Preparation of cobalt ferrite nanoparticles by high gravity liquid precipitation method

doi:10.16085/j.issn.1000-6613.2017-1343

Abstract

Abstract: Nanoparticles prepared by magnetic stirrer tend to have a wide particle size distribution and uneven dispersion. In order to address these problems,CoFe₂O₄ nanoparticles were prepared by chemical coprecipitation in impinging stream-rotating packed bed (IS-RPB) using aqueous solutions of Fe (NO₃)₃/Co (NO₃)₂ and NaOH as raw materials. The effects of rotational speed,liquid flow rate,NaOH concentration and crystallization time on the particle size of CoFe₂O₄ nanoparticles were examined,and their magnetic properties were compared with that prepared by magnetic stirrer. The particle size,morphology and magnetic properties of as prepared nanoparticles were characterized by X-ray diffraction (XRD),fourier infrared spectroscopy (FTIR),transmission electron microscopy (TEM),nanoparticle size analyzer and vibrating sample magnetometer (VSM). The results showed that the particle size of CoFe₂O₄ nanoparticles decreases with the increase of rotational speed,liquid flow rate and NaOH concentration,but increases with the increase of crystallization time. The optimum operating conditions are as follows:rotational speed 900r/min,liquid flow rate 60L/h,NaOH concentration 3mol/L,and crystallization time 6h. CoFe₂O₄ nanoparticles prepared under optimum operating conditions have an irregular shape with an average diameter of about 20nm and a saturation magnetization of 75.43emu/g,which is 40% higher than that prepared by magnetic stirrer.

Key words: high gravity, chemical coprecipitation, impinging stream-rotating packed bed, cobalt ferrite(CoFe₂O₄), nanoparticles

摘要： 针对磁力搅拌器制备纳米材料时存在粒径分布宽、分散不均匀的问题，采用撞击流-旋转填料床结合化学共沉淀法，以Fe（NO₃）₃·9H₂O、Co（NO₃）₂·6H₂O、NaOH为原料制备CoFe₂O₄纳米颗粒。研究了转速、液体流量、NaOH浓度以及晶化时间对CoFe₂O₄纳米颗粒粒径的影响；并与磁力搅拌器制备的CoFe₂O₄纳米颗粒在磁性能方面进行了对比。采用X射线衍射仪（XRD）、傅里叶红外光谱仪（FTIR）、透射电镜（TEM）、纳米粒度仪及振动样品磁强计（VSM）对产物的粒径形貌及磁性能进行表征。结果表明：CoFe₂O₄纳米颗粒的粒径随转速、液体流量和NaOH浓度的增加而减小，但随晶化时间的增加而增大。最佳工艺条件为：转速900r/min，液体流量60L/h，NaOH浓度3mol/L，晶化时间6h。此条件下制备的CoFe₂O₄纳米颗粒的粒径约为20nm，饱和磁化强度为75.43emu/g，较磁力搅拌器提高40%。

关键词: 超重力, 化学共沉淀, 撞击流-旋转填料床, 铁酸钴, 纳米粒子

CLC Number:

TQ586

QI Guisheng, WU Xiaoli, LIU Youzhi, ZHENG Qi, GUO Linya. Preparation of cobalt ferrite nanoparticles by high gravity liquid precipitation method[J]. Chemical Industry and Engineering Progress, 2018, 37(05): 1680-1686.

祁贵生, 武晓利, 刘有智, 郑奇, 郭林雅. 超重力液相沉淀法制备纳米铁酸钴[J]. 化工进展, 2018, 37(05): 1680-1686.

References

[1] GOLDMAN A.Modern ferrite technology[M].Berlin,Heidelberg:Springer,2006.
[2] CHANG S,QIAO H.Tuning magnetic properties of magnetic recording media cobalt ferrite nano-particles by co-precipitation method[C]//2009 Symposium on Photonics and Optoelectronics,IEEE Express Conference Publishing,2009:1-4.
[3] SODAEE T,GHASEMI A,RAZAVI R S.Microstructural characteristics and magnetic properties of gadolinium-substituted cobalt ferrite nanocrystals synthesized by hydrothermal processing[J]. Journal of Cluster Science,2015,27(4):1-13.
[4] CHINNASAMY C N,JEYADEVAN B,PERALES-PEREZ O,et al.Growth dominant co-precipitation process to achieve high coercivity at room temperature in CoFe₂O₄ nanoparticles[J].IEEE Transactions on Magnetics,2002,38(5):2640-2642.
[5] QU Y,YANG H,YANG N,et al.The effect of reaction temperature on the particle size,structure and magnetic properties of coprecipitated CoFe₂O₄,nanoparticles[J].Materials Letters,2006,60(29/30):3548-3552.
[6] VAZQUEZ-VAZQUEZ C,LOPEZ-QUINTELA M A,BUJAN-NUNEZ M C,et al.Finite size and surface effects on the magnetic properties of cobalt ferrite nanoparticles[J].Journal of Nanoparticle Research,2010,13(4):1663-1676.
[7] PENG J,HOJAMBERDIEV M,XU Y,et al.Hydrothermal synthesis and magnetic properties of gadolinium-doped CoFe₂O₄,nanoparticles[J].Journal of Magnetism & Magnetic Materials,2011,323(1):133-137.
[8] PILLAI V,SHAH D O.Synthesis of high-coercivity cobalt ferrite particles using water-in-oil microemulsions[J].Journal of Magnetism & Magnetic Materials,1996,163(1/2):243-248.
[9] PRABHAKARAN T,HEMALATHA J.Combustion synthesis and characterization of cobalt ferrite nanoparticles[J].Ceramics International,2016,42(12):14113-14120.
[10] SALUNKHE A B,KHOT V M,PHADATARE M R,et al.Combustion synthesis of cobalt ferrite nanoparticles——influence of fuel to oxidizer ratio[J].Journal of Alloys & Compounds,2012,514(2):91-96.
[11] ABBAS M,RAO B P,ISLAM M N,et al.Size-controlled high magnetization CoFe₂O₄,nanospheres and nanocubes using rapid one-pot sonochemical technique[J].Ceramics International,2014,40(2):3269-3276.
[12] ABBAS Y M,MANSOUR S A,IBRAHIM M H,et al.Microstructure characterization and cation distribution of nanocrystalline cobalt ferrite[J].Journal of Magnetism & Magnetic Materials,2011,323(22):2748-2756.
[13] AHN Y,CHOI E J,KIM S,et al.Magnetization and mössbauer study of cobalt ferrite particles from nanophase cobalt iron carbonate[J].Materials Letters,2001,50(1):47-52.
[14] JIAO W Z,LIU Y Z,QI G S.Micromixing efficiency of viscous media in novel impinging stream-rotating packed bed reactor[J].Industrial and Engineering Chemistry Research.2012,51(20):7113-7118.
[15] JIAO W Z,LIU Y Z,QI G S.A new impinging stream-rotating packed bed reactor for improvement of micromixing iodide and iodate[J].Chemical Engineering Journal,2010,157(1):168-173.
[16] SHEN Z G,CHEN J F,YUN J. Preparation and characterizations of uniform nanosized BaTiO₃,crystallites by the high-gravity reactive precipitation method[J].Journal of Crystal Growth,2004,267(1/2):325-335.
[17] 申红艳,刘有智. 纳米氢氧化镁的超重力沉淀法制备及沉降性能[J]. 化工进展,2016,35(10):3281-3287. SHEN H Y,LIU Y Z. Preparation of magnesium hydroxide nanoparticles by high gravity precipitation method and their settlement property[J]. Chemical Industry and Engineering Progress,2016,35(10):3281-3287.
[18] CHEN J,LI Y,WANG Y,et al. Preparation and characterization of zinc sulfide nanoparticles under high-gravity environment[J]. Materials Research Bulletin,2004,39(2):185-194.
[19] CHEN J F,SHAO L,GUO F,et al. Synthesis of nano-fibers of aluminum hydroxide in novel rotating packed bed reactor[J]. Chemical Engineering Science,2003,58(3):569-575.
[20] QIAN S,BO C,XI W,et al. Preparation of transparent suspension of lamellar magnesium hydroxide nanocrystals using a high-gravity reactive precipitation combined with surface modification[J]. Industrial & Engineering Chemistry Research,2014,54(2):150108153809007.
[21] CHEN J F,ZHOU M Y,SHAO L,et al. Feasibility of preparing nanodrugs by high-gravity reactive precipitation[J]. International Journal of Pharmaceutics,2004,269(1):267.
[22] 刘有智. 超重力撞击流-旋转填料床液-液接触过程强化技术的研究进展[J]. 化工进展,2009,28(7):1101-1108. LIU Y Z. Research progress of high gravity technology of IS-RPB to intensify liquid-liquid contact[J]. Chemical Industry and Engineering Progress,2009,28(7):1101-1108.
[23] 徐莉,张洪涛,洪健民,等. 铁酸钴纳米微粒的共沉淀法制备和磁性质[J]. 无机化学学报,2005,21(5):741-743. XU L,ZHANG H T,HONG J M,et al. Cobalt ferrite nanoparticles:coprecipitation synthesis and magnetic properties[J]. Chinese Journal of Inorganic Chemistry,2005,21(5):741-743.
[24] KOOTI M,AFSHARI M. Phosphotungstic acid supported on magnetic nanoparticles as an efficient reusable catalyst for epoxidation of alkenes[J]. Materials Research Bulletin,2012,47(11):3473-3478.
[25] FAN H L,ZHOU S F,QI G S,et al. Continuous preparation of Fe₃O₄ nanoparticles using impinging stream-rotating packed bed reactor and magnetic property thereof[J]. Journal of Alloys & Compounds,2016,662:497-504.
[26] HUA F,YIN C,ZHANG H,et al. Direct preparation of the nanocrystalline MnZn ferrites by using oxalate as precipitant[J]. Journal of Materials Science & Chemical Engineering,2015,3(12):23-29.
[27] MOHAMED M B,YEHIA M. Cation distribution and magnetic properties of nanocrystalline gallium substituted cobalt ferrite[J]. Journal of Alloys & Compounds,2014,615(8):181-187.
[28] 赵军,赵明静,刘小鱼. 晶化时间对Nd_9.2Fe_84.8-xZr_xB₆复相纳米永磁材料的影响[J]. 包钢科技,2011,37(4):47-49.. ZHAO J,ZHAO M J,LIU X Y. Effects of crystallization time on Nd_9.2Fe_84.8-xZr_xB₆ nanometer permanent-magnet materials with complex phase[J]. Science & Technology of Baotou Steel(Group) Corporation,2011,37(4):47-49.
[29] 艾伦弘,蒋静. 铁酸钴纳米晶的低温合成、谱学表征及磁性[J]. 应用化学,2010,27(1):78-81. AI L H,JIANG J. Low-temperature synthesis,spectral characterization and magnetic properties of CoFe₂O₄ nanocrystals[J]. Chinese Journal of Applied Chemistry,2010,27(1):78-81.
[30] 张梅梅,刘宏,刘建安. 混合碱媒介法制备磁性铁酸钴纳米粉体[J]. 人工晶体学报,2009,38(5):1231-1234. ZHANG M M,LIU H,LIU J A. Synthesis of magnetic cobalt ferrite nanomaterials by composite-hydroxide-mediate method[J]. Journal of Synthetic Crystals,2009,38(5):1231-1234.
[31] 国秋菊,郑少华,苏登成. 纳米CoFe₂O₄颗粒制备及性能研究[J]. 中国粉体技术,2007,13(1):16-19. GUO Q J,ZHENG S H,SU D C. Study on preparation and properties of CoFe₂O₄ nano-particles[J]. China Powder Science and Technology,2007,13(1):16-19.