透明AlON陶瓷凝胶浇注成型及其无压烧结制备

doi:10.15541/jim20220544

无机材料学报 ›› 2023, Vol. 38 ›› Issue (2): 193-198.DOI: 10.15541/jim20220544

透明AlON陶瓷凝胶浇注成型及其无压烧结制备

靳喜海¹^,²(), 董满江¹^,², 阚艳梅¹^,², 梁波³, 董绍明¹^,²()

1.中国科学院上海硅酸盐研究所, 上海 200050
2.中国科学院大学材料科学与光电工程中心, 北京 100049
3.燕山大学亚稳材料制备技术与科学国家重点实验室, 秦皇岛 066004

收稿日期:2022-09-19 修回日期:2022-11-17 出版日期:2023-02-20 网络出版日期:2022-11-21
通讯作者: 董绍明, 教授. E-mail: smdong@mail.sic.ac.cn
作者简介:靳喜海(1971-), 男, 研究员. E-mail: jinxhai@hotmail.com
基金资助:
国家自然科学基金(51872310)

Fabrication of Transparent AlON by Gel Casting and Pressureless Sintering

JIN Xihai¹^,²(), DONG Manjiang¹^,², KAN Yanmei¹^,², LIANG Bo³, DONG Shaoming¹^,²()

1. Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China
2. Center of Materials Science and Optoelectronics Engineering, University of Chinese Academy of Sciences, Beijing 100049, China
3. State Key Laboratory of Metastable Materials Science and Technology, Yanshan University, Qinhuangdao 066004, China

Received:2022-09-19 Revised:2022-11-17 Published:2023-02-20 Online:2022-11-21
Contact: DONG Shaoming, professor. E-mail: smdong@mail.sic.ac.cn
About author:JIN Xihai (1971-), male, professor. E-mail: jinxihai@hotmail.com
Supported by:
National Natural Science Foundation of China(51872310)

摘要/Abstract

摘要：

透明AlON具有优异的光学和力学性能, 应用前景广阔。但材料制备成本高昂, 限制了其应用发展。为解决上述问题, 本研究以透明AlON的凝胶浇注成型与无压烧结制备为核心目标, 就AlON细粉的低温合成及其抗水化处理展开重点研究。研究发现以有机聚合物包覆AlN/Al₂O₃为原料, 通过高温碳热-氮化工艺合成AlON, 可有效降低AlON的合成温度, 在1700 ℃即可合成近乎纯相的AlON粉体。所得粉体颗粒尺寸细小, 在亚微米级。通过对上述粉体进行聚氨酯包覆表面抗水化处理, 可大幅度提升其抗水化性能。即使历经长达72 h水中静置, 也不发生明显的水解。以此为基础, 通过凝胶浇注成型结合生坯的冷等静压后处理在1820~1850 ℃成功实现了透明AlON陶瓷的无压烧结制备。材料力学和光学性能优异, 其中1850 ℃烧结试样在紫外-中红外波段直线透过率达到83.1%~ 86.2%, 三点抗弯强度达到310 MPa。

关键词: 透明陶瓷, AlON, 粉体合成, 抗水化处理, 凝胶浇注, 无压烧结

Abstract:

Transparent AlON possesses good mechanical and optical properties, which shows great potential for application. However, high fabrication cost seriously restricts its wide usage. To solve this problem, gel-casting and pressureless sintering of transparent AlON was tentatively studied here, with emphasis on low temperature synthesis and anti-hydrolysis treatment of AlON powder. It was found that fine AlON powder could be readily synthesized at a low temperature of 1700 ℃ by a novel carbothermal nitridation technique, using polymer coated AlN/Al₂O₃ mixture as the starting materials. The powder obtained was submicron in size and its hydrolysis resistance could be significantly improved after surface coating with a polyurethane layer. On the basis of these findings, transparent AlON ceramics was successfully prepared through gel-casting and pressureless sintering. The material sintered at 1850 ℃ showed good optical and mechanical properties, with a high in-line transmittance of 83.1%-86.2% from ultraviolet to mid-infrared and three-point bending strength of 310 MPa.

Key words: transparent ceramics, AlON, powder synthesis, anti-hydrolysis treatment, gel casting, pressureless sintering

中图分类号:

TB333

靳喜海, 董满江, 阚艳梅, 梁波, 董绍明. 透明AlON陶瓷凝胶浇注成型及其无压烧结制备[J]. 无机材料学报, 2023, 38(2): 193-198.

JIN Xihai, DONG Manjiang, KAN Yanmei, LIANG Bo, DONG Shaoming. Fabrication of Transparent AlON by Gel Casting and Pressureless Sintering[J]. Journal of Inorganic Materials, 2023, 38(2): 193-198.

图/表 7

图1 不同条件下合成AlON粉体XRD图谱及其SEM照片

Fig. 1 XRD patterns and SEM images of AlON powder synthesized under different conditions (a) XRD patterns; (b) AlON powder synthesized at 1700 ℃, ball milled for 2 h; (c) AlON powder synthesized at 1700 ℃, ball milled for 15 h

图2 聚氨酯表面包覆对AlON粉体抗水化性能的影响

Fig. 2 Influence of polyurethane surface coating on the hydrolysis behavior of AlON powder (a) Hydrolysis curves of pristine AlON powder and AlON powder surfaces coated with 1.0% polyurethane; (b) pH variance of AlON slurries after 72 h setting

图3 (a)不同聚氨酯包覆量AlON粉体Zeta电位曲线; (b)不同pH条件下AlON浆料的流变曲线

Fig. 3 (a) Zeta potential curves of AlON powders after surface being coated with different mass amounts of polyurethane, and (b) rheological behavior of AlON slurry under different pH conditions Colorful figures are availuable on website

图4 干压-冷等静压(DP/CIP)、凝胶浇注(GC)以及凝胶浇注-冷等静压后处理(GC/CIP)成型AlON坯体的压汞测试曲线

Fig. 4 Mercury porosimetry curves of the AlON green bodies formed by dry pressing-cold isostatic pressing (DP/CIP), gel casting (GC) and gel-casting-cold isostatic pressing (GC/CIP) （a）Cumulative intrution;（b）Incremental intrution

图5 不同条件下烧结AlON陶瓷数码相机照片及SEM照片

Fig. 5 Photographs and SEM images of transparent AlON sintered under different conditions （a, c）1820 °C×10 h; （b, d）1850 °C×10 h

图6 不同温度下无压烧结透明AlON陶瓷直线透过率曲线(试样厚度2 mm)

Fig. 6 In-line transmittance of 2 mm thick transparent AlON pressurelessly sintered at different temperatures

表1 不同温度烧结的大尺寸透明AlON陶瓷的力学性能

Table 1 Mechanical properties of transparent AlON ceramics sintered at different temperatures

Sintering temperature/℃	Strength/ MPa	Toughness/ (MPa•m^1/2)	Hardness/ GPa
1820	325	2.3	17.5
1850	310	2.1	16.7

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透明AlON陶瓷凝胶浇注成型及其无压烧结制备

Fabrication of Transparent AlON by Gel Casting and Pressureless Sintering

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