CN101798214A - (Na1/2Bi1/2) TiO3/BaTiO3 ceramic dielectric material and preparation of capacitor thereof - Google Patents
(Na1/2Bi1/2) TiO3/BaTiO3 ceramic dielectric material and preparation of capacitor thereof Download PDFInfo
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- CN101798214A CN101798214A CN 201010116326 CN201010116326A CN101798214A CN 101798214 A CN101798214 A CN 101798214A CN 201010116326 CN201010116326 CN 201010116326 CN 201010116326 A CN201010116326 A CN 201010116326A CN 101798214 A CN101798214 A CN 101798214A
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Abstract
The invention relates to a (Na1/2Bi1/2) TiO3/BaTiO3 ceramic dielectric material and a preparation of a capacitor thereof. The ceramic dielectric material contains the following components of BaCO3, SrCO3, Bi2O3, SnO2, TiO2, (Na1/2Bi1/2) TiO3, Y2O3, ZnO and MnO2, and the sum of the mole percents of the components is 100%. The method for preparing the capacitor by using the material comprises the following steps of synthesizing the (Na1/2Bi1/2) TiO3; preparing a pre-synthesizing material by using the BaCO3, the SrCO3, the Bi2O3, the SnO2 and the TiO2, (Na1/2Bi1/2) TiO3; preparing a dry grinding material by using the Y2O3, the ZnO, MnO2and the pre-synthesizing material; adding a polyvinyl alcohol solution in the dry grinding material, and then pelleting, screening, pressing and sintering and preparing a silver electrode to obtain the capacitor. The ceramic dielectric material has the characteristics of high dielectric constant, low dielectric loss and low temperature change rate of the dielectric constant. The prepared capacitor has good performance parameters.
Description
Technical field
The present invention relates to a kind of (Na
1/2Bi
1/2) TiO
3/ BaTiO
3The preparation method of ceramic medium material and electrical condenser thereof belongs to the technology of ceramic dielectric material and electrical condenser.
Background technology
Electrical condenser is a requisite electron device in the electronics.Electrical condenser commonly used is distinguished by medium paper dielectric capacitance, mica capacitor, ceramic condenser, chemical capacitor etc.Wherein to have a volume little for ceramic dielectric capacitor, good heat resistance, insulation resistance height, lower-price characteristic.Along with the development of electronic industry, ceramic dielectric capacitor is widely applied in electronics.Contain in traditional ceramics dielectric material, especially the mesohigh ceramic condenser lead element that endangering environment and HUMAN HEALTH [Peng Jiagen, Wang Feng equality. high voltage capacitor is with ferroelectric ceramic(s) [J]. electronic component and material, 2006,25 (12): 16-19].In recent years, the scientist of countries in the world all at the lead-free ceramics dielectric material of development superior performance replacing traditional leaded ceramic medium material, but poor-performing still can not reach the dielectric properties of leaded ceramic medium material, as existing SrTiO
3(tan δ) is little for the dielectric loss of base ceramic dielectric material, but specific inductivity (ε
r) also less [[1] Xiao Jun, Zhang Qilong etc. novel B ST base high voltage capacitor pottery [J]. electronic component and material, 2006,25 (11): p47-49; [2] Wei Chen, Xi Yao and Xiaoyong Wei.Tunability and ferroelectric relaxorproperties of bismuth strontium titanate ceramics[J] .APPLIED PHYSICSLETTERS 2007, (9) 0182902]; BaTiO
3Base ceramic dielectric material specific inductivity (ε
r) big, but the rate of temperature change of dielectric loss (tan δ) and specific inductivity (Δ ε/ε) greatly [Zhang Jilin, Mao Zuyou etc. ac high-voltage dielectric ceramic composition [J]. electronic component and material, 2002,21 (6): p1-3].Facing to bigger electronic product market, the research and development of lead-free ceramics dielectric material has bigger society and economic worth undoubtedly.
Summary of the invention
The purpose of this invention is to provide a kind of (Na
1/2Bi
1/2) TiO
3/ BaTiO
3The preparation method of ceramic medium material and electrical condenser thereof.This ceramic medium material is the lead-free ceramics dielectric material, its specific inductivity (ε
r) height, (tan δ) is low for dielectric loss, change in dielectric constant rate (Δ ε/ε) little.Prepare electrical condenser with this ceramic medium material, process is simple, and the capacitor performance that makes is good.
The present invention is realized by the following technical programs, a kind of (Na
1/2Bi
1/2) TiO
3/ BaTiO
3Ceramic medium material is characterized in that, this ceramic medium material is made up of following component and molecular fraction thereof, and the molecular fraction sum of each component is 100%:
(Na
1/2Bi
1/2)TiO
3：11.41～11.44％，
BaCO
3：29.71～29.79％，
SrCO
3：13.56～13.60％，
Bi
2O
3：0.1990～0.1995％，
SnO
2：0.4423～0.4435％，
TiO
2：43.77～43.89％，
Y
2O
3：0.0558～0.333％，
ZnO：0.2971～0.2979％，
MnO
2：0.2781～0.2789％。
Prepare the method for electrical condenser with above-mentioned ceramic medium material, it is characterized in that comprising following process:
1. with Bi
2O
3With Na
2CO
3And TiO
2According to mol ratio is to prepare burden at 1: 1: 4, by this batching: agate ball: the mass ratio of deionized water is to mix and place nylon ball grinder wet ball grinding 4～36h at 1: 1: 1.5, abrasive material is in 110～120 ℃ of oven dry of temperature then, oven dry material is warming up to 820 ℃～870 ℃ synthetic (Na of insulation 1～4h with the temperature rise rate of 250 ℃/h～400 ℃/h in crucible
1/2Bi
1/2) TiO
3
2. according to ceramic medium material prescription mole percentage amounts weighing BaCO
3, SrCO
3, Bi
2O
3, SnO
2, TiO
2With step 1 synthetic (Na
1/2Bi
1/2) TiO
3Prepare burden, by this batching: agate ball: the mass ratio of deionized water is to mix and place nylon ball grinder wet ball grinding 2～36h at 1: 1: 1.5, abrasive material is in 110 ℃～120 ℃ oven dry down of temperature then, oven dry material in crucible, with the temperature rise rate of 300 ℃/h～400 ℃/h be warming up to 1030 ℃～1100 ℃ down insulation 1～4h carry out the synthetic in advance pre-synthetic material that obtains;
3. according to ceramic medium material prescription mole percentage amounts weighing Y
2O
3, ZnO, MnO
2Prepare burden with the pre-synthetic material of step 2 synthetic, by this batching: agate ball: the mass ratio of deionized water is to mix and place nylon ball grinder wet ball grinding 4～24h at 1: 1: 2, then 110～120 ℃ of temperature dry the dry grinding material;
4. get the dry grinding material that step 3 makes, by 5～8% of dry grinding material quality, in dry grinding material, add mass concentration and be 5% polyvinyl alcohol water solution tackiness agent, carry out granulation after mixing, the granulation material is by 40 mesh sieve branches, get particulate material and on shaper, suppress type in blocks with 150～300MPa, matrix band is placed on the aluminum oxide backing plate that the titanium dioxide zirconium powder is bedding and padding, separate with the titanium dioxide zirconium powder between two matrix bands, put into high-temperature electric resistance furnace then, the control heat-up rate is at 350～450 ℃/h, be warming up to 1250 ℃～1350 ℃ following sintering 1～4h, wherein at 150 ℃, respectively be incubated 10～30min when 250 ℃ and 350 ℃, sample furnace cooling behind the sintering arrives room temperature, after the zirconium dioxide bedding and padding removing of burning till on the ceramics, and even silver coating electrode slurry on ceramics two planes, prepare silver electrode at 830～870 ℃ of following burning infiltration 8～20min, obtain the lead-free ceramic capacitance device.
The BaTiO that is provided is provided outstanding advantage of the present invention
3Stupalith has the lower characteristics of rate of temperature change of high dielectric constant, low dielectric loss, specific inductivity.With the electrical condenser of this lead-free ceramics material preparation, specific inductivity (ε
r) be: 2330～2960, dielectric loss (tan δ) is: the rate of temperature change of 1.02%～1.40% ,-25 ℃～85 ℃ of temperature range specific inductivity (Δ ε/ε) be :-5.23%～-9.66%.
Embodiment
According to (Na
1/2Bi
1/2) TiO
3The needed Na of stoichiometric ratio weighing
2CO
3, Bi
2O
3And TiO
2Material, with batching: agate ball: the mass ratio of deionized water=1: 1: 1.5 places nylon ball grinder wet ball grinding 4h with batching, the ball milling material is dried under 110 ℃ of conditions of temperature, to dry material then and put into the alumina-ceramic crucible, the temperature rise rate with 300 ℃/h in electric furnace synthesizes Na at 850 ℃ of insulation 2h
1/2Bi
1/2TiO
3According to mole percentage amounts prescription 29.72mol%BaCO
3, 13.57mol%SrCO
3, 0.1991mol%Bi
2O
3, 0.4425mol%SnO
2, 43.80mol%TiO
2Na with 11.42mol%
1/2Bi
1/2TiO
3Carry out weigh batching, then with this batching: agate ball: the mass ratio of deionized water=1: 1: 1.5 places nylon ball grinder wet ball grinding 4h with batching.The ball milling material is dried under 110 ℃ of conditions.To dry material again and put into the alumina-ceramic crucible, and in electric furnace,, be warming up to 1080 ℃ of insulation 2h and carry out synthetic in advance with the temperature rise rate of 300 ℃/h.To allocate 0.2783mol%Y into according to mole percentage amounts prescription in the above-mentioned pre-synthetic material
2O
3, 0.2972mol%ZnO, 0.2782mol%MnO
2Carry out weigh batching, with batching: agate ball: the mass ratio of deionized water=1: 1: 2 places nylon ball grinder wet ball grinding 6h with batching, and the ball milling material is dried under 110 ℃ of conditions.With mass percent be 5～8%, concentration is that 5% polyvinyl alcohol water solution is that tackiness agent joins in this oven dry batching and mixes, and carries out granulation, the granulation material is by 40 mesh sieves.On shaper with pressure 170MPa with the compression moulding of granulation material
The shaped blank sheet of 15mm * 2mm.Sample after the moulding is placed on the aluminum oxide backing plate that the titanium dioxide zirconium powder is bedding and padding, separate with the titanium dioxide zirconium powder between matrix band and sheet, put into high-temperature electric resistance furnace then, 300 ℃/h of control heat-up rate, insulation 2h burns till when 1320 ℃ of temperature, wherein respectively be incubated 20min when 350 ℃ of 150 ℃ of temperature, 250 ℃ of temperature and temperature, the sample furnace cooling is to room temperature then.After the zirconium dioxide bedding and padding removing of burning till on the ceramics, even silver coating electrode slurry on ceramics two planes, burning infiltration 15min prepares silver electrode under 850 ℃ of conditions of temperature, makes lead-free ceramic capacitance device of the present invention.The performance of the lead-free ceramics dielectric material of making is: specific inductivity (ε
r): 2960, dielectric loss (tan δ): change in dielectric constant rate in 1.05% ,-25 ℃～85 ℃ temperature ranges (Δ ε/ε) :-9.19%.
Claims (2)
1. (Na
1/2Bi
1/2) TiO
3/ BaTiO
3Ceramic medium material is characterized in that, this ceramic medium material is made up of following component and molecular fraction thereof, and the molecular fraction sum of each component is 100%:
Na
1/2Bi
1/2TiO
3：11.41～11.44％，
BaCO
3：29.71～29.79％，
SrCO
3：13.56～13.60％，
Bi
2O
3：0.1990～0.1995％，
SnO
2：0.4423～0.4435％，
TiO
2：43.77～43.89％，
Y
2O
3：0.0558～0.333％，
ZnO：0.2971～0.2979％，
MnO
2：0.2781～0.2789％。
2. one kind with the described (Na of claim 1
1/2Bi
1/2) TiO
3/ BaTiO
3Ceramic medium material prepares the method for electrical condenser, it is characterized in that comprising following process:
1) with Bi
2O
3With Na
2CO
3And TiO
2According to mol ratio is to prepare burden at 1: 1: 4, by this batching: agate ball: the mass ratio of deionized water is to mix and place nylon ball grinder wet ball grinding 4～36h at 1: 1: 1.5, abrasive material is in 110～120 ℃ of oven dry of temperature then, oven dry material is warming up to 820 ℃～870 ℃ synthetic (Na of insulation 1～4h with the temperature rise rate of 250 ℃/h～400 ℃/h in crucible
1/2Bi
1/2) TiO
3
2) press ceramic medium material prescription mole percentage amounts weighing BaCO
3, SrCO
3, Bi
2O
3, SnO
2, TiO
2With step 1) synthetic (Na
1/2Bi
1/2) TiO
3Prepare burden, by this batching: agate ball: the mass ratio of deionized water is to mix and place nylon ball grinder wet ball grinding 2～36h at 1: 1: 1.5, abrasive material is in 110 ℃～120 ℃ oven dry down of temperature then, oven dry material in crucible, with the temperature rise rate of 300 ℃/h～400 ℃/h be warming up to 1030 ℃～1100 ℃ down insulation 1～4h carry out the synthetic in advance pre-synthetic material that obtains;
3) press ceramic medium material prescription mole percentage amounts weighing Y
2O
3, ZnO, MnO
2With step 2) the pre-synthetic material of synthetic prepares burden, by this batching: agate ball: the mass ratio of deionized water is to mix and place nylon ball grinder wet ball grinding 4～24h at 1: 1: 2, then 110～120 ℃ of temperature dry the dry grinding material;
4) get the dry grinding material that step 3) makes, by 5～8% of dry grinding material quality, in dry grinding material, add mass concentration and be 5% polyvinyl alcohol water solution tackiness agent, carry out granulation after mixing, the granulation material is by 40 mesh sieve branches, get particulate material and on shaper, suppress type in blocks with pressure 150～300MPa, matrix band is placed on the aluminum oxide backing plate that the titanium dioxide zirconium powder is bedding and padding, separate with the titanium dioxide zirconium powder between two matrix bands, put into high-temperature electric resistance furnace then, the control heat-up rate is at 350～450 ℃/h, be warming up to 1250 ℃～1350 ℃ following sintering 1～4h, wherein 150 ℃ of temperature, respectively be incubated 10～30min when 350 ℃ of 250 ℃ of temperature and temperature, sample furnace cooling behind the sintering arrives room temperature, after the zirconium dioxide bedding and padding removing of burning till on the ceramics, and even silver coating electrode slurry on ceramics two planes, 830～870 ℃ of following burning infiltration 8～20min prepare silver electrode in temperature, obtain the lead-free ceramic capacitance device.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010116326 CN101798214A (en) | 2010-03-03 | 2010-03-03 | (Na1/2Bi1/2) TiO3/BaTiO3 ceramic dielectric material and preparation of capacitor thereof |
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|---|---|---|---|
| CN 201010116326 CN101798214A (en) | 2010-03-03 | 2010-03-03 | (Na1/2Bi1/2) TiO3/BaTiO3 ceramic dielectric material and preparation of capacitor thereof |
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|---|---|
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|---|---|---|---|
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110254901A1 (en) * | 2010-04-14 | 2011-10-20 | Seiko Epson Corporation | Liquid ejecting head, liquid ejecting apparatus |
| CN103342556A (en) * | 2013-06-24 | 2013-10-09 | 湖北大学 | Preparation method of two-phase low-temperature co-sintered temperature stable dielectric ceramic material |
| CN103864418A (en) * | 2014-02-27 | 2014-06-18 | 天津大学 | Preparation method of ceramic capacitor dielectric with high dielectric constant and ultra-wide working temperature |
| CN105294101A (en) * | 2014-06-03 | 2016-02-03 | 上海帛汉新材料科技有限公司 | Dielectric material for high temperature stable type ceramic capacitor, and preparation method therefor and application thereof |
| CN108975912A (en) * | 2018-09-20 | 2018-12-11 | 歌尔股份有限公司 | Ternary system potassium niobate sodium-based leadless piezoelectric ceramic and preparation method thereof |
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2010
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110254901A1 (en) * | 2010-04-14 | 2011-10-20 | Seiko Epson Corporation | Liquid ejecting head, liquid ejecting apparatus |
| US8636342B2 (en) * | 2010-04-14 | 2014-01-28 | Seiko Epson Corporation | Piezoelectric device, liquid ejecting head, liquid ejecting apparatus, ultrasonic device sensor, and timing device |
| CN103342556A (en) * | 2013-06-24 | 2013-10-09 | 湖北大学 | Preparation method of two-phase low-temperature co-sintered temperature stable dielectric ceramic material |
| CN103342556B (en) * | 2013-06-24 | 2014-12-03 | 湖北大学 | Preparation method of two-phase low-temperature co-sintered temperature stable dielectric ceramic material |
| CN103864418A (en) * | 2014-02-27 | 2014-06-18 | 天津大学 | Preparation method of ceramic capacitor dielectric with high dielectric constant and ultra-wide working temperature |
| CN103864418B (en) * | 2014-02-27 | 2015-10-07 | 天津大学 | The preparation method of the ceramic capacitor dielectric of high-k ultra-wide working temperature |
| CN105294101A (en) * | 2014-06-03 | 2016-02-03 | 上海帛汉新材料科技有限公司 | Dielectric material for high temperature stable type ceramic capacitor, and preparation method therefor and application thereof |
| CN108975912A (en) * | 2018-09-20 | 2018-12-11 | 歌尔股份有限公司 | Ternary system potassium niobate sodium-based leadless piezoelectric ceramic and preparation method thereof |
| CN108975912B (en) * | 2018-09-20 | 2021-05-18 | 歌尔光学科技有限公司 | Ternary potassium sodium niobate based leadless piezoelectric ceramic and preparation method thereof |
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Application publication date: 20100811 |