CN103408302A - High permittivity and high temperature stability ceramic capacitor medium and its preparation method - Google Patents
High permittivity and high temperature stability ceramic capacitor medium and its preparation method Download PDFInfo
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- CN103408302A CN103408302A CN2013103048296A CN201310304829A CN103408302A CN 103408302 A CN103408302 A CN 103408302A CN 2013103048296 A CN2013103048296 A CN 2013103048296A CN 201310304829 A CN201310304829 A CN 201310304829A CN 103408302 A CN103408302 A CN 103408302A
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Abstract
Relating to the technical field of inorganic non-metallic materials, the invention in particular relates to a high permittivity and high temperature stability ceramic capacitor medium and its preparation method. According to a formula, the ceramic capacitor medium comprises, by weight: 55-90% of BaTiO3, 2-25% of SrTiO3, 2-15% of CaZrO3, 0.5-6% of Bi2O3.3TiO2, 0.1-8.5% of La2(ZrO3)3, 0.1-0.8% of Gd2O3, and 0.03-1.0% of MnO2. The invention employs a conventional ceramic capacitor medium preparation method, and uses a capacitor ceramic ordinary chemical raw material to prepare non-toxic and high temperature stability ceramic capacitor medium free of lead and cadmium. The medium is suitable for preparation of monolithic ceramic capacitors, can reduce the volume of ceramic capacitors and improve the withstand voltage, can greatly reduce the cost of ceramic capacitors and improve security, also has high temperature stability, and does not pollute the environment during preparation and use.
Description
Technical field
The present invention relates to technical field of inorganic nonmetallic materials, refer in particular to a kind of high Jie's high-temperature and stablize ceramic capacitor dielectric and preparation method thereof; It adopts conventional ceramic capacitor dielectric preparation method, utilize condenser ceramics general chemistry raw material, prepare unleaded, without height Jie high-temperature of cadmium, stablize ceramic capacitor dielectric, can also reduce the sintering temperature of condenser ceramics, this medium is suitable for preparing monolithic ceramic capacitor, the cost of ceramic condenser can be greatly reduced, temperature stability can be improved simultaneously to enlarge the range of application of ceramic condenser, and free from environmental pollution in preparation and use procedure.
Background technology
The fields such as colour TV, computer, communication, aerospace, guided missile, navigation are high in the urgent need to voltage breakdown, temperature stability good, reliability is high, miniaturization, jumbo ceramic condenser; The sintering temperature of general single-chip high voltage ceramic capacitor dielectric is 1350 ~ 1430 ℃, and ceramic capacitor dielectric sintering temperature of the present invention is 1200 ~ 1230 ℃, can greatly reduce the cost of high voltage ceramic capacitor like this, the not leaded and cadmium of this patent capacitor ceramic dielectric simultaneously, condenser ceramics is free from environmental pollution in preparation and use procedure; In addition, the specific inductivity of condenser ceramics of the present invention is higher, can improve like this capacity and the miniaturization of ceramic condenser, meets the development trend of ceramic condenser, equally also can reduce the cost of ceramic condenser.
Be generally used for producing in the medium of high voltage ceramic capacitor and contain a certain amount of lead, this not only produce, use and discarded process in human body and environment are worked the mischief, and stability is also had to detrimentally affect.
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 a literary composition, this dielectric material adopts 97.8wt.%BaTiO
3+ 0.8wt.%Bi
2O
3+ 0.7wt.%Nb
2O
5+ 0.5wt.%CeO
2+ 0.2wt.%MnO
2Formula, with conventional technique, prepare sample, its DIELECTRIC CONSTANT ε=2500 ~ 2600, tg δ=0.5-1.4%, DC break down voltage intensity is 7KV/mm; Though this medium belongs to unleaded dielectric material, it exists resistance to pressure poor, and specific inductivity is too little.Formula forms and is different from this patent.
Chinese patent " a kind of high-voltage ceramic condenser medium " (patent No. ZL00112050.6) is though disclosed capacitor ceramic dielectric belongs to unleaded dielectric material, but specific inductivity is 1860-3300, proof voltage can reach 10kV/mm above (direct current), sintering temperature is 1260-1400 ℃, higher than this patent, specific inductivity is too little, and far below this patent, and the formula composition is different from this patent.
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 a literary composition
3High Jie of middle easy fired meets the capacitor ceramics of X7R characteristic, and the formula of this dielectric material consists of (mass percent): (BaTiO
3+ Nd
2O
3) 89% ~ 92%+Bi
2O
32TiO
27.5 ~ 10%+ low melting glass material 0.8%+50%Mn (NO
3)
2(aqueous solution) 0.205%; Wherein, low melting glass material used is the lead borosilicate low melting glass, and medium is leaded, and does not relate to proof voltage, and specific inductivity is less than 3500, and much smaller than the specific inductivity of this patent, the formula of medium forms and also is different from patent of the present invention.
Patent " a kind of low-loss high-voltage ceramic condenser medium " (number of patent application: 201010588021.1) is separately arranged, although the medium dielectric loss of this patent is low, capacity temperature characteristic is poor, does not meet the X7R characteristic, specific inductivity is lower than this patent, and formula is different from this patent.
Patent " manufacture method of the high-voltage ceramic condenser medium " (patent No.: 91101958.8) is separately arranged, it adopts unconventional technique to prepare medium, be the flow casting molding film, then the laminated medium body, carry out the multilayered medium body the even pressure of heating under vacuum, punching, then carry out binder removal, burn till and obtain; The shortcoming of this patent is the process of preparing complexity, causes cost of goods manifactured to increase, the specific inductivity of manufacturing the high voltage capacitor pottery of gained by its medium formula is 1800-7200, specific inductivity is too little, and capacity temperature characteristic does not meet the X7R characteristic, and formula is different from this patent.
(number of patent application: 201010538725.8), although the medium specific inductivity of this patent is very high, hold temperature characteristics poor, do not meet the X7R characteristic, formula is different from this patent to also have patent " dielectric medium of a kind of ceramic condenser and preparation method thereof ".
Summary of the invention
The purpose of this invention is to provide a kind of high Jie's high-temperature and stablize ceramic capacitor dielectric.
The object of the present invention is achieved like this:
High Jie's high-temperature is stablized ceramic capacitor dielectric formula composition and is comprised (weight percent): BaTiO
355-90%, SrTiO
32-25%, CaZrO
32-15%, Bi
2O
33TiO
20.5-6%, La
2(ZrO
3)
30.1-8.5%, Gd
2O
30.1-0.8%, MnO
20.03-1.0%; BaTiO wherein
3, SrTiO
3, CaZrO
3, Bi
2O
33TiO
2, La
2(ZrO
3)
3Respectively to adopt conventional chemical feedstocks synthetic with solid phase method.
Bi used in medium of the present invention
2O
33TiO
2Adopt following technique to prepare: by conventional chemical feedstocks Bi
2O
3And TiO
2Press the 1:3 molar ratio ingredient, put into alumina crucible in 950 ℃-1100 ℃ insulations 120 minutes after ground and mixed is even, solid state reaction is synthesized Bi
2O
33TiO
2, ground 200 mesh sieves after cooling, standby.
La used in medium of the present invention
2(ZrO
3)
3Preparation process as follows: by conventional chemical feedstocks La
2O
3And ZrO
2Press the 1:3 molar ratio ingredient, put into alumina crucible in 1280 ℃-1300 ℃ insulations 120 minutes after ground and mixed is even, solid state reaction is synthesized La
2(ZrO
3)
3, ground 200 mesh sieves after cooling, standby.
The present invention adopts conventional high-voltage ceramic condenser medium preparation technology, namely at first adopts conventional chemical feedstocks to synthesize respectively BaTiO with solid phase method
3, SrTiO
3, CaZrO
3, Bi
2O
33TiO
2, La
2(ZrO
3)
3, then by the formula batching, by admixtion ball milling, pulverizing, mixing, after drying, add the tackiness agent granulation, then be pressed into green sheet, then in air, carry out binder removal and sintering, after insulation naturally cooling, obtain ceramic capacitor dielectric, on medium by electrode.
The formula of above-mentioned ceramic dielectic preferably adopts following three kinds of schemes (weight percent):
BaTiO
360-86%, SrTiO
33-22%, CaZrO
33-12%, Bi
2O
3·3TiO
2 0.5-6%, La
2(ZrO
3)
3 0.2-6.7%, Gd
2O
30.1-0.8%,MnO
20.03-1.0%；
BaTiO
3 65-83%, SrTiO
3 3-19%, CaZrO
3 4-10%, Bi
2O
3·3TiO
2 1-6%, La
2(ZrO
3)
3 0.2-5.2%, Gd
2O
30.1-0.8%, MnO
20.03-1.0%；
BaTiO
370-81%, SrTiO
34-17%, CaZrO
33-8%, Bi
2O
3·3TiO
2 1-5%, La
2(ZrO
3)
3 0.2-4.7%, Gd
2O
3 0.1-0.8%, MnO
20.03-1.0%。
The present invention compared with prior art, has following advantage:
1, the medium of this patent is sintering temperature lower (1200 ~ 1230 ℃ of sintering temperatures) barium strontium based capacitor pottery, can greatly reduce like this cost of high voltage ceramic capacitor, not leaded and cadmium in the media components of this patent, environmentally safe;
2, the specific inductivity of this medium is high, is more than 5600; Proof voltage is high, more than the direct current proof voltage can reach 14kV/mm; Dielectric loss is little, is less than 0.5%; The specific inductivity of this medium is higher, can realize miniaturization and the large capacity of ceramic condenser, can reduce costs equally;
3, the percentage of capacitance variation with temperature of this medium is little, holds the requirement that temperature characteristics meets the X7R characteristic; Dielectric loss is less than 0.5%, and use procedure performance good stability is safe;
4, main raw material employing ceramic condenser level is pure can produce ceramic dielectic of the present invention;
5, this medium adopts conventional solid phase method ceramic capacitor dielectric preparation technology to be prepared.
Embodiment
The invention will be further described in conjunction with the embodiments now.Table 1 provides the embodiments of the invention formula of totally 9 samples.
The embodiments of the invention main raw material of the formula of totally 9 samples adopt the ceramic condenser level pure, at first adopt in the preparation conventional chemical feedstocks to synthesize respectively BaTiO with solid phase method
3, SrTiO
3, CaZrO
3, Bi
2O
33TiO
2, La
2(ZrO
3)
3, then by above-mentioned formula batching, with distilled water or deionized water, adopt the planetary ball mill ball milling to mix in the material prepared, material: ball: water=1:3:(0.6 ~ 1.0) (mass ratio), after ball milling 4 ~ 8 hours, dry to obtain dry mash, in dry mash, adding the concentration that accounts for its weight 8 ~ 10% is 10% polyvinyl alcohol solution, carry out granulation, mixed rear mistake 40 mesh sieves, under 20 ~ 30Mpa pressure, carry out again dry-pressing and become green sheet, then in sintering temperature, be under 1200 ~ 1230 ℃, to be incubated 1 ~ 4 hour to carry out binder removal and sintering, silver ink firing was carried out in insulation in 15 minutes under 780 ~ 870 ℃ again, form silver electrode, solder taul again, seal, obtain ceramic condenser, test its dielectric properties.
Above-mentioned dielectric properties of respectively filling a prescription sample are listed in table 2, and prepared condenser ceramics proof voltage is high as can be seen from Table 2, can reach 14kV/mm (volts DS, DC) more than; Specific inductivity is more than 5600; Dielectric loss is less than 0.5%; Percentage of capacitance variation with temperature is little, meets the requirement of X7R characteristic.
Table 1 embodiments of the invention are the formula of totally 9 samples
Respectively the fill a prescription dielectric properties of sample of table 2
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (7)
1. one kind high Jie's high-temperature is stablized ceramic capacitor dielectric, and described ceramic capacitor dielectric specific inductivity is high, is more than 5600; Proof voltage is high, more than the direct current proof voltage can reach 14kV/mm; Dielectric loss is little, is less than 0.5%; Percentage of capacitance variation with temperature is little, meets the requirement of X7R characteristic; It is characterized in that: described ceramic capacitor dielectric formula composition calculates according to weight percent and is: BaTiO
355-90%, SrTiO
32-25%, CaZrO
32-15%, Bi
2O
33TiO
20.5-6%, La
2(ZrO
3)
30.1-8.5%, Gd
2O
30.1-0.8%, MnO
20.03-1.0%; BaTiO wherein
3, SrTiO
3, CaZrO
3, Bi
2O
33TiO
2, La
2(ZrO
3)
3Respectively to adopt conventional chemical feedstocks synthetic with solid phase method.
2. a kind of high Jie's high-temperature as claimed in claim 1 is stablized ceramic capacitor dielectric, it is characterized in that: described Bi
2O
33TiO
2Adopt following technique to prepare: by conventional chemical feedstocks Bi
2O
3And TiO
2Press the 1:3 molar ratio ingredient, put into alumina crucible in 950 ℃-1100 ℃ insulations 120 minutes after ground and mixed is even, solid state reaction is synthesized Bi
2O
33TiO
2, ground 200 mesh sieves after cooling, standby.
3. a kind of high Jie's high-temperature as claimed in claim 1 is stablized ceramic capacitor dielectric, it is characterized in that: described La
2(ZrO
3)
3Preparation process as follows: by conventional chemical feedstocks La
2O
3And ZrO
2Press the 1:3 molar ratio ingredient, put into alumina crucible in 1280 ℃-1300 ℃ insulations 120 minutes after ground and mixed is even, solid state reaction is synthesized La
2(ZrO
3)
3, ground 200 mesh sieves after cooling, standby.
4. a kind of high Jie's high-temperature as claimed in claim 1 is stablized ceramic capacitor dielectric, it is characterized in that: described ceramic capacitor dielectric formula composition calculates according to weight percent and is: BaTiO
360-86%, SrTiO
33-22%, CaZrO
33-12%, Bi
2O
33TiO
20.5-6%, La
2(ZrO
3)
30.2-6.7%, Gd
2O
30.1-0.8%, MnO
20.03-1.0%.
5. a kind of high Jie's high-temperature as claimed in claim 1 is stablized ceramic capacitor dielectric, it is characterized in that: described ceramic capacitor dielectric formula composition calculates according to weight percent and is: BaTiO
365-83%, SrTiO
33-19%, CaZrO
34-10%, Bi
2O
33TiO
21-6%, La
2(ZrO
3)
30.2-5.2%, Gd
2O
30.1-0.8%, MnO
20.03-1.0%.
6. a kind of high Jie's high-temperature as claimed in claim 1 is stablized ceramic capacitor dielectric, it is characterized in that: described ceramic capacitor dielectric formula composition calculates according to weight percent and is: BaTiO
370-81%, SrTiO
34-17%, CaZrO
33-8%, Bi
2O
33TiO
21-5%, La
2(ZrO
3)
30.2-4.7%, Gd
2O
30.1-0.8%, MnO
20.03-1.0%.
7. a kind of high Jie's high-temperature as claimed in claim 1 is stablized the preparation method of ceramic capacitor dielectric, it is characterized in that comprising the steps: at first to adopt conventional chemical feedstocks to synthesize respectively BaTiO with solid phase method
3, SrTiO
3, CaZrO
3, Bi
2O
33TiO
2, La
2(ZrO
3)
3, then by the formula batching, with distilled water or deionized water, adopt the planetary ball mill ball milling to mix in the material prepared, mass ratio material: ball: water=1:3:0.6 ~ 1.0, after ball milling 4 ~ 8 hours, dry to obtain dry mash, in dry mash, adding the concentration that accounts for its weight 8 ~ 10% is 10% polyvinyl alcohol solution, carry out granulation, mixed rear mistake 40 mesh sieves, under 20 ~ 30Mpa pressure, carry out again dry-pressing and become green sheet, then in sintering temperature, be under 1200 ~ 1230 ℃, to be incubated 1 ~ 4 hour to carry out binder removal and sintering, silver ink firing was carried out in insulation in 15 minutes under 780 ~ 870 ℃ again, form silver electrode, solder taul again, seal, obtain ceramic capacitor dielectric.
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| CN103408302B CN103408302B (en) | 2015-02-04 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105084892A (en) * | 2015-08-11 | 2015-11-25 | 电子科技大学 | High-medium single-layer miniature ceramic capacitor substrate material and preparation method thereof |
| CN105636275A (en) * | 2016-02-12 | 2016-06-01 | 慈溪锐恩电子科技有限公司 | Method for piezoelectric induction remote control LED lamp, piezoelectric induction remote control LED lamp and switch |
| CN106587988A (en) * | 2016-11-14 | 2017-04-26 | 江苏大学 | High-temperature stable ceramic capacitor dielectric |
| CN106854077A (en) * | 2016-12-29 | 2017-06-16 | 汕头市瑞升电子有限公司 | A kind of safety regulation ceramic capacitor medium material and preparation method thereof |
| CN107188562A (en) * | 2017-06-23 | 2017-09-22 | 汕头市瑞升电子有限公司 | Stable ceramic capacitor dielectric of a kind of high-k low loss and high temperature and preparation method thereof |
| CN108249915A (en) * | 2016-12-28 | 2018-07-06 | Tdk株式会社 | Dielectric composition and electronic unit |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105084892A (en) * | 2015-08-11 | 2015-11-25 | 电子科技大学 | High-medium single-layer miniature ceramic capacitor substrate material and preparation method thereof |
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| CN106854077A (en) * | 2016-12-29 | 2017-06-16 | 汕头市瑞升电子有限公司 | A kind of safety regulation ceramic capacitor medium material and preparation method thereof |
| CN106854077B (en) * | 2016-12-29 | 2019-06-14 | 汕头市瑞升电子有限公司 | A kind of safety regulation ceramic capacitor medium material and preparation method thereof |
| CN107188562A (en) * | 2017-06-23 | 2017-09-22 | 汕头市瑞升电子有限公司 | Stable ceramic capacitor dielectric of a kind of high-k low loss and high temperature and preparation method thereof |
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