CN100359612C - Medium low temperature sintered high voltage ceramic capacitor medium - Google Patents
Medium low temperature sintered high voltage ceramic capacitor medium Download PDFInfo
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- CN100359612C CN100359612C CNB200410041863XA CN200410041863A CN100359612C CN 100359612 C CN100359612 C CN 100359612C CN B200410041863X A CNB200410041863X A CN B200410041863XA CN 200410041863 A CN200410041863 A CN 200410041863A CN 100359612 C CN100359612 C CN 100359612C
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- low temperature
- solid solution
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Abstract
The present invention relates to a formulation for forming high-voltage ceramic capacitor media sintered at medium and low temperature. The present invention adopts a conventional method to prepare high-voltage ceramic capacitor media, and uses the general chemistry raw material of capacitor ceramics to prepare high-voltage high-stability ceramic capacitor media which have no lead, cadmium or toxin and are sintered at medium and low temperature ranging from 1100 to 1150 DEG C. The media which are suitable for preparing monolithic ceramic capacitors and multilayer sheet ceramic capacitors can greatly reduce the cost of ceramic capacitors, and do not pollute the environment in the courses of preparation and operation. The present invention is characterized in that the medium formulation comprises (by WT%) 60 to 90% of BaTiO3, 1 to 20% of SrTiO3, 0.1 to 10% of CaZrO3, 0.01 to 1% of Nb2O5, 0.01 to 1% of MgO, 0.01 to 0.8% of CeO2, 0.01 to 0.6% of ZnO, 0.03 to 1% of Co2O3, and 0.05 to 10% of Bi-Li solid solution, wherein BaTiO3, SrTiO3 and CaZrO3 are respectively synthesized by conventional chemical raw materials in a solid phase way. The present invention has the advantages of high voltage resistance (higher than 6.0KV /mm), large dielectric constant (ranging from 2000 to 3000), small change rate of capacitor temperature, coincidence to the requirements of X7R, Y5T and Y5U characteristics, stable performance during operation, high safety, and no environmental pollution.
Description
Technical field
The prescription that the invention relates to the low temperature sintering high-voltage ceramic condenser medium is formed, refer in particular to a kind of low temperature sintering high-voltage ceramic condenser medium, be suitable for preparing monolithic ceramic capacitor and multiple-layer sheet ceramic capacitor, can reduce the cost of ceramic capacitor greatly, and free from environmental pollution in preparation and use.
Technical background
Fields such as colour TV, computer, communication, space flight, guided missile, navigation press for puncture voltage height, temperature stability good (as X7R, Y5T and Y5U characteristic etc.), ceramic capacitor that reliability is high.The sintering temperature of general single-chip high voltage ceramic capacitor dielectric is generally 1300～1400 ℃, and the sintering temperature of low temperature sintering ceramic capacitor dielectric of the present invention is 1100～1150 ℃, can reduce the cost of high voltage ceramic capacitor so greatly, the not leaded and cadmium of while this patent capacitor ceramic dielectric, condenser ceramics is free from environmental pollution in preparation and use.
High speed development along with mobile electronic devices such as polytype electronic equipment such as digital camera, mobile phone, notebook computer, palmtop PCs, miniaturization and the lightness trend that is inevitable, the components and parts that constitute these electronic equipments also must reduce volume and weight, change the needs of surface mounting technology (SMD) into the mounting technique that adapts to electronic component, the components and parts that surface mounting technology requires are chip components and parts.Multilayer ceramic capacitor is that a most widely used class multilayer ceramic capacitor (Mulltilayer CeramicCapacitor) is called for short MLCC in the chip components and parts.It is that electrode material is replaced in parallel being superimposed together with ceramic body with multilayer, and burns till an integral body simultaneously.According to the international EIA of Electronic Industries Association standard, temperature-stable (X7R) MLCC is meant that the capacitance with 25 ℃ is a benchmark, in temperature in-55 ℃～+ 125 ℃ scope, temperature coefficient of capacitance＜=+/-15%, dielectric loss (DF)＜=2.5%.X7R type MLCC is divided into two big classes by component: a class is that leaded ferroelectric is formed, and another kind of is with BaTiO
3The non-lead of base is that ferroelectric is formed.And the latter is because environmentally safe, and mechanical strength and reliability be better than the former, and therefore non-lead is BaTiO
3Base high stable MLCC has broad application prospects.
Be generally used for producing in the medium of low temperature sintering 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 had harmful effect.
The firing temperature of chip multilayer ceramic capacitor medium is 1100～1150 ℃, and interior electrode can make the cost of MLCC chip multilayer ceramic capacitor reduce greatly with the silver content interior electrode higher than 70Ag/30Pd alloy electrode.
Chinese periodical " piezoelectricity and acousto-optic " the 23rd volume the 4th phase (August calendar year 2001) is at " intermediate sintering temperature BaTiO
3Ferroelectric-the glass ceramics dielectric property " literary composition discloses a kind of low temperature sintering BaTiO
3Ferroelectric ceramic, that it adopts is high-purity, the synthetic BaTiO of fine particle careless titanyl acid liquid phase method
3Be primary raw material, will prepared ceramic capacitor cost increased.The flux of Cai Yonging is the frit that contains a large amount of lead simultaneously, and the prescription of medium is formed and also is different from patent of the present invention, and this article does not relate to withstand voltage in performance test.
Chinese periodical " South China Science ﹠ Engineering University's journal (natural science edition) " the 24th volume the 3rd phase (in March, 1996) is at " intermediate sintering temperature BaTiO
3Quito mutually ferroelectric porcelain X7R characteristic " inquired into BaTiO in the literary composition
3Base porcelain intermediate sintering temperature mechanism has been analyzed intermediate sintering temperature BaTiO
3The composition and the uneven texture of base porcelain distribute to the influence of ε-T characteristic.Used BaTiO
3Raw material is to adopt the method for chemical coprecipitation to prepare, and can increase the cost of ceramic capacitor like this, and the used BaTiO of this patent
3, SrTiO
3, CaZrO
3All be to adopt conventional chemical raw material synthetic, between the room temperature dielectric constant 1500～2000 of the material that satisfies the X7R characteristic of this article announcement simultaneously, contain a certain amount of lead in the component, and do not relate to withstand voltage with solid phase method.
Other has patent " high Jie's high-performance intermediate sintering temperature chip multilayer ceramic capacitor porcelain " (number of patent application 97117286.2), and it is to adopt synthetic equivalence of solid phase method and different valency ion to replace (Sr simultaneously
2+, Zr
4+, Sn
4+, Nb
5+) BaTiO
3Solid solution adds an amount of boron-lead-zinc-copper glass agglutinant, makes porcelain at intermediate sintering temperature, and its performance is: dielectric constant is more than or equal to 16000, tan δ＜2.5%, and percentage of capacitance variation with temperature is at-78～+ 20% (30～+ 85 ℃), and withstand voltage is 700V/mm.Though this patent dielectric constant height, percentage of capacitance variation with temperature is big, considerably beyond X7R, Y5T and Y5U characteristic, can cause in the use performance inconsistency big, the material of being reported simultaneously withstand voltage too poor only is 700V/mm, and its component contains a certain amount of lead in addition.
Also have patent " high-performance intermediate sintering temperature chip multilayer ceramic capacitor porcelain " (number of patent application 97117287.0), it adopts unique prescription (BaTiO
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 that satisfies following performance of intermediate sintering temperature: dielectric constant is 3000, tan δ＜1.5%, and withstand voltage is 860V/mm, and does not satisfy X7R, Y5T and Y5U characteristic.The flux of this patent contains a certain amount of lead, the temperature stability of this patent and withstand voltage all poor.Cause in the use performance inconsistency big, prepared capacitor safety in utilization is poor.
Summary of the invention
The purpose of this invention is to provide a kind of low temperature sintering high-voltage ceramic condenser medium.
The object of the present invention is achieved like this:
Low temperature sintering high-voltage ceramic condenser medium prescription is formed and is comprised (percentage by weight): 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 solid solution 0.05-10%.
Used bismuth lithium solid solution is to adopt following prepared in the medium of the present invention: with the chemical raw material Bi of routine
2O
3And Li
2CO
3By 89: 11 molar ratio ingredients, ground and mixed was put into alumina crucible after evenly in 850 ℃ of insulations 30 minutes down, pours into subsequently and carries out quenching in the cold water, dry after grinding up to can crossing 200 mesh sieves, bismuth lithium solid solution.
The present invention adopts conventional high-voltage ceramic condenser medium preparation technology, promptly at first adopts conventional chemical raw material to synthesize BaTiO respectively with solid phase method
3, SrTiO
3, CaZrO
3, by prescription batching the batch ball mill grinding is mixed then, after drying, add the adhesive granulation, be pressed into green sheet again, sintering in air behind insulation and natural cooling, obtains ceramic capacitor dielectric then, on medium by top electrode.
The prescription of above-mentioned ceramic dielectric preferably adopts following three kinds of schemes (percentage by weight):
1) BaTiO
373-88%, SrTiO
33-18%, CaZrO
33-8%, Nb
2O
50.3-0.6%, MgO0.01-0.3%, CeO
20.2-0.5%, ZnO 0.2-0.5%, Co
2O
30.6-0.8%, bismuth lithium solid solution 0.05-3%.
2) BaTiO
370-86%, SrTiO
31-20%, CaZrO
36-10%, Nb
2O
50.3-0.6%, MgO0.01-0.3%, CeO
20.2-0.5%, ZnO 0.2-0.5%, Co
2O
30.6-0.8%, bismuth lithium solid solution 4-7%.
3) BaTiO
366-83%, SrTiO
31-20%, CaZrO
32-8%, Nb
2O
50.3-0.6%, MgO0.1-0.5%, CeO
20.2-0.5%, ZnO 0.2-0.5%, Co
2O
30.4-1%, bismuth lithium solid solution 6-9%.
The present invention compared with prior art has following advantage:
1. the medium of this patent is low temperature sintering (1100～1150 a ℃) barium strontium based capacitor pottery, can reduce the cost of high voltage ceramic capacitor so greatly, and is not leaded in the media components of this patent simultaneously, environmentally safe.
2. this dielectric withstanding voltage height can reach more than the 6KV/mm.
3. this dielectric capacitance rate of temperature change is little, and stability is good in the use, and is safe.
4. prepared medium cost is low, and primary raw material employing ceramic capacitor level is pure can to produce ceramic dielectric of the present invention.
5. this medium technology is simple, adopts conventional solid phase method ceramic capacitor dielectric preparation technology to be prepared.
6. this medium has adopted bismuth lithium solid solution as flux, realizes low temperature sintering.
Embodiment
The invention will be further described in conjunction with the embodiments now.
Table 1,2,3 provides three groups of embodiment of the present invention prescription of totally 9 samples.First group of embodiment (sample 1,2,3) has the Y5U temperature characterisitic; Second group of embodiment (sample 4,5,6) has Y5T and X7R temperature characterisitic; The 3rd group of embodiment (sample 7,8,9) has the X7R temperature characterisitic.
Table 1
| Specimen coding | Composition (weight %) | ||||||||
| BaTiO 3 | SrTiO 3 | CaZrO 3 | Nb 2O 5 | MgO | CeO 2 | ZnO | Co 2O 3 | Bismuth lithium solid solution | |
| 1 | 73.5 | 17.3 | 6 | 0.5 | 0.2 | 0.3 | 0.4 | 0.8 | 1 |
| 2 | 74 | 16.5 | 6 | 0.6 | 0.2 | 0.2 | 0.3 | 0.7 | 1.5 |
| 3 | 74.5 | 15 | 6.5 | 0.5 | 0.2 | 0.3 | 0.3 | 0.6 | 2.1 |
Table 2
| Specimen coding | Composition (weight %) | ||||||||
| BaTiO 3 | SrTiO 3 | CaZrO 3 | Nb 2O 5 | MgO | CeO 2 | ZnO | Co 2O 3 | Bismuth lithium solid solution | |
| 4 | 72.5 | 15.5 | 6 | 0.6 | 0.25 | 0.3 | 0.4 | 0.8 | 3.65 |
| 5 | 72 | 14.5 | 6.5 | 0.6 | 0.3 | 0.3 | 0.5 | 0.8 | 4.5 |
| 6 | 71 | 15 | 6.1 | 0.6 | 0.3 | 0.25 | 0.45 | 0.8 | 5.5 |
Table 3
| Specimen coding | Composition (weight %) | ||||||||
| BaTiO 3 | SrTiO 3 | CaZrO 3 | Nb 2O 5 | MgO | CeO 2 | ZnO | Co 2O 3 | Bismuth lithium solid solution | |
| 7 | 68 | 20 | 3 | 0.6 | 0.25 | 0.3 | 0.4 | 0.8 | 6.65 |
| 8 | 69 | 18 | 3 | 0.6 | 0.3 | 0.3 | 0.5 | 0.8 | 7.5 |
| 9 | 67 | 18 | 4 | 0.6 | 0.3 | 0.25 | 0.45 | 0.8 | 8.6 |
The primary raw material of above-mentioned prescription adopts capacitor level pure, at first adopts conventional chemical raw material to synthesize BaTiO respectively with solid phase method in the preparation
3, SrTiO
3, CaZrO
3Then by above-mentioned prescription batching, adopt the planetary ball mill ball milling to mix with distilled water or deionized water in the material for preparing, material: ball: water (weight ratio)=1: 3: (0.6～1.0), behind the ball milling 4～8 hours, dry dry mash, in dry mash, add the concentration account for its weight 10% and be 10% poly-vinyl alcohol solution, carry out granulation, 40 mesh sieves are crossed in the mixed back of grinding, and carry out dry-pressing again and become green sheet under 10～20Mpa pressure, and insulation was carried out binder removal in 0.5～4 hour and burnt till under temperature is 1100 ℃～1150 ℃ then, be incubated 15 minutes down at 780 ℃～870 ℃ again and carry out silver ink firing, form silver electrode, solder taul is sealed again, promptly get capacitor, can test its dielectric property.Above-mentioned dielectric property of respectively filling a prescription sample are listed in table 4.
Table 4
| Specimen coding | Dielectric constant (ε) | Dielectric loss (* 10 -4) | Insulation resistance (* 10 10 Ω·Cm) | Percentage of capacitance variation with temperature (%) (55 ℃～+ 125 ℃) | Anti-direct voltage (KV/mm) |
| 1 | 2800 | 210 | ＞30 | -43/+21 | ＞6.0 |
| 2 | 2670 | 190 | ＞30 | -40/+18 | ＞6.0 |
| 3 | 2710 | 165 | ＞30 | -35/+21 | ＞6.0 |
| 4 | 2509 | 156 | ＞20 | -31/+20 | ＞＝6.0 |
| 5 | 2520 | 143 | ＞20 | -22/+21 | ＞＝6.0 |
| 6 | 2300 | 200 | ＞20 | -14/+13 | ＞＝6.0 |
| 7 | 2208 | 220 | ＞18 | -12.5/+11 | ＞＝6.0 |
| 8 | 2160 | 233 | ＞17 | -13/+10 | ＞＝6.0 |
| 9 | 2078 | 245 | ＞18 | -11.5/+11.5 | ＞＝6.0 |
Claims (5)
1. a low temperature sintering high stable, high-voltage ceramic condenser medium is characterized in that described medium prescription represents to comprise with percentage by weight: 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 solid solution 0.05-10%.
2. low temperature sintering high-voltage ceramic condenser medium according to claim 1 is characterized in that described medium prescription represents to comprise with percentage by weight: BaTiO
373-88%, SrTiO
33-18%, CaZrO
33-8%, Nb
2O
50.3-0.6%, MgO 0.01-0.3%, CeO
20.2-0.5%, ZnO 0.2-0.5%, Co
2O
30.6-0.8%, bismuth lithium solid solution 0.05-3%.
3. low temperature sintering high-voltage ceramic condenser medium according to claim 1 is characterized in that described medium prescription represents to comprise with percentage by weight: BaTiO
370-86%, SrTiO
31-20%, CaZrO
36-10%, Nb
2O
50.3-0.6%, MgO 0.01-0.3%, CeO
20.2-0.5%, ZnO 0.2-0.5%, Co
2O
30.6-0.8%, bismuth lithium solid solution 4-7%.
4. low temperature sintering high-voltage ceramic condenser medium according to claim 1 is characterized in that described medium prescription represents to comprise with percentage by weight: BaTiO
366-83%, SrTiO
31-20%, CaZrO
32-8%, Nb
2O
50.3-0.6%, MgO 0.1-0.5%, CeO
20.2-0.5%, ZnO 0.2-0.5%, Co
2O
30.4-1%, bismuth lithium solid solution 6-9%.
5. according to claim 1,2,3 or 4 described high-voltage ceramic condenser mediums, it is characterized in that the preparation of bismuth lithium solid solution in the described medium comprises: with the chemical raw material Bi of routine
2O
3And Li
2CO
3By 89: 11 molar ratio ingredients, ground and mixed was put into alumina crucible after evenly in 850 ℃ of insulations 30 minutes down, pours into subsequently and carries out quenching in the cold water, dry after grinding up to can crossing 200 mesh sieves, bismuth lithium solid solution.
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| CNB200410041863XA CN100359612C (en) | 2004-09-03 | 2004-09-03 | Medium low temperature sintered high voltage ceramic capacitor medium |
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| CN100359612C true CN100359612C (en) | 2008-01-02 |
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Families Citing this family (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100427430C (en) * | 2005-01-04 | 2008-10-22 | 华南理工大学 | Dielectric ceramic materials for chip capacitor and method for preparing same |
| CN100457678C (en) * | 2006-06-19 | 2009-02-04 | 同济大学 | Dielectric adjustable material of ceramics burned together at low temperature, and preparation method |
| CN1889211B (en) * | 2006-07-17 | 2011-06-15 | 钱云春 | Barium titanate Y5U capacity material formula |
| CN101386534B (en) * | 2008-10-24 | 2012-07-04 | 江苏大学 | High performance middle and low temperature sintered high-voltage ceramic capacitor medium |
| CN102060522B (en) * | 2010-11-11 | 2013-04-17 | 汕头高新区松田实业有限公司 | Dielectric medium of ceramic capacitor and preparation method thereof |
| CN102176374B (en) * | 2011-03-10 | 2013-05-08 | 江苏大学 | High voltage ceramic capacitor dielectric sintered at low temperature |
| CN102557672B (en) * | 2012-01-05 | 2014-05-28 | 江苏大学 | Additive and application thereof to reduce sintering temperature of barium-strontium titanate capacitor ceramic |
| CN103113100B (en) * | 2013-03-01 | 2014-10-29 | 江苏大学 | High-temperature stabilization ceramic capacitor dielectric |
| CN105294097B (en) * | 2015-10-22 | 2017-06-23 | 江苏科技大学 | A kind of low-loss high-temp leadless capacitor material and preparation method thereof |
| CN105261480A (en) * | 2015-10-30 | 2016-01-20 | 广州新莱福磁电有限公司 | Capacitor and permanent magnetic direct-current motor |
| CN106565238B (en) * | 2016-11-16 | 2019-10-01 | 江苏大学 | A kind of low-temperature sintering high-voltage ceramic condenser medium |
| CN107226696A (en) * | 2017-05-19 | 2017-10-03 | 淄博高新技术产业开发区先进陶瓷研究院 | X7R types BaTiO3Based capacitor ceramic material and preparation method thereof |
| CN110922186B (en) * | 2019-12-10 | 2022-01-07 | 有研工程技术研究院有限公司 | Medium-low temperature sintered high-dielectric-constant ceramic dielectric material and preparation method thereof |
| CN113563066B (en) * | 2021-08-26 | 2022-11-29 | 四川特锐祥科技股份有限公司 | Dielectric material with dielectric constant larger than 12000 and preparation method thereof |
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| JPH10270284A (en) * | 1997-03-24 | 1998-10-09 | Tdk Corp | Manufacture of dielectric ceramic material |
| JP2001181027A (en) * | 1999-12-28 | 2001-07-03 | Tdk Corp | Composite dielectric material |
| CN1306288A (en) * | 2000-01-20 | 2001-08-01 | 江苏理工大学 | Medium for high-voltage ceramic capacitor |
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2004
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4861736A (en) * | 1986-08-11 | 1989-08-29 | Tdk Corporation | Semiconductive ceramic composition |
| JPH10270284A (en) * | 1997-03-24 | 1998-10-09 | Tdk Corp | Manufacture of dielectric ceramic material |
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| CN1306288A (en) * | 2000-01-20 | 2001-08-01 | 江苏理工大学 | Medium for high-voltage ceramic capacitor |
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Assignee: Shantou High-new Development Zone Songtian Enterprise Co., Ltd. Assignor: Jiangsu University Contract fulfillment period: 2009.7.10 to 2016.7.10 Contract record no.: 2009440001173 Denomination of invention: Medium low temperature sintered high voltage ceramic capacitor medium Granted publication date: 20080102 License type: Exclusive license Record date: 2009.8.11 |
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