摘 要

Abstract I

第一章 文献综述 2

1.1 探究背景与意义 2

1.2 电磁基础概述 3

1.2.1 磁性材料与磁导率 3

1.2.2 电介质与介电常数 4

1.3 CuCr₂Se₄的制备方法 5

1.4 CuCr₂Se₄磁性材料的应用 5

1.5 本文研究内容与意义 6

第二章 实验部分 7

2.1 实验试剂 7

2.2 实验仪器 7

2.3 实验方法 7

2.3.1 金属-油酸盐前驱体的制备 7

2.3.2 液相热注射法合成CuCr₂Se₄晶体 8

2.3.3 固相烧结法合成CuCr₂Se₄晶体 8

2.4 表征 9

2.4.1 X射线衍射(XRD) 9

2.4.2 扫描电子显微镜(SEM) 9

2.4.3 振动样品磁强计(VSM) 9

2.4.4 Agilent 4991阻抗分析仪 9

2.4.5 Agilent 4294阻抗分析仪 9

第三章 结果与讨论 10

3.1 晶体结构与形貌调控 10

3.1.1 反应投料比对晶体结构的影响 10

3.1.2 反应时间对晶体结构的影响 10

3.1.3 反应量对晶体结构的影响 12

3.1.4 反应溶剂对晶体形貌的影响 13

3.1.5 液相热注射与固相烧结合成的晶体结构对比 15

3.2 电磁性能分析 15

3.2.1 液相法与固相法合成的CuCr₂Se₄磁导率的比较 15

3.2.2 液相法与固相法合成的CuCr₂Se₄介电常数的比较 16

第四章 总结 18

参考文献 19

致谢 22

CuCr₂Se₄的制备及其电磁性能研究

摘 要

本文采用液相热注射方法和固相烧结方法合成了CuCr₂Se₄晶体颗粒，主要对液相热注射方法的反应条件和两种方法合成的CuCr₂Se₄晶体颗粒的电磁性能进行了研究。

在液相热注射方法中，采用金属-油酸盐配合物与硒的热分解反应合成了CuCr₂Se₄纳米晶体。X射线衍射光谱分析证实了纯尖晶石相CuCr₂Se₄纳米晶体的形成。合成的CuCr₂Se₄纳米晶体近似呈现扁平的三角形状或球体。对CuCr₂Se₄纳米晶体合成反应的Se与金属-油酸盐摩尔比、反应时间、反应量、反应溶剂进行研究，通过XRD分析证实了反应原料Se与金属-油酸盐摩尔比为4：1时得到的颗粒产物为CuCrSe₂晶体，反应原料Se与金属-油酸盐摩尔比为8：1时在合适的条件下可以得到CuCr₂Se₄晶体颗粒。在合成过程的不同时间0.5h、1h、1.5h、2h、3h高温取样，拍摄XRD对反应产物分析，证实了反应1小时即可得到CuCr₂Se₄纳米晶体。以反应原料投料2 mmol Se粉与0.25 mmol油酸盐为单位量，扩大反应量到2倍，4倍，5倍进行反应，确认在5倍范围内扩大反应仍可以得到纯相的CuCr₂Se₄纳米晶体颗粒。

对采用两种方法合成的CuCr₂Se₄晶体颗粒进行电磁性能测试，测试样品在1MHz-1GHz频率范围内的复相对磁导率和复相对介电常数。通过对不同尺寸的CuCr₂Se₄晶体的复相对磁导率和复相对介电常数随频率的变化情况分析得出结论：（1）CuCr₂Se₄晶体颗粒同时具有优良的电磁性能。（2）使用液相法合成的CuCr₂Se₄晶体颗粒具有使用固相法合成的CuCr₂Se₄晶体颗粒更高的复相对磁导率和复相对介电常数，CuCr₂Se₄晶体颗粒的尺寸降低将提高其电磁性能。

关键词：CuCr₂Se₄ 热注射 固相烧结 电磁性能

Preparation and Electromagnetic Properties of CuCr₂Se₄

Abstract

CuCr₂Se₄ crystal particles were synthesized by liquid phase thermal injection method and solid state reaction method. The reaction conditions of liquid phase thermal injection method and the electromagnetic properties of CuCr₂Se₄ crystal particles synthesized by two methods were studied.

In the liquid phase heat injection method, CuCr2Se4 nanocrystals were synthesized by thermal decomposition reaction of metal-oleate complex with selenium. X-ray diffraction spectroscopy confirmed the formation of pure spinel phase CuCr2Se4 nanocrystals. The synthesized CuCr2Se4 nanocrystals approximate a flat triangular shape or sphere. We studied the molar ratio of Se to metal-oleate, reaction time, reaction amount and reaction solvent in the liquid synthesis of CuCr2Se4 nanocrystals. XRD analysis confirmed that the molar ratio of Se and metal-oleate was 4:1. The granular product is CuCrSe₂ crystal, and the CuCr₂Se₄ crystal particles can be obtained under suitable conditions when the molar ratio of the reaction raw material Se to the metal-oleate is 8:1. At high temperature samples of 0.5h, 1h, 1.5h, 2h and 3h at different times of the synthesis process, XRD was used to analyze the reaction products, and it was confirmed that CuCr₂Se₄ nanocrystals were obtained after 1 hour of reaction. The reaction raw material was charged with 2 mmol Se powder and 0.25 mmol oleate as a unit amount, and the reaction amount was expanded to 2 times, 4 times, and 5 times to carry out a reaction, and it was confirmed that the pure phase CuCr₂Se₄ nanocrystal particles could be obtained by expanding the reaction in a range of 5 times. .

The CuCr₂Se₄ crystal particles synthesized by the two methods were tested for electromagnetic properties, and the complex magnetic permeability and complex relative dielectric constant of the sample in the frequency range of 1 MHz to 1 GHz were tested. By analyzing the changes of complex magnetic permeability and complex relative permittivity of different sizes of CuCr₂Se₄ crystals with frequency, it is concluded that: (1) CuCr₂Se₄ crystal particles have excellent electromagnetic properties at the same time. (2) The CuCr₂Se₄ crystal particles synthesized by the liquid phase method have higher complex magnetic permeability and complex relative dielectric constant of the CuCr₂Se₄ crystal particles synthesized by the solid phase method, and the reduction of the size of the CuCr₂Se₄ crystal particles will improve the electromagnetic properties.

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