细晶MgO·1.44Al2O3透明陶瓷的制备及其性能研究

doi:10.15541/jim20180589

摘要/Abstract

摘要：

晶粒细化是提高镁铝尖晶石透明陶瓷机械性能的有效途径之一。本研究采用单相MgO·1.44Al₂O₃陶瓷粉体, 首先通过放电等离子烧结进行成型和预致密化, 然后无压烧结达到烧结末期, 最终在180 MPa下1500 ℃热等静压烧结5 h, 制备出细晶MgO·1.44Al₂O₃透明陶瓷。无压烧结的结果表明: 缩窄气孔尺寸分布、降低平均气孔尺寸有助于显著促进陶瓷的致密化, 得到平均晶粒尺寸为1.4 μm、致密度为96.7%的闭气孔烧结体。透明陶瓷的平均晶粒尺寸为1.9 μm, 维氏硬度为(13.94±0.20) GPa, 杨氏模量为289 GPa。同时, 样品具有良好的光学透过率, 厚度为2 mm的样品在可见光和红外波段的最大直线透过率分别为70%和80%。

关键词: MgO·1.44Al₂O₃;, 坯体结构, 致密化, 细晶透明陶瓷, 硬度

Abstract:

Grain refinement is an effective way to enhance mechanical property of MgO·nAl₂O₃ spinel transparent ceramics. In this study, the porous body was firstly compacted and pre-densified by spark plasma sintering using pure phase MgO·1.44Al₂O₃ ceramic powder as raw material. Then, further densification at final stage has been achieved through pressureless sintering. Finally, a fine-grained MgO·1.44Al₂O₃ spinel transparent ceramic was fabricated by hot isostatic pressing at 1500 ℃ for 5 h under 180 MPa of argon. Pressureless sintering results show that narrowing the pore size distribution and reducing the average pore size can promote the densification process dramatically. And the pore-closed ceramic with average grain size of 1.4 μm and relative density of 96.7% was obtained. The transparent ceramic shows average grain size of 1.9 μm, Vickers hardness of (13.94±0.20) GPa and Young's modulus of 289 GPa. In addition, the 2-mm-thick product also displayed excellent optical transparency with the maximum transmittance 70% in visible region and 80% in infrared region, respectively.

Key words: MgO·1.44Al₂O₃;, microstructure of green body, densification, fine-grained transparent ceramic, hardness

中图分类号:

TQ174

郭胜强, 王皓, 涂兵田, 王斌, 徐鹏宇, 王为民, 傅正义. 细晶MgO·1.44Al₂O₃透明陶瓷的制备及其性能研究[J]. 无机材料学报, 2019, 34(10): 1067-1071.

GUO Sheng-Qiang, WANG Hao, TU Bing-Tian, WANG Bin, XU Peng-Yu, WANG Wei-Min, FU Zheng-Yi. Fabrication and Property of Fine-grained MgO·1.44Al₂O₃ Spinel Transparent Ceramic[J]. Journal of Inorganic Materials, 2019, 34(10): 1067-1071.

图/表 8

图1 合成MgO·1.44Al2O3粉体(a)和样品SPS-85 (b)的XRD图谱

Fig. 1 Typical XRD patterns of synthesized MgO·1.44Al2O3 powder (a) and sample SPS-85 (b)

图2 合成MgO·1.44Al2O3粉体的粒径分布曲线和SEM照片

Fig. 2 Particle size distribution and SEM image of synthesized MgO·1.44Al2O3 powder

图3 样品CIP-50、SPS-73和SPS-85的相对致密度随烧结时间的变化曲线

Fig. 3 Relative density of samples CIP-50, SPS-73 and SPS-85 changeed with soaking time

图4 多孔体CIP-50、SPS-73和SPS-85的气孔尺寸分布

Fig. 4 Pore size distribution of porous bodies CIP-50, SPS-73 and SPS-85

图5 样品CIP-50、SPS-73和SPS-85无压烧结前后的SEM照片

Fig. 5 SEM images of samples CIP-50, SPS-73 and SPS-85 before and after pressureless sintering (a-c): Fractured surface of samples CIP-50, SPS-73 and SPS-85; (d-e) Fractured surface of the samples CIP-50, SPS-73 pressureless sintered for 15 and 6 h; (f): Chemical etched surface of the sample SPS-85 pressureless sintered for 6 h

图6 透明陶瓷样品HIP-85的直线透过率图谱和样品照片

Fig. 6 In-line transmission spectrum and apparent photo of transparent ceramic HIP-85

图7 透明陶瓷样品HIP-85刻蚀表面的SEM照片

Fig. 7 SEM image of etched surface of transparent ceramic HIP-85

表1 MgO·nAl2O3透明陶瓷的晶粒尺寸与机械性能

Table 1 Grain size and mechanical properties of MgO·nAl2O3 transparent ceramics

n	Grain size/μm	Vickers hardness (9.8 N)/GPa	Young's modulus/GPa
1.5	>200	(12.75±0.12)^[12]	288.7^[10], 277^[12]
1.44	1.9	(13.94±0.20)	289
1.3^[3]	23	(12.8±0.3)	-

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细晶MgO·1.44Al₂O₃透明陶瓷的制备及其性能研究

Fabrication and Property of Fine-grained MgO·1.44Al₂O₃ Spinel Transparent Ceramic

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