宽光谱透过Mg0.9Al2.08O3.97N0.03透明陶瓷的制备与性能研究

doi:10.15541/jim20210771

无机材料学报 ›› 2022, Vol. 37 ›› Issue (9): 969-975.DOI: 10.15541/jim20210771

宽光谱透过Mg_0.9Al_2.08O_3.97N_0.03透明陶瓷的制备与性能研究

李文俊(), 王皓(), 涂兵田, 谌强国, 郑凯平, 王为民, 傅正义

武汉理工大学材料复合新技术国家重点实验室, 武汉 430070

收稿日期:2021-12-17 修回日期:2022-02-22 出版日期:2022-09-20 网络出版日期:2022-06-16
通讯作者: 王皓, 教授. E-mail: shswangh@whut.edu.cn
作者简介:李文俊(1996-), 男, 硕士研究生. E-mail: 15826911464@163.com
基金资助:
国家重点研发计划(2017YFB0310500);国家自然科学基金(51472195);三亚科教创新园开放基金(2020KF0018)

Preparation and Property of Mg_0.9Al_2.08O_3.97N_0.03 Transparent Ceramic with Broad Optical Transmission Range

LI Wenjun(), WANG Hao(), TU Bingtian, CHEN Qiangguo, ZHENG Kaiping, WANG Weiming, FU Zhengyi

State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070, China

Received:2021-12-17 Revised:2022-02-22 Published:2022-09-20 Online:2022-06-16
Contact: WANG Hao, professor. E-mail: shswangh@whut.edu.cn
About author:LI Wenjun (1996-), male, Master candidate. E-mail: 15826911464@163.com
Supported by:
National Key Research and Development Program of China(2017YFB0310500);National Natural Science Foundation of China(51472195);Sanya Science and Education Innovation Park Open Fundation(2020KF0018)

摘要/Abstract

摘要：

MgAl₂O₄透明陶瓷具有优异的光学性能, 但其较差的机械性能和成型过程中的水解问题限制了实际应用, 通过组成设计MgAlON四元尖晶石可以有效调节其综合性能。本研究采用凝胶注模成型、无压烧结和热等静压处理制备了一种具有宽光谱透过范围的新型Mg_0.9Al_2.08O_3.97N_0.03透明陶瓷, 系统比较其与MgAl₂O₄透明陶瓷的光学性能和机械性能, 分析了低应力下裂纹的缓慢扩展并预测使用寿命。研究表明：固相体积分数为50%的陶瓷浆料粘度最低, 为124 mPa·s, 满足凝胶注模成型的需求; 2 mm厚的Mg_0.9Al_2.08O_3.97N_0.03透明陶瓷样品在3.7 μm处的直线透过率达86.2%, 光学透过范围与MgAl₂O₄相比拟, 折射率和阿贝数略高于MgAl₂O₄; 同时, 该陶瓷具有和MgAl₂O₄相近的Weibull模数, 尽管裂纹缓慢扩展系数比MgAl₂O₄小, 但特征强度(210.6 MPa)和惰性强度(227.5 MPa)均高于MgAl₂O₄。包含少量N的MgAlON尖晶石较好地克服了陶瓷粉体的水解问题, 并在保持优越光学性能的前提下显著提高了透明陶瓷的机械性能。本研究为尖晶石型透明陶瓷的制备与性能的改善提供了新的途径。

关键词: 透明陶瓷, 凝胶注模成型, 机械性能, 光学性能

Abstract:

MgAl₂O₄ transparent ceramics possess excellent optical property, but their practical applications are somewhat restricted by the hydrolysis problem during the shaping process and limited mechanical property. Meanwhile, it has been demonstrated that the property of quaternary MgAlON spinel can be effectively adjusted via varying their composition. Accordingly, a novel Mg_0.9Al_2.08O_3.97N_0.03 transparent ceramic with a broad transmittance range was prepared by combining aqueous gel-casting, pressureless sintering, and hot isostatic pressing treatment. Optical and mechanical property of this transparent ceramic were systematically investigated and compared with those of MgAl₂O₄ transparent ceramic. Furthermore, the slow crack growth under low stress were analyzed, and the service life of transparent ceramic was predicted. It is shown that the viscosity of ceramic slurry with 50% (in volume) solid load was 124 mPa·s, which could meet the requirement of aqueous gel-casting. The in-line transmittance of 86.2% at 3.7 μm was obtained in the Mg_0.9Al_2.08O_3.97N_0.03 transparent ceramic sample with thickness of 2 mm, and the optical transmittance range was comparable to that of MgAl₂O₄, with slightly higher refractive index and Abbé number. Further, this ceramic showed a Weibull modulus similar to MgAl₂O₄, and although its crack slow growth coefficient is lower than MgAl₂O₄, but both the characteristic strength (210.6 MPa) and inert strength (227.5 MPa) were much higher. Therefore, in the quaternary MgAlON spinel with low nitrogen content, the hydrolysis problem of ceramic powders could be well overcome, while the mechanical property of transparent ceramic was remarkably improved without degradation of optical property. This research provides a new pathway toward obtaining the novel spinel transparent ceramics with improved preparation and property.

Key words: transparent ceramics, aqueous gel-casting, mechanical property, optical property

中图分类号:

TQ174

李文俊, 王皓, 涂兵田, 谌强国, 郑凯平, 王为民, 傅正义. 宽光谱透过Mg_0.9Al_2.08O_3.97N_0.03透明陶瓷的制备与性能研究[J]. 无机材料学报, 2022, 37(9): 969-975.

LI Wenjun, WANG Hao, TU Bingtian, CHEN Qiangguo, ZHENG Kaiping, WANG Weiming, FU Zhengyi. Preparation and Property of Mg_0.9Al_2.08O_3.97N_0.03 Transparent Ceramic with Broad Optical Transmission Range[J]. Journal of Inorganic Materials, 2022, 37(9): 969-975.

图/表 5

图1 Mg0.9Al2.08O3.97N0.03陶瓷粉体、浆料、坯体以及透明陶瓷的表征

Fig. 1 Characterization of Mg0.9Al2.08O3.97N0.03 powder, slurry, green body, and transparent ceramic (a) XRD patterns of powder and ceramic; (b) Relationship between viscosity of slurry and contents of TAC; (c) Morphology of green body; (d) SEM image of etched surface of transparent ceramic

图2 透明陶瓷光学性能比较

Fig. 2 Comparison of optical property of transparent ceramics (a) In-line transmittance of Mg0.9Al2.08O3.97N0.03, MgAl2O4, c-plane sapphire[1], Mg0.27Al2.58O3.73N0.27 transparent ceramics[14]; (b) Refractive index of Mg0.9Al2.08O3.97N0.03, MgAl2O4 transparent ceramics[19]

图3 Mg0.9Al2.08O3.97N0.03透明陶瓷的抗弯强度Weibull统计图(a)和断面SEM照片(b)

Fig. 3 Weibull plot of fracture strength (a) and SEM image of fractured surface (b) of Mg0.9Al2.08O3.97N0.03 transparent ceramic

图4 Mg0.9Al2.08O3.97N0.03和MgAl2O4透明陶瓷[27]在不同载荷速率下的抗弯强度(a)与强度-概率-时间关系图(b)

Fig. 4 Fractured strength under different load rates (a) and strength-probability-time diagram (b) of Mg0.9Al2.08O3.97N0.03 and MgAl2O4[27] transparent ceramics Colorful figures are available on website

表1 Mg0.9Al2.08O3.97N0.03和MgAl2O4透明陶瓷的性能

Table 1 Property of Mg0.9Al2.08O3.97N0.03 and MgAl2O4 transparent ceramic

Sample	Vickers hardness/GPa	Fracture toughness/(MPa·m^1/2)	Young’s modulus/GPa	Thermal expansion coefficient/(×10^-6, K^-1)
MgAl₂O₄^{[30⇓⇓-33]}	12.9±0.49	1.6±0.1	273	6.97
Mg_0.9Al_2.08O_3.97N_0.03	13.7±0.12	2.12±0.1	280	6.57

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宽光谱透过Mg_0.9Al_2.08O_3.97N_0.03透明陶瓷的制备与性能研究

Preparation and Property of Mg_0.9Al_2.08O_3.97N_0.03 Transparent Ceramic with Broad Optical Transmission Range

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