电泳沉积法制备纳米磁电多铁性复合薄膜的研究
详细信息    本馆镜像全文|  推荐本文 |  |   获取CNKI官网全文
摘要
本课题利用溶胶-凝胶法制备了纳米级的钛酸钡(BaTiO_3)粉体,利用共沉积法制备了钴铁氧体(CoFe_2O_4)粉体。
     对胶体悬浮液的配制进行了探索,采取乙醇加乙酰丙酮的体系,配制出了稳定的BaTiO_3、CoFe_2O_4、NiFe_2O_4胶体悬浮液。对胶体悬浮液的运动性质、电学性质和稳定性做了比较深入的研究,从微观上阐述了稳定的胶体悬浮液的形成机制。
     搭建了简易的电泳沉积平台,对电泳沉积用衬底电极材料Pt/Ti/SiO2/Si和ITO导电膜玻璃做了一定的比较研究。在ITO导电膜玻璃上电泳沉积出了BaTiO_3单层膜、CoFe_2O_4单层膜、NiFe_2O_4单层膜、BaTiO_3-CoFe_2O_4双层膜、BaTiO_3-NiFe_2O_4双层膜、BaTiO_3-CoFe_2O_4混合膜、BaTiO_3-NiFe_2O_4混合膜。对BaTiO_3单层膜而言,沉积电压30V,沉积时间10min可以得到比较合格的BaTiO_3单层膜。CoFe_2O_4单层膜的一般沉积电压为30V,沉积时间为3min。NiFe_2O_4单层膜的沉积电压是30V,沉积时间取2min。以上三种单层膜的退火工艺都是以250℃/h的升温速率,550℃下保温20min。制得合格的BaTiO_3单层膜后,在其上面继续电泳沉积CoFe_2O_4或者NiFe_2O_4,这样就得到了BaTiO_3-CoFe_2O_4双层膜或者BaTiO_3-NiFe_2O_4双层膜。用BaTiO_3粉体和CoFe_2O_4粉体配制成的混合悬浮液,可以电泳沉积得到BaTiO_3-CoFe_2O_4混合膜。BaTiO_3粉体和NiFe_2O_4粉体配制成的混合悬浮液,可电泳沉积BaTiO_3-NiFe_2O_4混合膜。
     对薄膜的表面形貌和电磁性能做了分析。BaTiO_3单层膜的铁电性能较好,CoFe_2O_4单层膜和NiFe_2O_4单层膜的铁磁性能较好。由于双层膜和混合膜表面都一定程度地存在漏电流,所以其铁电性能不理想。相比较而言,BaTiO_3-CoFe_2O_4双层膜和BaTiO_3-CoFe_2O_4混合膜的矫顽力和剩磁较大,但是漏电流过大,铁电性能不理想;BaTiO_3-NiFe_2O_4双层膜和BaTiO_3-NiFe_2O_4混合膜的矫顽力和剩磁很小,属于明显的软磁材料,其铁电性能比BaTiO_3-CoFe_2O_4双层膜和BaTiO_3-CoFe_2O_4混合膜的好一些。
Prepare nano-barium titanate (BaTiO_3) powders by a sol-gel method, and prepare ironcobalt (CoFe_2O_4) powders by a co-deposition method.
     Find out a suitable way to prepare colloidal suspensions, get a stable BaTiO_3suspension, CoFe_2O_4 suspension and NiFe_2O_4 suspension by the system of acetylacetoneand ethanol. Study the movement, electrical properties and stability of the suspensions,expla in the formation mecha nism of a stable colloidal suspension.
     Build a simple platform for the electrophoretic deposition, do some studies about thesubstrates such as Pt/Ti/SiO 2/Si and ITO conductive film glass. And then get a BaTiO_3single-la yer film, a CoFe_2O_4 single-la yer film, a NiFe_2O_4 single-la yer film, a BaTiO_3-CoFe_2O_4 double-la yer film, a BaTiO_3-NiFe_2O_4 double-la yer film, a BaTiO_3-CoFe_2O_4 mixedfilm, a BaTiO_3-NiFe_2O_4 mixed film by the electrophoretic deposition method on ITOconductive film glasses. For the BaTiO_3 single-la yer film, the most appropriate depositionvoltage is 30V, deposition time is 10min. For the CoFe_2O_4 single-la yer film, the commondeposition voltage is 30V, deposition time is 3min. For the NiFe_2O_4 single-la yer film, thecommon deposition voltage is 30V, deposition time is 2min. And their annealing conditionis sintered at 550℃for 20min.
     Analyse the surface morphology and electroma gnetic properties of the films. TheBaTiO_3 single-la yer film’s ferroelectric properties is not bad, so as the ferroma gneticproperties of the CoFe_2O_4 single-la yer film or NiFe_2O_4 single-la yer film. The hysteresis loopis not so well because of the leakage current on the surface of double-la yer and mixed films.Comparatively speaking, the coercivity(Hc) and resid ual ma gnetization(Mr) of BaTiO_3-CoFe_2O_4 double-la yer film and BaTiO_3-CoFe_2O_4 mixed film are higher, but theirferroelectric properties are bad for the large leakage current; the coercivity(Hc) and resid ualma gnetization(Mr) of BaTiO_3-NiFe_2O_4 double-la yer film and BaTiO_3-NiFe 2O4 mixed filmare very sma ll, but their ferroelectric properties are better.
引文
[1]吕文中,汪小红.电子材料物理,第1版.北京:电子工业出版社, 2002
    [2]陈辉.掺杂钴铁氧体CoxFe3-xO4纳米微晶结构与磁性研究. [硕士学位论文].合肥:安徽大学, 2006
    [3]路晓艳,刘玉岚,王彪.多重铁性材料的研究进展.材料导报, 2007, 21(3):17~20
    [4] Zhou J. P., He H. C., Shi Z. et al. Dielectric, ma gnetic, and ma gnetoelectricproperties of la minated PbZr0.52Ti0.48O3/CoFe2O4 composite ceramics. J. Appl. Phys.,2006, 100
    [5] Scott J. F.. Multiferroic memories. Nature Materia ls, 2007, 6: 256~257
    [6] Ramesh R., Spaldin N. A.. Multiferroics: progress and prospects in thin films.Nature Materia ls, 2007, 6: 21~29
    [7] Spaldin N. A., Fiebig M.. The Rena issa nce of Magnetoelectric Multiferroics.Science, 2005, 309: 391~392
    [8] Nan C. N., Bichurin M. I., Dong S. X. et al. Multiferroic ma gnetoelectric composites:Historica l perspective, status, and future directions. J. Appl. Phys., 2008, 103
    [9]展,王翠萍,刘兴军等.基于磁电复合材料的四态存储器.科学通报, 2008,53(10): 1177~1179
    [10]徐任信,王钧,周静等.室温磁电材料的制备与性能.材料导报, 2008, 22(7):8~13
    [11] Zurbuchen M. A., Wu T., Saha S., et al. Multiferroic composite ferroelectricferromagnetic films. Appl. Phys. Lett., 2005, 87
    [12] Eerenstein W., Mathur N. D., Scott J. F.. Multiferroic and ma gnetoelectric materia ls.Nature, 2006, 442: 759~765
    [13] Duong G. V., Groessinger R., Turtelli R. S.. Driving mecha nism for ma gnetoelectriceffect in CoFe2O4-BaTiO3 multiferroic composite. Journal of Magnetism andMagnetic Materia ls, 2007, 310: 1157~1159
    [14] Duong G. V., Groessinger R., Turtelli R. S.. Effect of structure on ma gnetoelectricproperties of CoFe2O4-BaTiO3 multiferroic composites. Journal of Magnetism andMagnetic Materia ls, 2007, 310: e361~e363
    [15] Fiebig M.. Revival of the ma gnetoelectric effect. J. Phys. D: Appl. Phys., 2005, 38:R123~R152
    [16]许雪芹.多铁性材料BiFeO3溶胶-凝胶制备及磁性研究. [博士学位论文].合肥:中国科学技术大学, 2006
    [17]印晓明.锰酸盐(稀土合金)-锆钛酸铅铁电铁磁多层膜中的磁电效应. [硕士学位论文].南京:南京师范大学, 2007
    [18]南策文.从非常规复合效应产生新型材料.自然科学进展, 2004, 14(4): 390~396
    [19]唐耀华. Sr0.5Ba0.5Nb2O6/CoFe2o4基铁电铁磁复合功能陶瓷. [硕士学位论文].杭州:浙江大学, 2005
    [20]周剑平,何泓材,展等. PMNNT/CoFe2O4复合材料的结构和磁电性能.硅酸盐学报, 2006, 34(10): 1213~1219
    [21] Zha ng S. T., Ding L. Y., Lu M. H. et al. Preparation and multiferroic properties ofBi0.8La0.2FeO3-CoFe2O4 ceramics. Solid State Communica tions, 2008, 148: 420~423
    [22]张善涛.复合相多铁性陶瓷(1-x)BaTiO3-xCoFe2O4的制备和性质.南京工业大学学报(自然科学版). 2008, 30(3): 1~5
    [23] Wan J. G., Liu J. M., Wang G. H. et al. Electric-field-induced ma gnetization inPb(Zr,Ti)O3/Terfenol-D composite structures. Appl. Phys. Lett., 2006, 88
    [24] Wan J. G., Wang X. W., Wu Y. J. et al. Magnetoelectric CoFe2O4-Pb(Zr,Ti)O3composite thin films derived by a sol-gel process. Appl. Phys. Lett., 2005, 86
    [25]林元华,姜庆辉,何泓材等.多铁性氧化物基磁电材料的制备及性能.硅酸盐学报, 2007, 35(S1): 10~21
    [26] Zheng H., Wang J., Lofla nd S. E. et al. Multiferroic BaTiO3-CoFe2O4 Nanostructures.Science, 2004, 303: 661~663
    [27] Chang K. S., Aronova M. A., Lin C. L. et al. Exploration of artificia l multiferroicthin-film heterostructures using composition spreads. Appl. Phys. Lett., 2004, 84(16):3091~3093
    [28]周剑平,展,刘刚等.铁电/铁磁1-3型结构复合材料磁电性能分析.物理学报, 2006, 55(7): 3766~3771
    [29] Nan C. W., Liu G., Lin Y. H. et al. Magnetic-Field-Induced Electric Polariza tion inMultiferroic Nanostructures. Physica l Review Letters, 2005, 94
    [30] Liu G., Nan C. W., Xu Z. K. et al. Coupling interaction in multiferroic BaTiO3-CoFe2O4 nanostructures. Journal of Physics D: Applied Physics, 2005, 38: 2321-2326
    [31]李扩社,李红卫,严辉等.磁电复合材料的研究进展.稀有金属, 2008, 32(3):369~374
    [32]何泓材,林元华,南策文.多铁性磁电复合薄膜.科学通报, 2008, 53(10):1136~1148
    [33]金沈贤,钟智勇,任学恒等. Fe3O4缓冲层对CoFe2O4薄膜磁性能的影响.功能材料, 2007,增刊(38): 1080~1083
    [34]李雁,方庆清,刘艳美等. Co0.7Fe2.3O4纳米晶颗粒与薄膜的结构及磁性.磁性材料及器件, 2006, 37(3): 28~42
    [35]李雁,方庆清,吕庆荣等. Co2+含量对钴铁氧体薄膜结构级磁性的影响.磁性材料及器件, 2006, 37(6): 30~33
    [36] Cheng F. X., Peng Z. Y., Xu Z. G. et al. The sol-gel preparation and AFM study ofspin CoFe2O4 thin film. Thin Solid Films, 1999, 339: 109~113
    [37] Lee J. G., Lee H. M., Kim C. S. et al. Magnetic properties of CoFe2O4 powders andthin film grown by a sol-gel method. Journal of Magnetism and Magnetic Materia ls,1998, 177-181: 900~902
    [38]刘红日. BiFeO3薄膜的溶胶凝胶方法的制备、掺杂及电磁性质的研究. [博士学位论文].武汉:华中科技大学, 2006
    [39] Liu M., Li X., Lou J. et al. A modified sol-gel process for multiferroicnanocomposite films. J. Appl. Phys., 2007,102
    [40] Thing P. D., Rijnders G., Bla nk D. H. A.. Stress-induced ma getic anisotropy ofCoFe2O4 thin film using pulsed laser deposition. Journal of Magnetism andMagnetic Materia ls, 2007, 310: 2621~2623
    [41] Singh M. P., Prellier W., Mechin L. et al. Effect of ferroelectric la yers on thema gnetocapacita nce properties of superlattices-based oxide multiferroics. Appl.Phys. Lett., 2006, 88
    [42] Zhou J. P., He H. C., Shi Z.. Magnetoelectric CoFe2O4/Pb(Zr0.52Ti0.48)O3 double-la yerthin film prepared by pulsed-laser deposition. Appl. Phys. Lett., 2006, 88
    [43] Deng C. Y., Zha ng Y., Ma J. et al. Magnetic-electric properties of epitaxialmultiferroic NiFe2O4-BaTiO3 heterostructure. J. Appl. Phys., 2007, 102
    [44] Tassel J. V., Randall C. A.. Electrophoretic Deposition and Sintering of Thin/ThickPZT Films. Journal of the European Ceramic Society, 19 (1999): 955~958
    [45]马亚鲁,孙小兵,王彦起等.应用电泳沉积技术制备钛酸钡铁电陶瓷薄膜.硅酸盐通报, 2002, 6: 13~26
    [46] Louh R. F., Hsu Y. H.. Fabrication of barium titanate ferroelectric la yers byelectrophoretic deposition technique. Materia ls Chemistry and Physics, 2003, 79:226–229
    [47]唐波,陈秀丽,刘来君等.电泳沉积技术制备铁电陶瓷薄膜的研究进展.材料导报, 2005, 19(1): 33~35
    [48]张瑞芳,张和平.电泳沉积法制备PZT厚膜及其性能.硅酸盐学报, 2004,32(12): 1486~1490
    [49]康妮.锆钛酸铅陶瓷厚膜电泳沉积技术研究. [硕士学位论文].北京:清华大学,2005
    [50] Wu Y. J., Li J., Tanaka H. et al. Preparation of nano-structured BaTiO3 thin film byelectrophoretic deposition and its characteriza tion. Journal of the European CeramicSociety, 2005, 25: 2041~2044
    [51]魏长松.溶胶电泳沉积法制备PZT膜材料技术及性能研究. [硕士学位论文].武汉:武汉理工大学, 2006
    [52] Zhao J. L., Wang X. H., Li L. T.. Electrophoretic deposition of BaTiO3 films fromaqueous suspensions. Materia ls Chemistry and Physics, 2006, 99: 350~353
    [53]王希林,薛昊,周和平.电泳沉积法制备Ba0.6Sr0.4TiO3厚膜及介电性能研究.稀有金属材料与工程, 2007, 36(增刊1): 935~938
    [54]闫小兵,刘保亭,边芳等.铁电/铁磁复合材料的制备及研究进展.河北大学学报(自然科学版), 2007, 27(2): 213~218
    [55]陈春芳.片式PTCR元件用粉体的Sol-gel法制备及性能研究: [硕士学位论文].武汉:华中科技大学, 2007
    [56]王欣.稀土改性钴镍铁氧体纳米粒子的制备及磁性能的研究. [硕士学位论文].上海:上海师范大学, 2003
    [57] Zha ng D. E., Zha ng X. J., Ni X. M. et al. Synthesis and characteriza tion of CoFe2O4octahedrons via an EDTA-assisted route. Journal of Magnetism and MagneticMateria ls, 2006, 305: 68~70
    [58]余之松,熊锐,周忠坡. CoFe2O4的制备及电子结构.信息记录材料, 2008, 9(1):60~64
    [59] Junior A. F., Lima E. C. O., Novak M. A. et al. Synthesis of nanoparticles of CoxFe(3-x)O4 by combustion reaction method. Journal of Magnetism and Magnetic Materia ls,2007, 308: 198~202
    [60]肖利.溶胶-凝胶法制备纳米级CoFe2O4尖晶石及掺杂导电聚乙二醇的研究. [硕士学位论文].长沙:中南大学
    [61] Turtelli R. S., Duong G. V., Nunes W. et al. Magnetic properties of nanocrystallineCoFe2O4 synthesized by modified citrate-gel method. Journal of Magnetism andMagnetic Materia ls, 2008, 320: e339~e342
    [62]陈辉,方庆清,李雁等.钴铁氧体CoxFe3-xO4结构和磁性研究.安徽大学学报(自然科学版), 2007, 31(4): 48~50
    [63]段红珍.铁氧体纳米粉体的制备与表征研究. [硕士学位论文].太原:华北工学院,2004
    [64]徐平,韩喜江,王晓红.无定形B-Co合金包覆对尖晶石钴铁氧体电磁性能的影响.功能材料, 2007,增刊(38): 997~999
    [65]曲玉秋.钛酸钡与铁氧体及其纳米复合颗粒的制备与表征. [硕士学位论文].长春:吉林大学, 2006
    [66]刘银,丘泰,沈春英等.纳米晶Co1-xNixFe2O4铁氧体的制备及Ni2+对其磁性能的影响.硅酸盐学报. 2007, 35(2): 160~163
    [67]吕庆荣,方庆清,李瑞等.钴铁氧体纳米晶粒的结构及磁性能研究.安徽大学学报(自然科学版), 2006, 30(2): 71~74
    [68] Kim Y., Kim D., Lee C. S.. Synthesis and characteriza tion of CoFe2O4 ma gneticnanoparticles prepared by temperature-controlled coprecipitation method. Physics B,2003, 337: 42~51
    [69] Maaz K., Mumtaz A., Hasanain S. K. et al. Synthesis and ma gnetic properties ofcobalt ferrite(CoFe2O4) nanoparticles prepared by wet chemica l route. Journal ofMagnetism and Magnetic Materia ls, 2007, 308: 289~295
    [70] Thang P. D., Rijnders G., Bla nk D. H. A.. Spinel cobalt ferrite by complexometricsynthesis. Journal of Magnetism and Magnetic Materia ls, 2005, 295: 251~256
    [71]邵海成,戴红莲,黄健等.化学共沉淀法合成CoFe2O4纳米颗粒及其磁性能.硅酸盐学报, 2005, 33(8): 959~962
    [72]车仁超,李永清,陈朝辉等.钴铁氧体微粉的化学法制备工艺及其吸波性能.宇航材料工艺, 1999, 6: 46~48
    [73] Besra L., Liu M. L.. A review on fundamenta ls and applica tions of electrophoreticdeposition(EPD). Materia ls Science, 2007, 52: 1~61.
    [74] Kanamura K., Hamagami J.. Innova tion of novel functiona l materia l processingtechnique by using electrophoretic deposition process. Solid State Ionics, 2004(172):303~308
    [75]陈宗淇,王光信,徐桂英.胶体与界面化学,第1版.北京:高等教育出版社,2004
    [76]赵振国.应用胶体与界面化学,第1版.北京:化学工业出版社, 2008
    [77]程书洁.基于阳极氧化铝模板的金属氧化物及其复合一维纳米材料的电泳沉积法制备和表征. [硕士学位论文].郑州:河南大学, 2007
    [78]赵建玲,王晓慧,郝俊杰等.电泳沉积及其在新型陶瓷工艺上的应用.功能材料, 2005, 2(36): 165~172
    [79]张道礼,胡云香,黎步银等.电泳沉积原理及其在陶瓷制备中的应用.现代技术陶瓷, 1999, 4: 22~25
    [80]符云飞,樊慧庆,邓永丽等.电泳沉积法制备Ba0.6Sr0.4TiO 3厚膜及其电学性能研究.无机材料学报,2008, 23(4): 687~690
    [81] Antonellia E., Silva R. S., Vicente F. S. et al. Electrophoretic deposition ofBa0.77Ca0.23TiO3 nanopowders. Journal of materia ls processing technology, 2008,203: 526~531
    [82] Zha ng L., Zha i J. W., Yao X.. Dielectric properties of barium strontium titanate thickfilms prepared by electrophoretic deposition. Materia ls Research Bulletin, 2008
    [83] Santilla n M. J., Caneiro A., Quaranta N. et al. Electrophoretic deposition ofLa0.6Sr0.4Co0.8Fe0.2O3-δcathodes on Ce0.9Gd0.1O1.95 substrates for intermed iatetemperature solid oxide fuel cell(IT-SOFC). Journal of the European CeramicSociety, 2008
    [84] Chen J., Fan H. Q., Chen X. L. et al. Fabrication of pyrochlore-free PMN-PT thickfilms by electrophoretic deposition. Journal of Alloys and Compounds, 2008
    [85]曹玉萍,李玉国,孙钦军.电泳沉积法制备MgO薄膜.微纳电子技术, 2007, 1:23~25
    [86]侯俊波,安茂忠.用电泳沉积方法制备LiCoO2薄膜.材料保护, 2005, 38(9):9~48
    [87]朱亚彬,周岳亮,成正维.电泳法制备YBCO超导厚膜的电阻特性研究.北京交通大学学报. 2005, 29(3): 1~3
    [88]关维晔. TiO2纳米薄膜的制备. [硕士学位论文].长春:吉林大学, 2004
    [89]周静,李君,魏长松等.溶胶电泳沉积法制备PZT压电厚膜及其性能研究.人工晶体学报, 2007, 36(1): 38~41

© 2004-2018 中国地质图书馆版权所有 京ICP备05064691号 京公网安备11010802017129号

地址:北京市海淀区学院路29号 邮编:100083

电话:办公室:(+86 10)66554848;文献借阅、咨询服务、科技查新:66554700