新型铋基低温烧结微波介质陶瓷研究
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摘要
近年来由于微波技术设备向小型化、集成化以及民用方向发展,国际上展开了大规模的对微波介质材料的研究工作。随着近年来LTCC(低温共烧陶瓷)技术的广泛使用,寻找、制备与研究中高介电常数(εr>10)、低损耗(Qf>5000GHz)、近零谐振频率温度系数(TCF≈0ppm/oC)、低烧结温度(低于Ag、Cu、Au、Al等常用金属的熔点)且跟金属电极烧结匹配、低成本(不含或者含有少量贵重金属)、环保(至少无铅,尽量不含或者含有较少有毒原材料)的新型微波介质陶瓷成为了人们研究的热点。
考虑到Bi基氧化物陶瓷一般具有较低烧结温度和较高介电常数等优点,本论文紧紧围绕各类Bi基氧化物陶瓷,应用固相反应烧结的方法和高能球磨的方法,通过多种离子取代以及氧化物掺杂的方式,对Bi基氧化物陶瓷的烧结温度、微波介电性能、金属电极匹配性等方面展开了研究,并尝试在陶瓷基板天线和多层共烧电容器等领域进行了原型器件设计和制作,得到了一系列兼具理论和工程应用价值的结果:
本文的第一章主要从基础介质物理理论出发,首先介绍了介质中最基本的极化现象,然后进一步引申出了在微波频段下(300MHz~300GHz)电介质的介电常数、介电损耗以及温度系数的具体表征以及含义,为后续具体工作提供了有力的理论依据。接下来详细介绍了低温共烧陶瓷(LTCC)技术的发展状况,其中包括常用的导体材料以及介质材料两部分的发展状况。在第一章的结束部分阐述了本文的主要研究内容及其意义。
本文的第二章主要是对Bi_2O_3-Nb_2O_5二元体系微波介质陶瓷的研究。首先通过V5+、Cu~(2+)、W~(6+)、Ta~(5+)等离子取代的方式,应用固相反应烧结和高能球磨等制备方法,系统研究了BiNbO_4和Bi_3NbO_7配方的相形成以及降温改性,得到了介电常数介于36~45、Qf介于5000~20000GHz、谐振频率温度系数近零的BiNbO_4基陶瓷以及介电常数介于65~95、Qf介于230GHz~560GHz、TCF在-115~-70ppm/oC的Bi_3(Nb,Ta)O_7基陶瓷。首次研究了BiNbO_4陶瓷跟Cu电极的共烧问题,发现在N_2气氛下共烧后并没有发生反应或者渗透的情况,奠定了BiNbO_4陶瓷在LTCC中的应用基础;首次尝试使用低温烧结的BiNbO_4陶瓷作为基板,设计了二维天线阵列,HFSS软件仿真结果跟网络分析仪的实际测量结果基本符合,为高介基板在微波频段的应用做了初步探索。
本文的第三章主要研究了Bi(Sb_xNb_yTa_z)O_4(x+y+z=1)三元体系的相组成、相变以及微波介电性能等问题。首次系统地研究了Bi(Sb_xNb_yTa_z)O_4(x+y+z=1)三元体系的相组成以及相变问题。将Bi(Sb_xNb_yTa_z)O_4(x+y+z=1)三元体系分为:I-单斜固溶体区域(x>0.78);II-单斜、正交同存的区域(0.78>x>0.55);III-正交三斜相变区域(x<0.55)三个区域(相图不随x和y的取值而发生大的变化)。从晶格结构、晶胞参数的角度出发,较为详细地阐述了三元相图中各个相区转变的过程,重点研究了在正交、三斜相变区域中正交相到三斜相之间的相变问题。发现了高温三斜相β-BiNbO_4向低温正交相α-BiNbO_4相转变现象,并确定了β-BiNbO_4陶瓷不能够稳定存在的温度范围700oC~1020oC。但该结论并不适用于粉末样品。并且在这个三元体系中开发出了一系列具有潜在应用价值的微波介质陶瓷:1080oC烧结的纯单斜相的BiSbO_4陶瓷,介电常数εr≈19.3、Qf≈70000GHz、TCF≈-62ppm/oC,不跟Ag发生明显反应;掺杂0.6wt.% ~1.2wt.%B_2O_3-CuO后930oC烧结的单斜相的BiSbO_4陶瓷,介电常数εr≈19.5、Qf≈45400GHz~33700GHz、TCF≈-65ppm/oC;960oC烧结的Bi(Sb_(0.6)Ta_(0.4))O_4陶瓷,εr≈27、Qf≈35000GHz、TCF=-12ppm/oC;960oC烧结的Bi{Sb_(0.6)(Nb_(0.992)V_(0.008))_(0.4)}O_4陶瓷,εr≈34.7、Qf≈16000GHz、TCF=+16.1ppm/oC。
在本文的第四章中,开发并研究了Bi_2O_3-MoO_3二元体系超低温烧结微波介质陶瓷的烧结特性、微波介电性能、金属电极烧结匹配问题以及多层电容器具体应用问题。首先,从Bi_2O_3-MoO_3二元体系的相图出发,设计并制备了一系列的二元氧化物,发现在xBi_2O_3-(1-x)MoO_3中,随着x值从0.2增加到0.5,样品的成瓷温度几乎线性地从600oC增加到了750oC。当x=0.875时,其烧结温度稳定在820oC附近。整体来讲,富含MoO_3的区域比富含Bi2O3的区域具有更低的烧结温度。这个体系中有三个具有良好微波介电性能的配方组成:620oC烧结的Bi_2Mo_3O_(12)陶瓷,εr≈19、Qf≈21800GHz、TCF≈-215ppm/oC,跟Ag发生反应但是跟Al不发生反应;640oC烧结的Bi_2Mo_2O_9陶瓷,εr≈38、Qf≈12500GHz、TCF≈+31ppm/oC,跟Ag发生反应但是跟Al不发生反应;750oC烧结的Bi_2MoO_6陶瓷,εr≈31、Qf≈16700GHz、TCF≈-114ppm/oC。使用等价镧系离子La~(3+)和Nd~(3+)对Bi_2Mo_2O_9中的Bi3+进行取代,来调节其微波介电性能,尤其是TCF值,获得的(Bi0.8La0.2)2Mo2O9陶瓷具有近零的温度系数TCF≈-4.6ppm/oC,其介电常数εr≈32.7、Qf≈13490GHz、烧结温度为650oC。在第四章的最后一小节中,初次尝试制备了Bi_2Mo_2O_9基、Al做内电极的超低温烧结多层电容器MLCC,在645oC下成功烧结制备了Bi_2Mo_2O_9多层电容器(共六层,每层厚度约90μm,电极厚度约为12μm)以及单层电容器(层厚约50μm,电极厚度约为12μm),这开拓了Al电极在LTCC领域中的应用。
在本文的最后一章,总结了全文的重要结论并阐明了进一步的工作方向。
With the rapid development of mobile communication and satellite communication, microwave electronic devices are required to be developed and fabricated for miniaturization and integration. The low temperature co-fired ceramic technology (LTCC) becomes an important fabricating technology that can integrate the passive components within a monolithic bulk module with IC chips mounted on its surface. By this technology, microwave dielectrics are stacked in multilayers and co-fired with internal electrodes, such as Ag, Cu, Au, Al, their alloys etc, in special patterns to fulfill different electrical functions. The microwave dielectric materials used in LTCC field must have a high dielectric permittivity (εr>10), a high Qf value (f=resonant frequency, Q=1/dielectric loss at f, Qf>5000GHz), a near zero temperature coefficient of resonant frequency (TCF≈0ppm/oC), a low sintering temperature (below the melting points of common electrode metals, such as silver, copper, gold, aluminum etc. ) and chemical compatibility with the metal electrodes. Besides that, considering the environment and economic elements, people prefer to explore microwave dielectric ceramics with low price (not contain rare metal oxides) and without toxicity (at least lead free).
Bismuth-based dielectric ceramics are well-known as low-fired materials and have been investigated in multilayer capacitors application for many years. According to Shanno’ns study, Bi~(3+) has a polarizability of 6.12(?)~3, which could account for the high permittivities in many bismuth based oxides. In this thesis, a series of new bismuth-based oxides prepared by solid state reaction method and high energy ball milling method were explored. Ionic substitution and oxides addition methods were used to lower the sintering temperature, adjust the microwave dielectric properties and their chemical compatibility with metal electrodes. The application of antenna substrate using high permittivity dielectric and the fabrication of multilayers co-fired capacitor using bismuth based oxides were also tried. A series of scientific and engineering results were obtained as follows:
1. The influence of V~(5+), Cu~(2+), W~(6+) and Ta~(5+) substitution on the sintering temperature, microwave dielectric properties and phase composition of BiNbO_4 and Bi_3NbO_7 compositions in the Bi_2O_3-Nb_2O_5 binary system prepared by solid state reaction method and high energy ball milling method were studied. A series of BiNbO_4 ceramics sintered at 850~960oC withεr≈36~45, Qf≈5000~20000GHz and TCF≈0ppm/oC and Bi_3(Nb,Ta)O_7 ceramics sintered at 900~990oC withεr≈65~95, Qf≈230~560GHz and TCF≈-115~-70ppm/oC were obtained. The co-firing between BiNbO_4 ceramics and copper electrode under N_2 atmosphere was first studied. The SEM and EDS results showed that there was no reaction and diffusion between the ceramic and electrode. This makes it possible for BiNbO4 ceramics to be used in LTCC technology. A two element antennas with centre frequency at 3.07 GHz and bandwidth of 34MHz at -10 dB attenuation were obtained using a BiNbO4 ceramic substrate with size 34mm×34mm×1mm. The primary study of BiNbO_4 ceramic in antenna will broaden the application field for microwave ceramics with high permittivity.
2. Based on the analysis on a number of Bi(Sb_xNb_yTa_z)O_4 (x+y+z=1) samples, a pseudo-ternary phase diagram of Bi(Sb,Nb,Ta)O_4 system is given below the melting point. It is composed of a monoclinic-phase region (x≥0.78), an orthorhombic-phase region (x≤0.55) and a monoclinic-orthorhombic coexisting phase region (0.55≤x≤0.78). The phase transformation from the monoclinic to orthorhombic structure can be attributed to the decrease of space occupied by the bismuth layers, which is caused by the increase of octahedra volumes when the Nb or Ta amount increases. In orthorhombic phase region, as the sintering temperature increases, the phase transformation to triclinic structure is observed and it is seriously affected by the sintering temperature and the Sb amount in Bi(Sb,Nb,Ta)O_4. Phase transformation fromβ-BiNbO_4 toα-BiNbO_4 in BiNbO_4 bulk samples was first reported and studied. From X-ray diffraction patterns, the transformation fromβtoαphase of BiNbO_4 could be observed by heating the bulk samples ofβ-BiNbO_4 from low temperatures to 700~1030oC. But such a transformation didn’t occur in powder samples and in the cooling course. This phenomenon might be related with associated activation of stress and heat energy in the heating course. Differential thermal analysis, shrinkage and dielectric properties as a function of temperature were carried out and all the results confirmed the transformation fromβtoαphase of BiNbO4. In addition, a series of promising candidates for LTCC were explored in Bi(SbxNbyTaz)O4 system: 1, the BiSbO_4 ceramic sintered at 1080oC withεr≈19.3, Qf≈70000GHz, TCF≈-62ppm/oC and chemical compatibility with silver; 2, the 930oC sintered BiSbO4 ceramics with 0.6wt.% ~1.2wt.%B_2O_3-CuO addition withεr≈19.5, Qf≈45400GHz~33700GHz and TCF≈-65ppm/oC; 3, the 960oC sintered Bi(Sb0.6Ta0.4)O_4 ceramic withεr≈27, Qf≈35000GHz and TCF=-12ppm/oC; 4, the 960oC sintered Bi、O_4 ceramic withεr≈34.7, Qf≈16000GHz, and TCF=+16.1ppm/oC.
3. The preparation, phase composition, microwave dielectric properties and chemical compatibility with silver and aluminum electrodes were investigated on a series of single phase compounds in the Bi2O3-MoO3 binary system. All materials have ultra low sintering temperatures lower than 820oC. Eight different xBi2O3-(1-x)MoO3 compounds with x value between 0.2≤x≤0.875 were fabricated and the associated microwave dielectric properties were studied. Theβ~Bi_2Mo_2O_9 single phase has a positive temperature coefficient of resonant frequency (TCF) about +31ppm/oC, with a permittivityεr=38 and a Qf=12500GHz at 300K at a frequency of 6.3GHz. Theα~Bi_2Mo_3O_(12) andγ~Bi2MoO6 compounds both have negative temperature coefficient values of TCF~-215ppmo/C and TCF~-114ppm/oC, with permittivities ofεr=19 and 31, Qf=21800GHz and 16700 GHz at 300K measured at resonant frequencies of 7.6 GHz and 6.4 GHz, respectively. Through sintering the B2iO3-2.2MoO3 at 620oC for 2hrs a composite dielectric containing bothαandβphase can be obtained with a near zero temperature coefficient of frequency TCF=-13ppm/oC and a relative dielectric constantεr=35, and a large Qf~12000 GHz is also obtained. Owing to the frequent difficulty of thermochemical interactions between low sintering temperature materials and the electrode materials during the cofiring, preliminary investigations are made to determine any major interactions with possible candidate electrode metals, Ag and Al. The results show thatβ~Bi_2Mo_2O_9 andα~Bi_2Mo_3O_(12) do not react with Al at their sintering temperatures. La and Nd were also used to substitute for the Bi in Bi_2Mo_2O_9. For (Bi_(1-x)Ln_x)_2Mo_2O_9 (Ln=La, Nd) ceramics, as the x value increased, the optimal sintering temperature increased. Substitution of La or Nd could stabilize the monoclinic phase and modify its microwave dielectric properties. The best microwave dielectric properties were obtained in (Bi0.8La0.2)2Mo2O9 ceramic with a permittivity of 32.7, Qf value of 13,490GHz and temperature coefficient about -4.6ppm/oC. From the above results, the low sintering temperature, good microwave dielectric properties, chemical compatibility with Al metal electrode, nontoxicity and price advantage of the Bi2O3-MoO3 binary system, all indicate the potential for a new material system with ultra-low temperature cofirng for multilayer devices application.
4. Fabrication of a new kind multlayer co-fired capacitor using Bi_2Mo_2O_9 dielectric and aluminum as internal electrode was studied. The Bi_2Mo_2O_9 powders was calcined at 600oC for 4hrs. The calcined powders were vibratory milled for 24hrs to obtain fine powders for tape-casting use. To obtain fine slurry, the milled Bi_2Mo_2O_9 powders (56wt.%) were added into a solution of MEK (Methyl Ethyl Ketone, 19wt.%), ethanol (19wt.%), and PVB (Polyvinyl Butyral, 6wt.%) mixture and ball-milled for 24hrs. Tape casting was performed on a laboratory-type tape-casting machine with a doctor blade casting head, using 75 microns thick silicone coated mylar (polyethylene terephthalate) as a carrier film. The casting speed was set as 420 cm/min. The cast slurries were dried at room temperature without additional air flow. Aluminum electrode was screen-printed on the tape and laminated before firing. To minimize the warpage of the Bi_2Mo_2O_9-Aluminum MLCCs in this study, we applied an external force during the sintering course. When the internal pressure was too large, the local compressive stresses in MLCC samples could cause the cracks during sintering course. Only when the proper pressure was applied, the warpage could be successfully limited. Scanning electron microscoy, dielectric spectroscopy, dielectric temperature dependence and P-E loop were measured on pellet samples, MLCC samples and monolayer samples. There is no reaction or interdiffusion between electrode layer and ceramic layer. The relative permittivities of multilayer, monolayer, and monolithic Bi_2Mo_2O_9 samples all stabilize at around 39, and the dielectric losses are near 0.001 at 1MHz. Temperature dependence is similar for both monolayer and monolithic Bi_2Mo_2O_9 samples. Energy density of the monolayer Bi_2Mo_2O_9 sample reaches 0.75J/cm~3 at 67kV/mm with a thickness of 46μm. This study extends the application of the ultra-low temperature firing Bi_2Mo_2O_9 with Al electrodes.
考虑到Bi基氧化物陶瓷一般具有较低烧结温度和较高介电常数等优点,本论文紧紧围绕各类Bi基氧化物陶瓷,应用固相反应烧结的方法和高能球磨的方法,通过多种离子取代以及氧化物掺杂的方式,对Bi基氧化物陶瓷的烧结温度、微波介电性能、金属电极匹配性等方面展开了研究,并尝试在陶瓷基板天线和多层共烧电容器等领域进行了原型器件设计和制作,得到了一系列兼具理论和工程应用价值的结果:
本文的第一章主要从基础介质物理理论出发,首先介绍了介质中最基本的极化现象,然后进一步引申出了在微波频段下(300MHz~300GHz)电介质的介电常数、介电损耗以及温度系数的具体表征以及含义,为后续具体工作提供了有力的理论依据。接下来详细介绍了低温共烧陶瓷(LTCC)技术的发展状况,其中包括常用的导体材料以及介质材料两部分的发展状况。在第一章的结束部分阐述了本文的主要研究内容及其意义。
本文的第二章主要是对Bi_2O_3-Nb_2O_5二元体系微波介质陶瓷的研究。首先通过V5+、Cu~(2+)、W~(6+)、Ta~(5+)等离子取代的方式,应用固相反应烧结和高能球磨等制备方法,系统研究了BiNbO_4和Bi_3NbO_7配方的相形成以及降温改性,得到了介电常数介于36~45、Qf介于5000~20000GHz、谐振频率温度系数近零的BiNbO_4基陶瓷以及介电常数介于65~95、Qf介于230GHz~560GHz、TCF在-115~-70ppm/oC的Bi_3(Nb,Ta)O_7基陶瓷。首次研究了BiNbO_4陶瓷跟Cu电极的共烧问题,发现在N_2气氛下共烧后并没有发生反应或者渗透的情况,奠定了BiNbO_4陶瓷在LTCC中的应用基础;首次尝试使用低温烧结的BiNbO_4陶瓷作为基板,设计了二维天线阵列,HFSS软件仿真结果跟网络分析仪的实际测量结果基本符合,为高介基板在微波频段的应用做了初步探索。
本文的第三章主要研究了Bi(Sb_xNb_yTa_z)O_4(x+y+z=1)三元体系的相组成、相变以及微波介电性能等问题。首次系统地研究了Bi(Sb_xNb_yTa_z)O_4(x+y+z=1)三元体系的相组成以及相变问题。将Bi(Sb_xNb_yTa_z)O_4(x+y+z=1)三元体系分为:I-单斜固溶体区域(x>0.78);II-单斜、正交同存的区域(0.78>x>0.55);III-正交三斜相变区域(x<0.55)三个区域(相图不随x和y的取值而发生大的变化)。从晶格结构、晶胞参数的角度出发,较为详细地阐述了三元相图中各个相区转变的过程,重点研究了在正交、三斜相变区域中正交相到三斜相之间的相变问题。发现了高温三斜相β-BiNbO_4向低温正交相α-BiNbO_4相转变现象,并确定了β-BiNbO_4陶瓷不能够稳定存在的温度范围700oC~1020oC。但该结论并不适用于粉末样品。并且在这个三元体系中开发出了一系列具有潜在应用价值的微波介质陶瓷:1080oC烧结的纯单斜相的BiSbO_4陶瓷,介电常数εr≈19.3、Qf≈70000GHz、TCF≈-62ppm/oC,不跟Ag发生明显反应;掺杂0.6wt.% ~1.2wt.%B_2O_3-CuO后930oC烧结的单斜相的BiSbO_4陶瓷,介电常数εr≈19.5、Qf≈45400GHz~33700GHz、TCF≈-65ppm/oC;960oC烧结的Bi(Sb_(0.6)Ta_(0.4))O_4陶瓷,εr≈27、Qf≈35000GHz、TCF=-12ppm/oC;960oC烧结的Bi{Sb_(0.6)(Nb_(0.992)V_(0.008))_(0.4)}O_4陶瓷,εr≈34.7、Qf≈16000GHz、TCF=+16.1ppm/oC。
在本文的第四章中,开发并研究了Bi_2O_3-MoO_3二元体系超低温烧结微波介质陶瓷的烧结特性、微波介电性能、金属电极烧结匹配问题以及多层电容器具体应用问题。首先,从Bi_2O_3-MoO_3二元体系的相图出发,设计并制备了一系列的二元氧化物,发现在xBi_2O_3-(1-x)MoO_3中,随着x值从0.2增加到0.5,样品的成瓷温度几乎线性地从600oC增加到了750oC。当x=0.875时,其烧结温度稳定在820oC附近。整体来讲,富含MoO_3的区域比富含Bi2O3的区域具有更低的烧结温度。这个体系中有三个具有良好微波介电性能的配方组成:620oC烧结的Bi_2Mo_3O_(12)陶瓷,εr≈19、Qf≈21800GHz、TCF≈-215ppm/oC,跟Ag发生反应但是跟Al不发生反应;640oC烧结的Bi_2Mo_2O_9陶瓷,εr≈38、Qf≈12500GHz、TCF≈+31ppm/oC,跟Ag发生反应但是跟Al不发生反应;750oC烧结的Bi_2MoO_6陶瓷,εr≈31、Qf≈16700GHz、TCF≈-114ppm/oC。使用等价镧系离子La~(3+)和Nd~(3+)对Bi_2Mo_2O_9中的Bi3+进行取代,来调节其微波介电性能,尤其是TCF值,获得的(Bi0.8La0.2)2Mo2O9陶瓷具有近零的温度系数TCF≈-4.6ppm/oC,其介电常数εr≈32.7、Qf≈13490GHz、烧结温度为650oC。在第四章的最后一小节中,初次尝试制备了Bi_2Mo_2O_9基、Al做内电极的超低温烧结多层电容器MLCC,在645oC下成功烧结制备了Bi_2Mo_2O_9多层电容器(共六层,每层厚度约90μm,电极厚度约为12μm)以及单层电容器(层厚约50μm,电极厚度约为12μm),这开拓了Al电极在LTCC领域中的应用。
在本文的最后一章,总结了全文的重要结论并阐明了进一步的工作方向。
With the rapid development of mobile communication and satellite communication, microwave electronic devices are required to be developed and fabricated for miniaturization and integration. The low temperature co-fired ceramic technology (LTCC) becomes an important fabricating technology that can integrate the passive components within a monolithic bulk module with IC chips mounted on its surface. By this technology, microwave dielectrics are stacked in multilayers and co-fired with internal electrodes, such as Ag, Cu, Au, Al, their alloys etc, in special patterns to fulfill different electrical functions. The microwave dielectric materials used in LTCC field must have a high dielectric permittivity (εr>10), a high Qf value (f=resonant frequency, Q=1/dielectric loss at f, Qf>5000GHz), a near zero temperature coefficient of resonant frequency (TCF≈0ppm/oC), a low sintering temperature (below the melting points of common electrode metals, such as silver, copper, gold, aluminum etc. ) and chemical compatibility with the metal electrodes. Besides that, considering the environment and economic elements, people prefer to explore microwave dielectric ceramics with low price (not contain rare metal oxides) and without toxicity (at least lead free).
Bismuth-based dielectric ceramics are well-known as low-fired materials and have been investigated in multilayer capacitors application for many years. According to Shanno’ns study, Bi~(3+) has a polarizability of 6.12(?)~3, which could account for the high permittivities in many bismuth based oxides. In this thesis, a series of new bismuth-based oxides prepared by solid state reaction method and high energy ball milling method were explored. Ionic substitution and oxides addition methods were used to lower the sintering temperature, adjust the microwave dielectric properties and their chemical compatibility with metal electrodes. The application of antenna substrate using high permittivity dielectric and the fabrication of multilayers co-fired capacitor using bismuth based oxides were also tried. A series of scientific and engineering results were obtained as follows:
1. The influence of V~(5+), Cu~(2+), W~(6+) and Ta~(5+) substitution on the sintering temperature, microwave dielectric properties and phase composition of BiNbO_4 and Bi_3NbO_7 compositions in the Bi_2O_3-Nb_2O_5 binary system prepared by solid state reaction method and high energy ball milling method were studied. A series of BiNbO_4 ceramics sintered at 850~960oC withεr≈36~45, Qf≈5000~20000GHz and TCF≈0ppm/oC and Bi_3(Nb,Ta)O_7 ceramics sintered at 900~990oC withεr≈65~95, Qf≈230~560GHz and TCF≈-115~-70ppm/oC were obtained. The co-firing between BiNbO_4 ceramics and copper electrode under N_2 atmosphere was first studied. The SEM and EDS results showed that there was no reaction and diffusion between the ceramic and electrode. This makes it possible for BiNbO4 ceramics to be used in LTCC technology. A two element antennas with centre frequency at 3.07 GHz and bandwidth of 34MHz at -10 dB attenuation were obtained using a BiNbO4 ceramic substrate with size 34mm×34mm×1mm. The primary study of BiNbO_4 ceramic in antenna will broaden the application field for microwave ceramics with high permittivity.
2. Based on the analysis on a number of Bi(Sb_xNb_yTa_z)O_4 (x+y+z=1) samples, a pseudo-ternary phase diagram of Bi(Sb,Nb,Ta)O_4 system is given below the melting point. It is composed of a monoclinic-phase region (x≥0.78), an orthorhombic-phase region (x≤0.55) and a monoclinic-orthorhombic coexisting phase region (0.55≤x≤0.78). The phase transformation from the monoclinic to orthorhombic structure can be attributed to the decrease of space occupied by the bismuth layers, which is caused by the increase of octahedra volumes when the Nb or Ta amount increases. In orthorhombic phase region, as the sintering temperature increases, the phase transformation to triclinic structure is observed and it is seriously affected by the sintering temperature and the Sb amount in Bi(Sb,Nb,Ta)O_4. Phase transformation fromβ-BiNbO_4 toα-BiNbO_4 in BiNbO_4 bulk samples was first reported and studied. From X-ray diffraction patterns, the transformation fromβtoαphase of BiNbO_4 could be observed by heating the bulk samples ofβ-BiNbO_4 from low temperatures to 700~1030oC. But such a transformation didn’t occur in powder samples and in the cooling course. This phenomenon might be related with associated activation of stress and heat energy in the heating course. Differential thermal analysis, shrinkage and dielectric properties as a function of temperature were carried out and all the results confirmed the transformation fromβtoαphase of BiNbO4. In addition, a series of promising candidates for LTCC were explored in Bi(SbxNbyTaz)O4 system: 1, the BiSbO_4 ceramic sintered at 1080oC withεr≈19.3, Qf≈70000GHz, TCF≈-62ppm/oC and chemical compatibility with silver; 2, the 930oC sintered BiSbO4 ceramics with 0.6wt.% ~1.2wt.%B_2O_3-CuO addition withεr≈19.5, Qf≈45400GHz~33700GHz and TCF≈-65ppm/oC; 3, the 960oC sintered Bi(Sb0.6Ta0.4)O_4 ceramic withεr≈27, Qf≈35000GHz and TCF=-12ppm/oC; 4, the 960oC sintered Bi、O_4 ceramic withεr≈34.7, Qf≈16000GHz, and TCF=+16.1ppm/oC.
3. The preparation, phase composition, microwave dielectric properties and chemical compatibility with silver and aluminum electrodes were investigated on a series of single phase compounds in the Bi2O3-MoO3 binary system. All materials have ultra low sintering temperatures lower than 820oC. Eight different xBi2O3-(1-x)MoO3 compounds with x value between 0.2≤x≤0.875 were fabricated and the associated microwave dielectric properties were studied. Theβ~Bi_2Mo_2O_9 single phase has a positive temperature coefficient of resonant frequency (TCF) about +31ppm/oC, with a permittivityεr=38 and a Qf=12500GHz at 300K at a frequency of 6.3GHz. Theα~Bi_2Mo_3O_(12) andγ~Bi2MoO6 compounds both have negative temperature coefficient values of TCF~-215ppmo/C and TCF~-114ppm/oC, with permittivities ofεr=19 and 31, Qf=21800GHz and 16700 GHz at 300K measured at resonant frequencies of 7.6 GHz and 6.4 GHz, respectively. Through sintering the B2iO3-2.2MoO3 at 620oC for 2hrs a composite dielectric containing bothαandβphase can be obtained with a near zero temperature coefficient of frequency TCF=-13ppm/oC and a relative dielectric constantεr=35, and a large Qf~12000 GHz is also obtained. Owing to the frequent difficulty of thermochemical interactions between low sintering temperature materials and the electrode materials during the cofiring, preliminary investigations are made to determine any major interactions with possible candidate electrode metals, Ag and Al. The results show thatβ~Bi_2Mo_2O_9 andα~Bi_2Mo_3O_(12) do not react with Al at their sintering temperatures. La and Nd were also used to substitute for the Bi in Bi_2Mo_2O_9. For (Bi_(1-x)Ln_x)_2Mo_2O_9 (Ln=La, Nd) ceramics, as the x value increased, the optimal sintering temperature increased. Substitution of La or Nd could stabilize the monoclinic phase and modify its microwave dielectric properties. The best microwave dielectric properties were obtained in (Bi0.8La0.2)2Mo2O9 ceramic with a permittivity of 32.7, Qf value of 13,490GHz and temperature coefficient about -4.6ppm/oC. From the above results, the low sintering temperature, good microwave dielectric properties, chemical compatibility with Al metal electrode, nontoxicity and price advantage of the Bi2O3-MoO3 binary system, all indicate the potential for a new material system with ultra-low temperature cofirng for multilayer devices application.
4. Fabrication of a new kind multlayer co-fired capacitor using Bi_2Mo_2O_9 dielectric and aluminum as internal electrode was studied. The Bi_2Mo_2O_9 powders was calcined at 600oC for 4hrs. The calcined powders were vibratory milled for 24hrs to obtain fine powders for tape-casting use. To obtain fine slurry, the milled Bi_2Mo_2O_9 powders (56wt.%) were added into a solution of MEK (Methyl Ethyl Ketone, 19wt.%), ethanol (19wt.%), and PVB (Polyvinyl Butyral, 6wt.%) mixture and ball-milled for 24hrs. Tape casting was performed on a laboratory-type tape-casting machine with a doctor blade casting head, using 75 microns thick silicone coated mylar (polyethylene terephthalate) as a carrier film. The casting speed was set as 420 cm/min. The cast slurries were dried at room temperature without additional air flow. Aluminum electrode was screen-printed on the tape and laminated before firing. To minimize the warpage of the Bi_2Mo_2O_9-Aluminum MLCCs in this study, we applied an external force during the sintering course. When the internal pressure was too large, the local compressive stresses in MLCC samples could cause the cracks during sintering course. Only when the proper pressure was applied, the warpage could be successfully limited. Scanning electron microscoy, dielectric spectroscopy, dielectric temperature dependence and P-E loop were measured on pellet samples, MLCC samples and monolayer samples. There is no reaction or interdiffusion between electrode layer and ceramic layer. The relative permittivities of multilayer, monolayer, and monolithic Bi_2Mo_2O_9 samples all stabilize at around 39, and the dielectric losses are near 0.001 at 1MHz. Temperature dependence is similar for both monolayer and monolithic Bi_2Mo_2O_9 samples. Energy density of the monolayer Bi_2Mo_2O_9 sample reaches 0.75J/cm~3 at 67kV/mm with a thickness of 46μm. This study extends the application of the ultra-low temperature firing Bi_2Mo_2O_9 with Al electrodes.
引文
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