球磨转速对Nd:YAG透明陶瓷的显微结构及光学性能的影响

doi:10.15541/jim20140621

无机材料学报 ›› 2015, Vol. 30 ›› Issue (6): 581-587.DOI: 10.15541/jim20140621

球磨转速对Nd:YAG透明陶瓷的显微结构及光学性能的影响

刘婧^{1, 2}, 刘军¹, 李江², 林丽^{1, 2}, 潘裕柏², 程晓农¹, 郭景坤²

(1. 江苏大学材料科学与工程学院, 镇江 210031; 2. 中国科学院上海硅酸盐研究所, 透明光功能无机材料重点实验室, 上海 200050)

收稿日期:2014-12-01 修回日期:2015-02-13 出版日期:2015-06-04 网络出版日期:2015-05-22
作者简介:刘婧(1986－), 女, 博士研究生. E-mail: liujing53302@163.com
基金资助:
国家自然科学基金(50990301, 51302298);2013年普通高校研究生科研创新计划项目(CXLX13_650)

Influence of Ball Milling Speed on Microstructure and Optical Transparency of Nd:YAG Ceramics

LIU Jing^{1, 2}, LIU Jun¹, LI Jiang², LIN Li^{1, 2}, PAN Yu-Bai², CHENG Xiao-Nong¹, GUO Jing-Kun²

(1. School of Materials Science and Engineering, Jiangsu University, Zhenjiang 210031, China; 2. Key Laboratory of Transparent Opto-functional Inorganic Materials, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China)

Received:2014-12-01 Revised:2015-02-13 Published:2015-06-04 Online:2015-05-22
About author:LIU Jing. E-mail: liujing53302@163.com
Supported by:
National Natural Science Foundation of China (50990301, 51302298);Colleges and Universities Plans to Graduate Resesrch and Innovation of 2013(CXLX13-650)

摘要/Abstract

摘要：

以高纯商业Y₂O₃、α-Al₂O₃和Nd₂O₃粉体为原料, 以TEOS(正硅酸乙酯)和MgO为烧结助剂, 采用固相反应和真空烧结技术制备了1.0at%Nd:YAG透明陶瓷。系统研究了球磨转速(球磨时间10 h)对混合粉体的尺寸以及对陶瓷样品致密化行为、显微结构和光学性能的影响。结果表明: 通过球磨过程可以充分细化原料粉体的颗粒; 随着球磨转速的提高, 陶瓷烧结时样品中的气孔能更好地排除。但是球磨转速过高时, 陶瓷烧结体中存在少量的富铝第二相会降低样品的光学透过率。当球磨转速为130 r/min时, 真空烧结(1760℃×50 h)所得Nd:YAG透明陶瓷的微结构均匀致密, 几乎没有晶界和晶内气孔存在, 样品在1064 nm处的直线透过率高达83%。

关键词: Nd:YAG激光陶瓷, 球磨转速, 显微结构, 光学性能

Abstract:

Transparent 1.0at%Nd:YAG ceramics were fabricated by the solid-state reaction and vacuum sintering method using Y₂O₃, α-Al₂O₃ and Nd₂O₃ as starting powders. These powders were mixed in ethanol with MgO and TEOS as sintering aids and ball milled at different speeds for 10 h. Effects of ball milling speed on the particle size of powder mixtures as well as the densification process, the microstructure and the optical transparency of Nd:YAG ceramics were mainly investigated. It is showed that coarse powders can be ground into fine particles with increase of the ball milling speed up to 130 r/min. Porosities of the sintered Nd:YAG ceramics decrease with the increase of ball milling speed. Al-rich secondary phase can be observed in the microstructure of Nd:YAG ceramics when the ball milling speed is over-high, and it will cause a decrease in the optical transmittance. For the sample sintered at 1760℃ for 50 h from the powder mixture ball milled at 130 r/min, the in-line transmittance reaches 83% at 1064 nm and there are almost no pores at the grain boundaries and inner grains.

Key words: Nd:YAG laser ceramics, ball milling speed, microstructure, optical transmittance

中图分类号:

TQ129

刘婧, 刘军, 李江, 林丽, 潘裕柏, 程晓农, 郭景坤. 球磨转速对Nd:YAG透明陶瓷的显微结构及光学性能的影响[J]. 无机材料学报, 2015, 30(6): 581-587.

LIU Jing, LIU Jun, LI Jiang, LIN Li, PAN Yu-Bai, CHENG Xiao-Nong, GUO Jing-Kun. Influence of Ball Milling Speed on Microstructure and Optical Transparency of Nd:YAG Ceramics[J]. Journal of Inorganic Materials, 2015, 30(6): 581-587.

图/表 11

图1 原料粉体的显微形貌照片

Fig. 1 FESEM micrographs of the raw powders (a) Y2O3; (b) Y2O3 (at high magnification); (c) α-Al2O3 and (d) Nd2O3

图2 经不同转速球磨(球磨10 h)后的混合粉体的FESEM形貌照片

Fig. 2 FESEM micrographs of the powder mixtures ball milled at different speeds for 10 h (a) 70 r/min; (b) 90 r/min; (c) 130 r/min; (d) 170 r/min

表1 经不同转速球磨后混合粉体的比表面积

Table 1 Specific surface areas (SBET) of powder mixtures ball milled at different speeds for 10 h

Ball milling speed/(r·min^-1)	70	90	110	130	150	170
S_BET /(m²·g^-1)	5.833	6.275	6.985	7.295	7.370	7.412

图3 不同转速球磨的混合粉体经1760 ℃×50 h真空烧结所得Nd:YAG陶瓷的实物照片

Fig. 3 Photographs of Nd:YAG ceramics sintered at 1760℃ for 50 h from the powder mixtures ball milled at different speeds

图4 不同转速球磨的混合粉体经1760℃×50 h真空烧结所得Nd:YAG陶瓷的透过率曲线

Fig. 4 In-line transmittances of Nd:YAG ceramics sintered at 1760℃ for 50 h from powder mixtures ball milled at different speeds (a) 190-1100 nm; (b) 1064 and 400 nm

图5 不同转速球磨的混合粉体在1550℃烧结不同时间所得Nd:YAG陶瓷的致密化曲线

Fig. 5 Relative density versus sintering time at 1550 ℃ for Nd:YAG ceramics from powder mixtures ball milled at different speeds

图 6 不同转速球磨的混合粉体在不同温度烧结2 h后Nd: YAG陶瓷样品的致密化曲线

Fig. 6 Relative density versus sintering temperature for Nd: YAG ceramics from powder mixtures ball milled at different speeds for 2 h

图7 不同转速球磨(球磨10 h)的混合粉体在1600℃×2 h真空烧结后所得陶瓷样品的热腐蚀表面形貌

Fig. 7 SEM micrographs of ceramics sintered at 1600℃ for 2 h from powder mixtures ball milled at different speeds for 10 h (a) 70 r/min; (b) 90 r/min; (c) 110 r/min; (d) 130 r/min; (e) 150 r/min; (f) 170 r/min

图8 不同转速球磨混合粉体在1500~1750℃之间烧结Nd: YAG陶瓷的轨线图

Fig. 8 Sintering trajectory for Nd:YAG ceramics sintered between 1500℃ and 1750℃ from powder mixtures ball milled at different speeds

图9 不同球磨转速所得混合粉体在1550℃真空烧结不同时间所得陶瓷样品的表面形貌

Fig. 9 SEM micrographs of ceramics sintered at 1550℃ for different time from powder mixtures ball milled at different speeds

图10 不同转速球磨所得混合粉体在1760℃×50 h真空烧结后陶瓷样品腐蚀后表面形貌

Fig. 10 EPMA micrographs of ceramics sintered at 1760℃ for 50 h from powder mixtures ball milled at different speeds (a) 70 r/min; (b) 90 r/min; (c) 130 r/min; (d) 170 r/min

参考文献 32

[1]	IKESUE A, AUNG Y L, TAIRA T, et al.Progress in ceramic lasers.Annu. Rev. Mater. Res., 2006, 36: 397-429.
[2]	IKESUE A, AUNG Y L.Ceramic laser materials.Nat. Photonics, 2008, 2(12): 721-727.
[3]	LI J, PAN Y B, ZENG Y P, et al.The history, development, and future prospects for laser ceramics: a review.Int. J. Refract. Met. Hard Mater., 2013, 39: 44-52.
[4]	YAGI H, YANAGITANI T, TAKAICHI K, et al.Characterizations and laser performances of highly transparent Nd3+: Y3Al5O12 laser ceramics.Opt. Mater., 2007, 29(10): 1258-1262.
[5]	IKESUE A, FURUSATO I, KAMATA K.Fabrication of polycrystalline, transparent YAG ceramics by a solid-state reaction method.J. Am. Ceram. Soc., 1995, 78(1): 225-228.
[6]	LU J R, UEDA K, YAGI H, et al.Neodymium doped yttrium aluminum garnet(Y3Al5O12)nano-crystalline ceramics—a new generation of solid state laser and optical materials.J. Alloys Compd., 2002, 341(1-2): 220-225.
[7]	BOULON G.Fifty years of advances in solid-state laser materials.Opt. Mater., 2012, 34(3): 499-512.
[8]	LI X D, LI J G, XIU Z M, et al.Transparent Nd: YAG ceramics fabricated using nanosized γ-alumina and yttria powders.J. Am. Ceram. Soc., 2009, 92(1): 241-244.
[9]	TANG F, CAO Y G, HUANG J Q, et al.Fabrication and laser behavior of composite Yb:YAG ceramic.J. Am. Ceram. Soc., 2012, 95(1): 56-59.
[10]	ZHANG W, LU T, MA B, et al.Improvement of optical properties of Nd: YAG transparent ceramics by post-annealing and post hot isostatic pressing.Opt. Mater., 2013, 35(12): 2405-2410.
[11]	CHEN J C, LI J, XU J L, et al.4350 W quasi-continuous-wave operation of a diode face-pumped ceramic Nd: YAG slab laser.Opt. Laser Technol., 2014, 63: 50-53.
[12]	LEE S H, KOCHAWATTANA S, MESSING G L, et al.Solid-state reactive sintering of transparent polycrystalline Nd: YAG.J. Am. Ceram. Soc., 2006, 89(6): 1945-1950.
[13]	LI J, WU Y S, PAN Y B, et al.Fabrication, microstructure and properties of highly transparent Nd:YAG laser ceramics.Opt. Mater., 2008, 31(1): 6-17.
[14]	SERANONI M, PIANCASTELLI A, COSTA A L, et al.Improvements in the production of Yb:YAG transparent ceramic materials: spray drying optimization. Opt. Mater., 2012, 34(6): 995-1001.
[15]	LIU W B, ZHANG W X, LI J, et al.Synthesis of Nd: YAG powders leading to transparent ceramics: the effect of MgO dopant.J. Eur. Ceram. Soc., 2011, 31(4): 653-657.
[16]	LI J, CHEN F, LIU W B, et al.Co-precipitation synthesis route to yttrium aluminum garnet (YAG) transparent ceramics.J. Eur. Ceram. Soc., 2012, 32(11): 2971-2979.
[17]	LV Y H, ZHANG W, LIU H, et al.Synthesis of nano-sized and highly sinterable Nd: YAG powders by the urea homogeneous precipitation method.Powder Technol., 2012, 217: 140-147.
[18]	CHEN X T, LU T C, WEI N, et al.Effect of ball-milling granulation with PVB adhesive on the sinterability of co-precipitated Yb: YAG nanopowders.J. Alloys Compd., 2014, 589: 448-454.
[19]	LI J, LIU W B, JIANG B X, et al.Synthesis of nanocrystalline yttria powder and fabrication of Cr, Nd:YAG transparent ceramics.J. Alloys Compd., 2012, 515: 49-56.
[20]	LIU B L, LI J, IVANOV M, et al.Solid-state reactive sintering of Nd:YAG transparent ceramics: the effect of Y2O3 powders pretreatment.Opt. Mater., 2014, 36(9): 1591-1597.
[21]	LI J, LIU J, LIU B L, et al.Influence of heat treatment of powder mixture on the microstructure and optical transmission of Nd:YAG transparent ceramics.J. Eur. Ceram. Soc., 2014, 34(10): 2497-2507.
[22]	EPICIER T, BOULON G, ZHAO W, et al.Spatial distribution of the Yb3+ rare earth ions in Y3Al5O12 and Y2O3 optical ceramics as analyzed by TEM.J. Mater. Chem., 2012, 22: 18221-18229.
[23]	STEVENSON A J, KUPP E R, MESSING G L.Low temperature, transient liquid phase sintering of B2O3-SiO2-doped Nd:YAG transparent ceramics.J. Mater. Res., 2011, 26(09): 1151-1158.
[24]	YANG H, QIN X P, ZHANG J, et al.Fabrication of Nd:YAG transparent ceramics with both TEOS and MgO additives.J. Alloys Compd., 2011, 509(17): 5274-5279.
[25]	GUO W, CAO Y G, HUANG Q F, et al.Fabrication and laser behaviors of Nd:YAG ceramic microchips. J. Eur. Ceram. Soc., 2011, 31(13): 2241-2246.
[26]	BA X W, LI J, ZENG Y P, et al.Transparent Y3Al5O12 ceramics produced by an aqueous tape casting method.Ceram. Int., 2013, 39(4): 4639-4643.
[27]	GE L, LI J, ZHOU Z W, et al.Fabrication of composite YAG/Nd: YAG/YAG transparent ceramic for planar waveguide laser.Opt. Mater. Express, 2014, 4(5): 1042-1049.
[28]	FU Y L, LI J, LIU Y, et al.Effect of air annealing on the optical properties and laser behavior of Nd:YAG transparent ceramics.Opt. Mater. Express, 2014, 4(10): 2108-2115.
[29]	LIU J, LIN L, LI J, et al.Effects of ball milling time on microstructure evolution and optical transparency of Nd:YAG ceramics.Ceram. Int., 2014, 40: 9841-9851.
[30]	STEVENSON A J, LI X, MARTINEZ M A, et al.Effect of SiO2 on densification and microstructure development in Nd:YAG transparent ceramics.J. Am. Ceram. Soc., 2011, 94(5): 1380-1387.
[31]	BOULESTEIX R, MAîTRE A, BAUMARD J F, et al. The Effect of silica doping on neodymium diffusion in yttrium aluminum garnet ceramics: implications for sintering mechanisms.J. Eur. Ceram. Soc., 2009, 29(12): 2517-2526.
[32]	KOCHAWATTANA S, STEVENSON A, LEE S H, et al.Sintering and grain growth in SiO2 doped Nd:YAG.J. Eur. Ceram. Soc., 2008, 28(7): 1527-1534.

球磨转速对Nd:YAG透明陶瓷的显微结构及光学性能的影响

Influence of Ball Milling Speed on Microstructure and Optical Transparency of Nd:YAG Ceramics

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