M型钡铁氧体及其复合材料的应用基础研究
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摘要
M型钡铁氧体因其具有较大的矫顽力和磁能积、单轴磁晶各向异性、优良的旋磁特性等特点，被广泛用在永磁、吸波、高密度垂直磁记录和微波毫米波器件等各个领域中。由于其烧结温度一般都要超过1000℃，作为高频材料应用时，无法与现有的片式元器件制造技术——低温共烧陶瓷与铁氧体(LTCC)工艺相适应；同时，随着高新技术的飞速发展，对材料的功能特性提出了更高、更严格的要求，M型钡铁氧体的性能多样性尤其是在与高分子材料复合后所具有的特殊电磁性能及其应用基础更是有待深入的研究。为此如何实现M型钡铁氧体的低温共烧、改性及解决材料的多功能性问题成为了制约此类材料及相关元器件向小型化、高频化、多功能化及高可靠性方向发展的技术瓶颈。本文的研究工作正是围绕M型钡铁氧体及其聚合物复合材料这一主体中的材料制备理论、复合方法、工艺及应用而展开的。旨在通过理论分析、材料研制以及器件应用验证三位一体的研究模式，实现从材料微观、宏观性能的分析到材料研制途径和工艺的优化的综合调控，重点探索M型钡铁氧体材料及其复合材料的高频与微波性能及其在LTCC高频片式器件等领域的应用基础技术，为开发高性能的M型钡铁氧体材料、复合材料及实现其在高频叠层片式元器件中的应用奠定理论和实践基础。
在理论研究方面，首先根据sol-gel法的基本原理从成胶的动力学与热力学角度分析了决定合成低温烧结M型钡铁氧体材料的关键影响因素，然后又从物质迁移的角度探讨了促进M型钡铁氧体低温烧结和致密化的有效途径。此外，为实现M型钡铁氧体的多功能化，从分子设计的思路出发，通过复合手段来赋予材料导电及光敏特性，并结合理论推导和数值拟合的方法得到了相关复合材料的热动力学方程，为提高复合材料的热稳定性及加工性能提供了理论依据。
在材料实验研究方面，本文采用了溶胶-凝胶法，通过加入阴离子表面活性剂及配合超声分散的方式，制备了粒径范围在60～80nm的M型钡铁氧体超细粉体。在此基础上，利用原位聚合法将棒状聚苯胺与M型钡铁氧体粉体进行复合，首次得到了棒状导电磁性复合材料，并对复合材料的磁电性能进行了深入的探索，为研制多功能化的铁氧体材料建立了一种新的实现途径。研究发现萘磺酸(NSA)在该方法中起到了反应控制剂及模板的作用，使得所形成的胶束能够沿某一方向生长，最终形成棒状结构和壳-核包覆结构。复合材料的电性能随着BaFe_(12)O_(19)含量的增加呈先上升后下降趋势，这是由于铁氧体的绝缘特性以及部分导电通道被铁氧体堵塞所造成。聚苯胺-钡铁氧体复合材料的M_s和H_c值均随BaFe_(12)O_(19)含量的增加明显下降。TG-DTG测试曲线表明：棒状PANI/BaFe_(12)O_(19)复合材料的热分解所需要的能量要远远高于PANI，具有优越的热稳定性，并通过建模及计算确定了其分解机理是三维扩散反应。
根据有机光化学原理，通过有机功能材料的分子设计，设计了具有肉桂酰基团新型结构的光敏性二胺。从有机合成的角度出发，成功地采用羟醛缩合技术与氨基保护技术，制备了此类光敏性二胺并通过溶液聚合法得到了相应的光敏聚酰胺酸，其紫外可见最大吸收波长在365nm处，重均分子量为3319，耐热温度超过400℃，分辨率可达4um，初步探索了纳米铁氧体微粉与光敏聚酰亚胺复合材料在构筑磁性阵列方面的应用。
在M型钡铁氧体低温烧结材料的研制过程中，根据M型钡铁氧体配方设计的基本原则，在sol-gel法制备的超细粉体的基础上，通过加入助熔剂BBSZ来实现材料在900℃的烧结。并详细研究了配方中BBSZ含量对材料烧结特性、微观形貌及电磁性能的影响，确定了当配方中BBSZ含量为2 wt％时能较好的兼顾材料低温烧结和高电磁性能的目标要求。此后通过对比实验详细研究了Co/Ti掺杂的低温烧结Ba(CoTi)_xFe_(12-2x)O_(19)钡铁氧体，明确了获得综合磁电性能较佳的掺杂模式为：x=1+3wt％BBSZ，材料的磁导率为13．5，截止频率可达800MHz以上。
为实现低温烧结的M型钡铁氧体在高频片式器件中的应用，本文首先在分析了各种添加剂对流延浆料性能影响规律的基础上，采用自制的分散剂、黏合剂、增塑剂及有机溶剂，得到了较佳流延的配方为：每100．0g铁氧体选用溶剂甲苯30．0g、乙醇20．0g、磷酸酯与脂肪醇聚氧乙烯醚分散剂5．5g、邻苯二甲酸丁酯增塑剂0．7g、聚乙烯醇缩丁醛粘结剂33．0g，粘度为2000cPs较佳。并通过流延膜片法从浆料配方角度解决了M型钡铁氧体与陶瓷两相材料的匹配共烧问题。然后基于电磁场仿真的思想，借助HFSS软件进行片式电感、滤波器结构与性能的优化设计。明确了于2．52uH、截止频率560MHz的0805型高频片式电感，采取银浆导体宽度200um，通孔半径100um，铁氧体膜片厚度27μm，保护层厚度130μm，有效图形层23层；对于截止频率为120MHz的0805型片式低通滤波器，电感采取银浆导体宽度200um，通孔半径100um，铁氧体膜片厚度20μm，保护层厚度40μm，有效图形层11层，电容采用7层极板，保护层厚度200μm、陶瓷膜片的厚度20μm。最后，采用自制的低温烧结Co/Ti掺杂钡铁氧体材料，按照优化的片式元器件结构，采用LTCC工艺进行了器件的研制工作。经验证，实际制备的高频片式电感，截止频率为548．3MHz，电感值为2．45μH；实际制备的低通滤波器，截止频率为130MHz，带外抑制在360MHz时大于20dB，实测结果均与仿真结果非常吻合，为电子元器件的高频化、小型化及器件参数的准确提取与建模仿真奠定了材料基础。
Due to the stronge uniaxial anisotropy, high coericitivity, (BH)_(max) value andexcellent gyromagnetic performances, M-type barium ferrite (BaFe_(12)O_(19)) has beenfound extensive applications in the fields of permanent magnets, wave-adsorbing,high-density magnetic recording and microwave devices. As the sintering temperaturefor the material is always higher than 1000℃and could not be satisfied with chipcomponents manufacturing technology, low-temperature co-fired ceramics and ferrites(LTCC) process, the problems of how to realize the low-temperature firing andmultifunctions of barium ferrite are becoming the key technologies for the adaption tothe developments of electronic components to the directions of sub-miniaturization,greater multifunctionality and excellent reliability. In this dissertation, the investigationswere focus on the theories, composition technics, processes and applications of theabove mentioned subjects. The research mode that combined theoretical analysis,materials preparation and components application was adopted to develop highperformance low-fired barium ferrite and multilayer chip components.
In the part of theoretical analysis, the key factors to determine the formation of thelow-fired barium ferrite were investigated firstly from the point of view of the kineticsand thermodynamics for the sol-gel method, which were very helpful to optimize theparameters of preparation process during experiments. Then the sintering kinetics of theferrite was analyzed to give directions to densify the ferrite under low sinteringtemperature. And in order to realize the multifuctions of the ferrite, after moleculardesign, the ferrte was endowed with conductivity and photosensitivity. Combined withthe deduce and data fitness means, the thermal kinetics equations for the compositeswere successfully got, which could direct the thermal stability of high temperatureperformances and the processing routes available for consolidating the composites.
In the part of experiments investigations, the sol-gel method was adopted toproduce the barium ferrite. After adding anionic surface active agent and by the meansof ultrasonic dispersing, the ultra-fine ferrites powders could be obtained with diametersof 60～80nm. On the basis of the results for the M-type barium ferrite, the rod-shaped polyaniline (PANI)-barium ferrite nanocomposites possessing the conductive andmagnetic performances were obtained by in situ polymerization method for the firsttime. The structure, morphology and properties of the composite were measured by allkinds of testing techniques, which indicated that it is a new and easy way to involve themultifuctions of ferrites. It is also found that the NSA plays a very important role as thereaction controlling agent and the template, which will guarantee the directional growthof micelle, the encapsulation of ferrite particles in the polymer chains and formation ofa "core-shell" structural mixture. The conductivity of the composites varied withdifferent BaFe_(12)O_(19) content with the trend of earlier increasement and later decrease. Itis believed that this is caused by the insulting behavior of the ferrite and partialblockage of conductive path by BaFe_(12)O_(19) in the core of the nanoparticles. The Ms andHc values were both obviously decreased with the increasement of the content ofBaFe_(12)O_(19). TG-DTG testing results showed that the apparent activation energies of thecomposites were higher than that of the pure PANI in a great degree with high thermalstability and the degradation mechanism is three-dimensional diffusion. According tothe principles of photochemistry and through the molecular design for organicfunctional materials, novel photosensitive diamines with the structure of cinnamoylgroup were designed and synthesized by the technology of the Aldol Condensation andprotection for amino group. And corresponding photosensitive PAA were prepared bythe means of solution polymerization with maximal absorption wavelength of UVspectrum at 365nm and weight-average molar mass of 3319. The heat-resistanttemperature of PI is over 400℃and the resolution can reach 4um. The magnetic arrayswere fabricated by the nano ferrites and the above photosensitive polyimide, whichsupply another method to involve the barium ferrites new multifuntions.
In order to realize the low-temperature sintered ferrites, by the references offomula of the materials designing, the BBSZ was adopted to the system. And theinfluences of compositions on the sintering behaviors, microstructures and magneticproperties of the ferrite were investigated. It was confirmed that 2wt% BBSZ contentwas appropriate to give attention to both low-fired characteristic and good magneticproperties. Then the low temperature sintered Co/Ti doped barium ferrite Ba(CoTi)_xFe_(12-2x)O_(19) were carefully researched after the comparing experiments and theoptimal doping mode was x=1+3wt% BBSZ. The permeability of the materials was 13.5 and the cut-off frequency could reach 800MHz.
In the part of LTCC application research, a research of the additives influences onthe slurry performances was carried out and the dispersant, binder, plasticizer andorganic solvent were added to adjust the slurry formula. The formula is as following.The amount of toluene is 30.0g, the alcohol is 20.0g, the dispersant is 5.5g, theplasticizer is 0.7g and the binder is 33.0g for 100.0g ferrites. The slurry viscosity is2000cPs. The co-firing behavior of different multilayer ceramic and ferrite sampleprepared by tape casting method was carried out and an improvement on the co-firingmatch between barium ferrite and the ceramic was established through the method ofadjusting the composition of the slurry for the first time. The HFSS software was usedto design, stimulate and optimize the multilayer chip components. It was confirmed thatfor the 0805-type multilayer chip inductor with the cut-off frequency at 560MHz andinductance of 2.52uH, the width of the silver was 200um, the radius of via holes was100um and the thickness of ferrite layer and protective layer was 27um, 130um withtwenty three figure layers. For the low-pass filter with the cut-off frequency at 120MHz,the inductor was constructed by eleven figure layer under the conditions of 200umsilver width, 100um via hole radius and 20um protective layer thickness and thecapacitor was constructed by seven figure layer under the conditions of 200um silverwidth, 20um layer thickness and 200um protective layer thickness. Then the preparedbarium ferfite was chosen to produce the multilayer chip inductors and low-pass filtersby LTCC technical line. The cut-off frequency and the inductance of the as-preparedinductors were 548.3 MHz and 5.45 uH respectively. And the cut-off frequency of thelow-pass filters and the attenuation were 130MHz and beyond 20dB. The performancesof the inductors and the low pass filter were in good agreements with that of the forecast,which benefits for the high-frequency, miniaturization of electronic components and theaccuate stimulation.
在理论研究方面，首先根据sol-gel法的基本原理从成胶的动力学与热力学角度分析了决定合成低温烧结M型钡铁氧体材料的关键影响因素，然后又从物质迁移的角度探讨了促进M型钡铁氧体低温烧结和致密化的有效途径。此外，为实现M型钡铁氧体的多功能化，从分子设计的思路出发，通过复合手段来赋予材料导电及光敏特性，并结合理论推导和数值拟合的方法得到了相关复合材料的热动力学方程，为提高复合材料的热稳定性及加工性能提供了理论依据。
在材料实验研究方面，本文采用了溶胶-凝胶法，通过加入阴离子表面活性剂及配合超声分散的方式，制备了粒径范围在60～80nm的M型钡铁氧体超细粉体。在此基础上，利用原位聚合法将棒状聚苯胺与M型钡铁氧体粉体进行复合，首次得到了棒状导电磁性复合材料，并对复合材料的磁电性能进行了深入的探索，为研制多功能化的铁氧体材料建立了一种新的实现途径。研究发现萘磺酸(NSA)在该方法中起到了反应控制剂及模板的作用，使得所形成的胶束能够沿某一方向生长，最终形成棒状结构和壳-核包覆结构。复合材料的电性能随着BaFe_(12)O_(19)含量的增加呈先上升后下降趋势，这是由于铁氧体的绝缘特性以及部分导电通道被铁氧体堵塞所造成。聚苯胺-钡铁氧体复合材料的M_s和H_c值均随BaFe_(12)O_(19)含量的增加明显下降。TG-DTG测试曲线表明：棒状PANI/BaFe_(12)O_(19)复合材料的热分解所需要的能量要远远高于PANI，具有优越的热稳定性，并通过建模及计算确定了其分解机理是三维扩散反应。
根据有机光化学原理，通过有机功能材料的分子设计，设计了具有肉桂酰基团新型结构的光敏性二胺。从有机合成的角度出发，成功地采用羟醛缩合技术与氨基保护技术，制备了此类光敏性二胺并通过溶液聚合法得到了相应的光敏聚酰胺酸，其紫外可见最大吸收波长在365nm处，重均分子量为3319，耐热温度超过400℃，分辨率可达4um，初步探索了纳米铁氧体微粉与光敏聚酰亚胺复合材料在构筑磁性阵列方面的应用。
在M型钡铁氧体低温烧结材料的研制过程中，根据M型钡铁氧体配方设计的基本原则，在sol-gel法制备的超细粉体的基础上，通过加入助熔剂BBSZ来实现材料在900℃的烧结。并详细研究了配方中BBSZ含量对材料烧结特性、微观形貌及电磁性能的影响，确定了当配方中BBSZ含量为2 wt％时能较好的兼顾材料低温烧结和高电磁性能的目标要求。此后通过对比实验详细研究了Co/Ti掺杂的低温烧结Ba(CoTi)_xFe_(12-2x)O_(19)钡铁氧体，明确了获得综合磁电性能较佳的掺杂模式为：x=1+3wt％BBSZ，材料的磁导率为13．5，截止频率可达800MHz以上。
为实现低温烧结的M型钡铁氧体在高频片式器件中的应用，本文首先在分析了各种添加剂对流延浆料性能影响规律的基础上，采用自制的分散剂、黏合剂、增塑剂及有机溶剂，得到了较佳流延的配方为：每100．0g铁氧体选用溶剂甲苯30．0g、乙醇20．0g、磷酸酯与脂肪醇聚氧乙烯醚分散剂5．5g、邻苯二甲酸丁酯增塑剂0．7g、聚乙烯醇缩丁醛粘结剂33．0g，粘度为2000cPs较佳。并通过流延膜片法从浆料配方角度解决了M型钡铁氧体与陶瓷两相材料的匹配共烧问题。然后基于电磁场仿真的思想，借助HFSS软件进行片式电感、滤波器结构与性能的优化设计。明确了于2．52uH、截止频率560MHz的0805型高频片式电感，采取银浆导体宽度200um，通孔半径100um，铁氧体膜片厚度27μm，保护层厚度130μm，有效图形层23层；对于截止频率为120MHz的0805型片式低通滤波器，电感采取银浆导体宽度200um，通孔半径100um，铁氧体膜片厚度20μm，保护层厚度40μm，有效图形层11层，电容采用7层极板，保护层厚度200μm、陶瓷膜片的厚度20μm。最后，采用自制的低温烧结Co/Ti掺杂钡铁氧体材料，按照优化的片式元器件结构，采用LTCC工艺进行了器件的研制工作。经验证，实际制备的高频片式电感，截止频率为548．3MHz，电感值为2．45μH；实际制备的低通滤波器，截止频率为130MHz，带外抑制在360MHz时大于20dB，实测结果均与仿真结果非常吻合，为电子元器件的高频化、小型化及器件参数的准确提取与建模仿真奠定了材料基础。
Due to the stronge uniaxial anisotropy, high coericitivity, (BH)_(max) value andexcellent gyromagnetic performances, M-type barium ferrite (BaFe_(12)O_(19)) has beenfound extensive applications in the fields of permanent magnets, wave-adsorbing,high-density magnetic recording and microwave devices. As the sintering temperaturefor the material is always higher than 1000℃and could not be satisfied with chipcomponents manufacturing technology, low-temperature co-fired ceramics and ferrites(LTCC) process, the problems of how to realize the low-temperature firing andmultifunctions of barium ferrite are becoming the key technologies for the adaption tothe developments of electronic components to the directions of sub-miniaturization,greater multifunctionality and excellent reliability. In this dissertation, the investigationswere focus on the theories, composition technics, processes and applications of theabove mentioned subjects. The research mode that combined theoretical analysis,materials preparation and components application was adopted to develop highperformance low-fired barium ferrite and multilayer chip components.
In the part of theoretical analysis, the key factors to determine the formation of thelow-fired barium ferrite were investigated firstly from the point of view of the kineticsand thermodynamics for the sol-gel method, which were very helpful to optimize theparameters of preparation process during experiments. Then the sintering kinetics of theferrite was analyzed to give directions to densify the ferrite under low sinteringtemperature. And in order to realize the multifuctions of the ferrite, after moleculardesign, the ferrte was endowed with conductivity and photosensitivity. Combined withthe deduce and data fitness means, the thermal kinetics equations for the compositeswere successfully got, which could direct the thermal stability of high temperatureperformances and the processing routes available for consolidating the composites.
In the part of experiments investigations, the sol-gel method was adopted toproduce the barium ferrite. After adding anionic surface active agent and by the meansof ultrasonic dispersing, the ultra-fine ferrites powders could be obtained with diametersof 60～80nm. On the basis of the results for the M-type barium ferrite, the rod-shaped polyaniline (PANI)-barium ferrite nanocomposites possessing the conductive andmagnetic performances were obtained by in situ polymerization method for the firsttime. The structure, morphology and properties of the composite were measured by allkinds of testing techniques, which indicated that it is a new and easy way to involve themultifuctions of ferrites. It is also found that the NSA plays a very important role as thereaction controlling agent and the template, which will guarantee the directional growthof micelle, the encapsulation of ferrite particles in the polymer chains and formation ofa "core-shell" structural mixture. The conductivity of the composites varied withdifferent BaFe_(12)O_(19) content with the trend of earlier increasement and later decrease. Itis believed that this is caused by the insulting behavior of the ferrite and partialblockage of conductive path by BaFe_(12)O_(19) in the core of the nanoparticles. The Ms andHc values were both obviously decreased with the increasement of the content ofBaFe_(12)O_(19). TG-DTG testing results showed that the apparent activation energies of thecomposites were higher than that of the pure PANI in a great degree with high thermalstability and the degradation mechanism is three-dimensional diffusion. According tothe principles of photochemistry and through the molecular design for organicfunctional materials, novel photosensitive diamines with the structure of cinnamoylgroup were designed and synthesized by the technology of the Aldol Condensation andprotection for amino group. And corresponding photosensitive PAA were prepared bythe means of solution polymerization with maximal absorption wavelength of UVspectrum at 365nm and weight-average molar mass of 3319. The heat-resistanttemperature of PI is over 400℃and the resolution can reach 4um. The magnetic arrayswere fabricated by the nano ferrites and the above photosensitive polyimide, whichsupply another method to involve the barium ferrites new multifuntions.
In order to realize the low-temperature sintered ferrites, by the references offomula of the materials designing, the BBSZ was adopted to the system. And theinfluences of compositions on the sintering behaviors, microstructures and magneticproperties of the ferrite were investigated. It was confirmed that 2wt% BBSZ contentwas appropriate to give attention to both low-fired characteristic and good magneticproperties. Then the low temperature sintered Co/Ti doped barium ferrite Ba(CoTi)_xFe_(12-2x)O_(19) were carefully researched after the comparing experiments and theoptimal doping mode was x=1+3wt% BBSZ. The permeability of the materials was 13.5 and the cut-off frequency could reach 800MHz.
In the part of LTCC application research, a research of the additives influences onthe slurry performances was carried out and the dispersant, binder, plasticizer andorganic solvent were added to adjust the slurry formula. The formula is as following.The amount of toluene is 30.0g, the alcohol is 20.0g, the dispersant is 5.5g, theplasticizer is 0.7g and the binder is 33.0g for 100.0g ferrites. The slurry viscosity is2000cPs. The co-firing behavior of different multilayer ceramic and ferrite sampleprepared by tape casting method was carried out and an improvement on the co-firingmatch between barium ferrite and the ceramic was established through the method ofadjusting the composition of the slurry for the first time. The HFSS software was usedto design, stimulate and optimize the multilayer chip components. It was confirmed thatfor the 0805-type multilayer chip inductor with the cut-off frequency at 560MHz andinductance of 2.52uH, the width of the silver was 200um, the radius of via holes was100um and the thickness of ferrite layer and protective layer was 27um, 130um withtwenty three figure layers. For the low-pass filter with the cut-off frequency at 120MHz,the inductor was constructed by eleven figure layer under the conditions of 200umsilver width, 100um via hole radius and 20um protective layer thickness and thecapacitor was constructed by seven figure layer under the conditions of 200um silverwidth, 20um layer thickness and 200um protective layer thickness. Then the preparedbarium ferfite was chosen to produce the multilayer chip inductors and low-pass filtersby LTCC technical line. The cut-off frequency and the inductance of the as-preparedinductors were 548.3 MHz and 5.45 uH respectively. And the cut-off frequency of thelow-pass filters and the attenuation were 130MHz and beyond 20dB. The performancesof the inductors and the low pass filter were in good agreements with that of the forecast,which benefits for the high-frequency, miniaturization of electronic components and theaccuate stimulation.
引文
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