CN101172849B - Low-temperature sintering high dielectric constant dielectric ceramic and method for producing the same - Google Patents

Low-temperature sintering high dielectric constant dielectric ceramic and method for producing the same Download PDF

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CN101172849B
CN101172849B CN200710031091A CN200710031091A CN101172849B CN 101172849 B CN101172849 B CN 101172849B CN 200710031091 A CN200710031091 A CN 200710031091A CN 200710031091 A CN200710031091 A CN 200710031091A CN 101172849 B CN101172849 B CN 101172849B
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dielectric constant
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srtio
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CN101172849A (en
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胡星
凌志远
何新华
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South China University of Technology SCUT
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Abstract

The invention discloses high dielectric constant dielectric medium ceramic sintered with low temperature and the preparation method thereof. The ceramic contains the components in weight percent as follows: CaTiSio5 of 53 to 81 percent, SrTiO3 of 5 to 34 percent, CaTiO3 of 0 to 36 percent, Bi2Ti3O9 of 0 to 2 percent, Bi2O3 of 0 to 2 percent, Nb2O5 of 0 to 0.5 percent, and glass component of 2 to 10 percent. The method comprises the steps as follows: mixing the raw material with planet ball grinder, drying, producing the wafers with the diameter being 10 to 20mm and the thickness being 2 to 3mmthrough the pressing of the single axis after adding the caking agent to produce the granule, and sintering for 3 hours under the atmosphere ambience of 880 to 1000 DEG C. The ceramic not contains lanthanon, and has cheap price and high dielectric constant compared with small dielectric constant temperature coefficient, therefore, the invention can be used in high frequency stable ceramic capacitors or temperature compensating ceramic capacitors, etc.

Description

A kind of low sintering high dielectric constant dielectric ceramic and preparation method thereof
Technical field
The present invention relates to a kind of low sintering high dielectric constant pottery and preparation method thereof, be used to make various high frequency capacitor devices.
Background technology
In recent years, along with electronics and IT products miniaturization day by day, little power consumptionization and installation densification, electronic devices and components constantly develop towards " thin; light, short, little; low cost " direction, and corresponding, the high-frequency high-permittivity ceramic condenser of cost degradation need be greatly developed.
High-k high frequency temperature-stable dielectric ceramics commonly used at present mainly contains BaO-Ln 2O 3-TiO 2, lead base composite perofskite, CaO-Li 2O-Ln 2O 3-TiO 2Series (Ln is that rare earth unit belongs to) etc.Because society is to the demand of environmental protection, the lead base material should not adopt.Other two kinds of materials all contain a large amount of rare earth elements, do not meet the low-cost requirement of developing material.
Summary of the invention
The objective of the invention is to overcome the shortcoming of prior art, a kind of rare earth element that do not contain is provided, have high-k and smaller temperature coefficient of permittivity dielectric ceramics.
Another purpose of the present invention is to provide the preparation method of above-mentioned dielectric ceramics.
Purpose of the present invention is achieved through the following technical solutions:
A kind of low sintering high dielectric constant dielectric ceramic, its recipe ingredient are CaTiSiO 5SrTiO 3CaTiO 3Bi 2Ti 3O 9, Bi 2O 3, Nb 2O 5And glass ingredient, in this pottery total weight percent, CaTiSiO 5Account for 53%～81%, SrTiO 3Account for 5%～34%, CaTiO 3Account for 0%～36%, Bi 2Ti 3O 9Account for 0%～2%, Bi 2O 3Account for 0～2%, Nb 2O 5Account for 0～0.5%, glass ingredient accounts for 2%～10%.
This ceramic specific inductivity is 53-98, and dielectric loss is less than 4 * 10 under the 1MHz -4, temperature coefficient of permittivity is-566～447ppm/ ℃.Specific inductivity that particularly should pottery can be 69, and temperature coefficient of permittivity is-28ppm/ ℃.
The preparation method of low sintering high dielectric constant dielectric ceramic: with CaTiSiO 5, SrTiO 3, CaTiO 3, Bi 2Ti 3O 9Account for this pottery total weight percent batch mixes by it, add the Bi that accounts for this pottery gross weight 0-2wt% simultaneously 2O 3, 0-0.5wt% Nb 2O 5And the glass ingredient of 2wt%-10wt%, carry out 1 hour planetary ball mill, powder after again oven dry being sieved after the granulation of adding binding agent, pressurizes by single shaft, prepare diameter 10-20mm, the disk of thickness 2-3mm, at last at 880-1000 ℃, sintering preparation in 3 hours media ceramic under the air atmosphere.
Described planetary ball mill is a ball milling in ball grinder, and wherein ball grinder is a tetrafluoroethylene, and ball-milling medium is a 1mm zirconium dioxide bead, and solvent is deionized water, wherein ball: powder: water=1: 1: 1-4.
Described CaTiSiO 5, SrTiO 3, CaTiO 3, Bi 2Ti 3O 9Be to be CaCO more than 99% with purity 3, TiO 2, SiO 2, Bi 2O 3, SrCO 3Press CaTiSiO respectively 5, SrTiO 3, CaTiO 3, Bi 2Ti 3O 9The molecular formula batch mixes, planetary ball mill 1 hour, after the oven dry, pre-burning made in 3 hours in 850 ℃ of-1100 ℃ of air respectively.
Described glass ingredient is for comprising oxide compound ZnO, B 2O 3, Zn/B=0.25～1 wherein.
Described binding agent is preferably paraffin.
Have following advantage and beneficial effect with respect to prior art the present invention:
(1) traditional dielectric materials is as TiO 2, SrTiO 3And CaTiO 3Have high-k and high quality factor, but bigger negative temperature coefficient of permittivity is arranged.The present invention is with CaTiSiO 5With SrTiO 3Or CaTiO 3Compound high-k and the smaller temperature coefficient of permittivity dielectric ceramics of obtaining.Its specific inductivity is 53-98, and dielectric loss is less than 4 * 10 under the 1MHz -4, temperature coefficient of permittivity is-566～447ppm/ ℃
(2) the present invention is with CaTiSiO 5With SrTiO 3Or CaTiO 3Compound with glassy phase, 1000 the degree or below carry out low-temperature sintering, developing low-cost frequency applications high-k multi-layer ceramic capacitor material.
(3) low-temperature sintering high dielectric ceramic provided by the invention does not contain expensive rare earth unit and belongs to, even only comprises the Bi of trace 2O 3Or Nb 2O 5, the prices of raw and semifnished materials are cheap, can be widely used in high frequency thermo-compensation capacitor or temperature-stable electrical condenser.
Embodiment
The present invention is described further below in conjunction with drawings and Examples, but protection scope of the present invention is not limited to the scope that embodiment represents.
Embodiment 1～8
With purity is CaCO more than 99% 3, TiO 2, SiO 2Press CaTiSiO 5The molecular formula batch mixes, planetary ball mill 1 hour (solvent is a deionized water, and rotating speed is 400 rev/mins), 1050 ℃ of pre-burnings 3 hours under atmospheric environment respectively after the oven dry.Planetary ball mill is a ball milling in ball grinder, and wherein ball grinder is a tetrafluoroethylene, and ball-milling medium is a 1mm zirconium dioxide bead, and solvent is deionized water, wherein ball: powder: water=1: 1: 4.
With purity is SrCO more than 99% 3, TiO 2Press SrTiO 3The molecular formula batch mixes, planetary ball mill 1 hour (solvent is a deionized water, and rotating speed is 400 rev/mins) is pressed SrTiO respectively after the oven dry 31100 ℃ of pre-burnings are 3 hours under atmospheric environment.Planetary ball mill is a ball milling in ball grinder, and wherein ball grinder is a tetrafluoroethylene, and ball-milling medium is a 1mm zirconium dioxide bead, and solvent is deionized water, wherein ball: powder: water=1: 1: 1.
With purity is CaCO more than 99% 3, TiO 2Press CaTiO 3The molecular formula batch mixes, planetary ball mill 1 hour (solvent is a deionized water, and rotating speed is 400 rev/mins), the 1100 ℃ of pre-burnings 3 hours under atmospheric environment of oven dry back.Planetary ball mill is a ball milling in ball grinder, and wherein ball grinder is a tetrafluoroethylene, and ball-milling medium is a 1mm zirconium dioxide bead, and solvent is deionized water, wherein ball: powder: water=1: 1: 2.
Press the listed weight ratio of table 1, preparation main component expression formula is mCaTiSiO 5NSrTiO 3PCaTiO 3Media ceramic, m, n and p represent CaTiSiO respectively in the formula 5, SrTiO 3And CaTiO 3Weight percent in media ceramic also comprises the Bi of t% weight in addition 2O 3, and the glass ingredient of 3wt%, wherein glass ingredient Zn: B: O=1: 4: 7, the value of m, n, p and t saw Table 1 among each embodiment.Press the listed part by weight of table 1 with CaTiSiO 5With SrTiO 3, CaTiO 3, Bi 2O 3Mix, add glass ingredient simultaneously, (solvent is a deionized water to carry out 1 hour planetary ball mill, rotating speed is 400 rev/mins), the powder after oven dry sieved, add the paraffin granulation after, pressurize by single shaft, prepare diameter 20mm, the disk of thickness 3mm, sintering prepared needed media ceramic in 3 hours under 950 ℃ of atmospheric environments at last.
Sample electrode was a fine silver, adopts typography, 650 ℃ of heating 15 minutes.Agilent4288A is adopted in the test of sintered ceramic dielectric properties, frequency 1MHz, and-55 ℃～+ 125 ℃ temperature ranges are obtained by GZ-ESPEC710P type environmental test chamber.Ceramic systems loss of the present invention is all less than 4 * 10 -4, specific inductivity and its temperature factor see Table 1.Ceramic systems of the present invention has obtained temperature factor seriation pottery, can be used for high frequency and stablizes ceramic condenser or temperature compensating ceramic capacit etc.And the raw materials used not containing rare earth of the present invention unit belongs to, and is cheap, again can low-temperature sintering, industrial great value arranged.
Table 1
Embodiment 9～12
With purity is CaCO more than 99% 3, TiO 2, SiO 2Press CaTiSiO 5The molecular formula batch mixes, planetary ball mill 1 hour (solvent is a deionized water, and rotating speed is 400 rev/mins), 1050 ℃ of pre-burnings 3 hours under atmospheric environment respectively after the oven dry.Planetary ball mill is a ball milling in ball grinder, and wherein ball grinder is a tetrafluoroethylene, and ball-milling medium is a 1mm zirconium dioxide bead, and solvent is deionized water, wherein ball: powder: water=1: 1: 3.
With purity is SrCO more than 99% 3, TiO 2Press SrTiO 3The molecular formula batch mixes, planetary ball mill 1 hour (solvent is a deionized water, and rotating speed is 400 rev/mins) is pressed SrTiO respectively after the oven dry 31100 ℃ of pre-burnings are 3 hours under atmospheric environment.
With purity is Bi more than 99% 2O 3, TiO 2Press Bi 2Ti 3O 9The molecular formula batch mixes, planetary ball mill 1 hour (solvent is a deionized water, and rotating speed is 400 rev/mins), the 850 ℃ of pre-burnings 3 hours under atmospheric environment of oven dry back.
Press the listed weight ratio of table 2, preparation main component expression formula is mCaTiSiO 5NSrTiO 3QBi 2Ti 3O 9Media ceramic, m, n and q represent CaTiSiO respectively in the formula 5, SrTiO 3And Bi 2Ti 3O 9Weight percent in media ceramic also comprises the Nb of s% in addition 2O 5, and the glass ingredient of 3wt%, wherein glass ingredient Zn: B: O=2: 2: 5.Press the listed part by weight of table 2 with CaTiSiO 5With SrTiO 3, Bi 2Ti 3O 9, Nb 2O 5Mix, add glass ingredient simultaneously, (solvent is a deionized water to carry out 1 hour planetary ball mill, rotating speed is 400 rev/mins), the powder after oven dry sieved, add the paraffin granulation after, pressurize by single shaft, prepare diameter 10mm, the disk of thickness 2mm, sintering prepared needed media ceramic in 3 hours under 950 ℃ of atmospheric environments at last.
Sample electrode was a fine silver, adopts typography, 650 ℃ of heating 15 minutes.Agilent4288A is adopted in the test of sintered ceramic dielectric properties, frequency 1MHz, and-55 ℃～+ 125 ℃ temperature ranges are obtained by GZ-ESPEC710P type environmental test chamber.Ceramic systems loss of the present invention is all less than 4 * 10 -4, specific inductivity and its temperature factor see Table 2.The dielectric properties of optimizing are on embodiment 12, and specific inductivity is 69, and temperature coefficient of permittivity is-28ppm/ ℃.
Table 2

Claims (4)

1. the preparation method of a low sintering high dielectric constant dielectric ceramic is characterized in that, with CaTiSiO 5, SrTiO 3, CaTiO 3, Bi 2Ti 3O 9Account for this pottery total weight percent batch mixes by it, add the Bi that accounts for this pottery gross weight 0-2wt% simultaneously 2O 3, 0-0.5wt% Nb 2O 5And the glass ingredient of 2wt%-10wt%, carry out 1 hour planetary ball mill, powder after again oven dry being sieved after the granulation of adding binding agent, pressurizes by single shaft, prepare diameter 10-20mm, the disk of thickness 2-3mm, at last at 880-1000 ℃, sintering preparation in 3 hours media ceramic under the air atmosphere;
This ceramic feed composition is CaTiSiO 5, SrTiO 3, CaTiO 3, Bi 2Ti 3O 9, Bi 2O 3, Nb 2O 5And glass ingredient; In this pottery total weight percent, CaTiSiO 5Account for 61%～81%, SrTiO 3Account for 16%～34%, CaTiO 3Account for 0%～11%, Bi 2Ti 3O 9Account for 0%～2%, Bi 2O 3Account for 0～2%, Nb 2O 5Account for 0～0.5%, glass ingredient accounts for 2%～10%;
Described glass ingredient is for comprising oxide compound ZnO and B 2O 3Glass ingredient.
2. the preparation method of low sintering high dielectric constant dielectric ceramic according to claim 1 is characterized in that, described CaTiSiO 5, SrTiO 3, CaTiO 3, Bi 2Ti 3O 9Be to be CaCO more than 99% with purity 3, TiO 2, SiO 2, Bi 2O 3, SrCO 3Press CaTiSiO respectively 5, SrTiO 3, CaTiO 3, Bi 2Ti 3O 9The molecular formula batch mixes, planetary ball mill 1 hour, after the oven dry, pre-burning made in 3 hours in 850 ℃ of-1100 ℃ of air respectively.
3. the preparation method of low sintering high dielectric constant dielectric ceramic according to claim 1 is characterized in that, described glass ingredient is for comprising oxide compound ZnO, B 2O 3, Zn/B=0.25～1 wherein.
4. the preparation method of low sintering high dielectric constant dielectric ceramic according to claim 1 is characterized in that, described binding agent is a paraffin.
CN200710031091A 2007-10-26 2007-10-26 Low-temperature sintering high dielectric constant dielectric ceramic and method for producing the same Expired - Fee Related CN101172849B (en)

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CN102627456B (en) * 2012-04-23 2014-06-25 江苏大学 Low-loss high-voltage ceramic capacitor dielectric
CN103274685A (en) * 2013-06-14 2013-09-04 龚建良 Dielectric ceramic and preparation method thereof
JP2016160133A (en) * 2015-03-02 2016-09-05 Tdk株式会社 Dielectric composition and electronic component
JP2016199446A (en) * 2015-04-14 2016-12-01 Tdk株式会社 Dielectric composition and electronic component
CN106892656A (en) * 2017-03-31 2017-06-27 天津大学 A kind of low temperature sintering high-dielectric constant capacitor dielectric material
CN109231977B (en) * 2018-11-02 2021-01-12 中国科学院上海硅酸盐研究所 High-temperature stable dielectric ceramic material and preparation method thereof
CN111925187A (en) * 2020-07-03 2020-11-13 成都宏科电子科技有限公司 Lead-free high-pressure medium-temperature sintered strontium bismuth titanium-based dielectric material and preparation method thereof
CN111943668B (en) * 2020-07-03 2022-09-13 成都宏科电子科技有限公司 Medium-temperature sintered high-dielectric low-loss negative temperature compensation type porcelain and preparation method thereof
CN115259677B (en) * 2022-06-15 2023-07-28 深圳顺络电子股份有限公司 Ultralow-temperature sintered low-dielectric high-heat-conductivity LTCC dielectric material and preparation method thereof

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