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材料研究学报  2025, Vol. 39 Issue (6): 455-462    DOI: 10.11901/1005.3093.2024.259
  研究论文 本期目录 | 过刊浏览 |
Er2O3 对二硅酸锂玻璃陶瓷的结构和性能的影响
袁新雨, 史非, 刘敬肖(), 张皓杰, 杨大毅, 王美玉, 任明
大连工业大学纺织与材料工程学院 辽宁省新材料与材料改性重点实验室 大连 116034
Effect of Er2O3 Addition on Crystallization Behavior and Properties of Lithium Disilicate Glass Ceramics
YUAN Xinyu, SHI Fei, LIU Jingxiao(), ZHANG Haojie, YANG Dayi, WANG Meiyu, REN Ming
School of Textile and Materials Engineering, Key Laboratory of New Materials and Material Modification in Liaoning Province, Dalian Polytechnic University, Dalian 116034, China
引用本文:

袁新雨, 史非, 刘敬肖, 张皓杰, 杨大毅, 王美玉, 任明. Er2O3 对二硅酸锂玻璃陶瓷的结构和性能的影响[J]. 材料研究学报, 2025, 39(6): 455-462.
Xinyu YUAN, Fei SHI, Jingxiao LIU, Haojie ZHANG, Dayi YANG, Meiyu WANG, Ming REN. Effect of Er2O3 Addition on Crystallization Behavior and Properties of Lithium Disilicate Glass Ceramics[J]. Chinese Journal of Materials Research, 2025, 39(6): 455-462.

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摘要: 

用熔融-析晶法制备掺杂Er2O3的Li2O-K2O-MgO-Al2O3-SiO2-ZrO2-CeO2-P2O5系二硅酸锂玻璃陶瓷,研究了Er2O3的加入量对其玻璃析晶行为和性能的影响。结果表明, 改变Er2O3的含量可调控玻璃陶瓷中二硅酸锂晶相的析出、玻璃陶瓷的微观结构和性能。在玻璃陶瓷中加入适量的Er2O3 (0.4%,摩尔分数)能降低Li2SiO3和Li2Si2O5的析晶活化能和促进玻璃析晶,使制备出的玻璃陶瓷中的晶粒互锁且玻璃相与晶相紧密结合,使玻璃陶瓷具有较好的半透明性。玻璃陶瓷中的晶粒互锁和玻璃相与晶相紧密结合,能阻止裂纹扩展而使其力学性能最佳:三点抗折强度平均达到(376±61) MPa,显微硬度达到(6423±284) MPa;但是,在玻璃陶瓷中加入过量的Er2O3使析出晶体的尺寸增大,从而使其力学性能和透光性降低。

关键词 无机非金属材料二硅酸锂Er2O3玻璃陶瓷抗弯强度半透性    
Abstract

Lithium disilicate glass-ceramics of Li2O-K2O-MgO-Al2O3-SiO2-ZrO2-CeO2-P2O5 were prepared by melting-crystallization method. The effect of Er2O3 addition on the crystallization, microstructure and properties of the glass-ceramics was investigated. The results show that Er2O3 has significant regulating effect on the precipitation, microstructure and properties of the glass ceramics. When an appropriate amount of Er2O3 (0.4%, mole fraction) was added to the glass, it could effectively reduce the crystallization activation energy of Li2SiO3 and Li2Si2O5, and promote glass crystallization. The prepared glass-ceramics have interlocked grains, while the glass phase is closely bound to the crystal phase, which helps to prevent crack extension and achieve the best mechanical properties. The average three-point flexural strength reaches (376±61) MPa, with the microhardness reaching (6423±284) MPa, and the glass ceramic exhibits good translucence. Whereas, when an excessive amount of Er2O3 is added to the glass, the increase in the size of the precipitated crystals and the enhancement of the coloring effect of Er3+ will lead to a decrease in the mechanical properties and transparency of lithium disilicate glass ceramics. This work is of great significance for developing lithium disilicate glass ceramics and promoting their application in dental prosthetics.

Key wordsinorganic non-metallic materials    lithium disilicate    Er2O3    glass-ceramic    flexural strength    translucency
收稿日期: 2024-06-12     
ZTFLH:  R783.1  
基金资助:辽宁省-沈阳材料科学国家研究中心联合研发基金(2019JH3/30100013)
通讯作者: 刘敬肖,教授,drliu-shi@dlpu.edu.cn,研究方向为无机功能材料
Corresponding author: LIU Jingxiao, Tel: (0411)86323708, E-mail: drliu-shi@dlpu.edu.cn
作者简介: 袁新雨,男,1998年生,硕士
SampleSiO2Li2OP2O5Al2O3Er2O3Other oxides
Er066.4027.101.21.403.91
Er0.466.0827.011.21.40.43.91
Er0.865.8226.861.21.40.83.91
Er1.265.5526.751.21.41.23.91
表1  不同Er2O3含量的Li2Si2O5基质玻璃的配方
图1  不同Er2O3含量的基质玻璃的DTA曲线
图2  不同Er2O3含量的基质玻璃的Li2SiO3和Li2Si2O5析晶峰的ln(β/Tp2)与1000/Tp关系的拟合曲线
Sample

Er2O3 content

/ %, mole fraction

Tg / oCTp1 / oCEk1 / kJ·mol-1Tp2 / oCEk2 / kJ·mol-1Tm / oC
Er00479.42631.12223.32±11.40839.27338.66±15.28957.26
Er0.40.4477.62638.61136.84±39.06848.31320.61±22.53954.06
Er0.80.8474.89640.56126.88±17.20856.14431.52±52.62942.84
Er1.21.2499.12664.43159.41±8.36857.10361.66±171943.02
表2  不同Er2O3含量的玻璃样品的特征温度和活化能
图3  不同Er2O3含量的基质玻璃经不同热处理后玻璃陶瓷样品的XRD谱
图4  不同Er2O3含量的基质玻璃分别在650 ℃保温1 h、在860 ℃保温20 min制备的玻璃陶瓷样品的SEM照片和EDS图像
图5  不同Er2O3含量的基质玻璃在650和860 ℃析晶热处理制备的玻璃陶瓷样品的三点抗折强度和显微硬度
图6  不同Er2O3加入量调控玻璃中Li2Si2O5晶体微观形貌的机理示意图
图7  不同Er2O3含量的基质玻璃及其在650和860 ℃两段析晶热处理制备的玻璃陶瓷样品的密度和热处理后密度的提高
图8  不同Er2O3含量的基质玻璃在650和860 ℃两段析晶热处理制备的玻璃陶瓷样品在乙酸溶液中的溶解性
图9  不同Er2O3含量的基质玻璃在650和860 ℃析晶热处理制备的玻璃陶瓷样品的透光性和实物照片
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