连续有序动态微液团混合法制备掺镧改性钛酸钡及钇铝石榴石纳米粉体的研究
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摘要
BaTiO_3材料具有铁电、压电、热电、介电等特性，广泛用于制造高介电容器、热敏电阻和换能器；YAG单晶是最重要的固体激光基质，在许多领域已得到了广泛的应用。与YAG激光晶体相比多晶YAG透明激光陶瓷具有高掺杂、掺杂均匀成本低等优点。
本论文首次采用导师周教授领导的课题组近年提出的“连续有序快速微液团混合沉淀法”制备了钛酸钡镧和钇铝石榴石纳米粉。采用了透射电镜(TEM)TG-DTA和X射线衍射等实验测试技术对制备的纳米粉体进行了表征。并将粉体压制成素坯进行烧结，并考察了各实验参数对粉体及瓷体的影响。
本文进行了以下研究工作：
1．确定制备纳米钛酸钡镧，钇铝石榴石纳米粉体的实验参数；
2．对所制备的纳米粉体进行TEM形貌分析，估算粒径及其分布情况，由本实验所得的纳米粉体的平均粒径：钛酸钡镧14nm—52nm；钇铝石榴石7nm—32nm；
3．对所制备的粉体进行了XRD物相分析，确定纳米钛酸钡镧为钙钛矿晶形纳米晶、钇铝石榴石为立方晶相纳米晶；
4．讨论了实验参数对于纳米粉体的形貌性质及瓷体的影响；
5．对纳米粉体的制备机理进行了研究，对影响纳米粉体制备的各个因素从根本上进行了分析；
BaTiO_3 materials have piezoelectricity, thermoelectricity, ferroelec- ricity, dielectric and other properties. And it was widely used to made high medium capacitor, thermistor and transducer; YAG is the most important solid-state laser matrix material, and there are wide applicant prospect in scientific research, environmental protection, laser curing and laser welding process."continuous-orderly-dynamic-micro-liquid-agglomerate-mixing" method provided by the research group leaded by prof. Zhou in recent years was firstly adopted to prepare nanoscale BaTiO_3 and yttrium aluminum garnet nanoparticles. The figures and structures of obtained nanocrystal were characterize respectively by TEM and XRD. The powders were compressed into green body and sintered, and also the influence of experimental parameters were investigated.The study described in this thesis consists of six parts:1. Experimental parameters of preparation of nanoscale BaTiO_3 and yttrium aluminum garnet nanoparticles are determined;2. The morphology analysis of the obtained nanopowders has been done by TEM (Transmitting Electronic Microscope), the particle diameters have been evaluated and the distributions of the particle diameter have been discussed as well. The average particle diameters of the obtained nanoparticles:La-BaTiO_3 14nm—52nm; yttrium aluminum garnet 7nm—32nm3. The XRD (X-Ray diffraction) has been performed for the phase analysis. The obtained nanoscale La-BaTiO_3 was perovskite type, yttrium aluminum garnet was cubic in structure.4. The experimental parameters, which have effect on the morphology and property of nanoparticles, have been discussed;5. The mechanism of the preparation of the nanoparticles has been studied and the factors affecting the preparation of nano-particles have been analysted fundamentally;
本论文首次采用导师周教授领导的课题组近年提出的“连续有序快速微液团混合沉淀法”制备了钛酸钡镧和钇铝石榴石纳米粉。采用了透射电镜(TEM)TG-DTA和X射线衍射等实验测试技术对制备的纳米粉体进行了表征。并将粉体压制成素坯进行烧结，并考察了各实验参数对粉体及瓷体的影响。
本文进行了以下研究工作：
1．确定制备纳米钛酸钡镧，钇铝石榴石纳米粉体的实验参数；
2．对所制备的纳米粉体进行TEM形貌分析，估算粒径及其分布情况，由本实验所得的纳米粉体的平均粒径：钛酸钡镧14nm—52nm；钇铝石榴石7nm—32nm；
3．对所制备的粉体进行了XRD物相分析，确定纳米钛酸钡镧为钙钛矿晶形纳米晶、钇铝石榴石为立方晶相纳米晶；
4．讨论了实验参数对于纳米粉体的形貌性质及瓷体的影响；
5．对纳米粉体的制备机理进行了研究，对影响纳米粉体制备的各个因素从根本上进行了分析；
BaTiO_3 materials have piezoelectricity, thermoelectricity, ferroelec- ricity, dielectric and other properties. And it was widely used to made high medium capacitor, thermistor and transducer; YAG is the most important solid-state laser matrix material, and there are wide applicant prospect in scientific research, environmental protection, laser curing and laser welding process."continuous-orderly-dynamic-micro-liquid-agglomerate-mixing" method provided by the research group leaded by prof. Zhou in recent years was firstly adopted to prepare nanoscale BaTiO_3 and yttrium aluminum garnet nanoparticles. The figures and structures of obtained nanocrystal were characterize respectively by TEM and XRD. The powders were compressed into green body and sintered, and also the influence of experimental parameters were investigated.The study described in this thesis consists of six parts:1. Experimental parameters of preparation of nanoscale BaTiO_3 and yttrium aluminum garnet nanoparticles are determined;2. The morphology analysis of the obtained nanopowders has been done by TEM (Transmitting Electronic Microscope), the particle diameters have been evaluated and the distributions of the particle diameter have been discussed as well. The average particle diameters of the obtained nanoparticles:La-BaTiO_3 14nm—52nm; yttrium aluminum garnet 7nm—32nm3. The XRD (X-Ray diffraction) has been performed for the phase analysis. The obtained nanoscale La-BaTiO_3 was perovskite type, yttrium aluminum garnet was cubic in structure.4. The experimental parameters, which have effect on the morphology and property of nanoparticles, have been discussed;5. The mechanism of the preparation of the nanoparticles has been studied and the factors affecting the preparation of nano-particles have been analysted fundamentally;
引文
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[2] Sugi moto, Yasutake[P]JP 2001 64 077
[3] Komatsu Kazuhiro, Kuramitsu Hideki[P].Jpn Kokai Tokyo Koho 2000 26 78 JP,2000,34,166
[4] Hood Christopher, Bultitude John, Chu Mike Ssu-HA[P] Eur Pat Appl,EP 726 235
[5] 张道礼等．钛酸钡系PTCR半导体陶瓷烧结过程的计算机模拟．烧结中后期及奥氏熟化过程中的晶粒生长[J]．功能材料，2001，31(5)：528—530
[6] 齐建全等．B_2O_3蒸汽掺杂的中低温烧结Y-BaTiO_3及其PTCR特性研究[J]．无机材料学报，1999，14(3)：408—411
[7] Yanovskaya M I,kotova N M,kovsman E P,et al[J]J Sol-Gel Sci Techno 1,1994,2(1/2/3):569—573
[8] 孔令兵，张良莹等．溶胶-凝胶制备铁电材料(Sr_((0.5))Ba_((0.5-x))Pb_x)TiO_3微粉及表征[J]．功能材料，1997，28(2)：146—149
[9] 刘静波，王智民等．掺镧改性钛酸钡纳米多晶粉体的制备和表征[J]．无机材料学报，2002，17(5)：945—951
[10] 范仰才，蒋力立等．溶胶凝胶法制备掺铅钛酸钡纳米晶及其结构相变[J] 无机材料学报，2000，15(5)：797—800
[11] 吴淑荣，李东升等不同Ti／Ba摩尔比的钛酸钡纳米晶粉体的Sol-gel法制备与表征．[J]．功能材料，1998，29(6)：609—612
[12] 吴淑荣，畅柱国等．不同稀土元素掺杂对钛酸钡陶瓷导电性的影响[J]．功能材料，1997，28(5)：509—510
[13] 吴明梅，李里，徐如人．(Ba，Pb)TiO_3的水热合成[J]．化学学报，1996，54，1181—1185
[14] Adair J H, Kerchner J A, Bell N S, et al[J]Acs Sym Ser, 1998,681:82—94
[15] 范素华，任嗥等．共沉淀法合成Bi掺杂钛酸钡基介电陶瓷的研究[J]．陶瓷学报，2003，24(4)：210—214
[16] 丁士文等，Ba_((1-1.5y))La_yZr_XTi_(1-x)O_3固溶体的合成、结构与介电特性．[J]．无机化学学报，1998，12(4)：445—448
[17] 沈志刚，陈建峰等．Ba_((1_x))Sr_xTiO_3纳米粉体的直接沉淀法合成结构与介电特性[J]．功能材料，2003，34(5)：556—558
[18] Hansen, D Hennings&H Schreinemacher. Dielectric properties of acceptor-doped (Ba, Ca) (Ti, Zr)O_3 ceramice [J]. Journal of Electroceramics,1998, (2):85-94
[19] kaya D Glinchuk, Lgor P Bykov&Sergei M Kornienko et al.Influence of impurities of the properties of rare-earth-doped barium-titanate sera mice[J].J.Mater.Chem.,2000,10:941-947
[20] Lei hang, Wei—Lie Zhong&Chun—Lei Wang et al. Finite—size effects in ferroelectxic solid solution Ba_xSr_(1-x)TiO_3[J].J. Phys.D. Appl.phys.,1999,32:546-551
[21] Xiaomei Guo and Kenji SKURAL.Jpan.J.Apply.Phys,2000(39):1230—34
[22] Qiwu Zhang,Fumio Saito,Powdex Technology,2003.129:86—91
[23] M.Sekita,H.Haneda,T.Yanagitani et al. J. Appl. Phys,1990.67(1):453—58
[24] T. Yanagitani, H. Yagi, M. Ichikawa Japan patent,1998:10—10133
[25] T. Yanagitani, H. Yagi, Y. Hiro. Japan patent,1998:10—101411
[26] J.Lu,M.Prubhu,J,Xu et al. Appl.Phys,Lett,2000.77(23):3707—09
[27] J.Lu,M.Prubhu,K.Ueda et al Laser Phys.,201.11(10):1053—57
[28] J.Lu,T.Murai,K.Takaichietal.Appl.Phys.Lett,2001.78(23):3586-88
[29] Ji—yong Park,Seong—Geun Oh. Bt al.1VHter. Letter,2002.56:429—34
[30] I. Matsubara. M. Paranthaman et al.1VHter. Res. Bull,2003.35:217—24
[31] Yukiya Hakuta, Kazuei Scino et al. J.1VHter. Che m.1999.9:2671-74
[32] Masashi Inoue,Hiroyuki Oksu et al.J.Am.Ceram.Soc,1991.74(6):1452—54
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