CN100358837C - Low temp, sintered bismuth base microwave medium ceramic material and preparation process thereof - Google Patents

Low temp, sintered bismuth base microwave medium ceramic material and preparation process thereof Download PDF

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CN100358837C
CN100358837C CNB2005100963344A CN200510096334A CN100358837C CN 100358837 C CN100358837 C CN 100358837C CN B2005100963344 A CNB2005100963344 A CN B2005100963344A CN 200510096334 A CN200510096334 A CN 200510096334A CN 100358837 C CN100358837 C CN 100358837C
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low
microwave
temperature
dielectric
sintered
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CN1793035A (en
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汪宏
周迪
张磊
姚熹
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Xian Jiaotong University
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Xian Jiaotong University
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Abstract

The present invention discloses a low-temperature sintered bismuth group microwave dielectric ceramic materials. On the basis of a bismuth niobate ceramic system, a dielectric ceramic material system using low-temperature normal alpha bismuth niobate phases as main crystal phases is formed by the replacement of a proper quantity of ions by a crystal chemistry principle. The structure expression of the materials is Bi(Nb<1-x>Vx)O4, wherein x is from 0.001 to 0.064. A small number of Nb<5+> ions in a B position are replaced by V<5+> ions, the traditional solid reaction synthesis technology is adopted, and the sintering temperature is from 810 to 980 DEG C. The low-temperature sintered bismuth base microwave dielectric ceramic materials of the present invention have the advantages of low sintering temperature, moderate dielectric constant, low dielectric loss, wide coverage area of dielectric constants and temperature coefficients, large insulation resistance, good microwave performance, low frequency temperature coefficient and simple chemical composition and preparing technology, can be sintered in reducing atmospheres such as air or nitrogen, and can be fired along with a silver electrode or a copper electrode. The present invention can be used for manufacturing microwave devices such as low-temperature cofired ceramic systems (LTCC), multi-layer dielectric resonators, microwave antennae, filters, etc.

Description

A kind of low temp, sintered bismuth base microwave medium ceramic material and preparation thereof
Technical field
The invention belongs to electronic ceramics and manufacturing field thereof, particularly a kind of bismuth base microwave medium ceramic material of agglomerating at low temperatures and preparation thereof.
Background technology
Along with the development of mobile communication, facility communication system has been proposed portable requirement, it is integrated that machine system moves towards, in the hope of obtaining small volume, light weight, high reliability, product cheaply.In the integrated process of microwave circuit, the appearance of metal wave-guide and microwave tube makes microwave circuit obtain to a certain degree integrated and miniaturization, but what a used heavy fat person's metal resonator cavity made microstrip circuit traditionally integratedly becomes a difficulty, with microwave-medium ceramics (microwave dielectric ceramics, MWDC) make resonator an outlet but is provided for this reason, microwave-medium ceramics has high-k (10＜ε r＜90), low-loss (tan δ＜3 * 10 -4), the little (10＜τ of frequency-temperature coefficient f＜10ppm/ ℃) etc. characteristics, therefore be widely used in the making of microwave device.
Various microwave devices based on dielectric resonator, be used widely in practice, but along with mobile communication striding forward to higher frequency, depend merely on the minimizing of tank circuit and can not satisfy the requirement of further microminiaturization of mobile communication terminal and portability, and new outlet has been opened up in passive integrated appearance for this reason.
The common burning temperature of LTCC system (LTCC) is generally between 800 ℃～950 ℃.Because sintering temperature is low, the low metal of available resistivity is as the conductor material of multilayer wiring, can improve packing density, signaling rate, and can in bury various laminar microwave electronic devices with the multilager base plate once-firing, therefore extensively be used in high-speed and high-density and interconnect among the polynary ceramic component (MCM).Because burning technology has the packing density height altogether, dielectric loss is low, can be used for high microwave frequency band, characteristics such as monolithic structure high reliability and IC heat match, therefore extremely wide application prospect is arranged, wherein first-elected again LTCC technology because it not only sintering temperature is low, but also be to adopt the metal electrode Au of high conductivity, Ag, Cu etc., wiring good conductivity, and with the Cu electrode time, cost also can be very low.
Therefore in microwave device research, can just obtain broad research, comprise the sheet medium resonator, wave filter, microwave-medium antenna and chip capacitor etc. with the chip multilayer microwave device that this multilayer circuit technology adapts.The sintering temperature of general microwave ceramics is mostly more than 1000 ℃, therefore and be not suitable for the LTCC technology with and the lowpriced metallization requirement, so microwave material system just very meaningful of R and D with sintering temperature and low.
Usually the method that reduces the sintering temperature of microwave dielectric material has, and adds oxide compound or low melting glass sintering aid, introduce chemical synthesis process, and superfine powder is made raw material etc.But when adding sintering aid, though can reduce sintering temperature, but the dielectric properties of reduction microwave dielectric material that all can be in various degree, the complex technical process then when synthetic with chemical process, manufacturing cost and cycle can rise, even and having adopted aforesaid method for present mostly microwave-medium system, its sintering temperature is high too and be difficult to meet the sintering process requirement that LTCC is lower than 1000 ℃.Therefore seek just very important of medium system that raw material itself has a sintering temperature and low, and Bi 2O 3-Nb 2O 5The so just individual system of system, the present invention is exactly the microwave dielectric ceramic materials of the low-temperature sintering high performance developed in this material system.
In sum, along with the fast development of microwave mobile communication, to the portability of microwave device, microminiaturization has proposed new requirement.Microwave dielectric resonator with the manufacturing of high-dielectric constant microwave material can reduce the microwave circuit size greatly, but further microminiaturized outlet is the development of MCM.When making MCM and use Mulitilayer circuit board, the LTCC technology demonstrates peculiar advantage, so has just obtained paying attention to widely and studying with multilayered medium device and material that the LTCC technology adapts.Exploitation be applicable to LTCC technology, microwave property excellence, can with silver or copper electrode altogether the simple novel microwave dielectric ceramic material of burning, chemical constitution and preparation technology be the novel material that a class has application prospect.
Summary of the invention
The objective of the invention is to, provide a kind of sintering at low temperatures to can be applicable to the high-performance low-temperature sintered bismuth base microwave medium ceramic material of LTCC.
An object of the present invention is to provide a kind of low temp, sintered bismuth base microwave medium ceramic material, the relative permittivity behind its sintering between 36～48, low dielectric loss (tan δ＜5 * 10 -4), big insulation resistance (ρ v〉=10 13Ω cm), and good microwave property (Qf=10000～25000GHz), low temperature coefficient of resonance frequency (τ f=0～+ 20ppm/ ℃), the adjustable (α of temperature factor ε=0ppm/ ℃～+ 500ppm/ ℃), except these performances, it can (810 ℃～980 ℃) carry out sintering under very low relatively temperature, can burning, chemical constitution and preparation technology are simple altogether with silver or copper electrode.
Another object of the present invention provides the preparation method of above-mentioned low temp, sintered bismuth base microwave medium ceramic material.
The present invention is by the existing low-temperature sintering dielectric ceramics Bi of the method improvement of ionic replacement 2O 3-Nb 2O 5Material system, widen its sintering range, its specific inductivity is along with the variation of replacement amount changes between 36～48, and measures to reduce significantly when higher in replacement and burnt junction temperature (minimum can sinter porcelain at 810 ℃), make it to adapt to the needs of LTCC technology, enlarge its range of application.
To achieve these goals, technical scheme of the present invention is, a kind of low temp, sintered bismuth base microwave medium ceramic material is characterized in that, the structure expression of this material is: Bi (Nb 1-xV x) O 4, in the formula: 0.001≤x≤0.064.
Realize the preparation method of above-mentioned low temp, sintered bismuth base microwave medium ceramic material, it is characterized in that, carry out according to the following steps:
1) with chemical feedstocks Bi 2O 3, V 2O 5, Nb 2O 5By prescription Formula B i (Nb 1-xV x) O 4Preparation, wherein 0.001≤x≤0.064;
2) chemical feedstocks after will preparing mixes, and puts into nylon jar ball milling 4 hours, and thorough mixing is levigate, takes out oven dry, is pressed into bulk after sieving;
3) Ya Zhi bulk is through 700 ℃～750 ℃ pre-burnings, and insulation 3h～4h, can obtain sample and burn piece;
4) will burn the pulverizing of piece sample, and carry out 4～5 hours secondary ball milling, thorough mixing is levigate, oven dry, granulation then, and granulation obtains required porcelain after 70 orders and 120 eye mesh screen bilayers sieve;
5) with porcelain compression moulding on demand, become porcelain at 810 ℃～980 ℃ following sintering 2～4h, can obtain low temp, sintered bismuth base microwave medium ceramic material.
Low temp, sintered bismuth base microwave medium ceramic material of the present invention has following characteristics: specific inductivity moderate (ε=36～48), little (tan δ＜3 * 10 of dielectric loss -4), the wide (α of temperature coefficient of permittivity coverage ε=0ppm/ ℃～+ 500ppm/ ℃), sintering temperature low (810 ℃～980 ℃), the big (ρ of insulation resistance v〉=10 13Ω cm), good (Qf=10000～25000GHz), the low (τ of temperature coefficient of resonance frequency of microwave property f=0ppm/ ℃～+ 20ppm ℃), can burning, chemical constitution and preparation technology be simple altogether with silver or copper electrode.
Embodiment
The present invention is further illustrated below in conjunction with specific embodiment that the contriver provides.
According to technical scheme of the present invention, the structure expression of low temperature sintered high frequency dielectric ceramic material of the present invention is: Bi (Nb 1-xV x) O 4, (0.001≤x≤0.064).
The concrete preparation process of low temperature sintered high frequency dielectric ceramic material of the present invention is: with chemical feedstocks Bi 2O 3, V 2O 5, Nb 2O 5By prescription Formula B i (Nb 1-xV x) O 4After the preparation, thorough mixing ball milling 4 hours, dry after levigate, sieve, then through 700 ℃～750 ℃ pre-burnings, and be incubated 3～4 hours, carry out secondary ball milling, granulation after the levigate oven dry after then the bulk sample after the pre-burning being pulverized, use 70 orders and 120 purpose screen cloth bilayers to sieve, can obtain required porcelain.As required after the compression moulding, sinter porcelain into porcelain at 810 ℃～980 ℃ then, can obtain low temp, sintered bismuth base microwave medium ceramic material.
Low temp, sintered bismuth base microwave medium ceramic material of the present invention is owing to comprised Bi 2O 3, V 2O 5, Nb 2O 5Deng composition, make that this media ceramic matrix material of sintering becomes possibility at low temperatures.
The present invention is relevant with dielectric medium theoretical according to the crystal chemistry principle, and the method that adopts ionic replacement is to existing Bi 2O 3-Nb 2O 5The base pottery improves.Use positively charged ion V 5+Small part replaces Bi 2O 3-Nb 2O 5In Nb 5+, Bi before and after research summary goes out to replace 2O 3-Nb 2O 5The rule relation that base ceramic structure and low frequency microwave frequency band dielectric properties change, sintering has gone out fine and close pottery in 810 ℃～980 ℃ temperature range, and the dielectric material that can be used as radio frequency laminated ceramic capacitor, chip microwave dielectric resonator or wave filter, LTCC system (LTCC), ceramic antenna etc. uses.
Be the embodiment that the contriver provides below.
Embodiment 1:
With chemical feedstocks Bi 2O 3, V 2O 5, Nb 2O 5By filling a prescription: Bi (Nb 1-xV x) O 4, x=0.002 wherein.After the preparation, thorough mixing ball milling 4 hours, the oven dry of levigate back is sieved, pre-burning is 3～4 hours under 700 ℃～750 ℃ air or nitrogen atmosphere, will burn piece then and pulverize back secondary ball milling, granulation again after the levigate oven dry, sieve with 70 orders and 120 eye mesh screen bilayers again, can obtain required porcelain.After porcelain compression moulding as required (sheet or column), under 950 ℃～980 ℃ air or nitrogen, sinter porcelain into then, can obtain low temp, sintered bismuth base microwave medium ceramic material.
The performance of this group stupalith reaches following index:
Sintered sample performance under the air: temperature coefficient of permittivity α ε=0～200ppm/ ℃ (under the 1MHz), DIELECTRIC CONSTANT=48 (under the 1MHz), dielectric loss tan δ=1 * 10 -4Dielectric properties ε under (under the 1MHz), microwave=39 (5.97GHz), quality factor q=2017, Qf＞12000GHz (f=3～6GHz), microwave frequency temperature factor τ f=+6ppm/oC (25 ℃～85 ℃).
Sintered sample performance under the nitrogen: DIELECTRIC CONSTANT=39 (5.09GHz), the quality factor q under the microwave=1980, Qf＞10000GHz (f=3～6GHz), microwave frequency temperature factor τ f=+8ppm/oC (25 ℃～85 ℃).
Embodiment 2:
With chemical feedstocks Bi 2O 3, V 2O 5, Nb 2O 5By filling a prescription: Bi (Nb 1-xV x) O 4, x=0.032 wherein.After the preparation, thorough mixing ball milling 4 hours, the oven dry of levigate back is sieved, pre-burning is 3～4 hours under 700 ℃～750 ℃ air atmospheres, will burn then that piece is pulverized after secondary ball milling, the oven dry granulation of levigate back, sieve with 70 orders and 120 eye mesh screen bilayers again, can obtain required porcelain.After porcelain compression moulding as required (sheet or column), under 830 ℃～890 ℃ air atmospheres, sinter porcelain into then, can obtain low temp, sintered bismuth base microwave medium ceramic material.
The performance of this group stupalith reaches following index:
Temperature coefficient of permittivity α ε=0～200ppm/ ℃ (under the 1MHz), DIELECTRIC CONSTANT=46.1 (under the 1MHz), dielectric loss tan δ=2 * 10 -4Dielectric properties ε under (under the 1MHz), microwave=44.39 (4.76GHz), quality factor q=2283, Qf＞10800GHz (f=3～6GHz), microwave frequency temperature factor τ 1=+11ppm/oC (25 ℃～85 ℃).
Embodiment 3:
With chemical feedstocks Bi 2O 3, V 2O 5, Nb 2O 5By filling a prescription: Bi (Nb 1-xV x) O 4, x=0.064 wherein.After the preparation, thorough mixing ball milling 4 hours, the oven dry of levigate back is sieved, pre-burning is 3～4 hours under 700 ℃～750 ℃ air atmospheres, will burn piece then and pulverize back secondary ball milling, granulation again after the levigate oven dry, sieve with 70 orders and 120 eye mesh screen bilayers again, can obtain required porcelain.After porcelain compression moulding as required (sheet or column), under 790 ℃～850 ℃ air atmospheres, sinter porcelain into then, can obtain low temp, sintered bismuth base microwave medium ceramic material.
The performance of this group stupalith reaches following index:
Temperature coefficient of permittivity α ε=0～200ppm/ ℃ (under the 1MHz), DIELECTRIC CONSTANT=47.5 (under the 1MHz), dielectric loss tan δ=2 * 10 -3Dielectric properties ε under (under the 1MHz), microwave=38.05 (5.12GHz), quality factor q=1971, Qf＞10000 (f=3～6GHz), microwave frequency temperature factor τ f=+16ppm/ ℃ (25 ℃～85 ℃).
It is pointed out that according to technical scheme of the present invention, the foregoing description can also be enumerated many, prove,, all can reach purpose of the present invention in the scope that claims of the present invention proposed according to applicant's lot of experiment results.

Claims (2)

1. a low temp, sintered bismuth base microwave medium ceramic material is characterized in that, the structure expression of this material is: Bi (Nb 1-xV x) O 4, in the formula: 0.001≤x≤0.064.
2. realize the preparation method of the described low temp, sintered bismuth base microwave medium ceramic material of claim 1, it is characterized in that, carry out according to the following steps:
1) with chemical feedstocks Bi 2O 3, V 2O 5, Nb 2O 5By prescription Formula B i (Nb 1-xV x) O 4Preparation, wherein 0.001≤x≤0.064;
2) chemical feedstocks after will preparing mixes, and puts into nylon jar ball milling 4 hours, and thorough mixing is levigate, takes out oven dry, is pressed into bulk after sieving;
3) Ya Zhi bulk is through 700 ℃～750 ℃ pre-burnings, and insulation 3h～4h, can obtain sample and burn piece;
4) will burn the pulverizing of piece sample, and carry out 4～5 hours secondary ball milling, thorough mixing is levigate, oven dry, granulation then, and granulation obtains required porcelain after 70 orders and 120 eye mesh screen bilayers sieve;
5) with porcelain compression moulding on demand, become porcelain at 810 ℃～980 ℃ following sintering 2～4h, can obtain low temp, sintered bismuth base microwave medium ceramic material.
CNB2005100963344A 2005-11-10 2005-11-10 Low temp, sintered bismuth base microwave medium ceramic material and preparation process thereof Expired - Fee Related CN100358837C (en)

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CN101462874B (en) * 2008-11-28 2012-05-23 西安交通大学 Low-temperature sintered medium-dielectric-constant microwave dielectric ceramic material and preparation method thereof
CN101531511B (en) * 2009-04-11 2011-11-09 桂林工学院 High thermal stability microwave dielectric ceramic material sintered at low temperature and preparation method thereof
CN101538158B (en) * 2009-04-11 2011-11-09 桂林工学院 Preparation method of composite niobate microwave dielectric ceramic material sintered at low temperature
CN101632935B (en) * 2009-07-19 2012-01-04 桂林理工大学 Compound oxide photocatalyst Bi4V(2-x)AxO(11-3x/2) and preparation method thereof
CN102718473B (en) * 2012-06-06 2013-11-06 西安交通大学 Bismuth-base microwave dielectric ceramic sintered at low temperature and preparation method thereof
CN102775144B (en) * 2012-07-18 2014-10-15 电子科技大学 BCZN microwave ceramic medium material and preparation method thereof
CN103145419B (en) * 2013-04-01 2014-07-02 桂林理工大学 Microwave dielectric ceramic Li3VO4 capable of being sintered at low temperature and preparation method thereof
CN103467092A (en) * 2013-08-27 2013-12-25 西安工业大学 Temperature stabilization type low-temperature sintering LTCC (low-temperature co-fired ceramic) microwave dielectric ceramic material as well as preparation method and application thereof
CN103539449B (en) * 2013-10-07 2015-11-25 桂林理工大学 Low temperature sintering microwave dielectric ceramic BiNbW 2o 10and preparation method thereof
CN104177085A (en) * 2014-08-27 2014-12-03 西安交通大学 Molybdenum-based temperature-stable microwave medium ceramic and preparation method thereof
CN106349756A (en) * 2016-08-27 2017-01-25 湖南汉瑞新材料科技有限公司 Yellow inorganic pigment taking bismuth and vanadium as basic adulterants as well as preparation method and application thereof
CN110156455B (en) * 2019-07-04 2021-10-26 贵州振华电子信息产业技术研究有限公司 Bismuth oxide-niobium oxide based LTCC substrate material and preparation method thereof

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