高饱和磁化强度的Fe_3O_4磁性颗粒的制备与研究
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摘要
采用水热法,以柠檬酸(Cit)为配位剂,使之与溶液中的亚铁离子形成配合物,通过改变水热反应时间合成出具有不同形貌和高饱和磁化强度的Fe_3O_4磁性粉体,以研究水热反应时间对合成Fe_3O_4磁性颗粒形貌及其磁性能的影响,从而确定最佳合成工艺.XRD衍射谱图分析结果表明柠檬酸配位体系水热合成产物为具有高纯度的面心立方结构的Fe_3O_4粉末;SEM图分析结果表明,随着反应时间的增加,Fe_3O_4的形状由正八面体消失,并先择优取向横向生长成纳米片结构,随后逐渐趋向于纵向生长,使片状生长为块状,最终生长为不规则的多面体结构.FT-IR分析结果表明,在柠檬酸体系合成Fe_3O_4的过程中,柠檬酸分子在合成的Fe_3O_4颗粒表面以配位状态存在.磁滞曲线分析结果表明,合成的Fe_3O_4样品具有超顺磁性,且当水热反应时间为14 h时,合成的Fe_3O_4粉体在300 K条件下饱和磁化强度高达97 emu/g,相比目前文献报道的最高的块状结构Fe_3O_4颗粒饱和磁化强度提高7.78%.
Fe_3O_4 powders with various morphologies and high magnetism were synthesized by controlling the reaction time of the hydrothermal process with the coordination of iron(Ⅱ) ion and citric acid(Cit). The influence of the reaction time on the morphology and magnetism of Fe_3O_4 synthesis was investigated,and the optimized synthesis protocol was determined. The XRD patterns showed that the products synthesized in the iron(Ⅱ)-Cit system were facecentered-cubic Fe_3O_4 powders of high purity. The SEM images illustrated that, with the increase of reaction time, octahedral Fe_3O_4 particles disappeared and grains exhibited lateral growth to form a nanoplate, and longitudinal growth to form a bulk structure and finally an irregular polyhedron structure. The FT-IR spectra indicated that coordinated Cit molecules existed on the surface of Fe_3O_4 particles. The hysteresis curves of the products showed that the maximum saturation magnetization of up to 97 emu/g at 300 K was observed at the hydrothermal reaction time of 14 h, which was 7.78% higher than that of the corresponding bulk Fe_3O_4.
Fe_3O_4 powders with various morphologies and high magnetism were synthesized by controlling the reaction time of the hydrothermal process with the coordination of iron(Ⅱ) ion and citric acid(Cit). The influence of the reaction time on the morphology and magnetism of Fe_3O_4 synthesis was investigated,and the optimized synthesis protocol was determined. The XRD patterns showed that the products synthesized in the iron(Ⅱ)-Cit system were facecentered-cubic Fe_3O_4 powders of high purity. The SEM images illustrated that, with the increase of reaction time, octahedral Fe_3O_4 particles disappeared and grains exhibited lateral growth to form a nanoplate, and longitudinal growth to form a bulk structure and finally an irregular polyhedron structure. The FT-IR spectra indicated that coordinated Cit molecules existed on the surface of Fe_3O_4 particles. The hysteresis curves of the products showed that the maximum saturation magnetization of up to 97 emu/g at 300 K was observed at the hydrothermal reaction time of 14 h, which was 7.78% higher than that of the corresponding bulk Fe_3O_4.
引文
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[3]Chen Y C,Gregori G,Leineweber A,et al.Unique high-temperature performance of highly condensed MnBi permanent magnets[J].Scripta Materialia,2015,107:131-135.
[4]Xu X,Dai Y,Yu J,et al.Metallic state FeSanchored(Fe)/Fe3O4/N-doped graphitic carbon with porous spongelike structure as durable catalysts for enhancing bioelectricity generation[J].ACS Applied Materials&Interfaces,2017,9(12):10777-10787.
[5]Jiang Y,Jiang J,Gao Q,et al.A novel nanoscale catalyst system composed of nanosized Pd catalysts immobilized on Fe3O4@Si O2-PAMAM[J].Nanotechnology,2008,19(7):075714.
[6]Issa B,Obaidat I M,Albiss B A,et al.Magnetic nanoparticles:Surface effects and properties related to biomedicine applications[J].International Journal of Molecular Sciences,2013,14(11):21266-21305.
[7]Wan J,Chen X,Wang Z,et al.A soft-templateassisted hydrothermal approach to single-crystal Fe3O4nanorods[J].Journal of Crystal Growth,2005,276(3):571-576.
[8]Liu Y,Cui T,Wu T,et al.Excellent microwaveabsorbing properties of elliptical Fe3O4 nanorings made by a rapid microwave-assisted hydrothermal approach[J].Nanotechnology,2016,27(16):165707.
[9]Khalil M I.Co-precipitation in aqueous solution synthesis of magnetite nanoparticles using iron(Ⅲ)salts as precursors[J].Arabian Journal of Chemistry,2015,8(2):279-284.
[10]Tajabadi M,Khosroshahi M E,Bonakdar S.An efficient method of SPION synthesis coated with third generation PAMAM dendrimer[J].Colloids and Surfaces A:Physicochemical and Engineering Aspects,2013,431(33):18-26.
[11]Hufschmid R,Arami H,Ferguson R M,et al.Synthesis of phase-pure and monodisperse iron oxide nanoparticles by thermal decomposition[J].Nanoscale,2015,7(25):11142-11154.
[12]Roca A,Morales M,O’Grady K,et al.Structural and magnetic properties of uniform magnetite nanoparticles prepared by high temperature decomposition of organic precursors[J].Nanotechnology,2006,17(11):2783-2788.
[13]Wongwailikhit K,Horwongsakul S.The preparation of iron(Ⅲ)oxide nanoparticles using W/O microemulsion[J].Materials Letters,2011,65(17):2820-2822.
[14]Wang J,Sun J,Sun Q,et al.One-step hydrothermal process to prepare highly crystalline Fe3O4 nanoparticles with improved magnetic properties[J].Materials Research Bulletin,2003,38(7):1113-1118.
[15]Zhu H,Yang D,Zhu L.Hydrothermal growth and characterization of magnetite(Fe3O4)thin films[J].Surface and Coatings Technology,2007,201(12):5870-5874.
[16]Jung H,Choi H.Hydrothermal fabrication of octahedral-shaped Fe3O4 nanoparticles and their magnetorheological response[J].Journal of Applied Physics,2015,117(17):17E708.
[17]Laurent S,Forge D,Port M,et al.Magnetic iron oxide nanoparticles:Synthesis,stabilization,vectorization,physicochemical characterizations,and biological applications[J].Chemical Reviews,2008,108(6):2064-2110.
[18]Soares P I,Alves A M,Pereira L C,et al.Effects of surfactants on the magnetic properties of iron oxide colloids[J].J Colloid Interface Sci,2014,419(4):46-51.
[19]Nikazar M,Alizadeh M,Lalavi R,et al.The optimum conditions for synthesis of Fe3O4/ZnO core/shell magnetic nanoparticles for photodegradation of phenol[J].Journal of Environmental Health Science and Engineering,2014,12(1):21-26.
[20]Wei Y,Han B,Hu X,et al.Synthesis of Fe3O4nanoparticles and their magnetic properties[J].Procedia Engineering,2012,27:632-637.
[21]Han D,Wang J,Luo H.Crystallite size effect on saturation magnetization of fine ferrimagnetic particles[J].Journal of Magnetism and Magnetic Materials,1994,136(1/2):176-182.
[22]Yang C,Hou Y L,Gao S.Nanomagnetism:Principles,nanostructures,and biomedical applications[J].Chinese Physics B,2014,23(5):057505.
[23]Goto K,Ito M,Sakurai T.Studies on magnetic domains of small particles of barium ferrite by colloidSEM method[J].Japanese Journal of Applied Physics,1980,19(7):1339-1346.
[24]Lee J,Isobe T,Senna M.Preparation of ultrafine Fe3O4particles by precipitation in the presence of PVA at high pH[J].Journal of Colloid and Interface Science,1996,177(2):490-494.
[25]Salado J,Insausti M,de Muro I G,et al.Synthesis and magnetic properties of monodisperse Fe3O4nanoparticles with controlled sizes[J].Journal of NonCrystalline Solids,2008,354(47):5207-5209.
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