ZnO SnO 2 Ta 2 O 5 ZnO JOURNAL OF THE CHINESE CERAMIC SOCIETY h α-fe/bafe 12 O 19

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1 ZnO SnO 2 Ta 2 O 5 ZnO JOURNAL OF THE CHINESE CERAMIC SOCIETY 821 Vol. 40 No. 6 June 2012 α-fe/bafe 12 O ( ) α-fe/bafe 12 O 19 X h α-fe/bafe 12 O A m 2 /kg ka/m 24.6 Am 2 /kg α- TQ171 A (2012) :37:07 Preparation and Magnetic Properties of α-fe/bafe 12 O 19 Composite Powders via Organic Gel Thermal Reduction Process YANG Xinchun 1 SHEN Xiangqian 1 SONG Fuzhan 1 LIU Ruijiang 1 CUI Xuewen 2 (1. Institute for Advanced Materials, Jiangsu University, Zhenjiang , Jiangsu, China; 2. Affiliated Hospital of Jiangsu University, Zhenjiang , Jiangsu, China) Abstract: The soft/hard α-fe/bafe 12 O 19 composites were prepared by an organic gel thermal reduction process with citric acid and metal salts as starting reagents. The phase, morphology and magnetic properties of the resultant products were analyzed by X-ray diffraction, scanning electron microscopy and vibrating sample magnetometer, respectively. The results showed that the magnetic properties was affected by the phase constituent and reduction process. The saturation magnetization of the α-fe/bafe 12 O 19 composites increased, and the coercivity firstly decreased and then increased with increasing the reduction temperature and time. The composites prepared in H 2 N 2 atmosphere at 375 for 1 h have the specific saturation magnetization of A m 2 /kg, coercivity of ka/m and specific remanence of 24.6 Am 2 /kg, respectively. Key words: composite powder; α-iron; barium ferrite; organic gel thermal reduction process; magnetic property 1991 Kneller [1] [2 4] [5] [6] [7] [8] [9] Bercoff [5] Fe/BaFe 12 O 19 ( K) Liu [9] ( ) (BK ) (1987 ) (1959 ) Received date: Revised date: First author: YANG Xinchun (1987 ), male, Master. yhuaze@163.com Correspondent author: SHEN Xiangqian (1959 ), male, professor. shenxq@ujs.edu.cn

2 α-fe/z Ba [10 13] / α-fe/bafe 12 O α-fe/bafe 12 O 19 α-fe/bafe 12 O 19 [12] (BaCO 3 ) [Fe(NO 3 ) 3 9H 2 O] (C 6 H 8 O 7 H 2 O) (Fe 2 O 3 BaFe 12 O 19 1:1) 24 h h h α-fe 2 O 3 /BaFe 12 O 19 α-fe 2 O 3 /BaFe 12 O 19 ( 1.0 L/min 5:4) α-fe/bafe 12 O D/max-rA X [Cu K α λ = nm 10 ma 50 kv 8( )/min 0.01( )/min] JEOL JSM-7001F (SEM) HH-15 (vibrating sample magnetometer VSM) α-fe 2 O 3 /BaFe 12 O h X (XRD) h α-fe α-fe BaFe 12 O 19 α-fe 2 O 3 [14 15] 1 α-fe 2 O 3 /BaFe 12 O 19 1 h XRD Fig. 1 XRD patterns of α-fe 2 O 3 /BaFe 12 O 19 composite precursor after reduction at different temperatures for 1 h α-fe 2 O 3 BaFe 12 O 19 α-fe BaFe 12 O 19 α-fe 2 α-fe 2 O 3 /BaFe 12 O XRD min α-fe 2 O 3 BaFe 12 O 19 α-fe α-fe α-fe 2 O 3 BaFe 12 O 19 2 α-fe 2 O 3 /BaFe 12 O XRD Fig. 2 XRD patterns of α-fe 2 O 3 /BaFe 12 O 19 composite precursor after reduction at temperature of 375 for different time

3 α-fe/bafe 12 O α-fe BaFe 12 O 19 1 Scherrer BaFe 12 O 19 α-fe 1 BaFe 12 O 19 α-fe 1 Table 1 α-fe BaFe 12 O 19 Grain size (D) of α-fe and BaFe 12 O 19 at different reduction conditions Reduction condition Phase constituent D (α Fe) /nm D (BaFe12O 19)/nm 375 /30 min BaFe 12 O 19, Fe 2 O /45 min BaFe 12 O 19, α-fe /1 h BaFe 12 O 19, α-fe /1 h BaFe 12 O 19, α-fe /1 h BaFe 12 O 19, α-fe α-fe/bafe 12 O min α-fe 2 O 3 α-fe 2 O 3 α-fe BaFe 12 O 19 α-fe 2 O 3 α-fe BaFe 12 O 19 α-fe h 2 Table 2 α-fe/bafe 12 O 19 Chemical compositions in α-fe/bafe 12 O 19 composites at different reduction conditions Reduction condition w(α-fe)/ % w(bafe 12 O 19 )/ % w(α-fe 2 O 3 )/ % 375 /30 min /45 min /1 h /1 h /1 h w(α-fe) represents mass fraction of (α-fe), other with this h α-fe BaFe 12 O 19 α-fe/bafe 12 O 19 SEM 3a α-fe 2 O 3 α-fe nm 3b BaFe 12 O 19 3c α-fe BaFe 12 O 19 α-fe/bafe 12 O h SEM Fig. 3 SEM morphologies of α-fe, BaFe 12 O 19 and α-fe/ BaFe 12 O 19 composite precursor after reduction at 375 for 1 h 1 h α-fe/bafe 12 O 19 SEM 3c α-fe 2 O 3 ( 3a) BaFe 12 O 19 ( 3b) 3c α-fe BaFe 12 O 19 BaFe 12 O 19 [2]

4 α-fe/bafe 12 O 19 3 (M s ) (H c ) (M r ) M S α-fe H c M r 3 α-fe/bafe 12 O 19 Table 3 Magnetic properties of α-fe/bafe 12 O 19 composites at different reduction conditions Reduction condition M s /(A m 2 kg 1 ) M r /(A m 2 kg 1 ) H c /(ka m 1 ) 350 /1 h /30 min /45 min /1 h /1 h /1 h M s Specific saturation magnetization; M r Specific remanence; H c Coercivity. 4 α-fe 2 O 3 /BaFe 12 O min 1 h α-fe 2 O 3 BaFe 12 O h min 1 α-fe obtained at 375 for 1 h; 2, 4 α-fe/bafe 12 O 19 composites obtained at 375 for 1 h and 30 min, respectively; 3 BaFe 12 O 19 obtained at 375 for 1 h. 4 α-fe BaFe 12 O 19 α-fe/bafe 12 O 19 Fig. 4 Hysteresis loops of α-fe, BaFe 12 O 19 and α-fe/bafe 12 O 19 composites α-fe 2 O h M s = 58.1A m 2 /kg H c = 32.5 ka/m M r = 24.5 A m 2 /kg α-fe BaFe 12 O α-fe/bafe 12 O 19 M S H C α-fe BaFe 12 O 19 M r α-fe BaFe 12 O 19 M r [2] Table 4 4 Magnetic properties of different powders Powder M s /(A m 2 kg 1 ) M r /(A m 2 kg 1 ) H c /(ka m 1 ) α-fe α-fe/bafe 12 O BaFe 12 O (α-fe) (BaFe 12 O 19 ) 3 [2,12] BaFe 12 O 19 α-fe BaFe 12 O 19 α-fe α-fe α-fe BaFe 12 O 19 α-fe/bafe 12 O ) α-fe/bafe 12 O 19

5 α-fe/bafe 12 O ) α-fe/bafe 12 O h α-fe/bafe 12 O 19 M s = 58.1 A m 2 /kg H c = 32.5 ka/m M r = 24.6 A m 2 /kg [1] KNELLER E F, HASIG R. The exchange-spring magnet: a new material principle for permanent magnets [J]. IEEE Trans Magn, 1991, 27(4): [2] ROY D, SHIVAKUMARA C, ANIL KUMAR P S. Observation of the exchange spring behavior in hard soft-ferrite nanocomposite [J]. J Magn Magn Mater, 2009, 321: L11 L14. [3] SONG F Z, SHEN X Q, LIU M Q, et al. One-dimensional SrFe 12 O 19 / Ni 0.5 Zn 0.5 Fe 2 O 4 composite ferrite nanofibers and enhancement magnetic property [J]. J Nanosci Nanotechnol, 2011, 11: 1 7. [4],,. Ni Co P [J]., 2009, 32(7): WU Xiaowei, FENG Yujie, LIU Yankun. J Chin Ceram Soc, 2009, 32(7): [5] BERCOFF P G, BERTORELLO H R. High-energy ball milling of Ba-hexaferrite/Fe magnetic composite [J]. J Magn Magn Mater, 1998, 187: [6] CHOI Y, LEE J J. Study of the synthesis mechanism and magnetic properties of quasi-nano-sized Ba Mg ferrite powders formed by self-propagating high-temperature synthesis [J]. Physica B, 2009, 404: [7] OHLAN A, SINGH K, CHANDRA A, et al. Microwave absorption behavior of core-shell structured poly (3,4-Ethylenedioxy thiophene)- barium ferrite nanocomposites [J]. ACS Appl Mater Int, 2010, 2(3): [8],,,. [J]., 2007, 35(6): CAO Huiqun, WEI Bo, LIU Jianhong, et al. J Chin Ceram Soc, 2007, 35(6): [9] LIU J R, ITOH M, MACHIDA K. Magnetic and electromagnetic wave absorption properties of α-fe/z-type Ba-ferrite nanocomposites [J]. Appl Phys Lett, 2006, 88: (1 3). [10] SONG F Z, SHEN X Q, LIU M Q, et al. Preparation and magnetic properties of SrFe 12 O 19 /Ni 0.5 Zn 0.5 Fe 2 O 4 nanocomposite ferrite microfibers via sol gel process [J]. Mater Chem Phys, 2011, 126: [11] WU K H, CHANG Y C, WANG G P. Preparation of NiZn ferrite/sio 2 nanocomposite powders by sol gel auto-combustion method [J]. J Magn Magn Mater, 2004, 269: [12] SONG F Z, SHEN X Q, LIU M Q, et al. Magnetic hard/soft nanocomposite ferrite aligned hollow microfibers and remanence enhancement [J]. J Colloid Interface Sci, 2010, 354: [13] HAZRA S, PATRA M K, VADERA S R, et al. A novel but simple one-pot synthetic route for preparation of (NiFe 2 O 4 ) x (BaFe 12 O 19 ) 1 x composites [J]. J Am Ceram Soc, 2012, 95(1): [14] WU H, ZHANG R, LIU X X, et al. Electrospinning of Fe, Co, and Ni nanofibers: Synthesis, assembly, and magnetic properties [J]. Chem Mater, 2007, 19: [15] BAHGAT M, RADWAN M, HESSIEN M M. Reduction behavior of barium hexaferrite into metallic iron nanocrystallites[j]. J Magn Magn Mater, 2007, 310:

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