock and ablation resistance for Gr/Al-Mg composites[D].Harbin:Harbin Institute of Technology,2008(in Chinese).
[24]CHANG Y B,SUN W,XIONG X,et al.A novel design of Al-Cr alloy surface sealing for ablation resistant C/C-ZrC-SiCcomposite[J].Journal of the European Ceramic Society,2017,37(2):859-864.
[25]PENG Z,SUN W,XIONG X,et al.A novel Cr-doped Al2O3-SiC-ZrC composite coating for ablative protection of C/C-ZrC-SiC composites[J].Journal of the European Ceramic Society,2018,38(7):2897-2902.
[26]中国国防科学技术工业委员会.烧蚀材料烧蚀试验方法:GJB 323A-96[S].北京:中国标准出版社,1996.China Commission of Science Technology and Industry for National Defense.Test methods for ablation of ablators:GJB323A-96[S].Beijing:China Standards Press,1996(in Chinese).
[27]SCHIEPERS R C J,VAN LOO F J J,DE WITH G.Reaction betweenα-silicon carbide ceramic and nickel or iron[J].Journal of the American Ceramic Society,2010,71(6):214-287.
[28]CHOU T C,JOSHI A,WADSWORTH J.Solid state of SiCwith Co,Ni and Pt[J].Journal of Materials Research,1991,6(4):796-809.
[29]GOTMAM I,GUTMANAS E Y.Microstructure and thermal stability of coated Si3N4and SiC[J].Acta Metallurgica et Materialia,1992,40(1):121-131.
[30]LACAZE J,SUNDMAN B.An assessment of the Fe-C-Si[J].Metallurgical Transactions A,1991,22(10):2211-2223.
[2]姜鹏,匡宇,谢小平,等.国外高超声速飞行器研究现状及发展趋势[J].飞航导弹,2017(7):19-24.JIANG P,KUANG Y,XIE X P,et al.Research status and development trend of hypersonic flight vehicles in abroad[J].Aerodynamic Missile Journal,2007(7):19-24(in Chinese).
[3]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 Q,HU L F,LUO X G,et al.Development of ceramic composite and hot structures for hypersonic vehicles[J].Journal of the Chinese Ceramic Society,2013,41(2):251-260(in Chinese).
[4]刘剑,刘伟强,王琴.C/C复合材料在高超声速飞行器中的应用[J].飞航导弹,2013(5):77-79.LIU J,LIU W Q,WANG Q.Applications of C/C composite materials in hypersonic aircraft[J].Aerodynamic Missile Journal,2013(5):77-79(in Chinese).
[5]曾毅,张武装,熊翔.C/C复合材料SiC/ZrB2-MoSi2复合材料涂层的抗氧化机制[J].复合材料学报,2010,27(3):50-55.ZENG Y,ZHANG W Z,XIONG X.Anti-oxidation mechanisms of the SiC/ZrB2-MoSi2coating on the carbon/carbon composites[J].Acta Materiae Compositae Sinica,2010,27(3):50-55(in Chinese).
[6]白宏德,张虹,叶益聪.浸渍熔渗复合法制备Cf/HfC复合材料及其性能[J].复合材料学报,2016,33(6):1259-1265.BAI H D,ZHANG H,YE Y C.Preparation and property of Cf/HfC composites by liquid impregnation combined reactive melt infiltration[J].Acta Materiae Compositae Sinica,2016,33(6):1259-1265(in Chinese).
[7]张强,崔红,朱阳,等.ZrB2-SiC复相陶瓷涂层制备及其保护C/C-SiC复合材料性能[J].复合材料学报,2018,35(3):640-646.ZHANG Q,CUI H,ZHU Y,et al.Preparation and properties of ZrB2-SiC compound ceramic coating for C/C-SiC composites[J].Acta Materae Compositae Sinica,2018,35(3):640-646(in Chinese).
[8]王少雷,李红,任幕苏,等.ZrC-SiC-C/C复合材料的制备及其烧蚀性能[J].复合材料学报,2017,34(5):1040-1047.WANG S L,LI H,REN M S,et al.Favrication and ablation performances of ZrC-SiC-C/C composites[J].Acta Materiae Compositae Sinica,2017,34(5):1040-1047(in Chinese).
[9]周立,周宇衡.非烧蚀防热材料在高超声速飞行器中的发展[J].飞航导弹,2018(1):14-24.ZHOU L,ZHOU Y H.Developments of nonablative thermal materials in hypersonic aircraft[J].Aerodynamic Missile Journal,2018(1):14-24(in Chinese).
[10]CHEN S A,ZHANG C R,ZHANG Y D,et al.Mechanism of ablation of 3DC/ZrC-SiC composite under an oxyacetylene flame[J].Corrosion Science,2013,68(11):168-175.
[11]YANG X,SU Z A,HUANG Q Z,et al.Microstructure and mechanical properties of C/C-ZrC-SiC composites fabricated by reactive melt infiltration with Zr,Si mixed powders[J].Journal of Materials Science&Technology,2013,29(8):702-710.
[12]WANG Y G,ZHU X J,ZHANG L T,et al.C/C-SiC-ZrCcomposites fabricted by reactive melt inhltration with Si0.87Zr0.13 alloy[J].Ceramics Internationl,2012,38(5):4337-4343.
[13]LI J,YANG X,SU Z A,et al.Effect of ZrC-SiC content on microstructure and ablation properties of C/C composites[J].Transaction of Nonferrous Metals Society of China,2016,26(10):2653-2664.
[14]XIE J,LI K Z,LI H J,et al.Microstructures and ablation resistence of ZrC coating for SiC-coated carbon/carbon composites prepared by supersonic plasma spraying[J].Journal of Thermal Spray Technology,2011,20(6):1286-1291.
[15]LIU C X,CAO L X,CHEN J X,et al.Microstructure and ablation behavior of SiC coated C/C-SiC-ZrC composites prepared by a hybrid infiltration process[J].Carbon,2013,65:196-205.
[16]王玲玲,嵇阿琳,崔红,等.ZrC改性C/C-SiC复合材料的力学性能和抗烧蚀性能[J].复合材料学报,2016,33(2):373-378.WANF L L,JI A L,CUI H,et al.Mechanical and anti-ablative performance of C/C-SiC composites modified by ZrC[J].Acta Materiae Compositae Sinica,2016,33(2):373-378(in Chinese).
[17]ZHANG L,FU Q G,TAN B Y,et al.Ablation behaviour of C/C and C/C-ZrC-SiC composites with cone-shaped holes under an oxyacetylene flame[J].Corrosion Science,2016,102:84-92
[18]LIU L,LI H J,FENG W,et al.Ablation in different heat fluxes of C/C composites modified by ZrB2-ZrC and ZrB2-ZrC-SiC particles[J].Corrosion Science,2013,74:159-167.
[19]WU G X,YAZHENSKIKH E,HACK K,et al.Viscosity model for oxide melts relevant to fuel slags Part 1:Pure oxides and binary systems in the system SiO2-Al2O3-CaO-MgO-Na2O-K2O[J].Fuel Processing Technology,2015,137:93-103.
[20]武高辉,康鹏超,张强.基于新型防热机理的防热材料的设计与试验验证[J].中国材料进展,2012,31(1):56-61.WU G H,KANG P C,ZHANG Q.The design and test verification of thermal protection materials based on new thermal mechanism[J].Materials China,2012,31(1):56-61(in Chinese).
[21]王梦得.Gr/Al-Si耗散防热材料的设计制备及性能研究[D].哈尔滨:哈尔滨工业大学,2016.WANG M D.Research design fabrication and an properties of Gr/Al-Si dissipative thermal protective materials[D].Harbin:Harbin Institute of Technology,2016(in Chinese).
[22]李冰清.Al20Si/Gr耗散防热材料氧-乙炔和发动机燃烧室烧蚀性能研究[D].哈尔滨:哈尔滨工业大学,2011.LI B Q.Research on the O2-C2H2and ramjet combustor ablation resistance of Al20Si/G transpiring coolant materials[D].Harbin:Harbin Institute of Technology,2011(in Chinese).
[23]姜鹤.Gr/Al-Mg复合材料抗热震性抗烧蚀性能研究[D].哈尔滨:哈尔滨工业大学,2008.JIANG H.Study on properties of thermal shock and ablation resistance for Gr/Al-Mg composites[D].Harbin:Harbin Institute of Technology,2008(in Chinese).
[24]CHANG Y B,SUN W,XIONG X,et al.A novel design of Al-Cr alloy surface sealing for ablation resistant C/C-ZrC-SiCcomposite[J].Journal of the European Ceramic Society,2017,37(2):859-864.
[25]PENG Z,SUN W,XIONG X,et al.A novel Cr-doped Al2O3-SiC-ZrC composite coating for ablative protection of C/C-ZrC-SiC composites[J].Journal of the European Ceramic Society,2018,38(7):2897-2902.
[26]中国国防科学技术工业委员会.烧蚀材料烧蚀试验方法:GJB 323A-96[S].北京:中国标准出版社,1996.China Commission of Science Technology and Industry for National Defense.Test methods for ablation of ablators:GJB323A-96[S].Beijing:China Standards Press,1996(in Chinese).
[27]SCHIEPERS R C J,VAN LOO F J J,DE WITH G.Reaction betweenα-silicon carbide ceramic and nickel or iron[J].Journal of the American Ceramic Society,2010,71(6):214-287.
[28]CHOU T C,JOSHI A,WADSWORTH J.Solid state of SiCwith Co,Ni and Pt[J].Journal of Materials Research,1991,6(4):796-809.
[29]GOTMAM I,GUTMANAS E Y.Microstructure and thermal stability of coated Si3N4and SiC[J].Acta Metallurgica et Materialia,1992,40(1):121-131.
[30]LACAZE J,SUNDMAN B.An assessment of the Fe-C-Si[J].Metallurgical Transactions A,1991,22(10):2211-2223.
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