Mn-Zn铁氧体纤维的制备与磁性能研究
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摘要
尖晶石型Mn-Zn铁氧体纤维是一种新型的陶瓷纤维材料,既具有铁氧体材料本身耐高温、耐腐蚀、耐氧化等特性,同时还具有纤维材料的各向异性和相对密度低的优点,在民用和国防高科技领域有广阔的应用前景。
本论文系统地研究了以金属盐和柠檬酸为原料,采用有机络合凝胶前驱体转化法制备Mn-Zn铁氧体纤维的过程。通过调节原料的配比及控制实验参数得到了可纺性较好的凝胶,并对纤维前驱体凝胶进行了红外光谱(FT-IR)、热重分析(TG/DSC)、X-射线衍射(XRO)分析,确定纤维前驱体凝胶是一种无定形非晶态物质,在凝胶中羧酸根以双齿配位于金属离子,形成线性分子结构。这种线性分子组成的凝胶显示出良好的可纺性。
通过热重-差示扫描量热(TG-DSC)分析了热处理过程中纤维前驱体的变化,包括脱水、分解、裂解等过程,并在此基础上制定了合理的热处理温度制度。通过扫描电镜(SEM)对纤维的形貌进行了表征。采用有机络合凝胶前驱体转化法可制备成分可控、直径细小、均匀、长径比大、表面光滑的尖晶石型Mn-Zn铁氧体纤维。尖晶石型铁氧体纤维的直径最小可达1μm以下,组成纤维的晶粒尺寸在纳米级,纤维的长度可达80cm。
通过振动样品磁强计(VSM)对纤维试样的磁性能进行了测试,分析研究了热处理工艺,Mn/Zn比例,掺杂Mg、Ce、Co对纤维磁性能的影响及其作用机理。适当的Co掺杂可以显著提高纤维的矫顽力,而适当的Ce掺杂则对纤维饱和磁化强度的提高有促进作用。
Spinel type Mn-Zn ferrite fibres are a kind of novel ceramic fibrous materials. They have not only the characteristics of excellent refractory, corrosion resistant, antioxidization as other ferrite powder materials but also the predominance of a high anisotropy and low relative density. So that, these novel materials will have potential applications in the national defence and high-tech area.
In this thesis, the organic complexation gel derived process has been developed and was used for the preparation of Mn-Zn ferrite fibers from the raw materials of citric acid and metal salts. Good spinnability gels were obtained by adjusting the proportion of raw materials and operational parameters. The gel precursors were characterized by FT-IR spectrum, X-ray diffraction (XRD) and thermo-analysis (TG/DSC). It is reasoned that these gel precuisors are formed by the carboxylic radiacl ligand reacting with metal ions in the aqueous solution throung a dual dentate model. These gel precursors with a linear type structure exhibited a very good spinnability.
The gel fibre precursors have been investigated by thermo-gravimetric analysis and differential scanning calorimetry (TG-DSC) and the process consisted of dehydration, decomposition, cracking and the heat treatment procedure was determined subsequently. The morphologies of Mn-Zn ferrite fibres were characterized by scanning electron microscopy (SEM). Through the organic complexation gel derived process, spinel type ferrite fibres with a precise composition, fine diamater,high aspect ratio(length/diameter) were prepared. In particular, diameters of the Mn-Zn ferrite fibres could be thinner than 1μm, the lenth upto 80cm and the fibres composed of grains in a nanometer level. Magnetic properties of the Mn-Zn ferrite fibres were characterized by a vibrating sample magnetometry (VSM). Effects of heat treatment, Mn/Zn proportion and Mg, Ce, Co doping on the Mn-Zn ferrite fibre's magnetism were discussed. Appropriate Co doping can improve the coercive significantly and Ce doping has an effect on the increase of the saturation magnetization.
本论文系统地研究了以金属盐和柠檬酸为原料,采用有机络合凝胶前驱体转化法制备Mn-Zn铁氧体纤维的过程。通过调节原料的配比及控制实验参数得到了可纺性较好的凝胶,并对纤维前驱体凝胶进行了红外光谱(FT-IR)、热重分析(TG/DSC)、X-射线衍射(XRO)分析,确定纤维前驱体凝胶是一种无定形非晶态物质,在凝胶中羧酸根以双齿配位于金属离子,形成线性分子结构。这种线性分子组成的凝胶显示出良好的可纺性。
通过热重-差示扫描量热(TG-DSC)分析了热处理过程中纤维前驱体的变化,包括脱水、分解、裂解等过程,并在此基础上制定了合理的热处理温度制度。通过扫描电镜(SEM)对纤维的形貌进行了表征。采用有机络合凝胶前驱体转化法可制备成分可控、直径细小、均匀、长径比大、表面光滑的尖晶石型Mn-Zn铁氧体纤维。尖晶石型铁氧体纤维的直径最小可达1μm以下,组成纤维的晶粒尺寸在纳米级,纤维的长度可达80cm。
通过振动样品磁强计(VSM)对纤维试样的磁性能进行了测试,分析研究了热处理工艺,Mn/Zn比例,掺杂Mg、Ce、Co对纤维磁性能的影响及其作用机理。适当的Co掺杂可以显著提高纤维的矫顽力,而适当的Ce掺杂则对纤维饱和磁化强度的提高有促进作用。
Spinel type Mn-Zn ferrite fibres are a kind of novel ceramic fibrous materials. They have not only the characteristics of excellent refractory, corrosion resistant, antioxidization as other ferrite powder materials but also the predominance of a high anisotropy and low relative density. So that, these novel materials will have potential applications in the national defence and high-tech area.
In this thesis, the organic complexation gel derived process has been developed and was used for the preparation of Mn-Zn ferrite fibers from the raw materials of citric acid and metal salts. Good spinnability gels were obtained by adjusting the proportion of raw materials and operational parameters. The gel precursors were characterized by FT-IR spectrum, X-ray diffraction (XRD) and thermo-analysis (TG/DSC). It is reasoned that these gel precuisors are formed by the carboxylic radiacl ligand reacting with metal ions in the aqueous solution throung a dual dentate model. These gel precursors with a linear type structure exhibited a very good spinnability.
The gel fibre precursors have been investigated by thermo-gravimetric analysis and differential scanning calorimetry (TG-DSC) and the process consisted of dehydration, decomposition, cracking and the heat treatment procedure was determined subsequently. The morphologies of Mn-Zn ferrite fibres were characterized by scanning electron microscopy (SEM). Through the organic complexation gel derived process, spinel type ferrite fibres with a precise composition, fine diamater,high aspect ratio(length/diameter) were prepared. In particular, diameters of the Mn-Zn ferrite fibres could be thinner than 1μm, the lenth upto 80cm and the fibres composed of grains in a nanometer level. Magnetic properties of the Mn-Zn ferrite fibres were characterized by a vibrating sample magnetometry (VSM). Effects of heat treatment, Mn/Zn proportion and Mg, Ce, Co doping on the Mn-Zn ferrite fibre's magnetism were discussed. Appropriate Co doping can improve the coercive significantly and Ce doping has an effect on the increase of the saturation magnetization.
引文
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