钴铁氧体的制备及其性能研究
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摘要
钴铁氧体在可见光区具有较大的磁光克尔效应,克服了目前市场上商用磁光存储材料非晶态稀土-过渡金属在短波长区的克尔旋转角小、抗氧化能力较差的缺点,再加上其温和的饱和磁化场、较大的矫顽力使其成为极具竞争力的新一代高密度磁光记录材料。但如何在保持钴铁氧体饱和磁化强度适当高的同时进一步提高其矫顽力,以期获得适合高密度信息存储水平的磁光读写特性,是目前的研究热点。
本研究采用低热固相-溶胶凝胶法、低热固相-自蔓延燃烧法制备出了高磁性能的钴铁氧体磁性材料。本文研究了改进后的耦合制备方法制取钴铁氧体的适宜工艺条件,并探讨了不同工艺条件对产物晶体结构和性能的影响机理。同时借助于TG-DSC、XRD、SEM和VSM等技术手段,对钴铁氧体的制备过程进行了跟踪检测,并对其微观结构、形貌和磁性能进行了表征,初步认识了产物的微观结构与其磁性能间的关系。
研究结果表明:制备工艺对产物的结构及磁性能影响很大;在本实验条件下,采用低热固相-溶胶凝胶法制备钴铁氧体的适宜工艺条件是钴铁比为1:2,柠檬酸配比为3,煅烧温度为700℃,煅烧时间为2h;采用低热固相-自蔓延燃烧法制备钴铁氧体的适宜工艺条件是钴铁比为1:2,柠檬酸配比为2,煅烧温度为600℃,煅烧时间为1h;在适宜工艺条件下,两种制备方法均可制得粒径均匀约40nm、物相纯净单一、结晶度高的纳米钴铁氧体,并在较大程度上改善其磁性能使其更适合于磁光记录。随着钴含量的增加产物的晶化程度逐渐提高,所以其粒径逐渐减小;随着柠檬酸用量增加,在反应过程中在反应物的液固界面之上的吸附作用越来越强促使所形成的液膜对于超微晶粒之间的相互接触以及积聚过程起到了很大的阻碍作用,并在颗粒间产生排斥力从而能抑制团聚体的形成,减小产物的晶粒尺寸;随着乙二醇的用量增加,它能更持久地固定聚合物中钴、铁离子的位置并且其分解气体产生压力会推动反应聚合,致使产品粒径趋于均匀且超细小化。所得产物的晶体粒度直接影响着其磁性能,相比较而言,柠檬酸适量增大时产物矫顽力提高显著,而乙二醇的加入虽然能有效地减轻颗粒间的软团聚细化颗粒,从而明显增大产物的矩形比在整体上改善其磁性能,却在一定程度上抑制了矫顽力的提高。本研究为制备高性能钴铁氧体磁性材料提供了一些有益的基础数据,具有很好的理论意义和可观的应用前景。
本文的创新之处主要在于:1、首次采用新的耦合法低热固相-溶胶凝胶法、低热固相-自蔓延燃烧法对钴铁氧体的制备工艺进行了研究并得出了适宜的工艺条件,并初步认识了不同制备工艺条件对产物结构、生成过程以及磁性能的影响机理。2、探索了分散剂乙二醇对产品性能的影响,发现随着乙二醇的用量增加,它能更持久地固定聚合物中钴、铁离子的位置并且其分解气体产生压力会推动反应聚合,并有效地减轻颗粒间的软团聚致使产品粒径趋于均匀且超细小化,从而明显增大产物的矩形比在整体上改善其磁性能。
Cobalt ferrite has a large magneto-optical Kerr effect in the visible region so that it overcomes the shortcomings of small Kerr rotation angle and less antioxidant capacity, which amorphous rare earth-transition metal of commercial magneto-optical storage materials in the current market has in the short wavelength region. In addition, the cobalt ferrite with a moderate saturation magnetization field and the larger coercivity become very competitive next-generation high-density magneto-optical recording materials. However, at present the current research focus is how to enhance its coercivity further while proper saturation magnetization of cobalt ferrite is maintained, in order to obtain magneto-optical read-write characteristics suitable for high density information storage levels.
In this study, cobalt ferrite as magnetic materials of high magnetic properties is prepared by low-heating solid-state sol-gel method and low-heating solid-state self-propagating combustion method respectively. This paper studies the appropriate process conditions of improved coupled preparation method to prepare cobalt ferrite, and the effect mechanism of different process conditions on the crystal structure and properties of the product is discussed. At the same time by means of TG-DSC, XRD, SEM and VSM technical means, the preparation of cobalt ferrite is tracked and detected, and its microstructure, morphology and magnetic properties are characterized further into preliminarily understanding the relationship between their microstructures and magnetic properties of the products.
The study results show that: preparation process has a great influence on the structure and magnetic properties of the product. Under the experimental conditions, the optimum conditions of cobalt ferrite prepared by low-heating solid-state sol-gel method are cobalt-iron ratio 1:2, citric acid ratio 3, calcination temperature 700℃, calcination time 2h. The optimum conditions of cobalt ferrite prepared by low-heating solid-state self-propagating combustion method are cobalt-iron ratio 1:2, citric acid ratio 2, calcination temperature 600℃, calcination time 1h. Under optimum conditions, the two preparation methods can obtain uniform size (about 40nm), single-phase pure, nano-crystalline cobalt ferrite of high crystallinity and improve its magnetic properties to a greater extent to make it more suitable for magnetic optical recording.
With the increase of cobalt content, the degree of crystallization of the product increases gradually, so the particle size decreases. With the increase of citric acid, the film, which is formed due to the adsorption growing on the liquid-solid interface of reactants during the reaction, plays a certain role in impeding ultrafine grains contacting and the accumulation process and generats repulsive force between particles. Therefore, it can inhibit the formation of aggregates and reduce the grain size of the product. With the increase of ethylene glycol, it fixes the position of cobalt and iron ions in the polymer more durably and the pressure of the decomposition gases will promote the polymerization reaction, resulting in the particle size of products ultra small and uniform. Crystal size of the products obtained directly affects their magnetic properties. Comparatively speaking, with the increase of citric acid coercivity of the product is increased significantly. However, the addition of ethylene glycol can effectively reduce soft agglomeration of particles to refine the grain, which significantly increases the squareness ratio of the product and improves its overall magnetic properties but to some extent inhibits the increase of coercivity. This paper provides some useful basic data for the preparation of high-performance cobalt ferrite magnetic materials, which has good theoretical and substantial applications.
In this paper, the innovation is that the preparations of cobalt ferrite are studied by low-heating solid-state sol-gel method and low-heating solid-state self-propagating combustion method respectively for the first time and that optimum conditions have been found out further into preliminarily understanding the effect mechanisms of different process conditions on the crystal structure, generation process and magnetic properties of the product. The impact of ethylene glycol as the dispersant on performances of the product is explored. And it is found out that with the increase of ethylene glycol, it fixes the position of cobalt and iron ions in the polymer more durably and the pressure of the decomposition gases will promote the polymerization reaction and effectively reduce soft agglomeration of particles, resulting in the particle size of products ultra small and uniform, which significantly increases the squareness ratio of the product and improves its overall magnetic properties.
本研究采用低热固相-溶胶凝胶法、低热固相-自蔓延燃烧法制备出了高磁性能的钴铁氧体磁性材料。本文研究了改进后的耦合制备方法制取钴铁氧体的适宜工艺条件,并探讨了不同工艺条件对产物晶体结构和性能的影响机理。同时借助于TG-DSC、XRD、SEM和VSM等技术手段,对钴铁氧体的制备过程进行了跟踪检测,并对其微观结构、形貌和磁性能进行了表征,初步认识了产物的微观结构与其磁性能间的关系。
研究结果表明:制备工艺对产物的结构及磁性能影响很大;在本实验条件下,采用低热固相-溶胶凝胶法制备钴铁氧体的适宜工艺条件是钴铁比为1:2,柠檬酸配比为3,煅烧温度为700℃,煅烧时间为2h;采用低热固相-自蔓延燃烧法制备钴铁氧体的适宜工艺条件是钴铁比为1:2,柠檬酸配比为2,煅烧温度为600℃,煅烧时间为1h;在适宜工艺条件下,两种制备方法均可制得粒径均匀约40nm、物相纯净单一、结晶度高的纳米钴铁氧体,并在较大程度上改善其磁性能使其更适合于磁光记录。随着钴含量的增加产物的晶化程度逐渐提高,所以其粒径逐渐减小;随着柠檬酸用量增加,在反应过程中在反应物的液固界面之上的吸附作用越来越强促使所形成的液膜对于超微晶粒之间的相互接触以及积聚过程起到了很大的阻碍作用,并在颗粒间产生排斥力从而能抑制团聚体的形成,减小产物的晶粒尺寸;随着乙二醇的用量增加,它能更持久地固定聚合物中钴、铁离子的位置并且其分解气体产生压力会推动反应聚合,致使产品粒径趋于均匀且超细小化。所得产物的晶体粒度直接影响着其磁性能,相比较而言,柠檬酸适量增大时产物矫顽力提高显著,而乙二醇的加入虽然能有效地减轻颗粒间的软团聚细化颗粒,从而明显增大产物的矩形比在整体上改善其磁性能,却在一定程度上抑制了矫顽力的提高。本研究为制备高性能钴铁氧体磁性材料提供了一些有益的基础数据,具有很好的理论意义和可观的应用前景。
本文的创新之处主要在于:1、首次采用新的耦合法低热固相-溶胶凝胶法、低热固相-自蔓延燃烧法对钴铁氧体的制备工艺进行了研究并得出了适宜的工艺条件,并初步认识了不同制备工艺条件对产物结构、生成过程以及磁性能的影响机理。2、探索了分散剂乙二醇对产品性能的影响,发现随着乙二醇的用量增加,它能更持久地固定聚合物中钴、铁离子的位置并且其分解气体产生压力会推动反应聚合,并有效地减轻颗粒间的软团聚致使产品粒径趋于均匀且超细小化,从而明显增大产物的矩形比在整体上改善其磁性能。
Cobalt ferrite has a large magneto-optical Kerr effect in the visible region so that it overcomes the shortcomings of small Kerr rotation angle and less antioxidant capacity, which amorphous rare earth-transition metal of commercial magneto-optical storage materials in the current market has in the short wavelength region. In addition, the cobalt ferrite with a moderate saturation magnetization field and the larger coercivity become very competitive next-generation high-density magneto-optical recording materials. However, at present the current research focus is how to enhance its coercivity further while proper saturation magnetization of cobalt ferrite is maintained, in order to obtain magneto-optical read-write characteristics suitable for high density information storage levels.
In this study, cobalt ferrite as magnetic materials of high magnetic properties is prepared by low-heating solid-state sol-gel method and low-heating solid-state self-propagating combustion method respectively. This paper studies the appropriate process conditions of improved coupled preparation method to prepare cobalt ferrite, and the effect mechanism of different process conditions on the crystal structure and properties of the product is discussed. At the same time by means of TG-DSC, XRD, SEM and VSM technical means, the preparation of cobalt ferrite is tracked and detected, and its microstructure, morphology and magnetic properties are characterized further into preliminarily understanding the relationship between their microstructures and magnetic properties of the products.
The study results show that: preparation process has a great influence on the structure and magnetic properties of the product. Under the experimental conditions, the optimum conditions of cobalt ferrite prepared by low-heating solid-state sol-gel method are cobalt-iron ratio 1:2, citric acid ratio 3, calcination temperature 700℃, calcination time 2h. The optimum conditions of cobalt ferrite prepared by low-heating solid-state self-propagating combustion method are cobalt-iron ratio 1:2, citric acid ratio 2, calcination temperature 600℃, calcination time 1h. Under optimum conditions, the two preparation methods can obtain uniform size (about 40nm), single-phase pure, nano-crystalline cobalt ferrite of high crystallinity and improve its magnetic properties to a greater extent to make it more suitable for magnetic optical recording.
With the increase of cobalt content, the degree of crystallization of the product increases gradually, so the particle size decreases. With the increase of citric acid, the film, which is formed due to the adsorption growing on the liquid-solid interface of reactants during the reaction, plays a certain role in impeding ultrafine grains contacting and the accumulation process and generats repulsive force between particles. Therefore, it can inhibit the formation of aggregates and reduce the grain size of the product. With the increase of ethylene glycol, it fixes the position of cobalt and iron ions in the polymer more durably and the pressure of the decomposition gases will promote the polymerization reaction, resulting in the particle size of products ultra small and uniform. Crystal size of the products obtained directly affects their magnetic properties. Comparatively speaking, with the increase of citric acid coercivity of the product is increased significantly. However, the addition of ethylene glycol can effectively reduce soft agglomeration of particles to refine the grain, which significantly increases the squareness ratio of the product and improves its overall magnetic properties but to some extent inhibits the increase of coercivity. This paper provides some useful basic data for the preparation of high-performance cobalt ferrite magnetic materials, which has good theoretical and substantial applications.
In this paper, the innovation is that the preparations of cobalt ferrite are studied by low-heating solid-state sol-gel method and low-heating solid-state self-propagating combustion method respectively for the first time and that optimum conditions have been found out further into preliminarily understanding the effect mechanisms of different process conditions on the crystal structure, generation process and magnetic properties of the product. The impact of ethylene glycol as the dispersant on performances of the product is explored. And it is found out that with the increase of ethylene glycol, it fixes the position of cobalt and iron ions in the polymer more durably and the pressure of the decomposition gases will promote the polymerization reaction and effectively reduce soft agglomeration of particles, resulting in the particle size of products ultra small and uniform, which significantly increases the squareness ratio of the product and improves its overall magnetic properties.
引文
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