Lu2O3-MgO纳米粉体合成及其复相红外透明陶瓷制备

doi:10.15541/jim20210149

无机材料学报 ›› 2021, Vol. 36 ›› Issue (12): 1263-1269.DOI: 10.15541/jim20210149

所属专题：【虚拟专辑】透明陶瓷与光学晶体；【信息功能】透明陶瓷与光学晶体

Lu₂O₃-MgO纳米粉体合成及其复相红外透明陶瓷制备

满鑫¹(), 吴南², 张牧¹^,³, 贺红亮⁴, 孙旭东³^,⁵, 李晓东¹^,³()

1.东北大学材料科学与工程学院, 沈阳 110819
2.沈阳大学机械工程学院, 沈阳 110044
3.东北大学材料各向异性与织构教育部重点实验室, 沈阳 110819
4.中国工程物理研究院流体物理研究所, 冲击波物理与爆轰物理重点实验室, 绵阳 621900
5.东北大学佛山研究生院, 佛山 528311

收稿日期:2021-03-11 修回日期:2021-04-27 出版日期:2021-12-20 网络出版日期:2021-05-10
通讯作者: 李晓东, 教授. E-mail: xdli@mail.neu.edu.cn
作者简介:满鑫(1995-), 男, 硕士研究生. E-mail: mxin0614@163.com
基金资助:
国家重点研发计划(2017YFB0310300);教育部基本科研业务费(N180212009);国家自然科学基金(51872033)

Lu₂O₃-MgO Nano-powder: Synthesis and Fabrication of Composite Infrared Transparent Ceramics

MAN Xin¹(), WU Nan², ZHANG Mu¹^,³, HE Hongliang⁴, SUN Xudong³^,⁵, LI Xiaodong¹^,³()

1. School of Materials Science and Engineering, Northeastern University, Shenyang 110819, China
2. School of Mechanical Engineering, Shenyang University, Shenyang 110044, China
3. Key Laboratory for Anisotropy and Texture of Materials (Ministry of Education), Northeastern University, Shenyang 110819, China
4. National Key Laboratory of Shock Wave and Detonation Physics, Institute of Fluid Physics, China Academy of Engineering Physics, Mianyang 621900, China
5. Foshan Graduate School, Northeastern University, Foshan 528311, China

Received:2021-03-11 Revised:2021-04-27 Published:2021-12-20 Online:2021-05-10
Contact: LI Xiaodong, professor. E-mail: xdli@mail.neu.edu.cn
About author:MAN Xin(1995-), male, Master candidate. E-mail: mxin0614@163.com
Supported by:
National Key R&D Program Project(2017YFB0310300);The Special Fund for Basic Research in Central Universities(N180212009);National Natural Science Foundation of China(51872033)

摘要/Abstract

摘要：

细化陶瓷微观结构至纳米级, 可以减少光的散射损失, 为开发新型光学陶瓷提供了一种有效的方法。本研究采用溶胶-凝胶法合成粉体, 结合热压烧结工艺制备出光学性能优异的新型Lu₂O₃-MgO纳米复合陶瓷, 研究了粉体合成条件及热压烧结工艺对样品微观结构的影响, 并对计算的理论透过率与样品的实际透过率进行了比较。研究结果表明: 采用优化后工艺制备的Lu₂O₃-MgO陶瓷具有均匀的相域分布, 晶粒尺寸约为123 nm, 3~5 μm波段的透过率高达84.5%~86.0%, 接近理论透过率; 维氏硬度为12.2 GPa, 断裂韧性为2.89 MPa·m^-1/2, 抗弯强度达到(221±12) MPa, 是一种潜在的红外透明窗口材料。

关键词: 溶胶-凝胶法, 热压烧结, Lu₂O₃-MgO, 纳米复合陶瓷, 红外窗口材料

Abstract:

Refining ceramic microstructures to nanometric range to minimize light scattering provides an effective methodology for developing novel optical ceramic materials. In this study, we reported the fabrication and properties of a new nanocomposite optical ceramic of Lu₂O₃-MgO by using nano powders synthesized via Sol-Gel method and hot-pressing sintering technology. Influence of powder synthesis conditions and hot-pressing sintering process on the microstructure of the sample was investigated, and the theoretical transmittance of the sample was calculated and compared with the measured transmittance. The results show that the Lu₂O₃-MgO ceramic fabricated by optimizing process exhibts a homogeneous phase domain distribution, a fine-grain size of 123 nm, a high transmittance of 84.5%-86.0% over the 3-5 μm wavelength range, close to the theoretical transmittance, and enhanced hardness value of 12.2 GPa, toughness value of 2.89 MPa·m^-1/2 and bending strength value of (221±12) MPa, indicating potential application in infrared transparent window material.

Key words: Sol-Gel method, hot-pressing sintering, Lu₂O₃-MgO, nano-composites, infrared window materials

中图分类号:

TQ174

满鑫, 吴南, 张牧, 贺红亮, 孙旭东, 李晓东. Lu₂O₃-MgO纳米粉体合成及其复相红外透明陶瓷制备[J]. 无机材料学报, 2021, 36(12): 1263-1269.

MAN Xin, WU Nan, ZHANG Mu, HE Hongliang, SUN Xudong, LI Xiaodong. Lu₂O₃-MgO Nano-powder: Synthesis and Fabrication of Composite Infrared Transparent Ceramics[J]. Journal of Inorganic Materials, 2021, 36(12): 1263-1269.

图/表 8

图1 前驱体泡沫的热分析曲线

Fig. 1 Thermal analysis curves of precursor foam

图2 不同温度煅烧粉体的XRD图谱

Fig. 2 XRD patterns of powders calcined at different temperatures

表1 不同煅烧温度合成粉体的比表面积、颗粒尺寸、晶粒尺寸及团聚因子

Table 1 Grain size and agglomeration factor φ of powders at different calcination temperatures

Temperature/℃	S_BET/(m²·g^-1)	D_BET/nm	D_XRD/nm	φ
400	58.2	15.9	7.2	2.21
500	54.3	17.0	8.6	1.98
600	51.1	18.1	9.3	1.95
700	41.9	22.0	10.6	2.08

图3 不同温度烧结样品的表面微观形貌、相对密度及平均晶粒尺寸

Fig. 3 SEM images, relative densites and average grain sizes of the samples sintered at different temperatures (a) 1200 ℃; (b) 1250 ℃; (c) 1300 ℃; (d) 1350 ℃; (e) 1400 ℃; (f) Relative densities and average grain sizes of the samples sintered at different temperatures

图4 不同升温速率烧结的样品的微观形貌、相对密度及平均晶粒尺寸

Fig. 4 SEM images, relative densites and average grain sizes of the samples sintered at different heating rates (a) 15 ℃/min; (b) 20 ℃/min; (c) 30 ℃/min; (d) Relative densities and average grain sizes of the samples sintered at different heating rates

图5 不同温度退火样品的微观形貌、相对密度及平均晶粒尺寸

Fig. 5 SEM images, relative densites and average grain sizes of the samples annealed at different temperatures (a) 1100 ℃; (b)1150 ℃; (c)1200 ℃; (d) Relative densities and average grain sizes of the samples annealed at different temperatures

图6 样品的理论透过率与实际透过率(厚度约2 mm); 插图为半透明Lu2O3-MgO纳米复相陶瓷实物照片

Fig. 6 Theoretical and actual transmittance of translucent Lu2O3-MgO nanocomposite ceramic (thickness≈2 mm) The inset shows the appearance of translucent Lu2O3-MgO nanocomposite ceramic

表2 样品的力学性能表征

Table 2 Mechanical properties of the sample

Sample	HV hardness/GPa	Fracture toughness/(MPa·m^-1/2)	Bending strength/MPa
Lu₂O₃-MgO	12.2	2.89	(221±12)

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Lu₂O₃-MgO纳米粉体合成及其复相红外透明陶瓷制备

Lu₂O₃-MgO Nano-powder: Synthesis and Fabrication of Composite Infrared Transparent Ceramics

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