Yb~（3+）：Y_2O_3透明陶瓷超细粉体的制备及性能研究
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摘要
Yb~(3+)：Y_2O_3激光透明陶瓷是一种新型激光工作物质，展示了潜在的应用前景。为了制备性能优异的陶瓷材料，其先决条件是制备出粒度均匀、分散性好、尺度小的超细Yb~(3+)：Y_2O_3粉体。本文采用液相共沉淀法与低温燃烧法制备Yb~(3+)：Y_2O_3超细粉体。
采用XRD、TG-DTA、TEM、FT-IR及荧光光谱分析等手段表征了Yb~(3+)：Y_2O_3超细粉体。系统地研究了共沉淀法中起始pH值、NH_4HCO_3的滴加速度、表面活性剂、反应温度、保温时间、陈化时间、Yb离子掺杂量等因素对Yb~(3+)：Y_2O_3粉体形貌、粒径大小及性能的影响，并对共沉淀法制备超细粉体中的团聚问题进行分析。在低温燃烧法中考察了点火温度、燃料用量和热处理温度对所获得的粉体特性的影响。
结果表明，采用共沉淀法制备Yb~(3+)：Y_2O_3超细粉体的粒径在100～200nm，最佳工艺参数是8Yb~(3+):Y_2O_3 ceramics is a new candidate for high power laser. Obtaining ultrafine powders with uniform size and good dispersion are the prerequisite for preparing transparent Yb~(3+):Y_2O_3 ceramics with high optical quality. In this thesis the liquid phase co-deposited method and LCS method were adopted to prepare the Yb~(3+):Y_2O_3 ultrafine powders.
XRD, TG-DTA, TEM, FT-IR and the fluorescence spectra analysis were employed to characterize the Yb~(3+):Y_2O_3 ultrafine powders. The influences of seven factors, including initial pH value , anti-aggregative agent, reaction temperature, holding time, Yb ion content on the morphology, size and property of the powders were systematically studied. The agglomeration phenomenon of the powders prepared by the co-precipitation method was analyzed. The influences of ignition temperature, fuel content and calcination temperature on the characteristics of the powders were investigated for the LCS method.
The particle diameters of Yb~(3+):Y_2O_3 ultrafine powders synthesized by the co-precipitation method were about 100 - 200nm. The optimum technology parameters were obtained as followings. The pH value is between 8 and 9. The titration velocity should be less than 2ml per minute. Surfactant (NH_4)_2SO_4 was 5mol% to Y(NO_3)_3. The calcining temperature and time of the powders were 1100℃and 4 hours, Yb content is 3at.%. The luminescence spectrum is consisted of three peaks at 976nm, 1030nm and 1075nm respectively under excitation of 514nm which is attributed to transition of ~2F_(5/2)→~2F_(7/2) of Yb~(3+). Among the three peaks 1030nm showed the strongest intensity.. Absolute ethyl alcohol decreased the conglobation phenomenon of the ultrafine powders. The particle diameters of Yb~(3+):Y_2O_3 ultrafine powders prepared by using the LCS method were about 15-30nm. The optimum technology parameters of LCS were that the value of nitrate : urea was 3:1, and the ignition temperature was about 600℃.
采用XRD、TG-DTA、TEM、FT-IR及荧光光谱分析等手段表征了Yb~(3+)：Y_2O_3超细粉体。系统地研究了共沉淀法中起始pH值、NH_4HCO_3的滴加速度、表面活性剂、反应温度、保温时间、陈化时间、Yb离子掺杂量等因素对Yb~(3+)：Y_2O_3粉体形貌、粒径大小及性能的影响，并对共沉淀法制备超细粉体中的团聚问题进行分析。在低温燃烧法中考察了点火温度、燃料用量和热处理温度对所获得的粉体特性的影响。
结果表明，采用共沉淀法制备Yb~(3+)：Y_2O_3超细粉体的粒径在100～200nm，最佳工艺参数是8
XRD, TG-DTA, TEM, FT-IR and the fluorescence spectra analysis were employed to characterize the Yb~(3+):Y_2O_3 ultrafine powders. The influences of seven factors, including initial pH value , anti-aggregative agent, reaction temperature, holding time, Yb ion content on the morphology, size and property of the powders were systematically studied. The agglomeration phenomenon of the powders prepared by the co-precipitation method was analyzed. The influences of ignition temperature, fuel content and calcination temperature on the characteristics of the powders were investigated for the LCS method.
The particle diameters of Yb~(3+):Y_2O_3 ultrafine powders synthesized by the co-precipitation method were about 100 - 200nm. The optimum technology parameters were obtained as followings. The pH value is between 8 and 9. The titration velocity should be less than 2ml per minute. Surfactant (NH_4)_2SO_4 was 5mol% to Y(NO_3)_3. The calcining temperature and time of the powders were 1100℃and 4 hours, Yb content is 3at.%. The luminescence spectrum is consisted of three peaks at 976nm, 1030nm and 1075nm respectively under excitation of 514nm which is attributed to transition of ~2F_(5/2)→~2F_(7/2) of Yb~(3+). Among the three peaks 1030nm showed the strongest intensity.. Absolute ethyl alcohol decreased the conglobation phenomenon of the ultrafine powders. The particle diameters of Yb~(3+):Y_2O_3 ultrafine powders prepared by using the LCS method were about 15-30nm. The optimum technology parameters of LCS were that the value of nitrate : urea was 3:1, and the ignition temperature was about 600℃.
引文
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5 G. E. Gazza and S. K. Dutta. U. S. Patent, 3767745,1973
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9 楼祺洪，马海霞，漆云凤等．Yb~(3+)：Y_2O_3透明陶瓷激光器获得5W连续激光输出[J]．光学学报．2004，24(3)： 431-432
10 漆云凤，楼祺洪，董景星等．Yb：Y_2O_3陶瓷薄片激光器获得10．5W连续激光输出[J]．光学学报．2006，26 (5)：797-798
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33 朴贤卿，刘景和，裴广庆等．稀土掺杂YAG透明激光陶瓷的粉体制备研究．2004,89(3)417-419
34 朴贤卿．Nd：YAG透明陶瓷的制各：[硕士论文]长春：长春理工大学材料系，2004
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38 Fu Y P , Lin C H , Hsu C S.Preparation of ultrafine CeO_2 powders by microwave2induced combustion and precipitation [J]. J .Alloys Compd.,2005,391 (1 - 2): 110
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2 刘军芳，傅正义，张东明等．透明陶瓷的研究现状与发展展望[J]．陶瓷学报．2002，23(4)：246-250
3 E. Carnall. Improved polycrystalline ceramics lasers[J]. Mater. sci. Res, 1966(3):165-173
4 J. Kong, D. Y. Tang, D. Y.Shen, et al. Diode pumped Yb:Y_2O_3 ceramic laser Proc. SPIE, 4914:69-76
5 G. E. Gazza and S. K. Dutta. U. S. Patent, 3767745,1973
6 C.Muller,N.Neuroth.Glass ceramic-a new laser host material[J].Apple.Phy.1973,44(5):2315-2318
7 C.Greskovich,J.P.Chernoch.Improved polycrystalline ceramic lasers[J].Apple.Phy. 1974,45(10): 4495-4502
8 朴贤卿，卢利萍，刘景和等．尿素共沉淀法制畚Yb：YAG透明激光陶瓷[J]．功能材料与器件学报．2004,10(2)：264- 268
9 楼祺洪，马海霞，漆云凤等．Yb~(3+)：Y_2O_3透明陶瓷激光器获得5W连续激光输出[J]．光学学报．2004，24(3)： 431-432
10 漆云凤，楼祺洪，董景星等．Yb：Y_2O_3陶瓷薄片激光器获得10．5W连续激光输出[J]．光学学报．2006，26 (5)：797-798
11 李劲东，姜本学，潘裕柏等．国产Nd：YAG陶瓷获得激光输出[J].中国激光．2006(6)：864
12 O ceramicJ. Kong, J. Lu, K. Takaichi, et al. Diode-pumped Yb:Y_2 O_3 laser[J].Appl.Phys. Lett.,2003,82:2556-2258
13 J.Lu,K. Takaichi, T.Uematsu, etal. Promising ceramic laser material.Highly transparent Nd-(3+):Lu_2O_3 ceramic[J]. Appl. Phys. Lett., 2002,23:4324-4326
14 J. Saikawa, Y. Sato, T. Taira, et al.Absorption, emission spectrum properties, and efficient laser performances of Yb:Y_3 ScAl_4O_(12) ceramics[J].Appl.Phys.Lett.,2004,85(1 1):1898- 1900
15 K. Takaichi, H. Yagi, J. Lu, et al. Highly efficient continuous-wave operation at 1030 and 1075 nm wavelengths of LD-pumped Yb-(3+): Y_2O_3 ceramic lasers[J]. Appl.Phys.Lett.,2004,84(3):317-319
16 J. Lu, J. F. Bisson, K. Takaichi, et al. Yb-(3+):Sc_2O_3 ceramic laser[J]. Appl. Phys.Lett,2003,83(6): 1101-1103
17 谢征芳，陈朝晖，李永清．特种陶瓷的发展与展望[J]．中国陶瓷工业．2000,7(1)：31-36
18 殷声．现代陶瓷及其应用[M]．北京：北京科学技术出版社．1990：256-258
19 李世普．特种陶瓷工艺学[M]．武汉：武汉工业出版社．1990：321-325
20 刘军芳，傅正义，张东明等．放电等离子烧结(SPS)技术烧结致密AIN陶瓷[J]．陶瓷学报．2001，22(3)：157-161．
21 De With Gand, Van Dijk. Transluent Y_3Al_5O_(12) ceramics [ J] .Mater Res Bull, 1984,29( 12): 1669-1674.
22 Roy D W, Hastert J L1 Polycrystalline MgAl_2O_4 spinel for use as windows and domes from 0. 3 to 6. 0 micrometers[J]. SPIE proc ,1983 ,400 .356-368
23 宋琼，苏春辉，张洪波等．均相沉淀法制备Nd：YAG透明激光陶瓷材料研究[J]．激光与红外．2006,36(1)：44-46
24 张希艳，田雪雁，刘全生．制备Nd~(3+)：Gd_3Ga_5O_(12)透明陶瓷的纳米粉体[J]．中国激光．2006,33(3)376-379
25 P. L acovara, H. K. Chai, C. A. W ang et al.. Room2tenperature diode2pumped Yb:YAG laser[ J]. Op t.L ett., 1991,16 (14):1089-1091
26 WILLIAM K F, CHASELL. Ground-state depleted solid-state lasers: principles, characteristics and scaling [J]. Opt Quantun Election,1990,22:S1-S22.
27 LACOVARA P, CHOI H K, WANG C A, et al. Room-temperature diocie-pumped Yb:YAG lasers [J]. Opt lett,1991,16(4):1089-1091.
28 M. Sekita ,H. Haneda ,T. Yanagitani et al. J. Appl. Phys, 1990.67 (1) :453
29 T. Yanagitani ,H. Yagi ,M. Ichikawa Japan patent, 1998 :10 -10133
30 T. Yanagitani ,H. Yagi ,Y. Hire. Japan patent ,1998 :10 - 101411
31 LU Jianren, Song Jie, M. Prabhu, et al. High-power Nd:Y_3Al_5O_(12) ceramic laser[J]. Jpn. Appl. Phy., 2000, 39(6): 1048-1050
32 LU Jianren, K. Ueda, H. Yagi, et al. Neodymium doped yttrium aluminum garnet (Y_3Al_5O_(12)) nanocrystalline ceramics a new generation of solid-state laser and optical materials[J]. J Alloy Compd, 2002,43(1 ):220-225
33 朴贤卿，刘景和，裴广庆等．稀土掺杂YAG透明激光陶瓷的粉体制备研究．2004,89(3)417-419
34 朴贤卿．Nd：YAG透明陶瓷的制各：[硕士论文]长春：长春理工大学材料系，2004
35 程永亮，宋武林，谢长生．燃烧法制备氧化物纳米材料的研究进展．2003，17(7)：70-72
36 Mokkelbost T , Kau I, Grande T , et al. Combustion synthesis and characterization of nanocrystalline CeO2based powders [J] .Chem. Mater. 2004,16 (25): 5489
37 Mahata T, Das G, Mishra R K, et al. Combustion synthesis of gadolinia doped ceria powder [J]. J. Alloys Compd., 2005,391(1 -2):129
38 Fu Y P , Lin C H , Hsu C S.Preparation of ultrafine CeO_2 powders by microwave2induced combustion and precipitation [J]. J .Alloys Compd.,2005,391 (1 - 2): 110
39 Aruna S T , Patil K C.Combustion synthesis and properties nanostructured of ceria2zirconia solid solutions [J].Nanostruct .Mater.1998,10 (6):955
40 Merzhanov A G,Shkiro V M,Borovinskaya I p. Method of producing refractory carbides,borides,silicides,and nitrides of groups Ⅳ,Ⅴ.and Ⅵ of Periodic Systems [J].U S Pat ,3726643.Apr.10,1973,1- 10.
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