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目的:研究不同含量氧化镧(La2O3)及氧化锂(Li2O)对ZTA复合陶瓷渗透玻璃粉性能的影响,并优选出性能最佳的玻璃组分。方法:通过熔融淬冷方法制备6组(Li1、Li2、Li3、La1、La2、La3)不同的玻璃粉,均匀涂布在经1200℃预烧结凝胶注模成型的ZTA陶瓷初坯上,经过1150℃玻璃渗透2次后,制得ZTA复合陶瓷。对玻璃试样进行差热分析及熔融范围测定,并对预烧结体及玻璃渗透ZTA复合陶瓷弯曲强度、线性收缩率进行测试,扫描电镜及能谱分析复合材料断面微观结构及元素变化,应用SPSS 13.0软件包对数据进行配对t检验和单因素方差分析,优选出性能最佳的渗透玻璃粉。结果:不同含量的La2O3和Li2O影响ZTA复合陶瓷渗透玻璃粉的性能。其中,Li1组复合陶瓷抗弯强度最高,可达(291.2±27.9)MPa,显著高于Li2组和La2组(P<0.05),且线性收缩率仅为(1.85±0.27)%。扫描电镜及能谱分析显示,该组断面结构较其他组致密,玻璃相充盈了陶瓷初坯的网络孔隙,玻璃与ZTA陶瓷界面过渡平滑,相互渗透,同时可见穿晶和沿晶断裂2种方式。结论:测试结果显示,Li1(30%La2O3-15%Al2O3-15%SiO2-15%B2O3-5%Li2O)组玻璃渗透ZTA复合陶瓷各项性能最佳。通过凝胶注模成型技术结合玻璃渗透制备ZTA复合陶瓷,能显著简化工艺,降低成本,为临床应用奠定了基础。
Objective: To study the effects of different contents of lanthanum oxide (La2O3) and lithium oxide (Li2O) on the properties of ZTA composite ceramic infiltrated glass frit, and optimize the glass component with the best performance. Methods: Six groups of glass powders (Li1, Li2, Li3, La1, La2, La3) were prepared by melt quenching method and uniformly coated on the blank of ZTA ceramic pre-sintered at 1200 ℃. After penetrating glass at 1150 ℃ for 2 times, ZTA composite ceramic was obtained. The differential thermal analysis and melting range of the glass samples were measured. The flexural strength and linear shrinkage of the pre-sintered and glass-infiltrated ZTA composite ceramics were tested. The microstructure and elemental changes of the composite were analyzed by scanning electron microscopy and energy dispersive spectroscopy. SPSS 13.0 software package paired t-test data and one-way analysis of variance, the best performance to optimize the penetration of glass powder. Results: The effects of different contents of La2O3 and Li2O on the properties of ZTA composite ceramic infiltrated glass powder. Among them, the bending strength of Li1 composite ceramics was the highest (291.2 ± 27.9) MPa, which was significantly higher than that of Li2 group and La2 group (P <0.05), and the linear shrinkage rate was only (1.85 ± 0.27)%. Scanning electron microscopy and energy spectrum analysis show that the cross-sectional structure of the group is more compact than the other groups, the glass phase fills the network pores of the ceramic primary blank, the interface between the glass and the ZTA ceramic is smooth and interpenetrated, and at the same time, transgranular and intergranular fracture are observed . CONCLUSION: The results show that the glass infiltrated ZTA composite with Li1 (30% La2O3-15% Al2O3-15% SiO2-15% B2O3-5% Li2O) has the best properties. Through the gel injection molding technology combined with glass infiltration preparation ZTA composite ceramic, can significantly simplify the process, reduce costs, and laid the foundation for clinical application.