硅酸盐学报

添加La₂O₃快速无压烧结制备高红外透过率AlON陶瓷

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郗雪敏 ¹ , 马莉娅 ¹ , 郭浩然 ¹ , 单英春 ¹ , 韩晓光 ¹ , 徐久军 ¹ , 李江涛 ²

硅酸盐学报 | 研究论文 2024,52(3): 794-803

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硅酸盐学报 |研究论文 2024 , 52 (3) : 794 -803

添加La₂O₃快速无压烧结制备高红外透过率AlON陶瓷

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郗雪敏¹, 马莉娅¹, 郭浩然¹, 单英春¹, 韩晓光¹, 徐久军¹, 李江涛²

作者信息

^1．大连海事大学材料系，辽宁大连 116026

^2．中国科学院理化技术研究所，北京 100080

通讯作者:

单英春（1977—），女，教授。

作者简介:

郗雪敏（1998—），女，硕士研究生。

Highly Infrared Transparent AlON Ceramics Doped with La₂O₃ via Fast Pressureless Sintering

Xuemin XI¹, Liya MA¹, Haoran GUO¹, Yingchun SHAN¹, Xiaoguang HAN¹, Jiujun XU¹, Jiangtao Li²

Affiliations

^1.Department of Materials Science and Engineering, Dalian Maritime University, Dalian 116026, Liaoning, China

^2.Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, Beijing 100080, China

Corresponding Author:

SHAN Yingchun (1977-), female, Professor. E-mail: shanychun@dlmu.edu.cn

XI Xuemin (1998-), female, Master candidate. E-mail: q1254869801@163.com

出版时间: 2024-03-20 doi: 10.14062/j.issn.0454-5648.20230634

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摘要

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利用La₂O₃作为烧结助剂，分别采用D₅₀为1.1 μm和2.0 μm的AlON粉体，在1 880 ℃保温2.5 h快速无压烧结成功制备了红外透过率达80%~84%（3 850 nm处）的AlON陶瓷。基于AlON粉体粒度研究了La₂O₃掺量对陶瓷透过率的影响规律，并通过研究高透光性AlON陶瓷烧结过程升温阶段的物相组成、微观结构及致密化进程，揭示了其致密化机制。结果表明，La₂O₃对AlON分解具有一定的抑制作用，使样品中的α-Al₂O₃含量较低，从而避免了颗粒的早期团聚、粗化等，为后期致密化烧结奠定了良好的基础，同时，高致密度高透光性AlON陶瓷的快速无压烧结制备表明La₂O₃能为后期烧结提供充足的动力。

关键词

氮氧化铝 / 氧化镧 / 烧结助剂 / 粉体粒度 / 透明陶瓷 / 无压烧结

Abstract

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Introduction

Transparent aluminum oxynitride (AlON) ceramics have superior optical transparency properties, high strength and hardness, having great potential applications as window, dome, and other optical components requiring high strength combined with optical transparency. Recent efforts are made to fabricate transparent AlON ceramics, i.e., synthesis of high purity AlON powder, optimization of the particle size distribution of AlON powder, and doping with various additives in different amounts. In these works, sintering additives, such as Y₂O₃, Y₂O₃/La₂O₃, Y₂O₃/La₂O₃/MgO, etc., are commonly used to accelerate densification process of AlON. However, a long dwelling duration of ≥6 h is generally required to eliminate pores to obtain a high transmittance in pressureless sintering. Although the dwelling duration of pressureless sintering AlON ceramics can be shortened to 2.5 h, it is crucial to carefully match the doping amount of Y₂O₃ with the particle size of AlON powder. The excessive Y₂O₃ doping can result in a significant decomposition of AlON into α-Al₂O₃ and AlN, and the massive formation of α-Al₂O₃ can lead to particle aggregation/coarsening, and even separation between components during the early stage of sintering, which in turn retards the subsequent densification process. Studies on using CaCO₃ as an additive to fabricate AlON ceramics indicate that it should be a promising way to fabricate highly transparent AlON ceramics via suppressing AlON decomposition during heating with sintering additive. In this paper, La₂O₃ was respectively doped to AlON powders with median particle size (D₅₀) of 1.1 μm and 2.0 μm to prepared transparent AlON ceramics via pressureless sintering (PS) at 1 880 ℃ for 2.5 h. The effect of La₂O₃ doping amount on the transmittance of AlON ceramics was investigated, and the phase composition, microstructure and densification process of samples during heating were monitored to investigate the fast densification mechanism of AlON.

Methods

Pure AlON powder and La₂O₃ powder were used as starting materials. The AlON powders doped with 0-0.50% La₂O₃ were ground in absolute ethyl alcohol in a grinding mill with Si₃N₄ balls, and AlON powder with D₅₀ of 1.1 μm and 2.0 μm were obtained, referred to as P1.1 and P2.0, respectively. The ground powders were loaded into a pellet of 13 mm in diameter at 50 MPa and then cold isostatically pressed at 120 MPa to prepare green bodies. The green bodies were pressureless sintered in N₂ in a graphite furnace at a heating rate of 20 ℃/min. One group of samples were sintered at 1 880 ℃ for 2.5 h to prepare transparent AlON ceramics, and another group samples were respectively heated to 1 400-1 900 ℃ (no dwelling) to investigate the phase transformation, microstructure evolution and densification process during heating. The transparent AlON ceramics were ground and mirror polished on the both sides to a thickness of 2 mm for the optical transmittance measurement. The polished samples were hot etched at 1 640 ℃ for 40 min to determine their microstructure.

Results and discussion

After a 2.5 h dwell at 1 880 ℃, all the La₂O₃ doped AlON ceramics prepared (i.e., P1.1 and P2.0) show higher transmittance than their undoped counterparts, and the transmittances at 3 850 nm enhance from 17% and 0% to 80% and 84%, respectively. Moreover, the doping of La₂O₃ broadens the transmission wavelength range of the fabricated samples at 2 500-6 000 nm for P1.1 and the optical range at 220-6 000 nm for P2.0. Doping amount of La₂O₃ has a similar effect on the transmittance of AlON ceramics prepared by P1.1 and P2.0. When the doping amount of La₂O₃ ≤0.15% in P1.1 and ≤0.40% in P2.0, increasing the doping amount of La₂O₃ contributes to the enhanced transmittance of the AlON ceramics. Doping 0.15%-0.25% and 0.40% La₂O₃ into P1.1 and P2.0, respectively, results in the transmittances of AlON ceramics up to 80%-84% at 3 850 nm. The high transmittance of fabricated AlON ceramics is mainly due to thehigh relative density. For the two highly transparent AlON ceramics prepared by P1.1 doped with 0.20% La₂O₃ and P2.0 doped with 0.40% La₂O₃, their average grain sizes are 97.3 μm and 60.2 μm, and their Vickers hardness values are (16.00±0.31) GPa and (16.36±0.31) GPa.

For the samples prepared by P1.1 doped with 0.20% La₂O₃ and by P2.0 doped with 0.40% La₂O₃, although AlON undergoes decomposition and reformation during heating. α-Al₂O₃ content in the samples does not exceed 25.1%. Moreover, a lower amount of α-Al₂O₃ appears in the sample P2.0, compared to the sample P1.1 at 1 400-1 700 ℃. Furthermore, compared to the samples without additive doping, the two samples above exhibit lower α-Al₂O₃ contents at ≤1 600 ℃. It is indicated that the decomposition of AlON during heating is slightly suppressed by doping La₂O₃ as an additive. No obvious particle aggregation/coarsening or no composition decomposition occur on the fracture surface of the samples due to the reduced α-Al₂O₃ content in the samples. It is beneficial for the subsequently densification process.

Conclusions

AlON ceramics with a high infrared transmittance of 80%-84% at 3 850 nm were fabricated via pressureless sintering at 1 880 ℃ for 2.5 h after doping 0.15%-0.25% and 0.40% La₂O₃ to AlON powders with D₅₀ of 1.1 μm and 2.0 μm, respectively. During heating, La₂O₃ could suppress the decomposition of AlON and lead to a lower amount of α-Al₂O₃ being decomposed from AlON. This could reduce the particle aggregation/coarsening and even the separation of composition at the early stage of sintering. The obtained exceptional microstructure was beneficial for the subsequent fast densification. Moreover, La₂O₃ could provide sufficient sintering kinetics to effectively eliminate pores at the later stage of sintering, thus promoting the densification of AlON.

Key words

aluminum oxynitride / lanthanum oxide / sintering additive / particle size of powder / transparent ceramics / pressureless sintering

引用本文

郗雪敏, 马莉娅, 郭浩然, 单英春, 韩晓光, 徐久军, 李江涛. 添加La₂O₃快速无压烧结制备高红外透过率AlON陶瓷. 硅酸盐学报, 2024 , 52 (3) : 794 -803 . DOI: 10.14062/j.issn.0454-5648.20230634

Xuemin XI, Liya MA, Haoran GUO, Yingchun SHAN, Xiaoguang HAN, Jiujun XU, Jiangtao Li. Highly Infrared Transparent AlON Ceramics Doped with La₂O₃ via Fast Pressureless Sintering[J]. Journal of the Chinese Ceramic Society, 2024 , 52 (3) : 794 -803 . DOI: 10.14062/j.issn.0454-5648.20230634

基金

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国家自然科学基金(52372058)
中央高校基本科研业务费专项资金资助(3132023515)
大连市科技创新基金重点学科重大课题项目(2021JJ11CG002)

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2024年第52卷第3期

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文章信息

doi: 10.14062/j.issn.0454-5648.20230634

接收时间：2023-08-25
首发时间：2026-10-22
出版时间：2024-03-20

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收稿日期：2023-08-25
修回日期：2023-09-08

基金

国家自然科学基金(52372058)

中央高校基本科研业务费专项资金资助(3132023515)

大连市科技创新基金重点学科重大课题项目(2021JJ11CG002)

作者信息

^1．大连海事大学材料系，辽宁大连 116026

^2．中国科学院理化技术研究所，北京 100080

通讯作者:

单英春（1977—），女，教授。

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2种不同金属材料的力学参数

科 Family	属数 Number of genus	种数 Number of species	占总种数比例 Percentage of total species (%)	属 Genus	种数 Number of species	占总种数比例 Percentage of total species (%)
鹅膏菌科Amanitaceae	2	11	5.26	鹅膏菌属 Amanita	10	4.78
小菇科 Mycenaceae	2	12	5.74	丝盖伞属 Inocybe	5	2.39
多孔菌科 Polyporaceae	8	14	6.70	蜡蘑属 Laccaria	5	2.39
红菇科 Russulaceae	3	23	11.00	小皮伞属 Marasmius	6	2.87
				小菇属 Mycena	11	5.26
				光柄菇属 Pluteus	5	2.39
				红菇属 Russula	17	8.13
				栓菌属 Trametes	5	2.39

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