ZrO2掺杂Y2O3-MgO纳米复相陶瓷的制备及性能研究

doi:10.15541/jim20240438

无机材料学报 ›› 2025, Vol. 40 ›› Issue (3): 281-289.DOI: 10.15541/jim20240438 CSTR: 32189.14.10.15541/jim20240438

ZrO₂掺杂Y₂O₃-MgO纳米复相陶瓷的制备及性能研究

穆浩洁¹(), 张源江¹, 喻彬², 付秀梅², 周世斌², 李晓东¹()

1.东北大学材料科学与工程学院, 先进陶瓷材料研究中心, 材料各向异性与织构教育部重点实验室, 沈阳 110819
2.成都东骏激光股份有限公司, 成都 611630

收稿日期:2024-10-17 修回日期:2024-11-22 出版日期:2025-03-20 网络出版日期:2025-03-12
通讯作者: 李晓东, 教授. E-mail:xdli@mail.neu.edu.cn
作者简介:穆浩洁(1999-), 女, 博士研究生. E-mail:2110169@stu.neu.edu.cn
基金资助:
国家自然科学基金(52472065)

Preparation and Properties of ZrO₂ Doped Y₂O₃-MgO Nanocomposite Ceramics

MU Haojie¹(), ZHANG Yuanjiang¹, YU Bin², FU Xiumei², ZHOU Shibin², LI Xiaodong¹()

1. Key Laboratory for Anisotropy and Texture of Materials (Ministry of Education), Research Center for Advanced Ceramic Materials, School of Materials Science and Engineering, Northeastern University, Shenyang 110819, China
2. Chengdu Dongjun Laser Co., Ltd., Chengdu 611630, China

Received:2024-10-17 Revised:2024-11-22 Published:2025-03-20 Online:2025-03-12
Contact: LI Xiaodong, professor. E-mail: xdli@mail.neu.edu.cn
About author:MU Haojie (1999-), female, PhD candidate. E-mail: 2110169@stu.neu.edu.cn
Supported by:
National Natural Science Foundation of China(52472065)

摘要/Abstract

摘要：

Y₂O₃-MgO纳米复相陶瓷与单相Y₂O₃陶瓷相比具有更高的机械强度、硬度、热导率以及优异的红外波段透光性, 是一种良好的红外窗口材料。然而, 恶劣的热、机械工作环境对红外窗口材料的光学和力学性能提出了更高的要求。本研究以高纯Y₂O₃-MgO纳米复合粉体为原料, 通过在球磨过程中添加硝酸锆水溶液制备了不同ZrO₂掺杂量(Zr⁴⁺离子分别占Y³⁺离子的1%、3%、5%)的Y₂O₃-MgO纳米复合粉体。利用该粉体成型后的坯体在1350 ℃、35 MPa条件下热压烧结30 min制备得到ZrO₂:Y₂O₃-MgO纳米复相陶瓷, 研究了ZrO₂掺杂量对陶瓷物相、微观结构、红外透光率、硬度和抗弯强度的影响。结果表明: ZrO₂掺杂改变了Y₂O₃-MgO纳米复相陶瓷的微观结构并引起了晶格畸变, 从而显著影响陶瓷的光学性能和力学性能。ZrO₂固溶并均匀分布在Y₂O₃晶格中, 对MgO相没有影响。微观结构观察结果显示, ZrO₂掺杂量增大, 抑制了陶瓷致密化, 因此在5%ZrO₂:Y₂O₃-MgO陶瓷中存在明显的孔洞。同时, ZrO₂掺杂可以强化Y₂O₃-MgO纳米复相陶瓷, 这是由于晶格畸变抑制了位错运动。当ZrO₂掺杂量为3%时, 致密的微观结构使其在3~5 μm波段的透过率达到~82%, 硬度和抗弯强度分别达到11.43 GPa和276.67 MPa。

关键词: 纳米复相陶瓷, 红外透明材料, ZrO₂掺杂, 微观结构, 力学性能, 晶格畸变

Abstract:

Compared with single-phase Y₂O₃ ceramics, Y₂O₃-MgO nanocomposite ceramics exhibit superior mechanical strength, hardness, thermal conductivity, and excellent infrared band transparency, endowing them a good infrared window material. However, harsh mechanical and thermal operating conditions impose stringent requirements on the optical and mechanical properties of infrared window materials. In this study, high-purity Y₂O₃-MgO nanocomposite powder was used as raw material, and Y₂O₃-MgO nanocomposite powders with different ZrO₂ contents, in which Zr⁴⁺ ions accounted for the percentage of Y³⁺ ions at 1%, 3% and 5%, were prepared by adding zirconium nitrate aqueous solution during ball milling. ZrO₂:Y₂O₃-MgO nanocomposite ceramics were fabricated by hot pressing sintering at 1350 ℃ and 35 MPa for 30 min. The influence of ZrO₂ content on the phase, microstructure, infrared transmittance, hardness, and bending strength of nanocomposite ceramics was systematically studied. The results showed that doping ZrO₂ dissolved and uniformly distributed in the Y₂O₃ lattice changed microstructure of Y₂O₃-MgO nanocomposite ceramics and caused lattice distortion, which had a significant impact on the optical and mechanical properties of Y₂O₃-MgO nanocomposite ceramics. The microstructures of ZrO₂:Y₂O₃-MgO nanocomposite ceramics reveal that increasing ZrO₂ content can hinder ceramic densification, resulting in obvious pores in 5%ZrO₂:Y₂O₃-MgO nanocomposite ceramic. Meanwhile, doping ZrO₂ can enhance the hardness and bending strength of Y₂O₃-MgO nanocomposite ceramics, which can be attributed to lattice distortion suppressing the dislocations’ motion. 3%ZrO₂:Y₂O₃-MgO nanocomposite ceramic has a dense microstructure, with a transmittance of ~82% in the range of 3-5 μm, while exhibiting a hardness of 11.43 GPa and a bending strength of 276.67 MPa.

Key words: nanocomposite ceramic, infrared transparent material, ZrO₂ doping, microstructure, mechanical property, lattice distortion

中图分类号:

TQ174

穆浩洁, 张源江, 喻彬, 付秀梅, 周世斌, 李晓东. ZrO₂掺杂Y₂O₃-MgO纳米复相陶瓷的制备及性能研究[J]. 无机材料学报, 2025, 40(3): 281-289.

MU Haojie, ZHANG Yuanjiang, YU Bin, FU Xiumei, ZHOU Shibin, LI Xiaodong. Preparation and Properties of ZrO₂ Doped Y₂O₃-MgO Nanocomposite Ceramics[J]. Journal of Inorganic Materials, 2025, 40(3): 281-289.

图/表 9

图1 商用Y2O3-MgO纳米复合粉体的(a)透射电子显微镜(TEM)照片和(b)选区电子衍射(SAED)图案

Fig. 1 (a) TEM image and (b) SAED pattern of commercial Y2O3-MgO nanocomposite powder

图2 不同ZrO2掺杂量(原子分数)的Y2O3-MgO纳米复合粉体的(a)XRD图谱和(b)晶粒尺寸及比表面积

Fig. 2 (a) XRD patterns, (b) crystalline sizes and specific surface areas of Y2O3-MgO nanocomposite powders doped with different ZrO2 concentrations (atom fraction)

图3 不同ZrO2掺杂量(原子分数)的Y2O3-MgO纳米复相陶瓷的(a)XRD图谱, (b)Y2O3(222)晶面和(c)MgO(200)晶面的衍射峰

Fig. 3 (a) XRD patterns and diffraction peaks of (b) Y2O3 (222) and (c) MgO (200) crystal planes of Y2O3-MgO nanocomposite ceramics doped with different ZrO2concentrations (atom fraction)

图4 (a, b) 3%ZrO2:Y2O3-MgO纳米复相陶瓷的明场像, (c)晶界的高分辨图像和(d~g) Mg、Y、Zr、O元素分布情况

Fig. 4 (a, b) Bright field images of 3%ZrO2:Y2O3-MgO nanocomposite ceramic, (c) high resolution image of grain boundary, and (d-g) element mappings of Mg, Y, Zr, and O

图5 ZrO2:Y2O3-MgO纳米复相陶瓷的表面形貌以及Y2O3相和MgO相的晶粒尺寸分布

Fig. 5 Surface morphologies and grain size distributions of Y2O3 and MgO phases of ZrO2:Y2O3-MgO nanocomposite ceramics (a-c) Surface morphologies of (a) 1%ZrO2:Y2O3-MgO, (b) 3%ZrO2:Y2O3-MgO and (c) 5%ZrO2:Y2O3-MgO nanocomposite ceramics; (d-f) Grain size distributions of Y2O3 phase in (d) 1%ZrO2:Y2O3-MgO, (e) 3%ZrO2:Y2O3-MgO and (f) 5%ZrO2:Y2O3-MgO nanocomposite ceramics; (g-i) Grain size distributions of MgO phase in (g) 1%ZrO2:Y2O3-MgO, (h) 3%ZrO2:Y2O3-MgO and (i) 5%ZrO2:Y2O3-MgO nanocomposite ceramics

图6 ZrO2:Y2O3-MgO纳米复相陶瓷的红外透过率图谱

Fig. 6 Infrared transmittance spectra of ZrO2:Y2O3-MgO nanocomposite ceramics

图7 ZrO2:Y2O3-MgO纳米复相陶瓷的硬度和抗弯强度

Fig. 7 Hardness and flexural strength of ZrO2:Y2O3-MgO nanocomposite ceramics

图8 3%ZrO2:Y2O3-MgO纳米复相陶瓷中(a~d)Y2O3和(e, f)MgO相的(a, e)明场像和(b~d, f)HAADF原子像

Fig. 8 (a, e) Bright field images and (b-d, f) HAADF atomic images of (a-d) Y2O3 phase and (e, f) MgO phase in 3%ZrO2:Y2O3-MgO nanocomposite ceramic

图9 ZrO2:Y2O3-MgO纳米复相陶瓷的断裂韧性

Fig. 9 Fracture toughness of ZrO2:Y2O3-MgO nanocomposite ceramics

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ZrO₂掺杂Y₂O₃-MgO纳米复相陶瓷的制备及性能研究

Preparation and Properties of ZrO₂ Doped Y₂O₃-MgO Nanocomposite Ceramics

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