SiO_2包覆磁性纳米粒子的制备及表征
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摘要
本论文工作的目标是采用反相微乳液的方法,制备出SiO2包覆的磁性纳米粒子,并利用TEM、SEM、XRD、FT-IR和VSM等手段表征这些磁性纳米复合粒子的结构、尺寸、形状及其磁学性质。具体内容如下：
一、采用化学共沉淀法制备出柠檬酸三铵改性的Fe3O4纳米粒子,并做为种子,在反相微乳液中制备了Fe3O4@SiO2纳米复合粒子。用X射线衍射(XRD)仪,透射电子显微镜(TEM),傅立叶—红外光谱仪(FT-IR)和振动样品磁强计(VSM)表征Fe3O4@SiO2磁性纳米复合粒子。结果表明,SiO2成功包覆在Fe3O4表面,且饱和磁化强度下降,但包覆前后Fe3O4纳米粒子矫顽力趋近于零,显示超顺磁性。
二、用乙酰丙酮铁(Fe(acac)3)和氯铂酸(H2PtCl6·6H2O)作为Fe源和Pt源,硼氢化钠(NaBH4)作为还原剂,通过湿化学还原法制备FePt纳米粒子做为种子,在OP-10／正丁醇／环己烷／浓氨水／的反相微乳液体系中,用油包水型反相微乳液法实现Si02对FePt纳米粒子的硅层包覆。用X射线衍射仪(XRD),透射电子显微镜(TEM),傅立叶—红外光谱仪(FT-IR)和振动样品磁强计(VSM)对FePt@SiO2纳米复合粒子进行了表征。结果表明,SiO2成功包覆在FePt表面,且磁性纳米复合粒子饱和磁化强度几乎不变,矫顽力趋近于零,仍显示超顺磁性。
In this thesis, the magnetic nanoparticles coated with silica were prepared via a reverse micelle method, and their crystalline structure, particle size, morphology and magnetic properties were characterized by XRD, TEM, FT-IR and VSM. The detailed content was given as follows:
1) Firstly, Fe3O4 nanoparticles were synthesized by a chemical coprecipitation method, and the triammonium citrate used as addition was added during this process. Then, Fe3O4 nanoparticles were coated with silica (Fe3O4@SiO2) via a reverse micelle method. The structure and magnetic properties of the Fe3O4@SiO2 nanoparticles were investigated by XRD, TEM, FT-IR, VSM respectively and the results showed:The silica were coated successfully on the surface of Fe3O4 nanoparticles; Since the coating of silica, the saturation magnetization showed a result of decrease; The coercivity of the Fe3O4 nanoparticles was near zero before and after coating performance, revealing the Fe3O4@SiO2 nanoparticles were of superparamagnetic properties.
2) Fe(acac)3 and H2PtCl6·6H2O were used as Fe ions and Pt ions sources. NaBH4 was used as reductant. FePt nanoparticles were prepared by wet chemical reduction method. Thereafter, FePt nanoparticles used as seed particles were added the reverse microemulsion which was made up of OP-10/buty alcohol/cyclohexane/water. FePt@SiO2 nanoparticles were successfully prepared by a water-in-oil microemulsion method. The structure and magnetic properties of the FePt@SiO2 nanoparticles were investigated by XRD, TEM, FT-IR, VSM and the results showed:the silica were coated successfully on the surface of FePt nanoparticles but their saturation magnetization changed scarely before and after coating performance; The coercivity of the FePt@SiO2 nanoparticles was near zero, indicating they were of superparamagnetic properties.
一、采用化学共沉淀法制备出柠檬酸三铵改性的Fe3O4纳米粒子,并做为种子,在反相微乳液中制备了Fe3O4@SiO2纳米复合粒子。用X射线衍射(XRD)仪,透射电子显微镜(TEM),傅立叶—红外光谱仪(FT-IR)和振动样品磁强计(VSM)表征Fe3O4@SiO2磁性纳米复合粒子。结果表明,SiO2成功包覆在Fe3O4表面,且饱和磁化强度下降,但包覆前后Fe3O4纳米粒子矫顽力趋近于零,显示超顺磁性。
二、用乙酰丙酮铁(Fe(acac)3)和氯铂酸(H2PtCl6·6H2O)作为Fe源和Pt源,硼氢化钠(NaBH4)作为还原剂,通过湿化学还原法制备FePt纳米粒子做为种子,在OP-10／正丁醇／环己烷／浓氨水／的反相微乳液体系中,用油包水型反相微乳液法实现Si02对FePt纳米粒子的硅层包覆。用X射线衍射仪(XRD),透射电子显微镜(TEM),傅立叶—红外光谱仪(FT-IR)和振动样品磁强计(VSM)对FePt@SiO2纳米复合粒子进行了表征。结果表明,SiO2成功包覆在FePt表面,且磁性纳米复合粒子饱和磁化强度几乎不变,矫顽力趋近于零,仍显示超顺磁性。
In this thesis, the magnetic nanoparticles coated with silica were prepared via a reverse micelle method, and their crystalline structure, particle size, morphology and magnetic properties were characterized by XRD, TEM, FT-IR and VSM. The detailed content was given as follows:
1) Firstly, Fe3O4 nanoparticles were synthesized by a chemical coprecipitation method, and the triammonium citrate used as addition was added during this process. Then, Fe3O4 nanoparticles were coated with silica (Fe3O4@SiO2) via a reverse micelle method. The structure and magnetic properties of the Fe3O4@SiO2 nanoparticles were investigated by XRD, TEM, FT-IR, VSM respectively and the results showed:The silica were coated successfully on the surface of Fe3O4 nanoparticles; Since the coating of silica, the saturation magnetization showed a result of decrease; The coercivity of the Fe3O4 nanoparticles was near zero before and after coating performance, revealing the Fe3O4@SiO2 nanoparticles were of superparamagnetic properties.
2) Fe(acac)3 and H2PtCl6·6H2O were used as Fe ions and Pt ions sources. NaBH4 was used as reductant. FePt nanoparticles were prepared by wet chemical reduction method. Thereafter, FePt nanoparticles used as seed particles were added the reverse microemulsion which was made up of OP-10/buty alcohol/cyclohexane/water. FePt@SiO2 nanoparticles were successfully prepared by a water-in-oil microemulsion method. The structure and magnetic properties of the FePt@SiO2 nanoparticles were investigated by XRD, TEM, FT-IR, VSM and the results showed:the silica were coated successfully on the surface of FePt nanoparticles but their saturation magnetization changed scarely before and after coating performance; The coercivity of the FePt@SiO2 nanoparticles was near zero, indicating they were of superparamagnetic properties.
引文
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[2]刑丽英.隐身材料.北京：化学工业出版社,2004,5
[3]Joseph L.Kirschvink, James L.Gould. Biogenic magnetite as a basis for magnetic field detection in animals. Biosystems,1981,13(3):181-201
[4]Shouheng Sun, C. B. Murray. Synthesis of monodisperse cobalt nanocrystals and their assembly into magnetic superlattices. Applied Physics,1999,85(8): 4325-4331
[5]Michael R.Diehl, Jae-Young Yu, James R.Heath, et al. Physical Chemistry,2001, 105(33):7913-7919
[6]Zhonglin Wang, Zurong Dai, Shouheng Sun. Polyhedral shapes of cobalt nanocrystals and their effect on ordered nanocrystal assembly. Advanced Materials, 2000,12(24):1944-1946
[7]Diandra L.Leslie-Pelecky, Reuben D.Rieke R. Magnetic properties of nanostructured materials. Chemistry Materials,1996,8(8):1770-1783
[8]Won Seok Seo, Hyong Hoon Jo, Kwangyeol Lee K, et al. Size-Dependent magnetic properties of colloidal Mn3O4 and MnO nanoparticles. Angewandte chemie,2004,43:1115-1117
[9]Shouheng Sun, Hao Zeng, David B.Robinson, et al. Monodisperse MFe2O4 (M= Fe, Co, Mn) Nanoparticles. The American Chemical,2004,126(1),273-279
[10]Comstock R L. Introduction to magnetism and magnetic recording. Wiley, New YOrk,1999
[11]R.A.McCurrie R. Ferromagnetic materials structure and properties. Academic press, London,1994
[12]Makino A, Inoue A, Masumoto T. Nanocrystalline soft magnetic Fe-M-B (M=Zr, Hf, Nb) alloys produced by crystallization of amorphous phase (Overview). Materials transations,1996,36(7):924-938
[13]Caiyin You, X K Sun, Wei Liu. Effect of Co and W additions on the structure and magnetic properties of Nd2Fe14B nanocomposite magnets.physics D:Applied Physics,2000,33(8),926-931
[14]侯鹤岚,张世伟,杨乃恒.磁流体技术的发展及应用.真空,1999,10(5)：8-12
[15]周寿曾.稀土永磁材料及其应用.北京：冶金工业出版社,1990,12
[16]杨毅,李凤生.超细粒子复合技术进展.材料导报,2001,15(3)：35-37
[17]穆加尼K,科埃J M D.磁性玻璃.北京：科学出版社,1989,61-97
[18]杨华,黄可龙,刘素琴,等.水热法制备的Fe304磁流体.Magn Mater Devices,2003,34(2)：4-6
[19]黄菁菁,徐祖顺,易昌风.化学共沉淀法制备纳米四氧化三铁粒子.湖北大学学报(自然科学版),2007,29(1)：50-52
[20]JunWang, Kai Zhang, Zhenmeng Peng, et al. Magnetic properties improvement in Fe3O4 nanopartic lesgrownunder magnetic fields. Crystal Growth,2004,266:500-504
[21]王全胜,刘颖,王建华,等.沉淀氧化法制备Fe304的影响因素研究.北京理工大学学报,1994,14(2)：200-205
[22]Laiqiong Yu, Luji Zheng, Jixiao Yang. Study of preparation and properties on magnetization and stability for ferromagnetic fluids. Materials Chemistry and Physics, 2000,66(1):6-9
[23]陈雷,杨文军,黄程,等.以高分子材料为介质制备纳米氧化铁颗粒.高分子材料科学与工程,1998,14(4)：53-55
[24]赵朝辉,姚素薇,张卫国.纳米Fe304磁性颗粒的制备及应用现状.化工进展,2005,24(8)：865-868
[25]Rong Fan, Xianhui Chen, Gui Zhou, et al. A new simplehy drothermal preparation of nanocrystalline magnetite Fe3O4. Materals Research Bulletin,2001,36:497-502
[26]Chun Feng, Baohe Li, Gang Han, et al. Effect of the underlayer(Ag,Ti or Bi)on the magnetic properties. Thin Soid Films,2007,515:8009-8012.
[27]Gopalan R, Kundig A A, Ohnuma M, et al. Scripta Mater,2005,52:761-765
[28]Nakagawa S, Kamiki T. Highly (001) oriented FePt ordered without seed layers. J Magn Magn Mater,2005,287:204-208.
[29]Tamada Y, Morimoto Y, Yamamoto S, et al. Effects of annealing time on structural and magnetic properties of Llo-FePt nanoparticles synthesized by the SiO2-nanoreactor method. J Magn Magn Mater,2007,310(2):2381-2383
[30]Bo Yao, Kevin R.Coffey. The influence of periodicity on the structures and properties of annealed [Fe/Pt]n multilayer films. J Magn Magn Mater,2008, 320(3):559-564.
[31]Gopalan R, Kundig A A, Ohnuma M, et al. Mechanically milled-and spark plasma sintered FePt-Based bulk magnets with high coercivity. Scripta Mater,2005, 52(8):761-765.
[32]Cagnon L, Dahmane Y, Voiron J, et al. Electrodeposited CoPt and FePt alloys nanowires.J Magn Magn Mater,2007,310(2):2428-2430.
[33]Leistner K, Backen, Schupp B, et al. Phase formation, microstructure, and hard magnetic properties of electrodeposited FePt films. J Appl Phys,2004,95: 7267-7270.
[34]Thongmee S, Ding J, Lin J Y, et al. FePt films fabricated by electrodeposition. Applied Physics,2007,101(9):9519-9521
[35]Svedberg E B, van de veerdonk R J M, Howard, et al. Quantifiable combinatorial materials science approach applied to perpendicular magnetic recording media. Appl Phys,2003,95:5519-5521
[36]Songzhu Chu, Satoru Inoue, Kenji Wada, et al. Fabrication of integrated arrays of ultrahigh density magnetic nanowires on glass by anodization and electrodeposition. Electrochim Acta,2005,51(5):820-826.
[37]Sun S, Murray C B, Weller D, et al. Monodisperse FePt nanoparticles and ferromagnetic FePt nanocrystal superlattices. Science,2000,287:1989-1992
[38]Howard L E M, Nguyen H L, Gibin S R, et al. A synthetic route to size-controlled fcc and fct FePt nanoparticles. American Chemical Society,2005,127(29): 10140-10141.
[39]Elkins K E, Vedantam T S, Liu J P, et al. Ultrafine FePt nanoparticles prepared by the chemical reduction method. Nano Letters,2003,3(12):1647-1649
[40]Guerrero-Ruiz A, Sepulveda-Escribano A, Rodriguez-Ramos I, et al. Cooperative action of cobalt and MgO for the catalysed reforming of CH4 with CO2. Catal. Today,1994,21(2):545-550
[41]Chao Liu, Xiaowei Wu, Timothy Klemmer, et al. Physical Chemistry B,2004, 108(20):6121-6123
[42]李玲.表面活性剂与纳米技术.北京：化学工业出版社,2004,145-150
[43]Jaeyun Kim, JI Eun Lee, Jinwoo Lee, et al. Magnetic fluorescent delivery vehicle using uniform mesoporous silica spheres embedded with monodisperse magnetic and semiconductor nanocrystal. Am Chem Soe,2006,128:688-692
[44]钱军民,李旭祥,黄海燕.纳米材料的性质及其制备方法.化工新型材料,2001,29(7)：1-5
[45]Mal N K, Fujiwara M, Tanaka Y. Photocont rolled reversible release of guest molecules from coumarinmodified mesoporous silica. Nature,2003,421: 350-353
[46]Yufang Zhu, Jianlin Shi, Weihua Shen, et al. Stimuli responsive cont rolled drug release f rom a hollow mesoporous silica sphere/polyelect rolyte multilayer core-shell st ructure. Angew Chem Int Ed,2005,44:5083-5085
[47]Arruebo M,.Galan M,.Navascues N, et al. Development of magnetic nanost ructured silica based materials as potentialvectors for drug delivery applications. Chem Mater,2006,18(7):1911-1914
[48]Butterwoth M D, Bell S A, Armes S P, et al. Synthesis and Characterization of Polypyrrole-Magnetite-Silica Particles. Colloid Interface Science,1996,183(1):91-99
[49]Xiaoqiao Liu, Jianmin Xing, Yueping Guan, et al. Collioid Surface A:Phys Eng Aspect, 2004,238:127-130
[50]Werner StOber, A Fink, E Bohn. Controlled growth of monodisperse sillica spheres in the micron size range. Colloid and Interface Science,1968,26(1): 62-69
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