【摘要】 背景:近年来的研究发现,Ti O₂和GeO₂共掺杂可提高氧化锆的超塑性。目的:探讨TiO₂和GeO₂共掺杂对3%氧化钇稳定氧化锆材料抗低温老化性能的影响。方法:使用机械球磨法、烘干、无压烧结制备共掺杂GeO₂和TiO₂的3%氧化钇稳定氧化锆材料,其中3%氧化钇稳定氧化锆的摩尔百分比均为98%,TiO₂粉末（纯度99.8%）与GeO₂粉末的摩尔百分比分别为1.5%,0.5%,记为1.5Ti-0.5Ge组;TiO₂粉末（纯度99.99%）与GeO₂粉末的摩尔百分比分别为1%,1%,记为1Ti-1Ge组;TiO₂粉末（纯度99.8%）与GeO₂的粉末摩尔百分比分别为0.5%,1.5%,记为0.5Ti-1.5Ge组。采用扫描透射电子显微镜、能谱仪等研究材料的微观结构;在高压釜中处理后,采用X射线衍射仪测量所有样品的转化量。结果与结论:（1）扫描透射电子显微镜下可见,GeO₂和TiO₂共掺3%氧化钇稳定氧化锆材料的复合粉体粒径均匀,分布在50 nm左右,颗粒形状基本呈球形,分散性好,但有少量团聚;X射线能谱仪检测显示,四价稳定剂(Ge⁴⁺,Ti⁴⁺)可以抑制氧化锆材料的低温老化效应,随着GeO₂掺杂量的增加,氧化锆的抗水热老化性能提高;能谱仪检测显示,随着掺杂剂含量的增加,晶界偏析程度增强,但即使Ge⁴⁺的掺杂量较小,晶界偏析程度也可与掺杂量大的Ti⁴⁺相媲美;（2）结果表明,添加GeO₂和TiO₂可提高3%氧化钇稳定氧化锆陶瓷的抗低温老化性能,其中GeO₂在抗低温老化方面优于Ti O₂,可作为首选。更多还原

【Abstract】 BACKGROUND:Many recent studies have found that zirconia co-doped with TiO₂ and GeO₂ exhibits excellent superplasticity.OBJECTIVE:To investigate the improvement of anti-cryogenic aging properties of zirconia materials sta bilized by 3% yttrium oxide co-doped with TiO₂ a nd GeO₂.METHODS:The 3% yttrium oxide stabilized zirconia material samples co-doped with GeO₂ and TiO₂ were prepared by mechanical ball milling,drying,and pressure free sintering.Among them,the mole percentage of 3% yttrium oxide stabilized zirconia was 98%.The mole percentages of TiO₂ powder（purity99.8%） and GeO₂ powder were 1.5% and 0.5%,respectively,which was recorded as the 1.5 Ti-0.5 Ge group.The mole percentages TiO₂ powder（purity） 99.99%)and GeO₂ powder were 1% and 1%,respectively,which was recorded as 1 Ti-1 Ge group,The mole percentages of TiO₂ powder（purity 99.8%） and Ge02 powder were 0.5%,1.5%,respectively,which was recorded as 0.5 Ti-1.5 Ge group.The microstructure of all samples was investigated by scanning transmission electron microscopy and ene rgy spectroscopy.After treatment in an autoclave,the conve rsion of all samples was measured by an X-ray diffractometer.RESULTS AND CONCLUSION:（1） Scanning transmission electron microscopy res ults showed that the composite powde rs of a 3% yttrium oxide stabilized zirconia material co-doped with GeO₂ and TiO₂ had uniform particle size and were distributed over a 50 nm;the particle shape was basically spherical and well dis persed,but there was a small amount of agglomeration.X-ray diffractometer exhibited that the Ge⁴⁺,Ti⁴⁺ stabilizers co uld inhibit the low-tempe rature aging effect of zirconia mate rials.With the increase of the doping amount of GeO₂,the low-tempe rature aging resistance of zirconia could be improved.Ene rgy spectrometer detection demonstrated that with the increase of dopant content,the degree of grain boundary segregation increased,but even if the doping amount of Ge⁴⁺ was small,the degree of grain boundary segregation could be comparable to that of Ti⁴⁺ with a large amount of doping.（2） The results suggest that the addition of GeO₂ and TiO₂ improved 3% yttrium oxide stabilized zirconia ce ramics against low-temperature aging properties.GeO₂ is superior to TiO₂ in resisting low-temperature aging and can be used as the first choice.更多还原