CN102101775B - Low-loss high-voltage ceramic capacitor dielectric - Google Patents
Low-loss high-voltage ceramic capacitor dielectric Download PDFInfo
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Abstract
The invention relates to a low-loss high-voltage ceramic capacitor dielectric which is characterized by comprising the following raw materials in percentage by weight: 58-91% of BaTiO3, 1-3% of SrTiO3, 4-20% of BaZrO3, 3-12% of CaZrO3, 0.03-1.0% of CeO2, 0.1-1.5% of ZnO and 0.5-4.5% of Bi2TiO5. The low-loss high-voltage ceramic capacitor dielectric provided by the invention has the advantages of high voltage resistance, low dielectric loss and no environment pollution in the preparation and use process, can lower the cost of the ceramic capacitor, and is suitable for preparing single-chip ceramic capacitors and multilayer chip ceramic capacitors.
Description
Technical field
The present invention relates to the dielectric medium of electrical condenser, specifically, relate to a kind of low-loss high-voltage ceramic condenser medium.
Background technology
The fields such as colour TV, computer, communication, aerospace, guided missile, navigation are in the urgent need to the ceramic condenser of high-performance (high such as voltage breakdown, temperature stability is good, reliability is high, miniaturization, capacity be large).In order to obtain high performance ceramic condenser, require the dielectric medium of ceramic condenser to have the characteristics such as loss is low, proof voltage is high; Simultaneously; along with the pay attention to day by day of people to healthy and environment protection; the dielectric medium that requires ceramic condenser preparation, use and discarded process in can not work the mischief to human body and environment, thereby require the dielectric medium of ceramic condenser not leaded, the metallic element such as cadmium.
At present, be generally used for producing in the dielectric medium of high voltage ceramic capacitor and contain a certain amount of lead, this not only the production of ceramic condenser, use and discarded process in human body and environment are worked the mischief, and the stability of ceramic condenser is also had detrimentally affect.For example, Chinese periodical " Jiangsu pottery " the 2nd phase in 1999 is at " BaTiO
3Be the high Jie X7R of easy fired capacitor ceramics " a kind of BaTiO is disclosed in the literary composition
3High Jie of middle easy fired satisfied the capacitor ceramics medium of X7R characteristic, and the contained low melting glass material of this medium is the lead borosilicate low melting glass, and medium is leaded, and does not relate to proof voltage, and dielectric loss is higher.And for example, Chinese periodical " Nanjing University of Chemical Technology's journal " the 4th phase in 1999 is at " SrTiO
3The composition and performance of based high-pressure porcelain capacitor material " a kind of capacitor ceramic dielectric of low consumption and high pressure resisting is disclosed in the literary composition, but this medium contains the lead titanate about 18mol%, and understanding in preparation and use procedure have pollution to environment and human body.And for example, (denomination of invention is " high Jie's high-performance medium temp. sintered chip multilayer ceramic capacitor porcelain " to Chinese invention patent application prospectus CN1212443A, number of patent application is 97117286.2), although disclosed ceramic condenser porcelain specific inductivity high (specific inductivity 〉=16000), but proof voltage relatively poor (proof voltage is 700V/mm), its component contains a certain amount of lead in addition.Also have, (denomination of invention is " high-performance medium temp. sintered chip multilayer ceramic capacitor porcelain " to Chinese invention patent application prospectus CN1212444A, number of patent application is 97117287.0), disclosed capacitor ceramics specific inductivity too little (specific inductivity is 3000), dielectric loss is higher, and proof voltage lower (proof voltage is 860V/mm), its component contains a certain amount of lead in addition.
Although the dielectric medium of some ceramic condenser is not leaded, the production of ceramic condenser, use and discarded process in less to the harm of human body and environment, its specific inductivity is too little, and/or proof voltage is lower.For example, Chinese periodical " electronic component and material " the 5th phase in 1989 is at " high Jie's high pressure 2B
4Media ceramic " a kind of high-voltage ceramic condenser medium material is disclosed in the literary composition; and this dielectric material is not leaded; but the too little (DIELECTRIC CONSTANT ε=2500-2600); tg δ=0.5-1.4%; resistance to pressure relatively poor (DC break down voltage intensity is 7KV/mm), and dielectric loss is higher of specific inductivity.And for example, (denomination of invention is " a kind of low temperature sintering high-voltage ceramic condenser medium " to Chinese invention patent application prospectus CN1619726A, number of patent application is 200410041863.x), the weight percent content of disclosed each component of ceramic capacitor dielectric is: BaTiO
360-90%, SrTiO
31-20%, CaZrO
30.1-10%, Nb
2O
50.01-1%, MgO 0.01-1%, CeO
20.01-0.8%, ZnO 0.01-0.6%, Co
2O
30.03-1%, bismuth lithium sosoloid 0.05-10%, its specific inductivity is 2000-3000, and proof voltage is more than the 6kV/mm, and specific inductivity and proof voltage are still not ideal enough, and dielectric loss is higher.
In sum, the existing various requirement that can't satisfy simultaneously the aspects such as low-loss, high withstand voltage and environmental protection for the dielectric medium of ceramic condenser.
Summary of the invention
Technical problem to be solved by this invention provides a kind of low-loss high-voltage ceramic condenser medium, and this ceramic capacitor dielectric loss is low, and proof voltage is high, and in preparation and use procedure environmentally safe.
The technical scheme that adopts is as follows:
A kind of low-loss high-voltage ceramic condenser medium is characterized in that being made by the raw material of following weight per-cent: BaTiO
358-91%, SrTiO
31-3%, BaZrO
34-20%, CaZrO
33-12%, CeO
20.03-1.0%, ZnO 0.1-1.5%, Bi
2TiO
50.5-4.5%.
In a kind of concrete scheme, preferred above-mentioned low-loss high-voltage ceramic condenser medium is made by the raw material of following weight per-cent: BaTiO
366.2-85%, SrTiO
31-3%, BaZrO
35-15%, CaZrO
35-10%, CeO
20.3-0.6%, ZnO 0.3-0.7%, Bi
2TiO
51.5-4.5%.
In another kind of concrete scheme, preferred above-mentioned low-loss high-voltage ceramic condenser medium is made by the raw material of following weight per-cent: BaTiO
373-88%, SrTiO
31-3%, BaZrO
34-14%, CaZrO
34-9%, CeO
20.3-0.6%, ZnO 0.3-0.7%, Bi
2TiO
51.5-4.5%.
Preferred above-mentioned BaTiO
3, SrTiO
3, BaZrO
3, CaZrO
3, Bi
2TiO
5Adopt respectively conventional chemical feedstocks synthetic with solid phase method.For example:
Above-mentioned BaTiO
3(barium titanate) can adopt following technique preparation: be equipped with BaCO by 1: 1 mol ratio
3And TiO
2, then to BaCO
3And TiO
2Grind and mix, again with BaCO
3And TiO
2Mixture put into alumina crucible, in 1260 ℃ of lower insulations 120 minutes, obtain BaTiO
3The BaTiO that obtains
3Through grinding and crossing 200 mesh sieves, for subsequent use.
Above-mentioned SrTiO
3(strontium titanate) can adopt following technique preparation: be equipped with SrCO by 1: 1 mol ratio
3And TiO
2, then to SrCO
3And TiO
2Grind and mix, again with SrCO
3And TiO
2Mixture put into alumina crucible, in 1260 ℃ of lower insulations 120 minutes, obtain SrTiO
3The SrTiO that obtains
3Through grinding and crossing 200 mesh sieves, for subsequent use.
Above-mentioned BaZrO
3(barium zirconate) can adopt following technique preparation: be equipped with BaCO by 1: 1 mol ratio
3And ZrO
2, then to BaCO
3And ZrO
2Grind and mix, again with BaCO
3And ZrO
2Mixture put into alumina crucible, in 1270 ℃ of lower insulations 120 minutes, obtain BaZrO
3The BaZrO that obtains
3Through grinding and crossing 200 mesh sieves, for subsequent use.
Above-mentioned CaZrO
3(calcium zirconate) can adopt following technique preparation: be equipped with CaCO by 1: 1 mol ratio
3And ZrO
2, then to CaCO
3And ZrO
2Grind and mix, again with CaCO
3And ZrO
2Mixture put into alumina crucible, in 1270 ℃ of lower insulations 120 minutes, obtain CaZrO
3The CaZrO that obtains
3Through grinding and crossing 200 mesh sieves, for subsequent use.
Above-mentioned Bi
2TiO
5(bismuth titanates) can adopt following technique preparation: be equipped with Bi by 1: 1 mol ratio
2O
3And TiO
2, then to Bi
2O
3And TiO
2Grind and mix, again with Bi
2O
3And TiO
2Mixture put into alumina crucible, in 950 ℃ of lower insulations 120 minutes, obtain Bi
2TiO
5The Bi that obtains
2TiO
5Through grinding and crossing 200 mesh sieves, for subsequent use.
In the above-mentioned various raw material: BaTiO
3Effect be to form principal crystalline phase; SrTiO
3And BaZrO
3As moving the peak agent, an amount of SrTiO
3And BaZrO
3The Curie temperature of ceramic capacitor dielectric can be moved near room temperature, improve the specific inductivity of ceramic capacitor dielectric etc.; CaZrO
3As moving peak agent and depressor, an amount of CaZrO
3Can improve the specific inductivity of ceramic capacitor dielectric and improve Jie's temperature characteristics of ceramic capacitor dielectric; An amount of CeO
2(cerium dioxide) can improve the specific inductivity of ceramic capacitor dielectric and reduce dielectric loss, improves Jie's temperature characteristics of ceramic capacitor dielectric; An amount of ZnO (zinc oxide) can crystal grain thinning, reduces the dielectric loss of ceramic capacitor dielectric, improves withstand voltage; An amount of Bi
2TiO
5Can reduce the dielectric loss of ceramic capacitor dielectric, improve withstand voltagely, reduce the sintering temperature of ceramic capacitor dielectric.
A kind of preparation method of the above-mentioned low-loss high-voltage ceramic condenser medium of brief description comprises the steps: successively
(1) is equipped with in proportion BaTiO
3, SrTiO
3, BaZrO
3, CaZrO
3, CeO
2, ZnO and Bi
2TiO
5
(2) BaTiO that step (1) is equipped with
3, SrTiO
3, BaZrO
3, CaZrO
3, CeO
2, ZnO and Bi
2TiO
5Pulverize and mix, obtain compound;
After above-mentioned various raw materials can being mixed, pulverize again; Subsequently, mix while pulverizing, or after finishing pulverizing various raw materials are mixed.Disintegrating apparatus can adopt ball mill, also can adopt other disintegrating apparatus;
After preferably above-mentioned various raw materials being mixed, adopt planetary ball mill to carry out ball milling and mix, by the part by weight of the raw material of ball milling, institute's water, balls be: raw material: ball: water=1: 3: (0.6-1), mechanical milling process continues 4-8 hour; The used water of ball milling is preferably distilled water or deionized water;
(3) compound that step (2) is obtained is dried; The purpose of oven dry is the moisture of removing in the compound; Preferred bake out temperature is 110 ℃, and drying time is 12 hours;
(4) in the compound of step (3) oven dry, adding tackiness agent and carrying out granulation, obtain granular material;
Above-mentioned tackiness agent can adopt polyvinyl alcohol water solution; It is the polyvinyl alcohol water solution of 10% (weight) that preferred adhesive adopts concentration, and the weight of the polyvinyl alcohol water solution that adds is the 8-10% through the weight of the compound of step (3) oven dry;
(5) granular material that step (4) is obtained is pressed into green sheet;
Can adopt dry-pressing formed technology that granular material is pressed into green sheet; Preferably under the pressure of 20-30Mpa, granular material is carried out dry-pressing formedly, obtain green sheet; Dry-pressing formed working temperature is generally room temperature;
(6) it is under 1250-1280 ℃ the environment, to be incubated 1-4 hour that the green sheet that step (5) is obtained places temperature, makes green sheet discharge tackiness agent and sintering, obtains the low-loss high-voltage ceramic condenser medium.The low-loss high-voltage ceramic condenser medium that obtains can be used for making ceramic condenser.
It is under the 780-870 ℃ of environment that the dielectric medium of above-mentioned ceramic condenser is placed temperature, is incubated 15 minutes and carries out silver ink firing, forms silver electrode, and welding lead and sealing namely gets ceramic condenser again.
Low-loss high-voltage ceramic condenser medium of the present invention has following advantage: not leaded and cadmium, in use environmentally safe; Proof voltage high (the direct current proof voltage can reach more than the 12kV/mm), percentage of capacitance variation with temperature little (meeting the requirement of Y5V characteristic), and dielectric loss little (dielectric loss is less than 0.2%), thereby ceramic condenser in use stability is good, safe, can enlarge the range of application of ceramic condenser.Low-loss high-voltage ceramic condenser medium of the present invention is in preparation process, and sintering temperature lower (adopt intermediate sintering temperature, sintering temperature is 1250-1280 ℃) reduces the cost of high voltage ceramic capacitor greatly; And utilize not leaded and condenser ceramics general chemistry raw material cadmium to prepare the dielectric medium of ceramic condenser, environmentally safe in preparation process.Generally speaking, low-loss high-voltage ceramic condenser medium proof voltage of the present invention is high, and dielectric loss is little, environmentally safe in preparation and use procedure, and can reduce the cost of ceramic condenser, be suitable for preparing monolithic ceramic capacitor and multiple-layer sheet ceramic capacitor.
Embodiment
Embodiment 1
At first, with the synthetic BaTiO of solid phase method
3, SrTiO
3, BaZrO
3, CaZrO
3, Bi
2TiO
5
BaTiO
3(barium titanate) adopts following technique preparation: be equipped with BaCO by 1: 1 mol ratio
3And TiO
2, then to BaCO
3And TiO
2Grind and mix, again with BaCO
3And TiO
2Mixture put into alumina crucible, in 1260 ℃ of lower insulations 120 minutes, obtain BaTiO
3The BaTiO that obtains
3Through grinding and crossing 200 mesh sieves, for subsequent use.
SrTiO
3(strontium titanate) adopts following technique preparation: be equipped with SrCO by 1: 1 mol ratio
3And TiO
2, then to SrCO
3And TiO
2Grind and mix, again with SrCO
3And TiO
2Mixture put into alumina crucible, in 1260 ℃ of lower insulations 120 minutes, obtain SrTiO
3The SrTiO that obtains
3Through grinding and crossing 200 mesh sieves, for subsequent use.
BaZrO
3(barium zirconate) adopts following technique preparation: be equipped with BaCO by 1: 1 mol ratio
3And ZrO
2, then to BaCO
3And ZrO
2Grind and mix, again with BaCO
3And ZrO
2Mixture put into alumina crucible, in 1270 ℃ of lower insulations 120 minutes, obtain BaZrO
3The BaZrO that obtains
3Through grinding and crossing 200 mesh sieves, for subsequent use.
CaZrO
3(calcium zirconate) adopts following technique preparation: be equipped with CaCO by 1: 1 mol ratio
3And ZrO
2, then to CaCO
3And ZrO
2Grind and mix, again with CaCO
3And ZrO
2Mixture put into alumina crucible, in 1270 ℃ of lower insulations 120 minutes, obtain CaZrO
3The CaZrO that obtains
3Through grinding and crossing 200 mesh sieves, for subsequent use.
Bi
2TiO
5(bismuth titanates) adopts following technique preparation: be equipped with Bi by 1: 1 mol ratio
2O
3And TiO
2, then to Bi
2O
3And TiO
2Grind and mix, again with Bi
2O
3And TiO
2Mixture put into alumina crucible, in 950 ℃ of lower insulations 120 minutes, obtain Bi
2TiO
5The Bi that obtains
2TiO
5Through grinding and crossing 200 mesh sieves, for subsequent use.
Then, prepare in the steps below successively the low-loss high-voltage ceramic condenser medium:
(1) is equipped with in proportion BaTiO
3, SrTiO
3, BaZrO
3, CaZrO
3, CeO
2, ZnO and Bi
2TiO
5
With reference to table 1, the weight percent of the various raw materials of outfit is as follows: BaTiO
381%, SrTiO
31.5%, BaZrO
38.2%, CaZrO
36.5%, CeO
20.4%, ZnO 0.4% and Bi
2TiO
52.0%;
(2) BaTiO that step (1) is equipped with
3, SrTiO
3, BaZrO
3, CaZrO
3, CeO
2, ZnO and Bi
2TiO
5Pulverize and mix, obtain compound;
In the present embodiment, after above-mentioned various raw materials mixing, adopt planetary ball mill to carry out ball milling and mix, by the part by weight of the raw material of ball milling, institute's water, balls be: raw material: ball: water=1: 3: 0.8, mechanical milling process continues 6 hours; The used water of ball milling is distilled water or deionized water;
(3) compound that step (2) is obtained is dried, and removes the moisture in the compound;
In the present embodiment, bake out temperature is 110 ℃, and drying time is 12 hours;
(4) in the compound of step (3) oven dry, adding tackiness agent and carrying out granulation, obtain granular material;
It is the polyvinyl alcohol water solution of 10% (weight) that tackiness agent adopts concentration, and the weight of the polyvinyl alcohol water solution that adds is through 10% of the weight of the compound of step (3) oven dry;
(5) granular material that step (4) is obtained is pressed into green sheet;
Present embodiment carries out dry-pressing formed under the pressure of 25Mpa to granular material, obtain green sheet;
(6) it is under 1260 ℃ the environment, to be incubated 3 hours that the green sheet that step (5) is obtained places temperature, makes green sheet discharge tackiness agent and sintering, obtains the low-loss high-voltage ceramic condenser medium.
Embodiment 2-9
Among the embodiment 2-9, the consumption of various raw materials is as shown in table 1.But utilize above-mentioned raw materials to prepare the method reference example 1 of low-loss high-voltage ceramic condenser medium, the processing condition such as the temperature in each step, time, pressure can be adjusted according to practical situation.
Dielectric performance perameter of the ceramic condenser that above-described embodiment 1-9 makes is as shown in table 2.
The proportioning raw materials of table 1 various embodiments of the present invention
The performance perameter of the low-loss high-voltage ceramic condenser medium that table 2 various embodiments of the present invention make
Claims (8)
1. a low-loss high-voltage ceramic condenser medium is characterized in that being made by the raw material of following weight per-cent: BaTiO
358-91%, SrTiO
31-3%, BaZrO
34-20%, CaZrO
33-12%, CeO
20.03-1.0%, ZnO 0.1-1.5%, Bi
2TiO
50.5-4.5%;
The preparation method of described low-loss high-voltage ceramic condenser medium comprises the steps: successively
(1) is equipped with in proportion BaTiO
3, SrTiO
3, BaZrO
3, CaZrO
3, CeO
2, ZnO and Bi
2TiO
5
(2) BaTiO that step (1) is equipped with
3, SrTiO
3, BaZrO
3, CaZrO
3, CeO
2, ZnO and Bi
2TiO
5Pulverize and mix, obtain compound;
(3) compound that step (2) is obtained is dried;
(4) in the compound of step (3) oven dry, adding tackiness agent and carrying out granulation, obtain granular material;
(5) granular material that step (4) is obtained is pressed into green sheet;
(6) it is under 1250-1280 ℃ the environment, to be incubated 1-4 hour that the green sheet that step (5) is obtained places temperature, makes green sheet discharge tackiness agent and sintering, obtains the low-loss high-voltage ceramic condenser medium.
2. low-loss high-voltage ceramic condenser medium according to claim 1, it is characterized in that: described low-loss high-voltage ceramic condenser medium is made by the raw material of following weight per-cent: BaTiO
366.2-85%, SrTiO
31-3%, BaZrO
35-15%, CaZrO
35-10%, CeO
20.3-0.6%, ZnO 0.3-0.7%, Bi
2TiO
51.5-4.5%.
3. low-loss high-voltage ceramic condenser medium according to claim 1, it is characterized in that: described low-loss high-voltage ceramic condenser medium is made by the raw material of following weight per-cent: BaTiO
373-88%, SrTiO
31-3%, BaZrO
34-14%, CaZrO
34-9%, CeO
20.3-0.6%, ZnO 0.3-0.7%, Bi
2TiO
51.5-4.5%.
4. each described low-loss high-voltage ceramic condenser medium is characterized in that: described BaTiO according to claim 1-3
3Adopt following technique preparation: be equipped with BaCO by 1: 1 mol ratio
3And TiO
2, then to BaCO
3And TiO
2Grind and mix, again with BaCO
3And TiO
2Mixture put into alumina crucible, in 1260 ℃ of lower insulations 120 minutes, obtain BaTiO
3
5. each described low-loss high-voltage ceramic condenser medium is characterized in that: described SrTiO according to claim 1-3
3Adopt following technique preparation: be equipped with SrCO by 1: 1 mol ratio
3And TiO
2, then to SrCO
3And TiO
2Grind and mix, again with SrCO
3And TiO
2Mixture put into alumina crucible, in 1260 ℃ of lower insulations 120 minutes, obtain SrTiO
3
6. each described low-loss high-voltage ceramic condenser medium is characterized in that: described BaZrO according to claim 1-3
3Adopt following technique preparation: be equipped with BaCO by 1: 1 mol ratio
3And ZrO
2, then to BaCO
3And ZrO
2Grind and mix, again with BaCO
3And ZrO
2Mixture put into alumina crucible, in 1270 ℃ of lower insulations 120 minutes, obtain BaZrO
3
7. each described low-loss high-voltage ceramic condenser medium is characterized in that: described CaZrO according to claim 1-3
3Adopt following technique preparation: be equipped with CaCO by 1: 1 mol ratio
3And ZrO
2, then to CaCO
3And ZrO
2Grind and mix, again with CaCO
3And ZrO
2Mixture put into alumina crucible, in 1270 ℃ of lower insulations 120 minutes, obtain CaZrO
3
8. each described low-loss high-voltage ceramic condenser medium is characterized in that: described Bi according to claim 1-3
2TiO
5Adopt following technique preparation: be equipped with Bi by 1: 1 mol ratio
2O
3And TiO
2, then to Bi
2O
3And TiO
2Grind and mix, again with Bi
2O
3And TiO
2Mixture put into alumina crucible, in 950 ℃ of lower insulations 120 minutes, obtain Bi
2TiO
5
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| CN102568821B (en) * | 2012-02-16 | 2015-02-04 | 江苏大学 | High-voltage ceramic capacitor dielectric with high dielectric constant |
| CN103242038A (en) * | 2013-05-31 | 2013-08-14 | 常州佳冠电子有限公司 | Ceramic capacitor medium and preparation method thereof |
| TWI573775B (en) * | 2015-07-16 | 2017-03-11 | Ceramic capacitor dielectric material | |
| CN105016727B (en) * | 2015-08-05 | 2017-08-11 | 天津大学 | The preparation method of high withstand voltage medium material for multilayer ceramic capacitors |
| CN105777115B (en) * | 2016-03-16 | 2018-06-15 | 江苏省陶瓷研究所有限公司 | It is a kind of to prepare the polynary barium strontium titanate doped method for preparing high-performance ceramic capacitor material of collaboration |
| CN112341187B (en) * | 2020-10-08 | 2022-09-13 | 重庆三峡学院 | Preparation method of barium titanate piezoelectric material for landslide displacement monitoring in three gorges reservoir area |
| 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 |
| CN114874007B (en) * | 2022-05-10 | 2022-12-09 | 河南科技大学 | Preparation method of calcium zirconate-strontium titanate high-efficiency energy-storage dielectric composite ceramic |
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