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Microstructure, composition and magnetic properties of Nd-(Fe1-xCox)-B oxide magnetic particles synthesized by Pechini-type chemical method
Advanced Powder Technology ( IF 5.2 ) Pub Date : 2021-09-15 , DOI: 10.1016/j.apt.2021.08.040
G. Ahmadpour 1 , A.Yu. Samardak 2 , V.V. Korochentsev 3 , I.S. Osmushko 3 , V.Yu. Samardak 2 , A.A. Komissarov 2, 3 , D.S. Shtarev 2 , A.S. Samardak 2, 4 , A.V. Ognev 2 , F. Nasirpouri 1
Affiliation  

This work deals with the investigation and optimization of the crystalline phases, magnetic properties, chemical composition and morphology of Nd-(Fe1-xCox)-B oxide magnetic particles (where x = 0, 0.05, 0.1, 0.15, 0.2, 0.3, 0.4, and 0.5) synthesized by Pechini method that can be used as a precursor for the production of Nd2(Fe,Co)14B hard magnetic phase. The polymerization mechanism of Pechini process was investigated by Fourier transform infrared (FTIR) and Raman spectroscopy to confirm the formation of metal-CA complexes and successive esterification reactions between citric acid (CA) and ethylene glycol (EG). The chemical composition of the synthesized samples was studied via energy dispersive (EDS) and X-ray photoelectro (XPS) spectroscopy methods. The structure, morphology, and the crystalline phase of resulting Nd-(Fe1-xCox)-B oxide magnetic particles were characterized by Rietveld refinement of X-ray diffraction (XRD) patterns, scanning electron microscopy ( SEM), and high-resolution transmission electron microscopy (HR-TEM) and its selected area electron diffractograms (SAED). The results obtained from the Rietveld refinement of XRD patterns show that (Fe2O3/Fe3O4) phase ratio decreases with the amount of cobalt that can be attributed to the reduction of enthalpy . The SEM micrographs indicate that the oxide particles have an elongated structure with irregular shapes supported by TEM observations. The results of structural analysis by HR-TEM and SAED are consistent with the Rietveld results which confirms the presence of different oxide phases in Nd-(Fe1-xCox)-B oxide particles. The magnetic behaviorstudied by VSM was interpreted by the variances of the morphology, structure and chemical composition of Nd-(Fe1-xCox)-B oxide particles, all of which were influenced by the cobalt content. First‐Order Reversal Curve (FORC) diagrams show that the magnetic interaction between oxide particles decreases as the cobalt content increases.



中文翻译:

Pechini型化学法合成的Nd-(Fe1-xCox)-B氧化物磁性颗粒的微观结构、组成和磁性能

这项工作涉及 Nd-(Fe 1-x Co x )-B 氧化物磁性颗粒(其中 x = 0, 0.05, 0.1, 0.15, 0.2, 0.3、0.4 和 0.5) 通过 Pechini 方法合成,可用作生产 Nd 2 (Fe,Co) 14的前体B 硬磁相。通过傅里叶变换红外光谱 (FTIR) 和拉曼光谱研究了 Pechini 过程的聚合机理,以确认金属-CA 配合物的形成以及柠檬酸 (CA) 和乙二醇 (EG) 之间的连续酯化反应。通过能量色散 (EDS) 和 X 射线光电 (XPS) 光谱方法研究合成样品的化学成分。所得 Nd-(Fe 1-x Co x)-B 氧化物磁性颗粒通过 X 射线衍射 (XRD) 图案的 Rietveld 精修、扫描电子显微镜 (SEM) 和高分辨率透射电子显微镜 (HR-TEM) 及其选区电子衍射图 (SAED) 进行表征。从 XRD 图案的 Rietveld 精修获得的结果表明 (Fe 2 O 3 /Fe 3 O 4) 相比随着可归因于焓降低的钴量而降低。SEM 显微照片表明氧化物颗粒具有由 TEM 观察支持的具有不规则形状的细长结构。HR-TEM 和 SAED 的结构分析结果与 Rietveld 结果一致,这证实了 Nd-(Fe 1-x Co x )-B 氧化物颗粒中存在不同的氧化物相。VSM研究的磁行为是通过Nd-(Fe 1-x Co x)-B 氧化物颗粒,所有这些都受钴含量的影响。一阶反转曲线(FORC)图显示,随着钴含量的增加,氧化物颗粒之间的磁相互作用会降低。

更新日期:2021-10-27
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