MgO·1.5Al2O3透明陶瓷的无压/热等静压烧结制备

doi:10.15541/jim20150010

无机材料学报 ›› 2015, Vol. 30 ›› Issue (8): 843-847.DOI: 10.15541/jim20150010

MgO·1.5Al₂O₃透明陶瓷的无压/热等静压烧结制备

袁泽¹, 王皓¹, 涂兵田¹, 刘鑫¹, 许春来², 王为民¹, 傅正义¹

(1. 武汉理工大学材料复合新技术国家重点实验室, 武汉 430070; 2. 中国运载火箭技术研究院, 北京 100076)

收稿日期:2015-01-07 修回日期:2015-02-28 出版日期:2015-08-20 网络出版日期:2015-07-21
作者简介:袁泽(1989–), 男, 硕士研究生. E-mail: yz0315@whut.edu.cn
基金资助:
国家自然科学基金 (51472195);中央高校基本科研业务费专项基金 (WUT: 2013-II-022)National Natural Science Foundation of China (51472195);Fundamental Research Funds for the Central Universities (WUT: 2013-II-022)

Preparation of MgO·1.5Al₂O₃ Transparent Ceramic by Pressureless Sintering and Hot Isostatic Pressing

YUAN Ze¹, WANG Hao¹, TU Bing-Tian¹, LIU Xin¹, XU Chun-Lai², WANG Wei-Ming¹, FU Zheng-Yi¹

(1. State Key Lab of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070, China; 2. China Academy of Launch Vehicle Technology, Beijing 100076, China)

Received:2015-01-07 Revised:2015-02-28 Published:2015-08-20 Online:2015-07-21
About author:YUAN Ze. E-mail: yz0315@whut.edu.cn

摘要/Abstract

摘要：

镁铝尖晶石透明陶瓷是典型的结构功能一体化材料, 具有优异的光学和机械性能。实验合成了颗粒细小、均匀的单相MgO·1.5Al₂O₃陶瓷粉末, 并且利用XRD全谱拟合软件Fullprof和尖晶石位置分配程序SIDR两步法确定其晶体结构为(Mg_0.46Al_0.54)^IV[Mg_0.26Al_1.64□_0.09]^VIO₄。再通过真空无压烧结结合热等静压烧结制备出了高性能的透明陶瓷, 热等静压18 MPa下1850℃烧结4 h所得样品的致密度达到99.75%, 厚度为2 mm的烧结样品可见光透过率达到65%, 红外波段透过率达到80%以上, 维氏硬度为(12.75±0.12) GPa, 杨氏模量为277 GPa。

关键词: MgO·1.5Al2O3, 透明陶瓷, 结构精修, 热等静压

Abstract:

Possessing unique optical and mechanical properties, magnesium aluminate spinel transparent ceramic has been regarded as an important multifunctional material. In this study, pure phase MgO·1.5Al₂O₃ ceramic powders with uniform and fine particle size were synthesized through solid-state reaction. A two-step structural refinement procedure, including XRD Rietveld analysis by Fullprof software and further refinement by spinel solid solutions structure modeling program SIDR, was utilized to resolve the crystal structure of synthesized powders. After refinement, the crystal structure was finally determined to be (Mg_0.46Al_0.54)^IV[Mg_0.26Al_1.64□_0.09]^VIO₄. Using the synthesized MgO·1.5Al₂O₃ ceramic powders, high performance transparent ceramic was fabricated by pressureless vacuum sintering and subsequent hot isostatic pressing sintering (HIP). The relative density of the sample HIP-sintered at 1850 ℃ for 4 h under 180 MPa Ar could reach 99.75%. In the meantime, the in-line transmittance measurement of the 2-mm-thick sample displayed good optical transparency from ultraviolet to middle-infrared wavelengths with the maximum transmittance 65% in visible region and 80% in infrared region. The MgO·1.5Al₂O₃ transparent ceramic also exhibited good mechanical properties of Vickers hardness ((12.75 ± 0.12) GPa) and Young's modulus (277 GPa).

Key words: MgO·1.5Al2O3, transparent ceramic, structure refinement, hot isostatic pressing

中图分类号:

TQ174

袁泽, 王皓, 涂兵田, 刘鑫, 许春来, 王为民, 傅正义. MgO·1.5Al₂O₃透明陶瓷的无压/热等静压烧结制备[J]. 无机材料学报, 2015, 30(8): 843-847.

YUAN Ze, WANG Hao, TU Bing-Tian, LIU Xin, XU Chun-Lai, WANG Wei-Ming, FU Zheng-Yi. Preparation of MgO·1.5Al₂O₃ Transparent Ceramic by Pressureless Sintering and Hot Isostatic Pressing[J]. Journal of Inorganic Materials, 2015, 30(8): 843-847.

图/表 6

图1 MgO·1.5Al2O3粉体(a)和烧结样品(b)的XRD图谱

Fig. 1 XRD patterns of synthesized MgO·1.5Al2O3 powder (a) and as-sintered sample (b)

表1 MgO·1.5Al2O3粉体的晶体结构精修结果

Table 1 Crystal structure refinement of MgO·1.5Al2O3 powders

First step: refined by Fullprof software
Crystal	Al^IV		□^IV		Al^VI		□^VI		a/nm		u		R_p		R_wp		χ²
MgO·1.5Al₂O₃	0.9721		0.0289		1.9185		0.08144		0.8030749		0.25991		5.30		6.90		1.39
Second step: refined by SIDR program
Crystal		Al^IV		Mg^IV		□^IV		Al^VI		Mg^VI		□^VI		a/nm		u		F(Xi)
MgO·1.5Al₂O₃		0.5397		0.4602		0		1.6397		0.2588		0.0906		0.803086		0.25939		2.2

图2 合成MgO·1.5Al2O3粉体的SEM照片

Fig. 2 SEM image of synthesized MgO·1.5Al2O3 powder

图3 (a)1650℃真空预烧后样品的断面SEM照片和(b) 1850℃热等静压烧结样品的刻蚀表面SEM照片

Fig. 3 SEM images of MgO·1.5Al2O3 ceramics (a) fractured surface after pressureless sintering at 1650 ℃ and (b) etched surface after HIP sintering at 1850 ℃

图4 MgO·1.5Al2O3透明陶瓷(样品厚度为2 mm)的(a)表观照片和(b)直线透过率图谱

Fig. 4 (a) Appearance and (b) in-line transmission spectrum of MgO·1.5Al2O3 transparent ceramic (thickness = 2 mm)

表2 MgO·1.5Al2O3和MgAl2O4透明陶瓷机械性能、热性能及介电性能的比较

Table 2 Comparison of mechanical, thermal, and dielectric properties between MgO·1.5Al2O3 and MgAl2O4 transparent ceramics

Sample	Vickers hardness (9.8 N) /GPa	Young's modulus /GPa	Specific heat capacity (20 ℃) /(J·g^-1·K^-1)	Thermal conductivity (20 ℃)/(W·m^-1·K^-1)	Dielectric constant (20℃, 1 MHz)
MgO·1.5Al₂O₃	12.75±0.12	277	0.83	16.3	9.70
MgAl₂O₄	12	267	~0.82	~25.0	8.33

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MgO·1.5Al₂O₃透明陶瓷的无压/热等静压烧结制备

Preparation of MgO·1.5Al₂O₃ Transparent Ceramic by Pressureless Sintering and Hot Isostatic Pressing

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