Y_2O_3耐火材料的制备及其与Zr合金界面反应研究
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摘要
通过在1650,1700,1750℃下烧结6 h制备纯Y_2O_3坩埚,并利用Y_2O_3坩埚真空感应熔炼Zr-4合金。借助X射线衍射(XRD),扫描电子显微镜(SEM),能谱分析仪(EDS)等手段研究了不同烧结温度下制备的Y_2O_3坩埚致密度变化,分析了Y_2O_3耐火材料与锆合金间的界面反应,研究了两者界面反应机制。研究结果表明:1650℃下烧成的坩埚晶粒生长不完全,团聚现象严重,致密度约为87%;1700℃下烧成的坩埚晶粒生长完整,未发现明显的团聚,致密度约为95%;1750℃下烧成的坩埚晶粒生长更加完整,无团聚与二次结晶现象,致密度约为97%;选用1750℃下制备的坩埚熔炼锆合金,熔炼后的坩埚结构完整,界面处没有新相生成,并未见合金熔体渗入现象;熔炼实验后,坩埚与合金界面处有黑色区域生成,可能是由于Y_2O_3坩埚微结构的变化引起;合金中分布有大量无规则Y的氧化夹杂物;由于Y_2O_3耐火材料在高温熔体作用下剥落,一部分耐火材料被搅拌入合金熔体中成为夹杂,另一部分分解为Y,O侵入合金熔体并重新结合生成稳定的Y_2O_3,过量的O以游离态存在于合金基体中。
Y_2O_3 crucible was prepared by sintering at 1650,1700,1750℃for 6 h,respectively.And Zr-4 alloy was melted in Y_2O_3 crucible with vacuum induction melting method.The density change of Y_2O_3 crucible prepared at different sintering temperature and the interface reaction between zirconium alloy and Y_2O_3 refractory were examined by X-ray diffraction(XRD),scanning electron microscope(SEM),energy dispersive spectroscope(EDS),then the interface reaction mechanism was explored.The results indicated the grain growth of crucible was incomplete and agglomeration was serious at 1650℃for 6 h,the relative density was approximately87%.The grain growth of crucible was complete and no agglomeration was observed at 1700℃for 6 h,the relative density was approximately 95%.The grain growth of crucible was more complete than that of crucible sintered at 1650 and 1700℃,no agglomeration and secondary crystallization was found at 1750℃for 6 h,and the relative density was approximately 97%.The crucible prepared at1750℃was selected for melting.The crucible structure was complete and no Zr-4 alloy melt penetration was observed after melting.However,some black area were generated at the interface of crucible and alloy,which might be due to the change of Y_2O_3 crucible microstructure.A large number of irregular Y oxide inclusions distributed in the alloy,which was due to that Y_2O_3 refractory was desquamated under the action of high temperature melt,and one part refractory was stirred into the melt alloy as inclusions,the other part refractory was decomposed into Y and O,and infiltrated into alloy melt and regenerated stable Y_2O_3 phase,meanwhile,excessive oxygen atoms existed in the alloy substrate as a free state.
Y_2O_3 crucible was prepared by sintering at 1650,1700,1750℃for 6 h,respectively.And Zr-4 alloy was melted in Y_2O_3 crucible with vacuum induction melting method.The density change of Y_2O_3 crucible prepared at different sintering temperature and the interface reaction between zirconium alloy and Y_2O_3 refractory were examined by X-ray diffraction(XRD),scanning electron microscope(SEM),energy dispersive spectroscope(EDS),then the interface reaction mechanism was explored.The results indicated the grain growth of crucible was incomplete and agglomeration was serious at 1650℃for 6 h,the relative density was approximately87%.The grain growth of crucible was complete and no agglomeration was observed at 1700℃for 6 h,the relative density was approximately 95%.The grain growth of crucible was more complete than that of crucible sintered at 1650 and 1700℃,no agglomeration and secondary crystallization was found at 1750℃for 6 h,and the relative density was approximately 97%.The crucible prepared at1750℃was selected for melting.The crucible structure was complete and no Zr-4 alloy melt penetration was observed after melting.However,some black area were generated at the interface of crucible and alloy,which might be due to the change of Y_2O_3 crucible microstructure.A large number of irregular Y oxide inclusions distributed in the alloy,which was due to that Y_2O_3 refractory was desquamated under the action of high temperature melt,and one part refractory was stirred into the melt alloy as inclusions,the other part refractory was decomposed into Y and O,and infiltrated into alloy melt and regenerated stable Y_2O_3 phase,meanwhile,excessive oxygen atoms existed in the alloy substrate as a free state.
引文
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[16]Ma L M,Zhang J Z,Yue G Q,Zhang H R,Zhou L,Zhang H.Improvement and application of Y2O3directional solidification crucible[J].Chinese Journal of Aeronautics,2016,29(2):554.
[2]Zhao J B,Wu L L,Zhang C J,Zeng B,Lv Y N,Li Z,Jiang Q L,Guo Z H.Highly efficient saturated visible up-conversion photoluminescent Y2O3:Er3+microspheres pumped with a 1.55μm laser diode[J].Journal of Materials Chemistry C,2017,5(16):3903.
[3]Rafiaei S M,Kim A,Shokouhimehr M.Enhanced luminescence properties of combustion synthesized Y2O3:Gd nanostructure[J].Current Nanoscience,2016,12(2):244.
[4]Lei L,Zhao G Y,Xu H,Wu N,Chen Y Q.Influences of Y2O3nanoparticle additions on the microstructure and superconductivity of YBCO films derived from low-fluorine solution[J].Materials Chemistry and Physics,2011,127(1-2):91.
[5]Kim C S,Kim I H.Effect of Al and Y2O3on mechanical properties in mechanically alloyed nanograin Ni-based alloys[J].Journal of Nanoscience and Nanotechnology,2015,15(8):6160.
[6]Wang C L,Gao Y,Zhang G Y.Effect of Y2O3addition on interface structure and corrosion resistance of laser additive manufacturing on the surface of Al alloys[J].Rare Metal Materials and Engineering,2017,46(3):812.(王成磊,高原,张光耀.Y2O3对铝合金表面激光增材制造组织及耐蚀性影响[J].稀有金属材料与工程,2017,46(3):812.)
[7]Zhang L,Li Z,Zhen F Z,Wang L X,Zhang Q T,Sun R,Selim F A,Wong C P,Chen H.High sinterability nano-Y2O3powders prepared via decomposition of hydroxyl-carbonate precursors for transparent ceramics[J].Journal of Materials Science,2017,52(14):8556.
[8]Jung W K,Ma H J,Jung S W,Kim D K.Effects of calcination atmosphere on monodispersed spherical particles for highly optical transparent yttria ceramics[J].Journal of the American Ceramic Society,2017,100(5):1876.
[9]Li J,Jang N,Xu S Q,Liu Q,Pan Y B.Resent development on infrared transparent Mg O-Y2O3nanocomposite ceramics[J].Journal of the Chinese Ceramic Society,2016,44(9):1302.(李江,姜楠,徐圣泉,刘强,潘裕柏.红外透明Mg O-Y2O3纳米复相陶瓷研究进展[J].硅酸盐学报,2016,44(9):1302.)
[10]Wang C L,Zhang G Y,Gao Y,Song Y Z.Mechanism of Y2O3affecting laser cladding of Ni-based coating on6063 Al alloy substrate[J].Chinese Journal of Rare Metals,2016,40(3):201.(王成磊,张光耀,高原,宋沂泽.Y2O3在6063铝合金表面激光熔覆Ni基熔覆层中的作用机制[J].稀有金属,2016,40(3):201.)
[11]Oh Y S,Chae J M,Choi S A,Han Y S,Kim S W,Lee S M,Kim H T,Ahn J K,Kim T H,Kim D H.Effect of powder composition on the failure and melting behavior of yttria stabilized zirconia ingot with a bimodal structure[J].Ceramics International,2017,43(1):1341.
[12]Chen G,Peng Y B,Zheng G,Qi Z X,Wang M Z,Yu H C,Dong C L,Liu C T.Polysynthetic twinned Ti Al single crystals for high-temperature applications[J].Nature Materials,2016,15(8):876.
[13]Mcdeavitt S M,Billings G W,Indacochea J E.High temperature interaction behavior at liquid metal-ceramic interfaces[J].Journal of Materials Engineering and Performance,2002,11(4):392.
[14]Xie H S,Liu H Y,Zhao J,Liu S B,Shi K.Interfacial reaction between zirconium alloy and graphite mold/yttrium oxide ceramic mold[J].China Foundry,2014,11(2):85.
[15]Kingery W D,Bowen H K,Uhlmann D R.Introduction to Ceramics[M].Beijing:Higher Education Press,2010.400.(金格瑞,鲍恩,乌尔曼.陶瓷导论[M].北京:高等教育出版社,2010.400.)
[16]Ma L M,Zhang J Z,Yue G Q,Zhang H R,Zhou L,Zhang H.Improvement and application of Y2O3directional solidification crucible[J].Chinese Journal of Aeronautics,2016,29(2):554.