反向微乳液法制备掺杂Co的锰锌铁氧体及其结构性能的研究

发布时间：2018-07-29 19:58

【摘要】： 本文在实验室条件下用三氯化铁,氯化锰,硫酸锌和氯化钴为原料制备高性能的掺杂钴的锰锌铁氧体。为制备高性能的锰锌铁氧体开启了一条新的工艺路线。而且为下一步利用金川公司的黄钠铁矾渣制备锰锌铁氧体作铺垫,也为西北永新集团制备掺杂纳米材料的高性能涂料埋下伏笔。实验采用可以控制粒径大小和形状的反向微乳液法制备锰锌钴铁氧体。重点研究用微乳液法制备掺杂不同含量的Co2+(X=0,0.1,0.2,0.3,0.4,0.5)对锰锌铁铁氧体纳米颗粒结构和磁性能的影响。同时研究了掺杂相同的Co2+含量在煅烧和未煅烧的条件下对锰锌铁氧体纳米颗粒结构和磁性能的影响。并用X射线衍射(XRD)、扫描电镜(SEM)、振动样品磁强计(VSM)和X-射线能量色散谱仪(EDS)对CoxZn0.5Mn1-xFe1.5O4进行了表征,结果表明：用微乳液法成功制备了掺杂不同Co2+含量的CoxZn0.5Mn1-xFe1.5O4,EDS的分析结果表明,Co元素取代了Mn元素并且确定了锰锌钴铁氧体的成分和分子式,随着Co元素含量的增加,Mn元素的含量减少,Fe元素和Zn元素基本保持不变。 XRD表明无论是煅烧还是未煅烧的样品均为单一的尖晶石结构,无其他杂相。同时适量的掺杂Co2+会使铁氧体颗粒变大,但是过量的掺杂反而会使颗粒粒径减小。XRD表征的结果和SEM表征的结果相一致。在未煅烧的情况下颗粒平均粒径小于15nm,颗粒呈球形,在煅烧的情况下颗粒的平均粒径小于30nm,颗粒也呈球形。研究了掺杂不同的Co2+含量在煅烧情况下和未煅烧情况下对锰锌铁氧体磁化强度和矫顽力的影响,研究结果表明：随着Co2+掺杂量的提高,煅烧和未煅烧样品的磁化强度和矫顽力都比未掺杂时有所提高,表明了掺杂Co2+可以增大颗粒的磁化强度和矫顽力。在煅烧情况下磁化强度和矫顽力都为波浪曲线呈现出先增大后减小再增大后减小的规律,并且矫顽力的最大值和最小值所对应的掺杂量都相一致,当X'=0.4时都达到最大值。在未煅烧的情况下磁化强度和矫顽力达到最大值时随对应的掺杂量也相一致,并在X=0.3时达到最大值。未煅烧情况下磁化强度要大于煅烧情况下的磁化强度,但是矫顽力却都小于煅烧情况下的矫顽力。
[Abstract]:In this paper, high performance cobalt-doped manganese zinc ferrites were prepared from ferric chloride, manganese chloride, zinc sulfate and cobalt chloride under laboratory conditions. A new process was opened for the preparation of high performance mn-Zn ferrite. It also lays the groundwork for the preparation of manganese zinc ferrite from jinchuan sodium ferrite slag and lays the groundwork for the preparation of high performance coatings doped with nanometer materials in northwest Yongxin group. Manganese zinc cobalt ferrite was prepared by reverse microemulsion method which can control particle size and shape. The effect of Co2 doped with different content on the structure and magnetic properties of ferrite nanocrystalline was studied by microemulsion method. At the same time, the effects of the same doped Co2 content on the structure and magnetic properties of MnZn ferrite nanocrystalline were investigated under calcined and uncalcined conditions. CoxZn0.5Mn1-xFe1.5O4 was characterized by X-ray diffraction (XRD),) scanning electron microscope (XRD),) (SEM), vibrating sample magnetometer (VSM) and X-ray energy dispersive spectrometer (EDS). The results show that CoxZn0.5Mn1-xFe1.5O4EDS doped with different Co2 content has been successfully prepared by microemulsion method. The results show that Co element has replaced mn element and the composition and molecular formula of mn Zn Co ferrite have been determined. With the increase of Co content, the content of Fe and Zn remained basically unchanged. XRD showed that both calcined and uncalcined samples had a single spinel structure and no other impurity phase. At the same time, proper doping of Co2 can make the ferrite particles larger, but excessive doping will reduce the particle size. The results of SEM characterization are consistent with the results of SEM characterization. The average particle size is less than 15nm without calcination, and the average particle size is less than 30nm under calcined condition, and the particle is spherical. The effects of doping different Co2 content on magnetization and coercivity of MnZn ferrite under calcined and uncalcined conditions were studied. The results showed that with the increase of Co2 doping amount, the magnetization and coercivity of Mn-Zn ferrite were increased. The magnetization and coercivity of calcined and uncalcined samples are higher than that of undoped samples, which indicates that doped Co2 can increase the magnetization and coercivity of particles. Both magnetization and coercivity show the law of first increasing and then decreasing under calcined condition, and the maximum and minimum of the coercivity are the same as the corresponding doping amount, and they all reach the maximum when XG is 0.4. When the magnetization and coercivity reach the maximum without calcination, the magnetization and coercivity are the same with the corresponding doping amount, and reach the maximum at XO 0.3. The magnetization of uncalcined is greater than that of calcined, but the coercivity is smaller than that of calcined.
【学位授予单位】：兰州大学
【学位级别】：硕士
【学位授予年份】：2010
【分类号】：O614

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