化学法制备Nd-Fe-B颗粒退火产物的物相调控
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摘要
为了制备具有优良性能的Nd-Fe-B颗粒,在等时变温退火和等温变时退火的基础上,深入研究了温度和时间对Nd-Fe-B氧化物物相组成和百分含量变化的影响,然后对物相进行调控。最终确定了合理的退火温度和退火时间,成功制备出了以Nd_2Fe_(14)B为主相的Nd-Fe-B纳米颗粒。通过XRD、Rietveld精修拟合、SEM、TEM、VSM检测分析,结果显示Nd-Fe-B氧化物主要由FeNdO_3,NdBO_3和α-Fe组成,最佳的退火温度为750℃,最佳的退火时间为5 h,最终获得的Nd-Fe-B氧化物分别为54.619%的FeNdO_3,19.901%的α-Fe,11.760%的NdBO_3。利用该氧化物成功制备出含有88.457%的Nd_2Fe_(14)B和11.543%的Fe_3B纳米粒子的Nd-Fe-B颗粒,该颗粒的矫顽力约206.96 kA/m。
Aiming to prepare Nd-Fe-B particles with excellent properties, based on the previous research on isochronous temperature annealing and isothermal annealing, the effects of temperature and time on the composition and percentage of Nd-Fe-B oxides were studied, respectively. Accordingly, the physical phase was adjusted. As a result, the optimal annealing temperature and time were determined. Nd-Fe-B nano particles with Nd_2Fe_(14)B as the main phase were prepared. Furthermore, the phase transition and magnetic properties were analyzed by X-ray diffractometer(XRD), Rietveld refinement fitting, scanning electron microscope(SEM), transmission electron microscope(TEM) and vibration sample magnetometer(VSM) detection. The results show that the Nd-Fe-B oxide mainly consisted of FeNdO_3, NdBO_3 and α-Fe. 750 ℃ and 5 h have been found to be the optimal annealing temperature and time, respectively. The Nd-Fe-B oxide obtained included 54.619%, FeNdO_3, 19.901% α-Fe, and 11.760% NdBO_3. Then this oxide was used to prepare Nd-Fe-B nanoparticles containing 88.457% of Nd_2Fe_(14)B and 11.543% of Fe_3B nanoparticles with the coercivity of 206.96 kA/m.
Aiming to prepare Nd-Fe-B particles with excellent properties, based on the previous research on isochronous temperature annealing and isothermal annealing, the effects of temperature and time on the composition and percentage of Nd-Fe-B oxides were studied, respectively. Accordingly, the physical phase was adjusted. As a result, the optimal annealing temperature and time were determined. Nd-Fe-B nano particles with Nd_2Fe_(14)B as the main phase were prepared. Furthermore, the phase transition and magnetic properties were analyzed by X-ray diffractometer(XRD), Rietveld refinement fitting, scanning electron microscope(SEM), transmission electron microscope(TEM) and vibration sample magnetometer(VSM) detection. The results show that the Nd-Fe-B oxide mainly consisted of FeNdO_3, NdBO_3 and α-Fe. 750 ℃ and 5 h have been found to be the optimal annealing temperature and time, respectively. The Nd-Fe-B oxide obtained included 54.619%, FeNdO_3, 19.901% α-Fe, and 11.760% NdBO_3. Then this oxide was used to prepare Nd-Fe-B nanoparticles containing 88.457% of Nd_2Fe_(14)B and 11.543% of Fe_3B nanoparticles with the coercivity of 206.96 kA/m.
引文
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[23] Guo Yaozu, Zhao Dong, You Junhua, et al. Evolution of microstructure and formation mechanism of Nd-Fe-B nanoparticles prepared by low energy consumption chemical method [J].RSC Advances,2018,8:38850-38859.
[2] Jack A G, Mecrow B C, Haylock J A. A comparative study of permanent magnet and switched reluctance motors for high-performance fault-tolerant applications [J]. IEEE Transactions on Industry Applications, 1996, 32 (4): 889-895.
[3] Kakosimos P E, Sarigian A G, Beniakar M E, et al. Induction motors versus permanent-magnet actuators for aerospace applications [J]. IEEE Transactions on Industrial Electronics, 2014, 61 (8): 4315-4325.
[4] Cao W, Mecrow B C, Atkinson G J, et al. Overview of electric motor technologies used for more electric aircraft (MEA) [J]. IEEE Transactions on Industrial Electronics, 2012, 59(9): 3523-3531.
[5] Beniakar M E, Sarigiannidis A G, Kakosimos P E, et al. Multiobjective evolutionary optimization of a surface mounted PM actuator with fractional slot winding for aerospace applications [J]. IEEE Transactions on Mganetics, 2014, 50(2): 665-668.
[6] Skomski R, Coey J M, Giant energy product in nanostructured two-phase magnets [J]. Physical Review B: Condensed Matter and Materials Physics, 1993, 48:15812-15816.
[7] Gschneidner K, Russell A, Pecharsky A, et al. A family of ductile intermetallic compounds [J]. Nature Materials, 2003, 2(9): 587-591.
[8] Inoue A, Shen B, Koshiba, et al. Cobalt-based bulk glassy alloy with ultrahigh strength and soft magnetic properties [J]. Nature Materials, 2003, 2(10): 661-663.
[9] Kim J J, Choi Y, Suresh S, et al. Nanocrystallization during nanoindentation of a bulk amorphous metal alloy at room temperature [J]. Science, 2002, 295(5555): 654-657.
[10] Kwon H W, Jeong I C, Thermomagnetic monitoring of nanocomposite formation in mechanically alloyed Nd-Fe-B alloys [J]. Physica Status Solidi, 2004, 201(8):1921-1925.
[11] Croat J J, Herbst J F, Lee R W, et al. Pr-Fe and Nd-Fe-B based materials: a new class of high performance permanent magnets (invited) [J]. Journal of Applied Physics,1984, 55(6): 2078-2082.
[12] Koon N C, Das B N. Crystallization of FeB alloys with rare earths to produce hard magnetic materials (invited) [J]. Journal of Applied Physics,1984, 55(6): 2063-2066.
[13] Cha H G,Kim Y H,Kim W, et al. Preparation and characterization of Nd2Fe14B/α-Fe nanocomposite magnetic material by reduction diffusion process [J]. Journal of Materials Research,2001,16(3):709-715.
[14] Swaminathan V, Deheri P K, Bhame S D, et al. Novel microwave assisted chemical synthesis of Nd2Fe14B hard magnetic nanoparticles[J]. Nanoscale, 2013, 5(7): 2718-2725.
[15] Yu L Q, Zhang Y P, Yang Z, et al. Chemical synthesis of Nd2Fe14B/Fe3B nanocomposites [J]. Nanoscale, 2016, 8(26): 12879-12884.
[16] Guo Yaozu, You Junhua, Pei Wenli,et al. Effect of (C2H5)3NBH3 content on microstructure and properties of Nd-Fe-B nanoparticles prepared by chemical and reduction-diffusion method [J]. Journal of Alloys and Compounds, 2019, 777: 850-859.
[17] Rahimi H, Ghasemi A, Mozaffarinia R, et al. Magnetic properties and magnetization reversal mechanism of Nd-Fe-B nanoparticles synthesized by a sol-gel method [J]. Journal of Geophysical Research Solid Earth, 1998, 103(B12): 30551-30560.
[18] Parmar H, Xiao T, Chaudhary V, et al. High energy product chemically synthesized exchange coupled Nd2Fe14B/α-Fe magnetic powders [J]. Nanoscale, 2017, 9(37):13956-13966.
[19] Chick L A, Pederson L R, Maupin G D, Exarhos, glycine-nitrate combustion synthesis of oxide ceramic powders [J]. Materials Letters, 1990, 10(1): 6-12.
[20] You Junhua, Zhao Dong, Guo Yaozu, et al. Preparation and reaction process of Nd2Fe14B magnetic powder synthesized by chemical method [J]. Rare Metal Materials and Engineering, 2018, 47(5):1643-1647(in Chinese).尤俊华,赵东,郭耀祖,等. 化学法制备Nd2Fe14B磁粉及其反应过程 [J]. 稀有金属材料与工程, 2018, 47(5):1643-1647.
[21] Rahimi H, Ghasemi A, Moza R, et al , On the magnetic and structural properties of neodymium iron boron nanoparticles [J]. Journal of Superconductivity and Novel Magnetic, 2016, 29(8): 1-11.
[22] Swaminathan V, Deheri P K, Bhame S D, et al. Novel microwave assisted chemical synthesis of Nd2Fe14B hard magnetic nanoparticles [J]. Nanoscale, 2013,3: 2718-2725.
[23] Guo Yaozu, Zhao Dong, You Junhua, et al. Evolution of microstructure and formation mechanism of Nd-Fe-B nanoparticles prepared by low energy consumption chemical method [J].RSC Advances,2018,8:38850-38859.