LiF对镁铝尖晶石透明陶瓷红外透过率的影响

doi:10.3724/SP.J.1077.2012.00417

无机材料学报 ›› 2012, Vol. 27 ›› Issue (4): 417-421.DOI: 10.3724/SP.J.1077.2012.00417 CSTR: 32189.14.SP.J.1077.2012.00417

LiF对镁铝尖晶石透明陶瓷红外透过率的影响

李法荟^1,2, 林红¹, 李俊峰¹, 雷牧云³, 李祯³, 李建保^1,4

(1. 清华大学材料科学与工程系, 新型陶瓷与精细工艺国家重点实验室, 北京100084; 2. 人工晶体研究院, 北京 100018; 3. 烁光特晶科技有限公司, 北京 100018; 4. 海南大学材料与化工学院, 海南优势资源化工材料应用技术教育部重点实验室, 海口 570228)

收稿日期:2011-05-09 修回日期:2011-06-17 出版日期:2012-04-10 网络出版日期:2012-03-12
作者简介:李法荟(1971-), 男, 博士. E-mail: lenad@163.com
基金资助:
科技部863项目(2007AA03Z524, 2006AA03Z218);973项目(2007CB607504)

Influence of LiF on the Infrared Transmissivity of Magnesia Alumina Spinel Transparent Ceramics

LI Fa-Hui^1,2, LIN Hong¹, LI Jun-Feng¹, LEI Mu-Yun³, LI Zhen³, LI Jian-Bao^1,4

(1. The State Key Lab of New Ceramics and Fine Processing, Department of Materials Science and Engineering, Tsinghua University, Beijing 100084, China; 2. Research Institute of Synthetic Crystals, Beijing 100018, China; 3. Bright Crystals Technology, Inc., Beijing 100018, China; 4. Key Laboratory of Ministry of Education for Application Technology of Chemical Materials in Hainan Superior Resources, School of Materials Science and Chemical Engineering, Hainan University, Haikou 570228, China)

Received:2011-05-09 Revised:2011-06-17 Published:2012-04-10 Online:2012-03-12
About author:LI Fa-Hui. E-mail: lenad@163.com

摘要/Abstract

摘要：

以溶胶-凝胶法制备镁铝尖晶石(以下简称“尖晶石”)粉末, 掺入0~2.5wt%的LiF, 经球磨后, 测试混合粉末的物相组成. 采用热压(HP; 32 MPa/1550℃)及热压结合热等静压(HP/HIP; 热等静压工艺条件为150 MPa/1700℃)工艺制备出尖晶石透明陶瓷. 分析测试了掺入不同LiF的尖晶石陶瓷的结构和红外透过率, 采用感应耦合等离子体(Inductively Coupled Plasma, 或ICP)方法测定了LiF掺杂后的粉料和透明陶瓷中的Li离子含量. 实验显示, LiF的加入促进了尖晶石晶粒长大和气孔的排除, 并促进了尖晶石陶瓷烧结的致密化进程. 添加1.0wt%~1.5wt% LiF的尖晶石透明陶瓷具有最高的红外透过率. LiF在尖晶石陶瓷中形成残余物质, 添加过量的LiF对尖晶石陶瓷的光学性能会产生不利影响.

关键词: 透明陶瓷, 镁铝尖晶石, LiF, 红外透过率, 感应耦合等离子体法

Abstract:

The influence of LiF as a sintering aidditive on the infrared transmissivity of magnesia alumina spinel (MgAl₂O₄; spinel, briefly) transparent ceramics was investigated. Spinel powders prepared by Sol-Gel method, were mixed with LiF of 0-2.5wt%, and then ball milled, tested by XRD for their phase compositions. Hot press (HP) or hot press combined with hot isostatic press (HP/HIP) technique was applied to sintering the powder mixtures into spinel ceramics, while HP under 32 MPa at 1550℃, and HIP under 150 MPa at 1700℃. The structures and infrared transmissions of the ceramic bodies were examined by SEM and IR spectrometer, respectively. Li contents in the spinel powder mixtures and in the resulted ceramics were detected by inductively coupled plasma (ICP) technique. The incorporation of LiF in the starting spinel powders facilitates the growth of grains and the expulsion of pores during sintering. And it shows LiF promotes the sintering of spinel ceramics. Spinel ceramics with LiF contents of 1.0wt%-1.5wt% exhibit optimal infrared transmissivity. While excess LiF acts adversly on the optical performances of spinel ceremics due likely to its remnant or derivative in the ceramic bodies.

Key words: transparent ceramics, magnesia alumina spinel, LiF, infrared transmissivity, ICP (Inductivity coupled plasma)

中图分类号:

TB383

李法荟, 林红, 李俊峰, 雷牧云, 李祯, 李建保. LiF对镁铝尖晶石透明陶瓷红外透过率的影响[J]. 无机材料学报, 2012, 27(4): 417-421.

LI Fa-Hui, LIN Hong, LI Jun-Feng, LEI Mu-Yun, LI Zhen, LI Jian-Bao. Influence of LiF on the Infrared Transmissivity of Magnesia Alumina Spinel Transparent Ceramics[J]. Journal of Inorganic Materials, 2012, 27(4): 417-421.

图/表 6

Table 1 Sample prepared by different sintering processes

No.	LiF addition/wt%	HP	HP/HIP
1#, 2#	0	1#	2#
3#, 4#	0.5	3#	4#
5#, 6#	1.0	5#	6#
7#, 8#	1.5	7#	8#
9#, 10#	2.0	9#	10#
11#, 12#	2.5	11#	12#

图1 不同LiF含量的尖晶石粉体的XRD图谱

Fig. 1 XRD patterns of spinel powders with different LiF concentrations

图2 不同LiF含量的尖晶石透明陶瓷的红外透过率

Fig. 2 IR transmission curves of spinel ceramics with different LiF concentrations

图3 未掺杂LiF的尖晶石陶瓷的SEM照片

Fig. 3 SEM images of spinel ceramics without LiF addition

图4 掺杂1wt%LiF的尖晶石陶瓷的SEM照片 (a) HP processed; (b) HP/HIP processed; (c) HP processed, fracture surface; (d) HP/HIP processed, fracture surface

Fig. 4 SEM images of spinel ceramics with 1wt% LiF addition

Table 2 LiF concentration test results of spinel powders and ceramics samples

No.	Preparation process	LiF addition/wt%	Li₂O detected /wt%	Equivalent LiF concentration/wt%^①
1#a	Powder	0	＜0.01	-
1#b	Powder	1.5	0.83	1.440
2#	HP	0.5	0.32	0.555
3#	HP	1.5	0.85	1.475
4#	HP/HIP	0.5	0.32	0.555
5#	HP/HIP	1.5	0.86	1.485

参考文献 20

[1]	Patterson M C L, Roy D W, Gilde G. An investigation of the transmission properties and ballistic performance of hot pressed spinel. Ceramic Transactions, 2002, 134: 595-608.
[2]	Gilde G, Patel P, Patterson M. Comparison of hot-pressing, rate-controlled sintering and microwave sintering of magnesium aluminate spinel for optical applications. Proc. SPIE, 1999, 3705: 94-104.
[3]	Patterson M C L, Caiazza J E, Roy D W. Transparent spinel development. Proc. SPIE, 2000, 4102: 59-68.
[4]	Cook R, Kochis M, Reimanis I. A new powder production route for transparent spinel windows: powder synthesis and window properties. Proc. SPIE, 2005, 5786: 41-47.
[5]	Suzuki Y. Reactive synthesis of a porous calcium zirconate/spinel composite with idiomorphic spinel grains. J. Am. Ceram. Soc., 2003, 86(7): 1128-1131.
[6]	Chiang Y M, Kingery W D. Grain-boundary migration in non-stoichiometric solid solutions of magnesium aluminate spinel: II, effects of grain-boundary non-stoichiometry. J. Am. Ceram. Soc., 1990, 73(5): 1153-1158.
[7]	Villalobos G, Sanghera J, Aggarwal I. Degradation of magnesium aluminum spinel by lithium fluoride sintering aid. J. Am. Ceram. Soc., 2005, 88(5): 1321-1322.
[8]	Huang J L, Sun S Y, Ko Y C. Investigation of high alumina-spinel: effects of LiF and CaCO3 addition. J. Am. Ceram. Soc., 1997, 80(12): 1153-1158.
[9]	Huang J L, Sun S Y, Chen C Y. Investigation of high alumina- spinel: effects of LiF and CaCO3 addition. Mater. Sci. Eng. A, 1999, 259(1): 1-7.
[10]	Roy D W, Hastert J L. Method for Manufacturing a Transparent Ceramic Body: U. S. Patent 3974249-264/65, 1976.
[11]	Lange F F, Clarke D R. Morphological changes of an intergranular film in a polycrystalline spinel. J. Am. Ceram. Soc., 1982, 65(10): 502-506.
[12]	Roy D W, Hastert J L. Polycrystalline MgAl2O4 spinel for high temperature windows. Ceram. Eng. Sci. Proc., 1983, 4(7/8): 502-509.
[13]	Lepkova D, Baatarjav A, Pavlova L. Effect of additives on the firing and the properties of magnesium spinel ceramics. Int. Ceram., 1993, 42(2): 89-92.
[14]	Gilde G, Patel P, Patterson P, et al. Evaluation of hot pressing and hot isostastic pressing parameters on the optical properties of spinel. J. Am. Ceram. Soc., 2005, 88(10): 2747-2751.
[15]	Villalobos G, Sanghera J S, Aggarwal I D, et al. Analysis of scattering sites in transparent magnesium aluminate spinel. Ceram. Eng. Sci. Proc., 2005, 26(7): 293-298.
[16]	Lin J N, Wu T B. Wetting reaction between lithium-fluoride and barium-titanate. J. Am. Ceram. Soc., 1989, 72(9): 1709-1712.
[17]	Kleebe H J, Reimanis I E, Cook R L. Processing and microstructure characterization of transparent spinel monoliths. Ceram. Trans., 2005, 157: 61-68.
[18]	Reimanis I E, Kleebe H J, Cook R L, et al. Transparent Spinel Fabricated from Novel Powders: Synthesis, Microstructure and Optical Properties. 10th DoD Electromagnetic Windows Symposium. Norfolk, 2004.
[19]	黄存新. 光学透明多晶尖晶石的制备及应用研究. 北京: 清华大学博士论文, 2005.
[20]	Rozenburg K, Reimanis I E, Kleebe H J, et al. Chemical interaction between LiF and MgAl2O4 spinel during sintering. J. Am. Ceram. Soc., 2007, 90(7): 2038-2042.

LiF对镁铝尖晶石透明陶瓷红外透过率的影响

Influence of LiF on the Infrared Transmissivity of Magnesia Alumina Spinel Transparent Ceramics

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