多孔金属陶瓷微结构调控及双负机理
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摘要
介电常数和磁导率是描述材料性能的两个重要物理性能参数。在不同应用领域,对材料介电常数和磁导率有不同的要求：电容器领域的高介电材料、透波领域的低介电材料、微波吸收领域的低介电常数和高磁导率匹配调控等。所以,电磁参数的调控是材料研究的重要方向。材料的介电常数ε和磁导率μ通常均为正值,近几年ε和μ均为负值的双负材料受到国内外学术界关注。这类材料表现出负折射等许多新颖性能,在新型谐振腔及滤波器、微带天线、电磁波衰减、电磁屏蔽和隐身、无线输电等领域有重要应用前景。
值得注意的是,目前的双负材料基本上都是基于周期性结构阵列的超构材料(metamaterials),其性质主要决定于阵列结构而非材料的组成和微观组织。因此,如果能从工程材料的角度,基于材料本征性质实现双负特性是一项非常有意义的工作。
综合国内外研究现状认为,超构材料实际上是一类有序的导体-绝缘体复合结构,如果将导电的金属和绝缘的陶瓷复合并对其微观组织进行调控,无序的、随机复合的金属陶瓷也有可能具有双负性质。基于这种思路,本文提出了多孔化、网络状金属陶瓷,通过对其组分和微结构进行调控,在MHz频段实现了双负性质。这种金属陶瓷是利用液相浸渍工艺制备的,与传统的金属陶瓷制备工艺相比,可以比较方便的对材料微结构进行调控。
我们首先利用造孔剂法制备了多孔陶瓷,然后利用浸渍-煅烧工艺在多孔陶瓷中负载金属相得到多孔金属陶瓷,通过改变工艺参数制备了不同物相组成和微观形貌的多孔金属陶瓷。利用X射线衍射(XRD)、穆斯堡尔谱、振动样品磁强计(VSM)和扫描电镜(SEM)等对金属陶瓷的物相组成及微观结构进行了表征。利用热重-差热仪(TG-DTA)和程序控温还原(TPR)对材料煅烧和还原过程中的物理及化学反应过程进行了分析。利用阻抗分析仪测试了多孔金属陶瓷的介电性能和磁性能,详细研究了金属陶瓷微观结构与其电磁性能的关系。最后,利用Drude模型、等效电路、HFSS高频电磁结构仿真、有效介质理论(EMT)等理论和模型对金属陶瓷双负机理进行了分析。本文主要研究内容如下。
(1)以碳粉为造孔剂,制备不同气孔率的多孔氧化铝及多孔钇铁石榴石。研究了造孔剂含量、粒径及烧结温度对多孔陶瓷气孔率的影响。利用浸渍-煅烧工艺在多孔陶瓷中负载金属,研究了浸渍溶液组分和浓度、陶瓷类别及气孔率煅烧温度及时间等对金属陶瓷微观形貌的影响。这种多孔金属陶瓷及其浸渍-煅烧工艺,可以制备片状、絮状和网络状等金属相,低温制备使金属粒径更小
(2)利用浸渍-还原工艺在多孔氧化铝内部负载磁性金属镍和铁,制备了不同金属含量的Fe/Al2O3和Ni/Al2O3金属陶瓷。结果表明,金属含量低于逾渗阂值时,电导机制为电子跳跃电导,电导率随频率增加而增加；金属含量超过但仍然接近逾渗阈值时,金属颗粒相互接触形成网络结构,电导率随频率增加而减小。高频电磁场作用下,金属导电网络中自由电子的等离体子振荡导致负介电常数,金属导电网络产生的附加感应磁场以及磁性金属的磁共振共同产生负磁导率。法诺(Fano)型介电共振和磁共振频率可调。
(3)利用浸渍-煅烧工艺侄亚铁磁性的多孔钇铁石榴石中负载银和铜分别得到不同金属含量的Ag/YIG和Cu/YIG金属陶瓷。研究发现,其负介电机理与上述A1203基金属陶瓷类似,但是除了金属导电网络的抗磁性外,YIG基体的磁共振也可以产生负磁导率。
(4)利用等效电路法分析了金属陶瓷的阻抗谱。分析认为,金属含量较低时,可以等效为电容和电阻的并联电路；当金属含量较高超过逾渗阈值时,可以等效为电容、电阻和电感组成的电路,并联电感的出现是产生负介电常数的原因。HFSS数值仿真和有效介质理论计算的结果也与实验结果符合。
(5)计算了钇铁石榴石在0.1MHz-10GHz频段的磁谱,认为钇铁石榴石的畴壁共振和自然共振产生负磁导率,且可以通过外加磁场对其负磁导率进行调控。
论文工作得到国防项目、国家自然科学基金、教育部新世纪优秀人才支持计划、山东省科技攻关计划、山东大学自主创新基金杰出青年培育项目、山东大学研究生自主创新基金等科研项目的资助。
Permittivity (ε) and permeability (μ) are the basic parameters to describe the response of a material to the external electromagnetic field. In different application fields, the permittivity and permeability should satisfy requirements of corresponding conditions. For example, high permittivity was needed for capacitors, low permittivity was needed for wave-transmitting materials, and permittivity should match well with permeability for microwave absorbing materials. Therefore, much attention has been paid to the investigations on the adjustment of the electromagnetic parameters of materials. Generally, the ε and μ of a conventional material are both positive. In recent years, much attention has been paid to double negative materials (DNMs) with simultaneously negative permittivity and permeability. DNMs have many unique electromagnetic properties, such as negative refraction effects. And, they have various novel potential applications, such as novel cavity resonators, microstrip antenna and microwave attenuation, etc.
It is worth noting that, the double negative property of DNMs is usually provided by artificial structures (metamaterials) rather than directly from the materials' composition and micro structure. Therefore, it is also interesting to investigate the possibility of realizing double negative property from the point of "real" random materials rather than periodic artificial structures.
In fact, metamaterial is a kind of ordered conductor-insulator composite structure. Therefore, cermets consisting of metal and ceramic could be a potential candidate for the realization of double negative property by tailoring the microstructure of the cermet. From this point of view, porous cermet is proposed to obtain double negative property in this work, and double negative property is realized in MHz frequency. In this work, cermets were prepared via a wet chemical process. The composition and microstructure of the cermets could be easily tuned.
Porous ceramics are prepared using pore former method. Then, metallic phase is loaded into porous ceramics via impregnation-calcination technique, forming porous cermets. The composition and microstructure of the porous cermets can be tailored by changing experimental parameters. The composition and microstructure of the cermets are characterized using X-ray diffraction (XRD), Mossbauer spectra. Vibrating Sample Magnetometer (VSM) and Scanning Electron Microscope (SEM). The physical and chemical reactions during the calcinations and reduction processes are analyzed using Thermogravimetric and differential thermal analysis (TG-DTA) and Temperature Programmed Reduction (TPR). The dielectric and magnetic properties of the porous cermets are tested using impedance analyzer. The relationship between the microstructure of the cermets and its electromagnetic properties are investigated. Finally, the double negative mechanism of the cermets is analyzed using Drude model, equivalent circuits, HFSS simulation, and Effective Medium Theory (EMT), etc. The main contents are summarized as follows:
(1) Carbon was selected as the pore former, and porous alumina and porous yttrium iron garnets with different porosities were prepared. The influences of pore former content, particles size and sintereing temperature on the porosity of the porous ceramic were investigared. Metals were loaded into porous ceramics using impregnation-calcination process. And the influences of impregnation solution, porous matrix composition and porosity, calcination temperature and time on the microsturctures of the supported metals were investigated.
(2) Fe/Al2O3and Ni/Al2O3composites were prepared using impregnation-calcination process. For the composites with low metal content, the conductive mechanism is hopping conduction. For the composites exceeded the percolation threshold, metallic networks were formed, and the conductivity decreases with increasing frequency due to the skin effects. The plasma oscillation of delocalized electrons in the current loops leads to the negative permittivity. Meanwhile, the combined effects of the diamagnetic response of current loops and magnetic resonances of ferromagnetic metals lead to the negative permeability. Porous cermets can be prepared via low temperature reduction in the impregnation-calcination process, leading to small metal particls. The fano resonance frequency and magnetic resonance frequency can be tunable.
(3) Silver and copper were hosted in prous YIG matrix using impregnation-calcination process, forming Ag/YIG and Cu/YIG composites. The negative mechanism of the YIG matrix cermet is the same as the alumina matrix ceremt. However, in addition to the diamagnetic response of metallic networks, negative permeability can also be obtained by the magnetic resonances of ferrimagnetic YIG matrix.
(4) The impedance spectra of cermets were investigated using equivalent circuit analysis. The results indicated that, composites with low metal content can be simulated by an equivalent circuit model composed of a parallel combination of resistor R and capacitor C. For the composites with high metal content, current loops will be induced in the composites, and the composites can be simulated by an equivalent circuit model composed of inductor L, resistor R and capacitor C. The appearance of shunt inductances is the origin of negative permittivity. The HFSS simulation and Effectivbe Medium Theory (EMT) calculation results agrees well with the experimental results.
(5) The permeability spectra of YIG in the frequency band of0.1MHz-10GHz were calculated. Negative permeability can be realized by the domain wall resonance and nature resonance of YIG, and the negative permeability is tunable with external bias magnetic field.
This work was supported by National Natural Science Foundation of China (50772061,51172131), Program for New Century Excellent Talents in University (NCET-10-518), Independent Innovation Foundation of Shandong University (GIIFSDU-YZC12076, GIIFSDU-YYX10011), and Shandong S&T Plan (2007GG10003007),973Project of China (2012CB825702).
值得注意的是,目前的双负材料基本上都是基于周期性结构阵列的超构材料(metamaterials),其性质主要决定于阵列结构而非材料的组成和微观组织。因此,如果能从工程材料的角度,基于材料本征性质实现双负特性是一项非常有意义的工作。
综合国内外研究现状认为,超构材料实际上是一类有序的导体-绝缘体复合结构,如果将导电的金属和绝缘的陶瓷复合并对其微观组织进行调控,无序的、随机复合的金属陶瓷也有可能具有双负性质。基于这种思路,本文提出了多孔化、网络状金属陶瓷,通过对其组分和微结构进行调控,在MHz频段实现了双负性质。这种金属陶瓷是利用液相浸渍工艺制备的,与传统的金属陶瓷制备工艺相比,可以比较方便的对材料微结构进行调控。
我们首先利用造孔剂法制备了多孔陶瓷,然后利用浸渍-煅烧工艺在多孔陶瓷中负载金属相得到多孔金属陶瓷,通过改变工艺参数制备了不同物相组成和微观形貌的多孔金属陶瓷。利用X射线衍射(XRD)、穆斯堡尔谱、振动样品磁强计(VSM)和扫描电镜(SEM)等对金属陶瓷的物相组成及微观结构进行了表征。利用热重-差热仪(TG-DTA)和程序控温还原(TPR)对材料煅烧和还原过程中的物理及化学反应过程进行了分析。利用阻抗分析仪测试了多孔金属陶瓷的介电性能和磁性能,详细研究了金属陶瓷微观结构与其电磁性能的关系。最后,利用Drude模型、等效电路、HFSS高频电磁结构仿真、有效介质理论(EMT)等理论和模型对金属陶瓷双负机理进行了分析。本文主要研究内容如下。
(1)以碳粉为造孔剂,制备不同气孔率的多孔氧化铝及多孔钇铁石榴石。研究了造孔剂含量、粒径及烧结温度对多孔陶瓷气孔率的影响。利用浸渍-煅烧工艺在多孔陶瓷中负载金属,研究了浸渍溶液组分和浓度、陶瓷类别及气孔率煅烧温度及时间等对金属陶瓷微观形貌的影响。这种多孔金属陶瓷及其浸渍-煅烧工艺,可以制备片状、絮状和网络状等金属相,低温制备使金属粒径更小
(2)利用浸渍-还原工艺在多孔氧化铝内部负载磁性金属镍和铁,制备了不同金属含量的Fe/Al2O3和Ni/Al2O3金属陶瓷。结果表明,金属含量低于逾渗阂值时,电导机制为电子跳跃电导,电导率随频率增加而增加；金属含量超过但仍然接近逾渗阈值时,金属颗粒相互接触形成网络结构,电导率随频率增加而减小。高频电磁场作用下,金属导电网络中自由电子的等离体子振荡导致负介电常数,金属导电网络产生的附加感应磁场以及磁性金属的磁共振共同产生负磁导率。法诺(Fano)型介电共振和磁共振频率可调。
(3)利用浸渍-煅烧工艺侄亚铁磁性的多孔钇铁石榴石中负载银和铜分别得到不同金属含量的Ag/YIG和Cu/YIG金属陶瓷。研究发现,其负介电机理与上述A1203基金属陶瓷类似,但是除了金属导电网络的抗磁性外,YIG基体的磁共振也可以产生负磁导率。
(4)利用等效电路法分析了金属陶瓷的阻抗谱。分析认为,金属含量较低时,可以等效为电容和电阻的并联电路；当金属含量较高超过逾渗阈值时,可以等效为电容、电阻和电感组成的电路,并联电感的出现是产生负介电常数的原因。HFSS数值仿真和有效介质理论计算的结果也与实验结果符合。
(5)计算了钇铁石榴石在0.1MHz-10GHz频段的磁谱,认为钇铁石榴石的畴壁共振和自然共振产生负磁导率,且可以通过外加磁场对其负磁导率进行调控。
论文工作得到国防项目、国家自然科学基金、教育部新世纪优秀人才支持计划、山东省科技攻关计划、山东大学自主创新基金杰出青年培育项目、山东大学研究生自主创新基金等科研项目的资助。
Permittivity (ε) and permeability (μ) are the basic parameters to describe the response of a material to the external electromagnetic field. In different application fields, the permittivity and permeability should satisfy requirements of corresponding conditions. For example, high permittivity was needed for capacitors, low permittivity was needed for wave-transmitting materials, and permittivity should match well with permeability for microwave absorbing materials. Therefore, much attention has been paid to the investigations on the adjustment of the electromagnetic parameters of materials. Generally, the ε and μ of a conventional material are both positive. In recent years, much attention has been paid to double negative materials (DNMs) with simultaneously negative permittivity and permeability. DNMs have many unique electromagnetic properties, such as negative refraction effects. And, they have various novel potential applications, such as novel cavity resonators, microstrip antenna and microwave attenuation, etc.
It is worth noting that, the double negative property of DNMs is usually provided by artificial structures (metamaterials) rather than directly from the materials' composition and micro structure. Therefore, it is also interesting to investigate the possibility of realizing double negative property from the point of "real" random materials rather than periodic artificial structures.
In fact, metamaterial is a kind of ordered conductor-insulator composite structure. Therefore, cermets consisting of metal and ceramic could be a potential candidate for the realization of double negative property by tailoring the microstructure of the cermet. From this point of view, porous cermet is proposed to obtain double negative property in this work, and double negative property is realized in MHz frequency. In this work, cermets were prepared via a wet chemical process. The composition and microstructure of the cermets could be easily tuned.
Porous ceramics are prepared using pore former method. Then, metallic phase is loaded into porous ceramics via impregnation-calcination technique, forming porous cermets. The composition and microstructure of the porous cermets can be tailored by changing experimental parameters. The composition and microstructure of the cermets are characterized using X-ray diffraction (XRD), Mossbauer spectra. Vibrating Sample Magnetometer (VSM) and Scanning Electron Microscope (SEM). The physical and chemical reactions during the calcinations and reduction processes are analyzed using Thermogravimetric and differential thermal analysis (TG-DTA) and Temperature Programmed Reduction (TPR). The dielectric and magnetic properties of the porous cermets are tested using impedance analyzer. The relationship between the microstructure of the cermets and its electromagnetic properties are investigated. Finally, the double negative mechanism of the cermets is analyzed using Drude model, equivalent circuits, HFSS simulation, and Effective Medium Theory (EMT), etc. The main contents are summarized as follows:
(1) Carbon was selected as the pore former, and porous alumina and porous yttrium iron garnets with different porosities were prepared. The influences of pore former content, particles size and sintereing temperature on the porosity of the porous ceramic were investigared. Metals were loaded into porous ceramics using impregnation-calcination process. And the influences of impregnation solution, porous matrix composition and porosity, calcination temperature and time on the microsturctures of the supported metals were investigated.
(2) Fe/Al2O3and Ni/Al2O3composites were prepared using impregnation-calcination process. For the composites with low metal content, the conductive mechanism is hopping conduction. For the composites exceeded the percolation threshold, metallic networks were formed, and the conductivity decreases with increasing frequency due to the skin effects. The plasma oscillation of delocalized electrons in the current loops leads to the negative permittivity. Meanwhile, the combined effects of the diamagnetic response of current loops and magnetic resonances of ferromagnetic metals lead to the negative permeability. Porous cermets can be prepared via low temperature reduction in the impregnation-calcination process, leading to small metal particls. The fano resonance frequency and magnetic resonance frequency can be tunable.
(3) Silver and copper were hosted in prous YIG matrix using impregnation-calcination process, forming Ag/YIG and Cu/YIG composites. The negative mechanism of the YIG matrix cermet is the same as the alumina matrix ceremt. However, in addition to the diamagnetic response of metallic networks, negative permeability can also be obtained by the magnetic resonances of ferrimagnetic YIG matrix.
(4) The impedance spectra of cermets were investigated using equivalent circuit analysis. The results indicated that, composites with low metal content can be simulated by an equivalent circuit model composed of a parallel combination of resistor R and capacitor C. For the composites with high metal content, current loops will be induced in the composites, and the composites can be simulated by an equivalent circuit model composed of inductor L, resistor R and capacitor C. The appearance of shunt inductances is the origin of negative permittivity. The HFSS simulation and Effectivbe Medium Theory (EMT) calculation results agrees well with the experimental results.
(5) The permeability spectra of YIG in the frequency band of0.1MHz-10GHz were calculated. Negative permeability can be realized by the domain wall resonance and nature resonance of YIG, and the negative permeability is tunable with external bias magnetic field.
This work was supported by National Natural Science Foundation of China (50772061,51172131), Program for New Century Excellent Talents in University (NCET-10-518), Independent Innovation Foundation of Shandong University (GIIFSDU-YZC12076, GIIFSDU-YYX10011), and Shandong S&T Plan (2007GG10003007),973Project of China (2012CB825702).
引文
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