CN102568821B - High-voltage ceramic capacitor dielectric with high dielectric constant - Google Patents
High-voltage ceramic capacitor dielectric with high dielectric constant Download PDFInfo
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- CN102568821B CN102568821B CN201210034278.1A CN201210034278A CN102568821B CN 102568821 B CN102568821 B CN 102568821B CN 201210034278 A CN201210034278 A CN 201210034278A CN 102568821 B CN102568821 B CN 102568821B
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Abstract
The invention relates to the technical field of inorganic non-metal material, in particular to a high-voltage ceramic capacitor dielectric with high dielectric constant, wherein the capacitor dielectric comprises following components in percentages by weight: 55-90% of BaTiO3, 2-25% of SrTiO3, 2-15% of MgZrO3, 2-10% of Bi3NbZrO3, 0.1-1.0% of CeO2, 0.5-1.5% of ZnO, 0.2-1.0% of MnCO3; the BaTiO3, SrTiO3, MgZrO3 and Bi3NbZrO3 are synthesized by normal chemical materials through a solid state method. The prepared capacitor ceramic material resists high voltage and more than 10kV/mm of direct-current voltage, has high dielectric constant which can reach more than 10000, small capacitance temperature change rate, meets requirement of Y5U characteristic, has less than 0.5% of dielectric loss, has good stable performance, high safety and no environment pollution during the usage.
Description
Technical field
The present invention relates to technical field of inorganic nonmetallic materials, refer in particular to a kind of high dielectric high-voltage ceramic condenser medium; Its adopts conventional ceramic capacitor dielectric preparation method, utilizes condenser ceramics general chemistry raw material, prepare unleaded, without height Jie high-voltage ceramic condenser medium of cadmium, the sintering temperature of condenser ceramics can also be reduced; This medium is suitable for preparing monolithic ceramic capacitor and multiple-layer sheet ceramic capacitor, greatly can reduce the cost of ceramic capacitor, can improve proof voltage to expand the range of application of ceramic capacitor simultaneously, and free from environmental pollution in preparation and use procedure.
Background technology
The field such as colour TV, computer, communication, Aero-Space, guided missile, navigation is high in the urgent need to puncture voltage, temperature stability good, reliability is high, miniaturized, jumbo ceramic capacitor; The sintering temperature of general single-chip high voltage ceramic capacitor dielectric is 1300 ~ 1430 DEG C, and ceramic capacitor dielectric sintering temperature of the present invention is 1250 ~ 1270 DEG C, greatly can reduce the cost of high voltage ceramic capacitor like this, the simultaneously not leaded and cadmium of this patent capacitor ceramic dielectric, condenser ceramics is free from environmental pollution in preparation and use procedure; In addition, the dielectric constant of condenser ceramics of the present invention is high, can improve the capacity of ceramic capacitor like this and miniaturized, meets the development trend of ceramic capacitor, equally also can reduce the cost of ceramic capacitor.
Be generally used for containing a certain amount of lead in the medium of production high voltage ceramic capacitor, this not only works the mischief to human body and environment in production, use and waste procedures, and also has harmful effect to stability.
Chinese periodical " electronic component and material " the 5th phase in 1989 is at " high Jie's high pressure 2B
4media ceramic " disclose a kind of high-voltage ceramic condenser medium material 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, prepare sample with the technique of routine, 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 is poor that it exists resistance to pressure, and dielectric constant is too little.Formula composition 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 dielectric constant is 1860-3300, proof voltage can reach more than 10kV/mm (direct current), sintering temperature is 1260-1400 DEG C, higher than this patent; Dielectric constant is too little, and far below this patent, and formula composition is different from this patent.
Chinese periodical " Jiangsu pottery " the 2nd phase in 1999 is at " BaTiO
3be easy fired height Jie X7R capacitor ceramics " disclose a kind of BaTiO in a literary composition
3middle easy fired height is situated between and 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 lead borosilicate low-melting glass, and medium is leaded, and does not relate to proof voltage, and dielectric constant is less than 3500, and much smaller than the dielectric constant of this patent, the formula composition of medium is also different from patent of the present invention.
Chinese periodical " South China Science & Engineering University's journal (natural science edition) " the 3rd phase in 1996 is at " intermediate sintering temperature BaTiO
3quito mutually ferroelectric porcelain X7R characteristic " inquire into BaTiO in a literary composition
3base porcelain intermediate sintering temperature mechanism, analyzes intermediate sintering temperature BaTiO
3the composition of base porcelain and uneven texture distribution are on the impact of dielectric constant and temperature characterisitic; BaTiO used
3raw material adopts the method for chemical coprecipitation to prepare, and can increase the cost of ceramic capacitor like this, and the BaTiO that this patent is used
3, SrTiO
3, CaZrO
3be adopt conventional chemical raw material with Solid phase synthesis respectively, composition is different from this patent, containing a certain amount of lead in component, and does not relate to proof voltage.
(number of patent application: 97117286.2), simultaneously it adopt Solid phase synthesis equivalence and aliovalent ion to replace (Sr separately patent " high Jie's high-performance medium temp. sintered chip multilayer ceramic capacitor porcelain "
2+, Zr
4+, Sn
4+, Nb
5+) BaTiO
3solid solution, add appropriate boron-lead-zinc-copper glass agglutinant, make porcelain at intermediate sintering temperature, its performance is: dielectric constant is more than or equal to 16000, and withstand voltage is 700V/mm; Although this patent dielectric constant is high, the material reported withstand voltage too poor, be only 700V/mm, its component contains a certain amount of lead in addition.
Separately have patent " manufacture method of high-voltage ceramic condenser medium " (patent No. 91101958.8), it adopts unconventional technique to prepare medium, i.e. flow casting molding film, then laminated medium body, carries out the even pressure of heating in vacuum, punching, then carries out binder removal, burns till and obtain by multilayer dielectricity body; The shortcoming of this patent is process of preparing complexity, causes cost of goods manufactured to increase, and the dielectric constant manufacturing the HV hall of gained by its medium formula is 1800-7200, and dielectric constant is too little, does not have the dielectric constant of this patent high.
(number of patent application: 97117287.0), it adopts unique formula (percentage by weight) (BaTiO to also have Chinese patent " high-performance medium temp. sintered chip multilayer ceramic capacitor porcelain "
393 ~ 96%+Nb
2o
50.8 ~ 1.5%+Bi
2o
31.0 ~ 2.2%+ flux, 1.8 ~ 3.5%+ modifier 0.25 ~ 1.0%) obtain the condenser ceramics meeting following performance of intermediate sintering temperature: dielectric constant is 3000, and dielectric loss is less than 1.5%, and withstand voltage is 860V/mm; The flux of this patent contains a certain amount of lead, and the proof voltage of this patent is too poor, and dielectric constant is too low simultaneously, much smaller than this patent.
Also have Chinese patent " a kind of low temperature sintering high-voltage ceramic condenser medium " (number of patent application: 200410041863.x), it adopts unique formula (percentage by weight) (BaTiO
360-90%, SrTiO
31-20% CaZrO
30.1-10%, Nb
2o
50.01-1%, MgO0.01-1%, CeO
20.01-0.8%, ZnO0.01-0.6%, Co
2o
30.03-1%, bismuth lithium solid solution 0.05-10%) obtain the condenser ceramics meeting following performance of intermediate sintering temperature: dielectric constant is 2000 ~ 3000, proof voltage is more than 6kV/mm, the additive reducing sintering temperature is bismuth lithium solid solution, dielectric constant and the proof voltage of this patent are high less than this patent, and the formula composition of this patent is different from this patent.
Summary of the invention
The object of this invention is to provide a kind of high dielectric high-voltage ceramic condenser medium.
The object of the present invention is achieved like this:
Described high dielectric high-voltage ceramic condenser medium formula constituent counts by weight percentage: BaTiO
355-90%, SrTiO
32-25%, MgZrO
32-15%, Bi
3nbZrO
92-10%, CeO
20.1-1.0%, ZnO 0.5-1.5%, MnCO
30.2-1.0%; Wherein BaTiO
3and SrTiO
3, MgZrO
3, Bi
3nbZrO
9adopt conventional chemical raw material with Solid phase synthesis respectively.
MgZrO used in medium of the present invention
3following technique is adopted to prepare: by chemical raw material MgO and ZrO of routine
2by 1:1 molar ratio ingredient, put into alumina crucible after ground and mixed is even in 1200 DEG C-1230 DEG C insulations 120 minutes, solid state reaction kinetics MgZrO
3, ground 200 mesh sieves after cooling, for subsequent use.
Bi used in medium of the present invention
3nbZrO
9following technique is adopted to prepare: by the chemical raw material Bi of routine
2o
3, Nb
2o
5and ZrO
2by 3/2:1/2:1 molar ratio ingredient, put into alumina crucible after ground and mixed is even in 900 DEG C-960 DEG C insulations 120 minutes, solid state reaction kinetics Bi
3nbZrO
9, ground 200 mesh sieves after cooling, for subsequent use.
The present invention adopts conventional high-voltage ceramic condenser medium preparation technology, namely first adopts conventional chemical raw material solid phase method to synthesize BaTiO respectively
3, SrTiO
3, MgZrO
3, Bi
3nbZrO
9, then by formula batching, batch ball mill grinding is mixed, after drying, add adhesive granulation, then be pressed into green sheet, then carry out binder removal and sintering in atmosphere, through insulation and naturally, after cooling, acquisition ceramic capacitor dielectric, by electrode on medium.
The formula of above-mentioned ceramic dielectric preferably adopts following three kinds of schemes (percentage by weight):
BaTiO
360-86%,SrTiO
33-22%,MgZrO
33-12%,Bi
3NbZrO
93-8%,CeO
20.2-0.6%,ZnO0.8-1.3% , MnCO
30.2-0.8%；
BaTiO
365-83%,SrTiO
33-19%,MgZrO
34-10%,Bi
3NbZrO
93-8%,CeO
20.2-0.6%,ZnO0.9-1.2%, MnCO
30.4-0.7%；
BaTiO
370-81%,SrTiO
35-15%,MgZrO
33-8%,Bi
3NbZrO
94-7%,CeO
20.2-0.6%,ZnO0.9-1.2% , MnCO
30.5-0.7%。
Compared with prior art, tool has the following advantages in the present invention:
1, the medium of this patent is intermediate sintering temperature (1250 ~ 1280 DEG C) barium strontium based capacitor pottery, greatly can reduce the cost of high voltage ceramic capacitor like this, not leaded and cadmium in the media components of this patent, environmentally safe.
2, the dielectric constant of this medium is high, is more than 10000; Proof voltage is high, and direct current proof voltage can reach more than 10kV/mm; Dielectric loss is little, is less than 0.5%; The dielectric constant of this medium is high, can realize miniaturization and the Large Copacity of ceramic capacitor, can reduce costs equally.
3, the percentage of capacitance variation with temperature of this medium is little, meets the requirement of Y5U characteristic; Dielectric loss is less than 0.5%, and in use procedure, stability is good, and fail safe is high.
4, primary raw material employing ceramic capacitor level is pure can produce ceramic dielectric 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 formula of embodiments of the invention totally 9 samples.
The primary raw material of the embodiments of the invention formula of totally 9 samples adopts ceramic capacitor level pure, first adopts conventional chemical raw material solid phase method to synthesize BaTiO respectively in the preparation
3, SrTiO
3, MgZrO
3, Bi
3nbZrO
9, then by above-mentioned formula batching, the material distilled water prepared or deionized water are adopted the mixing of planetary ball mill ball milling, material: ball: mass ratio=1:3:(0.6 ~ 1.0 of water), ball milling is after 4 ~ 8 hours, dry to obtain dry mash, in dry mash, add the concentration accounting for its weight 8 ~ 10% is the poly-vinyl alcohol solution of 10%, carry out granulation, mixed rear mistake 40 mesh sieve, under 20 ~ 30Mpa pressure, carry out dry-pressing again become green sheet, then at temperature is 1250 ~ 1270 DEG C, insulation carries out binder removal and sintering in 1 ~ 4 hour, at 780 ~ 870 DEG C, insulation carries out silver ink firing in 15 minutes again, form silver electrode, solder taul again, encapsulate, obtain ceramic capacitor, test its dielectric property, the dielectric property of above-mentioned each formula sample list in table 2, and condenser ceramics proof voltage prepared is as can be seen from Table 2 high, can reach more than 10kV/mm (direct voltage, DC), dielectric constant is more than 10000, dielectric loss is less than 0.5%, percentage of capacitance variation with temperature is little, meets the requirement of Y5U characteristic.
The formula of table 1 embodiments of the invention totally 9 samples
The dielectric property of table 2 each formula sample
Claims (6)
1. a high dielectric high-voltage ceramic condenser medium, is characterized in that: the component of described condenser dielectric counts by weight percentage as BaTiO
355-90%, SrTiO
32-25%, MgZrO
32-15%, Bi
3nbZrO
92-10%, CeO
20.1-1.0%, ZnO 0.5-1.5%, MnCO
30.2-1.0%; Wherein BaTiO
3, SrTiO
3, MgZrO
3and Bi
3nbZrO
9adopt conventional chemical raw material with Solid phase synthesis respectively.
2. a kind of high dielectric high-voltage ceramic condenser medium as claimed in claim 1, is characterized in that: BaTiO
360-86%, SrTiO
33-22%, MgZrO
33-12%, Bi
3nbZrO
93-8%, CeO
20.2-0.6%, ZnO0.8-1.3%, MnCO
30.2-0.8%.
3. a kind of high dielectric high-voltage ceramic condenser medium as claimed in claim 1, is characterized in that: BaTiO
365-83%, SrTiO
33-19%, MgZrO
34-10%, Bi
3nbZrO
93-8%, CeO
20.2-0.6%, ZnO0.9-1.2%, MnCO
30.4-0.7%.
4. a kind of high dielectric high-voltage ceramic condenser medium as claimed in claim 1, is characterized in that: BaTiO
370-81%, SrTiO
35-15%, MgZrO
33-8%, Bi
3nbZrO
94-7%, CeO
20.2-0.6%, ZnO0.9-1.2%, MnCO
30.5-0.7%.
5. a kind of high dielectric high-voltage ceramic condenser medium as claimed in claim 1, is characterized in that: described MgZrO
3following technique is adopted to prepare: by chemical raw material MgO and ZrO of routine
2by 1:1 molar ratio ingredient, put into alumina crucible after ground and mixed is even in 1200 DEG C-1230 DEG C insulations 120 minutes, solid state reaction kinetics MgZrO
3, ground 200 mesh sieves after cooling, for subsequent use.
6. a kind of high dielectric high-voltage ceramic condenser medium as claimed in claim 1, is characterized in that: described Bi
3nbZrO
9following technique is adopted to prepare: by the chemical raw material Bi of routine
2o
3, Nb
2o
5and ZrO
2by 3/2:1/2:1 molar ratio ingredient, put into alumina crucible after ground and mixed is even in 900 DEG C-960 DEG C insulations 120 minutes, solid state reaction kinetics Bi
3nbZrO
9, ground 200 mesh sieves after cooling, for subsequent use.
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| CN103408301B (en) * | 2013-07-19 | 2015-04-22 | 江苏大学 | Ultrahigh voltage ceramic capacitor medium and preparation method thereof |
| CN104692800B (en) * | 2015-02-04 | 2016-08-24 | 桂林理工大学 | A kind of temperature-stable unleaded huge dielectric constant ceramic material |
| CN106587996B (en) * | 2016-11-14 | 2020-03-31 | 江苏大学 | High-frequency grain boundary layer ceramic capacitor medium |
| CN106587989B (en) * | 2016-11-15 | 2019-08-02 | 江苏大学 | A kind of high dielectric property grain boundary layer ceramic capacitor medium |
| CN107369554A (en) * | 2017-08-30 | 2017-11-21 | 苏州惠华电子科技有限公司 | A kind of manufacture method of capacitor |
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| CN102101775B (en) * | 2010-12-08 | 2013-03-13 | 汕头高新区松田实业有限公司 | Low-loss high-voltage ceramic capacitor dielectric |
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