成分优化对软磁MnZn铁氧体的影响规律  

Influence of composition optimization on soft magnetic MnZn ferrites

作　　者：徐展源 赵伟 史湘石 张振宇 王中钢[1] 韩勇[3] 范景莲[3] XU Zhanyuan;ZHAO Wei;SHI Xiangshi;ZHANG Zhenyu;WANG Zhonggang;HAN Yong;FAN Jinglian(School of Traffic&Transportation Engineering,Central South University,Changsha 410075,China;Farsoon Technologies Company Limited,Changsha 410006,China;State Key Laboratory of Powder Metallurgy,Central South University,Changsha 410083,China)

机构地区：[1]中南大学交通运输工程学院,湖南长沙410075 [2]湖南华曙高科技股份有限公司,湖南长沙410006 [3]中南大学粉末冶金国家重点实验室,湖南长沙410083

出　　处：《中南大学学报（自然科学版）》2024年第8期2900-2909,共10页Journal of Central South University:Science and Technology

基　　金：国家重点研发计划项目(2022YFB4300101);中南大学博士后科研启动经费资助项目(140050022)。

摘　　要：采用“化学溶胶—喷雾干燥—煅烧”方法制备Mn_(0.5−y)Zn_(0.5)Fe_(2+y)O_(4)(y=0,0.01,0.03,0.05,0.07,0.09)软磁MnZn铁氧体,利用X射线衍射(XRD)、红外光谱(FTIR)、拉曼光谱(Raman)、X射线光电子能谱(XPS)、扫描电镜(SEM)、透射电镜(TEM)和超导量子干涉磁测量系统等检测方法对其进行表征。研究结果表明:当y=0~0.07时,样品均只含有MnZn铁氧体单相;而当y=0.09时,将析出α-Fe_(2)O_(3)杂质相,此现象得到了XRD和Raman光谱结果验证。随着Fe含量的增加,平均晶粒度先减小再增大,当y=0.03时,平均晶粒度最小。样品中的Fe呈+3价,Zn呈+2价,而Mn则存在+2、+3和+4这3种价态,其中,当y=0.09时,样品中Fe^(3+)位于MnZn铁氧体和α-Fe_(2)O_(3)中的环境不同,其Fe2p_(3/2)峰存在结合能分别为710.09、711.16和713.71 eV的3个子峰。样品中Mn^(2+)的含量先增加再减少,在y=0.07时最大。所有样品均呈细小颗粒组成的空心球壳形貌,几乎不存在非空心球壳粉末形貌,且元素均匀化分布。当y=0~0.09时,比饱和磁化强度(M_(s))为41.15~54.58 A·m^(2)/kg,剩磁(M_(r))为0.91~6.50 mA/m,矫顽力(H_(c))为2242.4~8917.6 A/m,矩形比(M_(r)/M_(s))为0.02~0.12。其中,当Fe过量时,M_(s)呈先增大再减小的趋势;当y=0.07时,MnZn铁氧体的综合特性最优。The soft magnetic MnZn ferrite materials Mn_(0.5−y)Zn_(0.5)Fe_(2+y)O_(4)(y=0,0.01,0.03,0.05,0.07,0.09)were prepared by the chemical sol-spray drying-calcination method.X-ray diffraction(XRD),Fourier transform infrared(FTIR)spectroscopy,Raman spectroscopy,X-ray photon-electron spectroscopy(XPS),scanning electron microscope(SEM),transmission electron microscopy(TEM),and superconducting quantum interference magnetic measurement system were used to characterize the samples.The results indicate that the samples are all single-phase MnZn ferrite when y=0−0.07.When y=0.09,α-Fe_(2)O_(3) impurity phase will appear,which is supported by the XRD and Raman spectroscopy results.With the increase of Fe content,the average crystallite size decreases and then increases.The average crystallite size reaches minimum value when y=0.03.The valences of Fe and Zn are+3 and+2 respectively,while Mn exhibits three valence states of+2,+3,and+4.When y=0.09,the environment in which Fe^(3+)is located in MnZn ferrite andα-Fe_(2)O_(3) phase is different,and the Fe2p_(3/2) peak has three sub peaks with binding energies of 710.09,711.16 and 713.71 eV,respectively.The content of Mn^(2+)in the samples first increases and then decreases,reaching its maximum at y=0.07.The samples all present hollow spherical shell morphology composed of small particles,with highly uniform distribution of elements.Also,there is almost no non-hollow spherical shell morphology.When y=0−0.09,the specific saturation magnetizations(M_(s))are 41.15−54.58 A·m^(2)/kg,the remanences(M_(r))are 0.91-6.50 mA/m,the coercivities(H_(c))are 2242.4~8917.6 A/m,and the squareness ratios(M_(r)/M_(s))are 0.02−0.12.When the content of Fe is excessive,specific saturation magnetization(M_(s))shows a trend of first increasing and then decreasing.And when y=0.07,the comprehensive characteristics of MnZn ferrite are optimal.

关 键 词：MNZN铁氧体 磁性能 软磁 Fe含量 

分 类 号：TB34[一般工业技术—材料科学与工程]