Nd3+:Lu2O3放电等离子烧结及光学性能

doi:10.15541/jim20170110

无机材料学报 ›› 2017, Vol. 32 ›› Issue (12): 1315-1320.DOI: 10.15541/jim20170110 CSTR: 32189.14.10.15541/jim20170110

Nd³⁺:Lu₂O₃放电等离子烧结及光学性能

安丽琼^1,2, 章健², 范润华¹, GOTO Takashi³, 王士维²

1. 上海海事大学海洋科学与工程学院, 上海 201306;
2. 中国科学院上海硅酸盐研究所,高性能陶瓷和超微结构国家重点实验室, 上海 200050;
3. 日本东北大学金属材料研究所, 仙台 980-8577

收稿日期:2017-03-09 修回日期:2017-04-13 出版日期:2017-12-20 网络出版日期:2017-11-21
作者简介:安丽琼(1979-),女,副教授. E-mail: anlq@shmtu.edu.cn
基金资助:
高性能陶瓷和超微结构国家重点实验室开放课题(SKL201501SIC);上海市青年东方学者(QD2015043);国家自然科学基金青年基金(51602194);上海市自然科学基金(15ZR1419600);The Open Project of State Key Laboratory of High Performance Ceramics and Superfine Microstructure (SKL201501SIC);Young Eastern Scholar at Shanghai Institutions of Higher Learning (QD2015043);National Natural Science Foundation of China (51602194);Natural Science Foundation of Shanghai (15ZR1419600)

Sintering and Optical Property of Nd³⁺:Lu₂O₃ Fabricated by Spark Plasma Sintering

AN Li-Qiong^1,2, ZHANG Jian², FAN Run-Hua¹, GOTO Takashi³, WANG Shi-Wei²

1. College of Ocean Science and Engineering, Shanghai Maritime University, Shanghai 201306, China;
2. The State Key Lab of High Performance Ceramics and Superfine Microstructure, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China;
3. Institute for Materials Research, Tohoku University, Sendai 980-8577, Japan

Received:2017-03-09 Revised:2017-04-13 Published:2017-12-20 Online:2017-11-21

摘要/Abstract

摘要：

Lu₂O₃是具有高热导率而成为极具潜力的高功率激光介质材料。实验以商用氧化物粉体为原料, LiF为烧结助剂, 采用放电等离子烧结法制备了不同Nd³⁺掺杂浓度(C_Nd=0, 1at%, 3at%和5at%) Lu₂O₃透明陶瓷, 并研究了Nd³⁺掺杂浓度对Lu₂O₃陶瓷的物相、烧结性能、微观结构及光学性能的影响。结果表明：在高Nd³⁺浓度(5at%)掺杂后烧结样品仍为纯Lu₂O₃相;Nd³⁺掺杂对Lu₂O₃陶瓷烧结性能及微观形貌的影响有限;所有样品最终均表现出高致密性(99.5%以上)和优异的透光性能, 其中3at% Nd³⁺:Lu₂O₃的透过率最高, 在1064和2000 nm处的透过率分别为82.7和83.2%。Nd³⁺:Lu₂O₃透明陶瓷的最强发射峰位于1076和1080 nm;且随着Nd³⁺掺杂浓度的增加, 荧光强度降低, 寿命变短, 发生浓度淬灭。

关键词: 放电等离子烧结, Nd³⁺:Lu₂O₃, Nd³⁺掺杂浓度

Abstract:

Lu₂O₃ is a novel material for high-power solid-state lasers due to its high thermal conductivity. In present work, Nd³⁺:Lu₂O₃ transparent ceramics with different Nd³⁺ doping concentration (C_Nd = 0, 1at%, 3at% and 5at%) were fabricated by spark plasma sintering, using commercial oxides as raw materials and LiF as sintering aid. The effect of Nd³⁺ doping concentration on phase, sintering property, microstructure and optical properties was investigated. X-ray powder diffraction (XRD), scanning electron microscopy (SEM), UV-VIS-NIR spectroscopy, and fluorescence spectroscopy were used for characterization. The results show that the sintered body exhibits pure Lu₂O₃ phase even with high Nd³⁺ doping concentration (5at%). The Nd³⁺ doping concentration has little influence on densification behavior and microstructure of Nd³⁺:Lu₂O₃ ceramics. All the sintered bodies have a high relative density above 99.5% and excellent transparency, in which 3at% Nd³⁺:Lu₂O₃ body shows highest transmittance, with values of 82.7% and 83.2% at 1064 and 2000 nm, respectively. Nd³⁺:Lu₂O₃ transparent ceramics show strongest emission bands located at 1076 and 1080 nm, which are attributed to the ⁴F_3/2→⁴I_11/2 transition of Nd³⁺ ions. The emission intensity and decay time decrease with increasing Nd³⁺ doping concentration, which indicates concentration quenching.

Key words: spark plasma sintering, Nd³⁺:Lu₂O₃, Nd³⁺ doping concentration

中图分类号:

TQ174

安丽琼, 章健, 范润华, GOTO Takashi, 王士维. Nd³⁺:Lu₂O₃放电等离子烧结及光学性能[J]. 无机材料学报, 2017, 32(12): 1315-1320.

AN Li-Qiong, ZHANG Jian, FAN Run-Hua, GOTO Takashi, WANG Shi-Wei. Sintering and Optical Property of Nd³⁺:Lu₂O₃ Fabricated by Spark Plasma Sintering[J]. Journal of Inorganic Materials, 2017, 32(12): 1315-1320.

图/表 9

图1 Nd3+:Lu2O3透明陶瓷所采用的放电等离子烧结分段烧结制度

Fig. 1 Sintering profile of Nd3+:Lu2O3 transparent ceramics produced by spark plasma sintering

图2 (a) 5at% Nd3+:Lu2O3透明陶瓷的XRD图谱和(b)不同Nd3+掺杂浓度Lu2O3透明陶瓷的晶格常数

Fig. 2 (a) Typical XRD pattern of the 5at% Nd3+:Lu2O3 transparent ceramic and (b) lattice parameters of Lu2O3 transparent ceramics with different Nd3+ doping concentration Inset in (a) shows the fine XRD patterns of Lu2O3 transparent ceramics with different Nd3+ doping concentrations in the 2θ range of 77°-80°

图3 不同Nd3+掺杂浓度Lu2O3透明陶瓷的相对致密度曲线

Fig. 3 Relative density of Lu2O3 transparent ceramics with different Nd3+ doping concentrations

图4 5at% Nd3+:Lu2O3透明陶瓷的热腐蚀表面(a)和断口(b)SEM照片

Fig. 4 SEM images of thermally etched (a) and fracture (b) surfaces of the 5at% Nd3+:Lu2O3 transparent ceramic

图5 退火前后不同Nd3+掺杂浓度Lu2O3透明陶瓷的样品照片

Fig. 5 Photographs of Lu2O3 transparent ceramics with different Nd3+ doping concentrations before and after annealing

图6 (a) 退火前后5 at%Nd3+:Lu2O3透明陶瓷的透过率曲线和(b)退火前(红色标记)后(黑色标记)不同掺杂浓度Nd3+:Lu2O3透明陶瓷在代表波长处(1064和2000 nm)的透过率曲线

Fig. 6 (a) Transmittance spectra of the 5 at%Nd3+:Lu2O3 transparent ceramics before and after annealing and (b) transmittance at representative wavelengths (1064 and 2000 nm) for Nd3+:Lu2O3 transparent ceramics with different doping concentrations before (red) and after annealing (dark) The dot line refers to theoretical transmission of Lu2O3 calculated from ref[19]

图7 (a) 不同Nd3+掺杂浓度Lu2O3透明陶瓷退火后的吸收光谱曲线和(b)退火前后Nd3+: Lu2O3透明陶瓷在806 nm处的吸收系数

Fig. 7 (a) Absorption coefficient spectra of Lu2O3 transparent ceramics with different Nd3+ doping concentration after annealing and (b) absorption coefficient at 806 nm for the Lu2O3 transparent ceramics with different Nd3+ doping concentrations before and after annealing

图8 不同Nd3+掺杂浓度Lu2O3透明陶瓷在808 nm激光激发下的常温发射光谱

Fig. 8 Emission spectra of Lu2O3 transparent ceramics with different Nd3+ doping concentration irradiated by an 808 nm diode laser at room temperature

图9 不同Nd3+掺杂浓度Lu2O3透明陶瓷的荧光寿命。实线为拟合曲线

Fig. 9 Fluorescence lifetime of Lu2O3 transparent ceramics with different Nd3+ doping concentration and the fitted curve (solid line)

参考文献 26

[1]	GRIEBNER U, PETROV V, PETERMANN K,et al. Passively mode-locked Yb:Lu2O3 laser. Opt. Express, 2004, 12(14): 3125-3130.
[2]	LU J, TAKAICHI K, UEMATSU T,et al. Promising ceramic laser material: highly transparent Nd3+: Lu2O3 ceramic. Appl. Phys. Lett., 2002, 81(23): 4324-4326.
[3]	ZHOU X Q, YI H L, ZHOU G H,et al. Highly transmitting ZrO2-doped Lu2O3 ceramics from combustion synthesized powders. J. Am. Ceram. Soc., 2011, 94(9): 2772-2774.
[4]	ANTIPOV O L, NOVIKOV A A, ZAKHARO N G,et al. Optical properties and efficient laser oscillation at 2066 nm of novel Tm: Lu2O3 ceramics. Opt. Mater. Express, 2012, 2(2): 183-189.
[5]	QIAO X B, HUANG H T, YANG H,et al. Fabrication, optical properties and LD-pumped 2.7 μm laser performance of low Er3+ concentration doped Lu2O3 transparent ceramics. J. Alloy. Comp., 2015, 640(8): 51-55.
[6]	SANGHERA J, FRANTZ J, KIM W,et al. 10% Yb3+- Lu2O3 ceramic laser with 74% efficiency. Opt. Lett., 2011, 36(4): 576-578.
[7]	KIM W, BAKER C, BOWMAN S,et al. Laser oscillation from Ho3+ doped Lu2O3 ceramics. Opt. Mater. Express, 2013, 3(7): 913-919.
[8]	AN L Q, ITO A, ZHANG J,et al. Highly transparent Nd3+: Lu2O3 produced by spark plasma sintering and its laser oscillation. Opt. Mater. Express, 2014, 4(7): 1420-1426.
[9]	ITO A, AN LQ, GOTO T.Laser oscillation and luminescence of Nd3+- and Eu3+-doped Lu2O3 transparent ceramics fabricated by spark plasma sintering.J. Ceram. Soc. Jpn., 2016, 124(4): 313-320.
[10]	TOCI G, VANNINI M, CIOFINI M,et al. Nd3+-doped Lu2O3 transparent sesquioxide ceramics elaborated by the Spark Plasma Sintering (SPS) method. Part 1: Structural, thermal conductivity and spectroscopic characterization. Opt. Mater., 2015, 41(S1): 3-11.
[11]	TOCI G, VANNINI M, CIOFINI M,et al. Nd3+-doped Lu2O3 transparent sesquioxide ceramics elaborated by the Spark Plasma Sintering (SPS) method. Part 2: First laser output results and comparison with Nd3+-doped Lu2O3 and Nd3+-Y2O3 ceramics elaborated by a conventional method. Opt. Mater., 2015, 41(3): 12-16.
[12]	XU C W, YANG C D, ZHANG H,et al. Efficient laser operation based on transparent Nd: Lu2O3 ceramic fabricated by spark plasma sintering. Opt. Express, 2016, 24(18): 20571-20579.
[13]	BOULESTEIX R, EPHERRE R, NOYAU S,et al. Highly transparent Nd: Lu2O3 ceramics obtained by coupling slip-casting and spark plasma sintering. Scr. Mater. 2014, 75(3): 54-57.
[14]	KAMINSKII A A.Laser crystal and ceramics: recent advances.Laser Photon. Rev., 2007, 1(2): 93-177.
[15]	TAIRA T.Domain-controlled laser ceramics toward giant micro- photonics.Opt. Mater. Express, 2011, 1(5): 1040-1050.
[16]	ZHOU D, SHI Y, XIE J,et al. Fabrication and luminescent properties of Nd3+-doped Lu2O3 transparent ceramics by pressureless sintering. J. Am. Ceram. Soc., 2009, 92(10): 2182-2187.
[17]	ZHOU D, SHI Y, YUN P,et al. Effect of precipitants on the properties of Nd3+:Lu2O3 nano-powders. J. Inorg. Mater., 2009, 24(4): 764-768.
[18]	LIU J, LIU Q, LI J,et al Influence of doping concentration on microstructure evolution and sintering kinetics of Er:YAG transparent ceramics.Opt. Mater., 2014, 37(11): 706-713.
[19]	KAMINSKII A A, AKCHURIN M S, BECKER P,et al. Mechanical and optical properties of Lu2O3 host-ceramics for Ln3+ lasants. Laser Phys. Lett., 2008, 5(4): 300-303.
[20]	JIANG D, HULLERT D M, ANSELMI-TAMBURINI U,et al. Optically transparent polycrystalline Al2O3 produced by spark plasma sintering. J. Am. Ceram. Soc., 2008, 91(1): 151-154.
[21]	ANSELMI-TAMBURINI U, WOOLMAN J, MUNIR Z.Transparent nanometric cubic and tetragonal zirconia obtained by high-pressure pulsed electric current sintering.Adv. Funct. Mater., 2007, 17(16): 3267-3273.
[22]	SHANNON R D.Dielectric polarizabilities of ions in oxides and fluorides, J. Appl. Phys., 1993, 73(1): 348-366.
[23]	HAO L, WU K, CONG H,et al. Spectroscopy and laser performance of Nd: Lu2O3 crystal. Opt. Express, 2011, 19(18): 17774-17779.
[24]	SATO Y, TAIRA T, IKESUE A.Spectral parameters of Nd3+-ions in the polycrystalline solid-solution composed of Y3Al5O12 and Y3Sc2Al3O12.Jpn. J. Appl. Phys., 2003, 42(8): 5071-5074.
[25]	HOU X R, ZHOU S M, JIA T T,et al. Effect of Nd concentration on structural and optical properties of Nd:Y2O3 transparent ceramic. J. Luninescence, 2011, 131(9): 1953-1958.
[26]	POWELL R C.Physics of Solid-state Laser Materials. New York: Springer, 1998: 335.

Nd³⁺:Lu₂O₃放电等离子烧结及光学性能

Sintering and Optical Property of Nd³⁺:Lu₂O₃ Fabricated by Spark Plasma Sintering

RichHTML

PDF (PC)

可视化

摘要/Abstract

引用本文

使用本文

图/表 9

参考文献 26

相关文章 15

编辑推荐

Metrics

本文评价

[1]	李俊生, 曾良, 刘荣军, 王衍飞, 万帆, 李端. 锶钽氧氮化物功能陶瓷的高效合成、致密化及介电性能研究[J]. 无机材料学报, 2023, 38(8): 885-892.
[2]	万朋, 李勉, 黄庆. 熔盐辅助合成Dy₃Si₂C₂包裹SiC粉体及其陶瓷的烧结行为[J]. 无机材料学报, 2021, 36(1): 49-54.
[3]	赵占奎, 李涛, 鲁书含, 王明罡, 张京京, 程道文, 吴臣, 迟悦, 王虹力. SPS界面反应增强机制调控的软磁复合材料磁性能和电阻率[J]. 无机材料学报, 2020, 35(11): 1223-1226.
[4]	王伟, 罗世阶, 鲜聪, 肖群, 杨洋, 欧云, 刘运牙, 谢淑红. 水热合成BiCl₃/Bi₂S₃复合材料的热电性能[J]. 无机材料学报, 2019, 34(3): 328-334.
[5]	王明辉, 钟洪彬, 范宇驰, 陈婷. SPS烧结制备生物活性镁黄长石陶瓷[J]. 无机材料学报, 2017, 32(8): 825-830.
[6]	李松浩, 张忻, 刘洪亮, 郑亮, 张久兴. Ag掺杂SnSe化合物的制备及热电性能[J]. 无机材料学报, 2016, 31(7): 751-755.
[7]	姚铮, 仇鹏飞, 李小亚, 陈立东. n型填充方钴矿热电材料的快速制备研究[J]. 无机材料学报, 2016, 31(12): 1375-1382.
[8]	邢志波, 李敬锋. AgSn₁₈SbTe₂₀无铅中温热电材料的粉末冶金法制备工艺及其对性能的影响[J]. 无机材料学报, 2015, 30(8): 872-876.
[9]	梁超龙, 张忻, 张久兴, 张繁星, 王杨. La_1-_xNd_xB₆阴极材料的制备及性能研究[J]. 无机材料学报, 2015, 30(4): 363-368.
[10]	唐云山, 柏胜强,任都迪,廖锦城,张澜庭, 陈立东. Yb_0.3Co₄Sb₁₂/Mo-Cu热电元件的界面结构与界面电阻[J]. 无机材料学报, 2015, 30(3): 256-260.
[11]	黄林芸, 李晨辉, 柯文明, 史玉升, 贺智勇, 张启富. 稀土氧化物对SPS烧结AlN陶瓷电性能的影响[J]. 无机材料学报, 2015, 30(3): 267-271.
[12]	韩志明, 张忻, 路清梅, 张久兴, 张飞鹏. (Mg₂Si_1-xSb_x)_0.4-(Mg₂Sn)_0.6固溶体合金的制备及热电输运特性[J]. 无机材料学报, 2012, 27(8): 822-826.
[13]	林挺, 许志斌, 邓莲芸, 任玉英, 施鹰, 谢建军. Ce:Lu₂SiO₅闪烁陶瓷的放电等离子烧结与发光性能[J]. 无机材料学报, 2011, 26(11): 1210-1214.
[14]	包黎红, 张久兴, 周身林. Ba掺杂对稀土硼化物GdB₆结构, 晶粒取向和热发射性能的影响[J]. 无机材料学报, 2011, 26(10): 1116-1120.
[15]	王磊1,2, 路清梅1,2, 张忻1,2, 张久兴1,2. 快淬和球磨时间对p型(Bi_0.25Sb_0.75)₂Te₃合金热电性能的影响[J]. 无机材料学报, 2010, 25(6): 588-592.