纳米铁氧体(Co, Mn)的制备及其磁性研究

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纳米铁氧体(Co, Mn)的制备及其磁性研

究

摘要

本文建立了一种以二价铁离子为铁前驱体，在没有外加氧化剂的条件下，制

备铁氧体纳米材料的水-乙二醇溶剂热法。并着重探讨了其在制备

CoFe2O4、MnFe2O4中的操作参数。通过研究发现在比较温和、简单的条件下制备

出尖晶石结构的 CoFe2O4、MnFe2O4的纳米材料，建立了制备 CoFe2O4和MnFe2O4

的溶剂热制备工艺。在此基础上，又对其他金属的铁酸盐进行了尝试性的制备及

研究。产品的形貌、组成、磁性主要用 SEM、XRD、TEM、VSM 等进行表征。

1、单分散 CoFe2O4纳米晶体的制备

本文采用水热法以硝酸钴、氯化亚铁、HMTA 为原料在反应釜中，以乙二醇

和去离子 5:2 为溶剂一步合成 CoFe2O4纳米晶体。将高压反应釜密封严实，置于

温度和时间都可控的恒温干燥箱中 160oC反应 6h，反应结束后取出反应釜，使之

自然冷却至室温成功制备出 CoFe2O4纳米晶体，其中反应温度、时间及表面活性

剂对纳米晶体的形貌、大小、分布均匀度和磁性质有一定的影响。

2、MnFe2O4纳米粒子的水热法制备

在成功制备 CoFe2O4的工艺流程的基础上，探讨 MnFe2O4纳米材料的合成工

艺。研究了反应时间、添加剂对样品的形貌、分散度及室温磁性的影响。

1) MnFe2O4的形貌和饱和磁化强度可以通过延长反应时间和加入添加剂来改变。

2) 随着但有时间的延长，MnFe2O4的饱和磁化强度会有一个最低值。

3) 随着反应时间的延长，MnFe2O4的矫顽力不断减小。

3、水热法制备 Ba, Zn, Sr, Cr, Cu, Ni 和Ca 金属的铁酸盐。

利用建立的溶剂热途径对类似铁氧体纳米材料制备做了一些尝试，取得一些

初步结果。

关键词: 溶剂热纳米材料磁性质氧化物

ABSTRACT

In this paper, a facile solvothermal approach is firstly demonstrated for preparing

cobalt and manganese ferrite nanoparticles. Fe2+ salts are used as iron source without

extraneous oxidant help via the synthesis system in water-glycol solution. Some effect

factors are researched including reaction temperature, reaction time, surfactant and

solution on the size, morphologies and magnetic properties of the sample. The sample is

characterized by a X-ray powder diffraction (XRD), a scanning electron microscopy

(SEM), a transmission electron microscopy (TEM), and a vibrating sample

magnetometer (VSM).

Monodisperse cobalt ferrite nanoparticles is synthesized

In this paper, FeCl2•4H2O, Co(NO3)2•6H2O, hexamethylenetetramine (HMTA) are

used as precursor, 50 ml glycol and 20 ml deionized water are used as solution. The

precursors are placed into a 100 ml Teflon-lined stainless-steel autoclave, and after the

mixture is agitated vigorously about 20 min, the autoclaves are sealed and settled in a

digital-controlled constant temperature at 160oC for six hours. The autoclave is took out

and cooled to room temperature naturally. The result predicts that the size,

morphologies and magnetic properties of cobalt ferrite are effect by reaction

temperature, reaction time, surfactants.

The synthesis approach of CoFe2O4 is applied to prepare MnFe2O4 and the effects

of some action parameter are studied. The Ms and Hc of MnFe2O4 can be changed by

increase reaction time and add some additives. We can obtain a sample with the lowest

Ms and super-paramagnetic by increase the reaction time.

The solvothermal method is tried to construct other metal (Ba, Zn, Sr, Cr, Cu, Ni

and Ca) ferrite nanoparticles, and some valuble results are obtained.

Key word: nanoparticles, magnetic, solvothermal, oxide

中文摘要

ABSTRACT

第一章绪论...............................................................................................................1

1.1 纳米材料的概述..............................................................................................1

1.2 纳米材料的特殊性能......................................................................................3

1.2.1 热学性能...................................................................................................3

1.2.2 光学性能...................................................................................................3

1.2.3 磁学性能...................................................................................................4

1.2.4 电学性能...................................................................................................5

1.2.5 力学性能...................................................................................................5

1.2.6 光催化性能...............................................................................................5

1.3 纳米材料的应用..............................................................................................6

1.3.1 医药和生物方面的应用...........................................................................6

1.3.2 催化剂方面的应用...................................................................................7

1.3.3 磁记录和共振成像的应用.......................................................................7

1.3.4 其他方面的应用.......................................................................................7

1.4 纳米铁酸盐的制备方法..................................................................................8

1.4.1 气相法制备纳米材料...............................................................................8

1.4.1.1 蒸发凝聚法........................................................................................8

1.4.1.2 化学气相沉积法................................................................................9

1.4.2 固相法制备纳米材料...............................................................................9

1.4.2.1 高能球磨法........................................................................................9

1.4.2.2 非晶晶化法......................................................................................10

1.4.2.3 机械-化学法....................................................................................10

1.4.2.4 深度塑性变形法..............................................................................10

1.4.3 液相法制备纳米材料.............................................................................10

1.4.3.1 共沉淀法..........................................................................................11

1.4.3.2 溶胶-凝胶法....................................................................................11

1.4.3.3 微乳液法..........................................................................................12

1.4.3.4 超声化学法......................................................................................13

1.4.3.5 溶剂热/水热法................................................................................14

1.5 本课题的研究意义和创新点........................................................................15

1.5.1 本课题的研究意义.................................................................................15

1.5.2 本课题的创新点.....................................................................................15

第二章铁酸钴纳米粒的溶剂热法制备.................................................................16

2.1 CoFe2O4纳米粒的制备.................................................................................16

2.1.1 实验试剂、仪器及设备.........................................................................16

2.1.2 实验仪器及设备.....................................................................................16

2.2 实验原理........................................................................................................16

2.3 实验步骤........................................................................................................17

2.4 CoFe2O4晶体合成的工艺讨论....................................................................17

2.5 分析与讨论....................................................................................................18

2.5.1 反应时间对粒子形貌和大小的影响.....................................................18

2.5.2 反应温度对铁酸盐制备的影响.............................................................20

2.5.3 碱和溶剂对铁酸盐的影响.....................................................................20

2.5.4 表面活性剂对粒子形貌的影响.............................................................21

2.5.5 反应时间对铁酸钴磁性质的影响.........................................................24

2.5.6 表面活性剂对铁酸钴磁性的影响.........................................................25

2.6 小结................................................................................................................26

第三章 MnFe2O4纳米微粒的水热法制备.............................................................28

3.1 实验试剂........................................................................................................28

3.2 主要仪器........................................................................................................28

3.3 实验原理........................................................................................................28

3.4 实验步骤........................................................................................................28

3.5 工艺路程研究................................................................................................28

3.6 实验结果与讨论............................................................................................30

3.6.1 反应温度对粒子的影响.........................................................................30

3.6.2 反应时间对粒子的影响.........................................................................31

3.6.3 表面活性剂对粒子的影响 (1)...............................................................31

3.6.4 表面活性剂对粒子的影响 (2)...............................................................33

3.6.5 溶剂对 MnFe2O4晶体制备的影响........................................................33

3.6.6 反应时间对 MnFe2O4磁性质的影响....................................................34

3.6.7 表面活性剂对磁性的影响.....................................................................35

3.7 反应机制的探讨............................................................................................35

3.8 小结................................................................................................................36

第四章尝试水热法制备钙、锌、锶、钡、铜和镍金属的铁酸盐及简单表征..37

4.1 实验用品论....................................................................................................37

4.2 实验方案........................................................................................................37

4.3 检测仪器........................................................................................................38

4.4 结果与讨论....................................................................................................38

4.4.1 钡-铁酸盐的简单表征...........................................................................38

4.4.2 钙-铁酸盐的简单表征...........................................................................39

4.4.3 锶-铁酸盐的简单表征...........................................................................41

4.4.4 锌-铁酸盐的简单表征...........................................................................44

第五章结论及进一步工作....................................................................................44

5.1 结论................................................................................................................44

5.2 进一步研究建议............................................................................................44

参考文献..................................................................................................................46

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摘要：

纳米铁氧体(Co,Mn)的制备及其磁性研究摘要本文建立了一种以二价铁离子为铁前驱体，在没有外加氧化剂的条件下，制备铁氧体纳米材料的水-乙二醇溶剂热法。并着重探讨了其在制备CoFe2O4、MnFe2O4中的操作参数。通过研究发现在比较温和、简单的条件下制备出尖晶石结构的CoFe2O4、MnFe2O4的纳米材料，建立了制备CoFe2O4和MnFe2O4的溶剂热制备工艺。在此基础上，又对其他金属的铁酸盐进行了尝试性的制备及研究。产品的形貌、组成、磁性主要用SEM、XRD、TEM、VSM等进行表征。1、单分散CoFe2O4纳米晶体的制备本文采用水热法以硝酸钴、氯化亚铁、HMTA为原料在反应釜中，以乙二...

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