环氧树脂改性自发凝固成型制备YAG透明陶瓷

doi:10.15541/jim20210790

无机材料学报 ›› 2022, Vol. 37 ›› Issue (9): 941-946.DOI: 10.15541/jim20210790 CSTR: 32189.14.10.15541/jim20210790

环氧树脂改性自发凝固成型制备YAG透明陶瓷

母利成¹^,²^,³(), 杨金萍¹(), 王俊平², 赵瑾², 刘梦玮², 汪德文², 章健²()

1.华北理工大学材料科学与工程学院, 唐山 063210
2.中国科学院上海硅酸盐研究所, 高性能陶瓷和超微结构国家重点实验室, 上海 201899
3.固体激光技术重点实验室, 北京 100015

收稿日期:2021-12-27 修回日期:2022-03-03 出版日期:2022-09-20 网络出版日期:2022-06-16
通讯作者: 杨金萍, 副教授. E-mail: imjp_yang@163.com;
章健, 研究员. E-mail: jianzhang@mail.sic.ac.cn
作者简介:母利成(1997-), 男, 硕士研究生. E-mail: mulicheng1997@163.com
基金资助:
固体激光技术重点实验室开放基金(6142404190201);国家自然科学基金(52130207)

Preparation of YAG Transparent Ceramics by Epoxy Resin Modified Spontaneous Coagulation Casting

MU Licheng¹^,²^,³(), YANG Jinping¹(), WANG Junping², ZHAO Jin², LIU Mengwei², WANG Dewen², ZHANG Jian²()

1. College of Materials Science and Engineering, North China University of Science and Technology, Tangshan 063210, China
2. The State Key Laboratory of High Performance Ceramics and Superfine Microstructure, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 201899, China
3. Key Laboratory of Solid State Laser Technology, Beijing 100015, China

Received:2021-12-27 Revised:2022-03-03 Published:2022-09-20 Online:2022-06-16
Contact: YANG Jinping, associate professor. E-mail: imjp_yang@163.com;
ZHANG Jian, professor. E-mail: jianzhang@mail.sic.ac.cn
About author:MU Licheng (1997-), male, Master candidate. E-mail: mulicheng1997@163.com
Supported by:
Science and Technology on Solid-State Laser Laboratory(6142404190201);National Natural Science Foundation of China(52130207)

摘要/Abstract

摘要：

YAG透明陶瓷具有良好的光学和力学性能, 广泛应用于激光增益介质与光学窗口等领域, 制备大尺寸/复杂形状YAG透明陶瓷是目前研究的热点与难点。作为一种新型胶态成型技术, 自发凝固成型在制备大尺寸陶瓷方面已显示出一定优势, 然而该体系存在浆料固化速率慢、素坯强度低等问题。本工作以水溶性环氧树脂乙二醇二缩水甘油醚(EGDGE)对自发凝固成型体系进行改性, 采用高温固相合成法制备了不同EGDGE含量的YAG透明陶瓷, 研究EGDGE对浆料流变性、凝胶强度、素坯孔隙率和烧结后陶瓷微结构与光学性能的影响。结果表明: 添加EGDGE有效增强了浆料的凝胶固化能力, 解决了YAG素坯干燥变形和开裂等问题。当EGDGE添加量为质量分数0.8%时, 在1700 ℃下真空烧结6 h并在1650 ℃下180 MPa热等静压烧结3 h, 成功制备了90 mm×30 mm×4.5 mm的YAG透明陶瓷, 它在1064 nm处直线透过率为80.8%。这为大尺寸/复杂形状YAG透明陶瓷的制备提供了新途径。

关键词: YAG, 环氧树脂, 自发凝固成型, 透明陶瓷

Abstract:

YAG transparent ceramics have been widely used in the fields of laser medium and optical windows due to their excellent optical and mechanical property. The research of large-scale and complex shape YAG transparent ceramics has become a hot and difficult point of current research. As an important colloidal based forming method, spontaneous coagulation casting has shown big potentials for preparing large-scale ceramics. However, long gel curing time and low green strength are main challenges for applications. Here, water soluble epoxy glycol diglycidyl ether (EGDGE) was used to modify the spontaneous solidification forming system, and YAG transparent ceramics with different EGDGE contents were prepared by high temperature solid phase synthesis method. The influence of EGDGE addition on slurry rheology, gel strength, green porosity, ceramic microstructure, and optical property after sintering was analyzed. The results showed that the addition of EGDGE enhanced the gel curing ability of the slurry, and deformation and cracking of YAG ceramic green body were overcame. The prepared YAG green body with 0.8% (in mass) EGDGE can be sintered at 1700 ℃ for 6 h in vacuum and followed by hot isostatic press sintering at 1650 ℃ for 3 h, under 180 MPa argon pressure. The obtained YAG transparent ceramic with dimension of 90 mm×30 mm× 4.5 mm has an in-line transmittance of 80.8% at 1064 nm. This research provides a new way for the preparation of YAG transparent ceramics with large-size/complex structure.

Key words: YAG, epoxy resin, spontaneous coagulation casting, transparent ceramics

中图分类号:

TQ174

母利成, 杨金萍, 王俊平, 赵瑾, 刘梦玮, 汪德文, 章健. 环氧树脂改性自发凝固成型制备YAG透明陶瓷[J]. 无机材料学报, 2022, 37(9): 941-946.

MU Licheng, YANG Jinping, WANG Junping, ZHAO Jin, LIU Mengwei, WANG Dewen, ZHANG Jian. Preparation of YAG Transparent Ceramics by Epoxy Resin Modified Spontaneous Coagulation Casting[J]. Journal of Inorganic Materials, 2022, 37(9): 941-946.

图/表 7

图1 浆料固化能力测试示意图[25]

Fig. 1 Schematic diagram of slurry consolidation test[25]

图2 EGDGE对浆料流变性的影响

Fig. 2 Effects of EGDGE on the rheology of slurry (a) Viscosity curve of EGDGE; (b) Viscosity curves of the slurry after adding different contents of EGDGE; (c) Storage modulus of the slurry after adding different contents of EGDGE; (d) Load-displacement curves of the slurry (solid content 80%, IB104 0.25%, IB600 0.55% (in mass)). Colorful figures are available on website

图3 添加不同量EGDGE干燥后的样品照片

Fig. 3 Photographs of samples adding different EGDGE contents after drying (a, b) 0; (c) 0.8%; (d) 1.6%, (in mass)

图4 EGDGE对素坯特性的影响

Fig. 4 Influence of EGDGE on the green body property (a) Pore size distribution; (b) Porosity

图5 不同EGDGE含量的YAG透明陶瓷直线透过率

Fig. 5 In-line transmittance curves of YAG ceramics adding different EGDGE Colorful figures are available on website

图6 不同EGDGE含量的YAG透明陶瓷SEM照片

Fig. 6 SEM images of YAG transparent ceramics adding different contents of EGDGE (a) 0; (b) 0.4%; (c) 0.8%; (d) 1.6% (in mass)

图7 HIP后不同EGDGE含量的YAG透明陶瓷照片

Fig. 7 Photos of YAG transparent ceramics adding different contents of EGDGE (a) 0; (b) 0.8% (in mass)

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环氧树脂改性自发凝固成型制备YAG透明陶瓷

Preparation of YAG Transparent Ceramics by Epoxy Resin Modified Spontaneous Coagulation Casting

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