亚微米球形Y2O3粉体及其透明陶瓷的制备

doi:10.15541/jim20230514

无机材料学报 ›› 2024, Vol. 39 ›› Issue (6): 691-696.DOI: 10.15541/jim20230514 CSTR: 32189.14.10.15541/jim20230514

所属专题：【信息功能】透明与闪烁陶瓷（202506）

亚微米球形Y₂O₃粉体及其透明陶瓷的制备

刘焱¹^,²(), 覃显鹏¹(), 甘霖²(), 周国红¹, 章天金², 王士维¹, 陈鹤拓¹

1.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 200050
2.湖北大学材料科学与工程学院, 武汉 430062

收稿日期:2023-11-03 修回日期:2024-01-12 出版日期:2024-06-20 网络出版日期:2024-01-22
通讯作者: 覃显鹏, 副研究员. E-mail: xpqin@mail.sic.ac.cn;
甘霖, 副教授. E-mail: ganlin@hubu.edu.cn
作者简介:刘焱(1999-), 男, 硕士研究生. E-mail: ly8267426@163.com
基金资助:
国家自然科学基金(52130207);国家自然科学基金(51902093);国家自然科学基金(52103357)

Preparation of Sub-micron Spherical Y₂O₃ Particles and Transparent Ceramics

LIU Yan¹^,²(), QIN Xianpeng¹(), GAN Lin²(), ZHOU Guohong¹, ZHANG Tianjin², WANG Shiwei¹, CHEN Hetuo¹

1. State Key Laboratory of High Performance Ceramics and Superfine Microstructure, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China
2. School of Material Science and Engineering, Hubei University, Wuhan 430062, China

Received:2023-11-03 Revised:2024-01-12 Published:2024-06-20 Online:2024-01-22
Contact: QIN Xianpeng, associate professor. E-mail: xpqin@mail.sic.ac.cn;
GAN Lin, associate professor. E-mail: ganlin@hubu.edu.cn
About author:LIU Yan (1999-), male, Master candidate. E-mail: ly8267426@163.com
Supported by:
National Natural Science Foundation of China(52130207);National Natural Science Foundation of China(51902093);National Natural Science Foundation of China(52103357)

摘要/Abstract

摘要：

Y₂O₃以其优良的物理化学性质和在280 nm~8 μm宽频段内的高透明性, 而广泛应用于激光介质或光学窗口等领域。制备高透明的Y₂O₃陶瓷是目前的研究热点和难点, 而高质量的粉体是制备高透明Y₂O₃陶瓷的关键, 尿素均相沉淀法以其爆发成核和均匀可控的阴离子释放机制成为制备单分散颗粒的主要方法。本工作以硝酸钇和尿素为原料, 采用尿素均相沉淀法制备了单分散、亚微米级的球形Y₂O₃粉体。采用不同方法研究了Y₂O₃前驱体和煅烧后粉体的结构、物相演变和形貌。前驱体的颗粒尺寸约为330 nm, 800 ℃煅烧2 h得到的Y₂O₃粉体尺寸约为260 nm。在800 ℃煅烧后即可得到纯相的Y₂O₃粉体, 粉体呈球形, 分散性好, 且粒径均匀。以该Y₂O₃粉体为原料, 添加原子分数0.3%的Nb₂O₅为烧结助剂, 在1780 ℃通过真空无压烧结成功制备了透明Y₂O₃陶瓷。材料的光学性质优良, 即样品(厚度1 mm)的直线透过率在1100 nm处达到76.9%, 在400 nm处达到65.6%。本工作为制备性能优良的Y₂O₃透明陶瓷提供了一种新的方法。

关键词: 尿素均相沉淀法, 亚微米球形Y₂O₃粉体, 透明Y₂O₃陶瓷, Nb₂O₅, 真空烧结

Abstract:

Y₂O₃ ceramics is widely used as laser medium or optical window due to its excellent physical and chemical properties and high transparency in wide frequency band of 280 nm-8 μm. However, preparation of highly transparent Y₂O₃ ceramics still remains challenge due to its synthetic precursor and nano-powders difficult to meet the requirements. In this work, a spherical monodispersed and submicron-sized Y₂O₃ powder was prepared by a homogeneous precipitation method using yttrium nitrate and urea as raw materials. Structure, phase evolution and morphology of Y₂O₃ precursor and the calcined powder were studied by different methods. The synthesized particle precursor exhibits a sphere morphology with diamension around 330 nm, and Y₂O₃ powder calcined at 800 ℃ for 2 h shows spherical, well-dispersed and uniformed particles with dimension around 260 nm. Based on this spherical Y₂O₃ powder, transparent Y₂O₃ ceramics were fabricated by vacuum sintering at 1780 ℃ using 0.3% (in atom) Nb₂O₅ as sintering additive. The in-line transmittances of Y₂O₃ ceramics with thickness of 1 mm reach 76.9% at a wavelength of 1100 nm and 65.6% at a wavelength of 400 nm. In conclusion, this study provides a new promising method for preparing Y₂O₃ transparent ceramics with excellent properties.

Key words: urea homogeneous precipitation method, submicron-sized spherical Y₂O₃ powder, transparent Y₂O₃ceramic, Nb₂O₅, vacuum sintering

中图分类号:

TQ174.75

刘焱, 覃显鹏, 甘霖, 周国红, 章天金, 王士维, 陈鹤拓. 亚微米球形Y₂O₃粉体及其透明陶瓷的制备[J]. 无机材料学报, 2024, 39(6): 691-696.

LIU Yan, QIN Xianpeng, GAN Lin, ZHOU Guohong, ZHANG Tianjin, WANG Shiwei, CHEN Hetuo. Preparation of Sub-micron Spherical Y₂O₃ Particles and Transparent Ceramics[J]. Journal of Inorganic Materials, 2024, 39(6): 691-696.

图/表 7

图1 前驱体的TG/DSC曲线

Fig. 1 TG/DSC curves of the precursor

图2 前驱体和800℃煅烧后粉体的FT-IR谱图

Fig. 2 FT-IR spectra of the precursor and powder calcined at 800 ℃

图3 前驱体和800℃煅烧后粉体的XRD图谱

Fig. 3 XRD patterns of the precursor and powder calcined at 800 ℃

图4 Y2O3前驱体可能的形成示意图

Fig. 4 Illustration of the possible formation process of Y2O3 precursor

图5 前驱体(a)、800 ℃煅烧2 h(b~c)以及进一步球磨后(d)粉体的SEM照片

Fig. 5 SEM images of the precursor (a), Y2O3 powders calcined at 800 ℃ for 2 h (b-c) and powders after further ball milling (d)

图6 Y2O3陶瓷样品的直线透过率曲线

Fig. 6 In-line transmittance of the Y2O3 ceramic sample Inset: the picture of sample

图7 Y2O3陶瓷样品抛光表面的SEM照片

Fig. 7 SEM image of the mirror-polished surface of Y2O3 ceramic sample

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亚微米球形Y₂O₃粉体及其透明陶瓷的制备

Preparation of Sub-micron Spherical Y₂O₃ Particles and Transparent Ceramics

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