CN102531592B - Reduction-resistant Y5P ceramic capacitor dielectric porcelain - Google Patents
Reduction-resistant Y5P ceramic capacitor dielectric porcelain Download PDFInfo
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- CN102531592B CN102531592B CN201110355871.1A CN201110355871A CN102531592B CN 102531592 B CN102531592 B CN 102531592B CN 201110355871 A CN201110355871 A CN 201110355871A CN 102531592 B CN102531592 B CN 102531592B
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Abstract
The invention relates to a reduction-resistant ceramic dielectric material and a preparation method thereof. Ba1-xZnxTi1-yZryO3 (wherein x is more than or equal to 0.001 and less than or equal to 0.10 and y is more than or equal to 0.005 and less than or equal to 0.10) which is synthesized by a solid state reaction is taken as a main crystal phase material which accounts for 88 to 98 mass percent of the dielectric material; and three or more than three of CaO, MgO, Y2O3, Nb2O5, MnO2, SiO2, Al2O3 and R2O3 (R refers to at least one of Eu, Ho, Dy and Yb), which serve as modifiers, are added into the main crystal phase material, wherein the modifiers accounts for 2 to 12 mass percent of the dielectric material. Therefore, the ceramic dielectric material with Y5P temperature characteristic and capable of being sintered in reducing atmosphere is obtained.
Description
Technical field
The present invention relates to a kind of anti-reduction ceramic dielectric material and preparation method thereof, be specifically related to ceramic medium material of a kind of Y5P temperature characterisitic and preparation method thereof, further relate to a kind of manufacture method of ceramic dielectric capacitor.
Background technology
Along with developing rapidly of electronics and information industry, the application of ceramic dielectric capacitor is more and more wider.One class be take ceramic medium material that barium titanate has Y5P temperature characterisitic as base with advantages such as its high-k, low dielectric loss, high-temperature stabilities, has had the larger market demand; Meanwhile, such traditional ceramic medium material, owing to not having resistance to reduction, can only carry out sintering in air atmosphere, while being made into layered ceramic electric capacity, must do extraction electrode with noble silver or silver alloy.At present, because the price of precious metal material silver is higher, the cost of the material of ceramic capacitor is remained high.In the face of the market competition that is growing more intense, each manufacturer is for development better, all reduces production costs seeking various ways; In this case, with relatively inexpensive metallic copper or copper alloy, as electrode, by increasing producer, paid attention to, the more important thing is that this alternative energy is significantly declined the material cost of ceramic condenser; But then, while applying as electrode with copper or copper alloy slurry, must in reducing atmosphere, carry out fired electrodes; And in reducing atmosphere during fired electrodes, the ceramic medium material of traditional coupling noble metal can reduce, cause the electrical property degradation phenomena such as insulation resistance decline, loss tangent rising of electric capacity, therefore, while selecting copper or copper alloy as electrode, require ceramic medium material used must there is resistance to reduction, to guarantee that corresponding electric capacity product still has good dielectric property in reducing atmosphere after high-temperature process.
Summary of the invention
Object of the present invention, is that a kind of anti-reduction ceramic dielectric material and preparation method thereof will be provided, and it adopts the synthetic single compd B a of solid phase method
1-xzn
xti
1-yzr
yo
3as principal crystalline phase composition; The ceramic medium material providing has good dispersiveness, uniformity and technology stability; During for the preparation of monolithic ceramic capacitor, can be with copper or copper alloy as extraction electrode, and there are good dielectric property.
The present invention is achieved in that described a kind of anti-reduction ceramic dielectric material, it is characterized in that: principal crystalline phase composition and property-modifying additive, consist of; With the synthetic Ba of solid phase method
1-xzn
xti
1-yzr
yo
3(wherein 0.001≤x≤0.10,0.005≤y≤0.10) as principal crystalline phase composition, principal crystalline phase composition by mass percentage in the composition of dielectric material shared umber be 88～98%; Property-modifying additive is selected from CaO, MgO, Y
2o
3, Nb
2o
5, MnO
2, SiO
2, Al
2o
3, R
2o
3in (R is at least one in Eu, Ho, Dy, Yb) more than three kinds or three kinds; Various oxides in property-modifying additive shared mass percent in described dielectric material is: 0.1～5% CaO, 0～3% MgO, 0～2% Y
2o
3, 0～1% Nb
2o
5, 0～0.6% MnO
2, 0.1～2% SiO
2, 0～1.5% Al
2o
3, 0.1～2.5% R
2o
3; Property-modifying additive by mass percentage in the composition of dielectric material shared umber be 2～12%.
The preparation method of a kind of anti-reduction ceramic dielectric material of the present invention, is characterized in that: described principal crystalline phase composition Ba
1-xzn
xti
1-yzr
yo
3the acquisition of (wherein 0.001≤x≤0.10,0.005≤y≤0.10) is BaCO
3, ZnO, TiO
2and ZrO
2be placed in ball mill, in mass ratio for material: deionized water=1: the ratio of (1.0～2.0) adds deionized water to carry out wet ball grinding to mix, then be dried, pulverize to obtain powder mixture, then the temperature range calcining 1～4 hour of 1100 ℃～1250 ℃ is synthetic in high temperature resistance furnace; With together with above-mentioned property-modifying additive, amount by formula Design is weighed respectively, be placed in ball mill, it is material in mass ratio: deionized water=1: the ratio of (0.8～1.5) adds deionized water to carry out wet ball grinding, then the good material of ball milling is dried, obtains anti-reduction ceramic dielectric material of the present invention.
Anti-reduction ceramic dielectric material of the present invention has more than at least 3000 dielectric constants; The temperature range that is adapted in reducing atmosphere 1150 ℃～1300 ℃ is carried out sintering, can coated copper or copper alloy slurry as outside extraction electrode, the temperature range of 800 ℃～950 ℃, carry out fired electrodes; To make the capacitor of ceramic dielectric.
The invention has the beneficial effects as follows, prepared ceramic dielectric powder has good dispersiveness, uniformity, wider technique accommodation; During for the preparation of ceramic capacitor, can be in reducing atmosphere sintering; Can use copper or copper alloy as outside extraction electrode, and ceramic capacitor have good dielectric property; Compare the noble silver of current use or the similar capacitor product that silver alloy is done extraction electrode, can reduce significantly the material cost of product, highlight the market competition advantage of product.
Embodiment
A kind of anti-reduction ceramic dielectric material of the present invention, is comprised of principal crystalline phase composition and property-modifying additive; With the synthetic Ba of solid phase method
1-xzn
xti
1-yzr
yo
3(wherein 0.001≤x≤0.10,0.005≤y≤0.10) as principal crystalline phase composition, principal crystalline phase composition by mass percentage in the composition of dielectric material shared umber be 88～98%; ; Property-modifying additive is selected from CaO, MgO, Y
2o
3, Nb
2o
5, MnO
2, SiO
2, Al
2o
3, R
2o
3in (R is at least one in Eu, Ho, Dy, Yb) more than three kinds or three kinds; Various oxides in property-modifying additive shared mass percent in described dielectric material is: 0.1～5% CaO, 0～3% MgO, 0～2% Y
2o
3, 0～1% Nb
2o
5, 0～0.6% MnO
2, 0.1～2% SiO
2, 0～1.5% Al
2o
3, 0.1～2% R
2o
3; ; Property-modifying additive by mass percentage in the composition of dielectric material shared umber be 2～12%.
The preparation method of a kind of anti-reduction ceramic dielectric material of the present invention, described principal crystalline phase composition Ba
1-xzn
xti
1-yzr
yo
3the acquisition of (wherein 0.001≤x≤0.10,0.005≤y≤0.10) is BaCO
3, ZnO, TiO
2and ZrO
2be placed in ball mill, in mass ratio for material: deionized water=1: the ratio of (1.0～2.0) adds deionized water to carry out wet ball grinding to mix, then the slurry mixing is dried, pulverizes to obtain powder mixture, in high temperature resistance furnace, the temperature range of 1100 ℃～1250 ℃ calcining is synthesized for 1～4 hour again, obtains Ba
1-xzn
xti
1-yzr
yo
3powder; With together with above-mentioned property-modifying additive, requirement by formula Design is weighed respectively, be placed in ball mill, it is material in mass ratio: deionized water=1: the ratio of (0.8～1.5) adds deionized water to carry out wet ball grinding, requirement mixing of materials is even, and reach the powder granularity of designing requirement, preferably make powder average particle size particle size after ball milling lower than 1.5 microns.Slurry after ball milling is dried, obtains ceramic medium material powder of the present invention.
Ceramic medium material of the present invention can be in reducing atmosphere the temperature range of 1150 ℃～1300 ℃ realize sintering, room temperature dielectric constant is 3000～4000, capacitance temperature characterisitic reaches the requirement of Y5P.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described, but the present invention is not limited to these embodiment.
Embodiment
(1) at principal crystalline phase composition Ba of the present invention
1-xzn
xti
1-yzr
yo
3in (wherein 0.001≤x≤0.10,0.005≤y≤0.10), according to mass percent, weigh BaCO
3, ZnO, TiO
2and ZrO
2prepare burden, by the proportion of composing of table 1, mix and be placed in ball mill, add in mass ratio equal deionized water, mixing and ball milling 12 hours, then dries slurry, pulverizes, and is placed in high temperature resistance furnace and sets 4 hours synthetic Ba of 1200 ℃ of insulations
1-xzn
xti
1-yzr
yo
3powder.
(2) with CaO, MgO, Y
2o
3, Nb
2o
5, MnO
2, SiO
2, Al
2o
3, R
2o
3(R is at least one in Eu, Ho, Dy, Yb) is raw material, press the proportion of composing of table 1, mix and be placed in ball mill, add the deionized water of equal portions to carry out wet ball grinding, slurry particle size distribution after ball milling meets after designing requirement, slurry is dried with drying equipment, pulverize, finally obtain ceramic medium material powder of the present invention.
(3) prepare the process of capacitor sample:
Get the ceramic medium material powder obtaining in (2), add in mass ratio 10% PVA based adhesive to carry out granulation, dry-pressing formed, obtain disc-shaped green compact; This green compact exemplar be placed in can controlled atmospher high temperature furnace, by N
2, H
2and H
2in the mixed atmosphere that O forms, with the heating rates of 100 ℃/h, from normal temperature, be raised to 500 ℃ of insulations 5 hours, with the adhesive composition in burn off exemplar, then with the heating rate of 150 ℃/h, be warming up to high temperature (1150 ℃～1300 ℃) insulation and carry out sintering in 3 hours, obtain the potsherd for ceramic capacitor dielectric; This potsherd is carried out to surface cleaning and process rear surface uniform coated copper or copper alloy slurry toward two opposition, then in nitrogen atmosphere stove, be warming up to 850 ℃ of insulations and within 20 minutes, carry out fired electrodes, obtain the ceramic capacitor sample the present invention relates to.
To carrying out electric performance test with the ceramic capacitor sample that said method obtains, the results are shown in Table 2.
The composition of table 1 embodiment of the present invention
The respective electrical the performance test results of table 2 embodiment of the present invention
Claims (3)
1. a ceramic medium material with resistance to reduction, is characterized in that: comprise that mass percent is the Ba of 88～98 %
1-xzn
xti
1-yzr
yo
3, 0.001≤x≤0.10 wherein, 0.005≤y≤0.10 and 2～12% modifier, described modifier comprises that mass percent is the CaO of 0.1～5 %, the MgO of 0～3 %, the Y of 0～2 %
2o
3, the Nb of 0～1 %
2o
5, the MnO of 0～0.6 %
2, the SiO of 0.1～2 %
2, 0～1.5% Al
2o
3, 0.2～2.5% R
2o
3, R is at least one in Eu, Ho, Dy, Yb; Wherein, principal crystalline phase composition Ba
1-xzn
xti
1-yzr
yo
3acquisition be: BaCO
3, ZnO, TiO
2and ZrO
2be placed in ball mill, in mass ratio for material: ratio deionized water=1:(1.0～2.0) add deionized water to carry out ball milling to mix, then the slip mixing is dried, in high temperature resistance furnace, the temperature range of 1100 ℃～1250 ℃ calcining is 1～4 hour, obtains described principal crystalline phase composition; The mode that adds of described modifier is: according to formula Design, various oxides are added respectively or be pre-mixed evenly after add again, by mass percentage by the Ba of 88～98 %
1-xzn
xti
1-yzr
yo
3mixing and be placed in ball mill with 2～12% modifier, is material in mass ratio: ratio deionized water=1:(0.8～1.5) add deionized water carry out wet-mixed evenly, ultra-fine grinding, dry, there is the ceramic medium material of resistance to reduction described in acquisition.
2. a preparation method with the ceramic medium material of resistance to reduction, is characterized in that:
1) preparation of principal crystalline phase composition:
Described principal crystalline phase composition Ba
1-xzn
xti
1-yzr
yo
3acquisition, 0.001≤x≤0.10 wherein, 0.005≤y≤0.10, is BaCO
3, ZnO, TiO
2and ZrO
2be placed in ball mill, in mass ratio for material: ratio deionized water=1:(1.0～2.0) add deionized water to carry out ball milling to mix, then the slip mixing is dried, in high temperature resistance furnace, the temperature range of 1100 ℃～1250 ℃ calcining is 1～4 hour, obtains described principal crystalline phase composition;
2) in principal crystalline phase composition, add modifier:
The mode that adds of described modifier is, according to formula Design, various oxides are added respectively or be pre-mixed evenly after add again, this oxide and formula Design specifically: mass percent is the CaO of 0.1～5 %, the MgO of 0～3 %, the Y of 0～2 %
2o
3, the Nb of 0～1 %
2o
5, the MnO of 0～0.6 %
2, the SiO of 0.1～2 %
2, 0～1.5% Al
2o
3, 0.2～2.5% R
2o
3, R is at least one in Eu, Ho, Dy, Yb, by mass percentage by the Ba of 88～98 %
1-xzn
xti
1-yzr
yo
3mixing and be placed in ball mill with 2～12% modifier, is material in mass ratio: ratio deionized water=1:(0.8～1.5) add deionized water carry out wet-mixed evenly, ultra-fine grinding, dry, there is the ceramic medium material of resistance to reduction described in acquisition.
3. a kind of preparation method with the ceramic medium material of resistance to reduction according to claim 2, it is characterized in that: described in there is resistance to reduction ceramic medium material make ceramic capacitor green compact, can be in reducing atmosphere the temperature range of 1150 ℃～1300 ℃ carry out sintering, be then incubated 2～5 hours; Ceramic dielectric after sintering has more than 3000 dielectric constants, and temperature characterisitic meets the requirement of Y5P in EIA standard.
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| CN201110355871.1A CN102531592B (en) | 2011-11-10 | 2011-11-10 | Reduction-resistant Y5P ceramic capacitor dielectric porcelain |
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| CN201110355871.1A CN102531592B (en) | 2011-11-10 | 2011-11-10 | Reduction-resistant Y5P ceramic capacitor dielectric porcelain |
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| CN102531592B true CN102531592B (en) | 2014-10-29 |
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| CN114394832B (en) * | 2022-01-19 | 2022-11-29 | 江苏科技大学 | Barium zirconate titanate based porcelain with stable dielectric temperature and preparation method thereof |
| CN114591079B (en) * | 2022-03-11 | 2023-04-28 | 汕头市瑞升电子有限公司 | High-voltage low-loss ceramic capacitor medium and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1635592A (en) * | 2003-12-29 | 2005-07-06 | 广东风华高新科技集团有限公司 | High dielectric and reduction resistant ceramic material and prepared ceramic capacitor |
| CN101492293A (en) * | 2009-03-09 | 2009-07-29 | 陕西科技大学 | Barium titanate based Y5P ceramic dielectric material and method of producing the same |
| CN101654360A (en) * | 2008-08-19 | 2010-02-24 | 达方电子股份有限公司 | Ceramic powder composition, ceramic material and multilayer ceramic capacitor made thereby |
| CN102030526A (en) * | 2010-11-11 | 2011-04-27 | 厦门松元电子有限公司 | Anti-reduction ceramic dielectric material and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1635592A (en) * | 2003-12-29 | 2005-07-06 | 广东风华高新科技集团有限公司 | High dielectric and reduction resistant ceramic material and prepared ceramic capacitor |
| CN101654360A (en) * | 2008-08-19 | 2010-02-24 | 达方电子股份有限公司 | Ceramic powder composition, ceramic material and multilayer ceramic capacitor made thereby |
| CN101492293A (en) * | 2009-03-09 | 2009-07-29 | 陕西科技大学 | Barium titanate based Y5P ceramic dielectric material and method of producing the same |
| CN102030526A (en) * | 2010-11-11 | 2011-04-27 | 厦门松元电子有限公司 | Anti-reduction ceramic dielectric material and preparation method thereof |
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Denomination of invention: Reduction-resistant Y5P ceramic capacitor dielectric porcelain Effective date of registration: 20170302 Granted publication date: 20141029 Pledgee: Jimei Xiamen District Finance Company limited by guarantee Pledgor: Xiamen Wanming Electronics Co.,Ltd. Registration number: 2017990000148 |
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Date of cancellation: 20190129 Granted publication date: 20141029 Pledgee: Jimei Xiamen District Finance Company limited by guarantee Pledgor: Xiamen Wanming Electronics Co.,Ltd. Registration number: 2017990000148 |