CN101386534B - High performance middle and low temperature sintered high-voltage ceramic capacitor medium - Google Patents
High performance middle and low temperature sintered high-voltage ceramic capacitor medium Download PDFInfo
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- CN101386534B CN101386534B CN2008101550569A CN200810155056A CN101386534B CN 101386534 B CN101386534 B CN 101386534B CN 2008101550569 A CN2008101550569 A CN 2008101550569A CN 200810155056 A CN200810155056 A CN 200810155056A CN 101386534 B CN101386534 B CN 101386534B
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Abstract
The invention provides a medium of a high-voltage ceramic capacitor with high performance and middle-low temperature sintering, which relates to the technical field of inorganic non-metal material. The invention adopts the prior method for preparing the medium of the high-voltage ceramic capacitor to prepare the medium of the high-voltage high-stability ceramic capacitor containing no lead, cadmium or other toxicities, and having high performance and middle-low temperature sintering (the sintering temperature is between 1,100 and 1,150 DEG C) by the prior chemical raw materials of capacitor ceramics. The medium is applicable to the preparation of single-chip ceramic capacitor and multi-layer tablet ceramic capacitor so as to greatly reduce the cost for the ceramic capacitor and avoid environmental pollution during preparation and application. The medium is characterized in that the medium comprises the following compositions (in weight percentage): 58 to 92 percent of BaTiO3, 2 to 19 percent of SrTiO3, 0.5 to 10 percent of CaZrO3, 0.05 to 1 percent of Nb2O5, 0.03 to 1.0 percent of Y2O3, 0.03 to 1.0 percent of Co2O3, and 6 to 30 percent of Bi2Sn2O7, wherein each of the BaTiO3, the SrTiO3 and the CaZrO3 is synthesized by a solid phase method by the prior chemical materials. The medium has high voltage resistance reaching over 10 kilovolt/millimeter, specific inductive capacity of between 2,200 and 3,500 and small variance ratio of capacitance temperature, accords with the requirement on X7R property, Y5T and Y5U property, has excellent stability and high security when used, and does not pollute environment.
Description
Technical field
The present invention relates to technical field of inorganic nonmetallic materials, refer in particular to a kind of high-performance low temperature sintering high-voltage ceramic condenser medium.It adopts conventional ceramic capacitor dielectric preparation method; Utilize condenser ceramics general chemistry raw material; Prepare high-performance low temperature sintering (sintering temperature is 1100～1150 ℃) high pressure high stable ceramic capacitor dielectric unleaded, no cadmium; This medium is 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, Aero-Space, guided missile, navigation press for puncture voltage height, temperature stability good (like X7R characteristic etc.), ceramic capacitor that reliability is high.The sintering temperature of general single-chip high voltage ceramic capacitor dielectric is 1300～1400 ℃; And low temperature sintering ceramic capacitor dielectric temperature 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 development 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 the multilayer sheet type components and parts.Multilayer ceramic capacitor is most widely used one type of multilayer ceramic capacitor (MLCC) in the chip components and parts.It is that electrode material is replaced parallelly connected 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 smaller or equal to+/-15%, dielectric loss is smaller or equal to 2.5%.X7R type MLCC is divided into two big types by component: one type 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 the property examined be superior to 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 sintering temperature of 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 " electronic component and material " the 4th phase in 1993 discloses a kind of BaTiO at " a kind of X7R porcelain that is used for multilayer chip capacitor " literary composition
3-PbBi
4Ti
4O
15-PbNb
2O
6The low temperature sintering condenser dielectric though be the X7R porcelain of low temperature sintering, contains a large amount of lead in the prescription.
Chinese periodical " piezoelectricity and acousto-optic " the 4th phase of calendar year 2001 is at " intermediate sintering temperature BaTiO
3Ferroelectric-the glass ceramics dielectric properties " a kind of low-temperature sintering BaTiO is disclosed in the literary composition
3Ferroelectric ceramics, that it adopts is high-purity, the synthetic BaTiO of fine grained careless titanyl acid liquid phase method
3Be primary raw material, will prepared ceramic capacitor cost increased.The flux that adopts simultaneously is the frit that contains great quantity of Pb, 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 " 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 of X7R characteristic, and the prescription 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, used low-melting glass material is the lead borosilicate low-melting glass, and medium is leaded, and the prescription of medium is formed and also is different from patent of the present invention, and the dielectric withstanding voltage of being announced is relatively poor.
Chinese periodical " silicate circular " the 1st phase in 1999 discloses the influence of technology to the high Jie's high stable of intermediate sintering temperature MLC medium electrical property in " influence of technology high Jie's high stable MLC medium electrical property to intermediate sintering temperature " literary composition, and unexposed prescription is formed.
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 " 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 dielectric constant and temperature characterisitic.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
3Be respectively to adopt conventional chemical raw material synthetic, form and be different from this patent, 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 ", and (number of patent application: 97117286.2), 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, and percentage of capacitance variation with temperature is at-78～+ 20% (30～+ 85 ℃), and withstand voltage is 700V/mm.Though this patent dielectric constant is high, percentage of capacitance variation with temperature is big, does not satisfy X7R, Y5T, Y5U characteristic, can cause in the use performance inconsistency big, and the material of being reported simultaneously withstand voltage too poor is merely 700V/mm, and its component contains a certain amount of lead in addition.
(number of patent application: 97117287.0), it adopts unique prescription (percentage by weight) (BaTiO to also have Chinese patent CN1212444A " high-performance intermediate sintering temperature 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 that satisfies following performance of intermediate sintering temperature: dielectric constant is 3000; Dielectric loss is less than 1.5%; 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, the capacitor of gained uses stability poor.
(number of patent application: 200410041863.x), it adopts unique prescription (percentage by weight) (BaTiO to also have Chinese patent " a kind of low temperature sintering high-voltage ceramic condenser medium "
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 that satisfies following performance of intermediate sintering temperature: dielectric constant is 2000～3000, and withstand voltage is more than the 6kV/mm, and the additive that reduces sintering temperature is a bismuth lithium solid solution; Concrete prescription is formed and is different from this patent; And the condenser ceramics that satisfies following performance of the intermediate sintering temperature that this patent obtains: dielectric constant is 2200～3500, and withstand voltage is more than the 10kV/mm, and the additive that reduces sintering temperature is Bi
2Sn
2O
7The dielectric constant of this patent and withstand voltage higher than this patent.
Summary of the invention
The purpose of this invention is to provide a kind of high-performance low temperature sintering high-voltage ceramic condenser medium.
The objective of the invention is to realize like this:
Low temperature sintering high-voltage ceramic condenser medium prescription is formed and is comprised (percentage by weight):
BaTiO
358-92％，SrTiO
32-19％，CaZrO
30.5-10％，Nb
2O
50.05-1％，Y
2O
30.03-0.8％，Co
2O
30.3-0.8％，Bi
2Sn
2O
76-30％；
BaTiO wherein
3, SrTiO
3, CaZrO
3Be respectively to adopt conventional chemical raw material synthetic with solid phase method.Bi
2Sn
2O
7Consist of (mol ratio): Bi
2O
3/ SnO
2=1:2.
Used Bi in the medium of the present invention
2Sn
2O
7Be to adopt following prepared: with the chemical raw material Bi of routine
2O
3And SnO
2Press the 1:2 molar ratio ingredient, put into alumina crucible in 1000 ℃ of insulations 600 minutes after ground and mixed is even, solid phase reaction is synthesized Bi
2Sn
2O
7, ground 200 mesh sieves, subsequent use.
The present invention adopts conventional high-voltage ceramic condenser medium preparation technology, promptly at first adopts conventional chemical raw material with the synthetic respectively BaTiO of 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 then, behind insulation and natural cooling, the acquisition ceramic capacitor dielectric, on medium by electrode.
The prescription of above-mentioned ceramic dielectric preferably adopts following three kinds of schemes (percentage by weight):
BaTiO
366-82％，SrTiO
32-19％，CaZrO
33-7％，Nb
2O
50.5-0.8％，Y
2O
30.3-0.6％，
Co
2O
30.3-0.7％，Bi
2Sn
2O
76-8％；
BaTiO
370-84％，SrTiO
32-19％，CaZrO
35-8％，Nb
2O
50.5-0.8％，Y
2O
30.3-0.6％，
Co
2O
30.5-0.7％，Bi
2Sn
2O
710-20％；
BaTiO
376-87％，SrTiO
35-16％，CaZrO
33-8％，Nb
2O
50.5-0.8％，Y
2O
30.3-0.6％，
Co
2O
30.3-0.7％，Bi
2Sn
2O
720-30％。
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, environmentally safe.
2, the withstand voltage height of this medium can reach more than the 10kV/mm.The dielectric constant of this medium is high, can realize the miniaturization of ceramic capacitor.
3, the percentage of capacitance variation with temperature of this medium is little, and stability is good in the use, and is safe.
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 prepare.
6, this medium adopts Bi
2Sn
2O
7As modification and flux, can keep realizing low temperature sintering on the high performance basis.
Embodiment
Combine embodiment that the present invention is done further description now.
Table 1 provides the embodiments of the invention prescription of totally 6 samples.
The embodiments of the invention primary raw material of the prescription of totally 6 samples adopt the ceramic capacitor level pure, at first adopt conventional chemical raw material with the synthetic respectively BaTiO of solid phase method in the preparation
3, SrTiO
3, CaZrO
3, then by above-mentioned prescription batching, the material for preparing is adopted the planetary ball mill ball mill mixing with distilled water or deionized water, material: ball: water=1:3: (0.6～1.0), ball milling is after 4～8 hours, dry dry mash, in dry mash, add and account for its weight
Table 1 embodiments of the invention are the prescription of totally 6 samples
8～10% concentration is 10% poly-vinyl alcohol solution, carries out granulation, and 40 mesh sieves are crossed in the mixed back of grinding; Under 10～20Mpa pressure, carry out dry-pressing again and become green sheet, binder removal and sintering were carried out in insulation in 1～4 hour under temperature is 1100～1150 ℃ then, were incubated 15 minutes down at 780～870 ℃ again and carried out silver ink firing; Form silver electrode, solder taul is sealed again; Promptly get ceramic capacitor, test its dielectric property.Above-mentioned dielectric property of respectively filling a prescription sample are listed in table 2.
Respectively the fill a prescription dielectric property of sample of table 2
| ? | Dielectric constant | Dielectric loss (* 10 -4) | Insulation resistance (* 10 10Ohmcm) | Percentage of capacitance variation with temperature (%) (55～+ 125 ℃) | Anti-direct voltage (kV/mm) |
| 1 | 3406 | 205 | >;60 | -52/+23 | >;10 |
| 2 | 3210 | 200 | >;60 | -42/+19 | >;10 |
| 3 | 2860 | 183 | >;50 | -36/+28 | >;10 |
| 4 | 2730 | 201 | >;50 | -24/+26 | >;10 |
| 5 | 2436 | 210 | >;42 | -13/+14 | >;10 |
| 6 | 2260 | 224 | >;42 | -12/+10.3 | >;10 |
Claims (5)
1. a low temperature sintering high stable, high-voltage ceramic condenser medium is characterized in that said medium prescription representes to comprise with percentage by weight: BaTiO
358-92%, SrTiO
32-19%, CaZrO
30.5-10%, Nb
2O
50.05-1%, Y
2O
30.03-0.8%, Co
2O
30.3-0.8%, Bi
2Sn
2O
76-30%, the weight percentage sum of each component is 100%.
2. a kind of low temperature sintering high stable according to claim 1, high-voltage ceramic condenser medium is characterized in that: BaTiO
3, SrTiO
3, CaZrO
3Be respectively to adopt conventional chemical raw material synthetic with solid phase method, Bi
2Sn
2O
7Composition Bi
2O
3And SnO
2Mol ratio be 1: 2.
3. a kind of low temperature sintering high stable according to claim 1, high-voltage ceramic condenser medium is characterized in that said medium prescription representes to comprise with percentage by weight: BaTiO
366-82%, SrTiO
32-19%, CaZrO
33-7%, Nb
2O
50.5-0.8%, Y
2O
30.3-0.6%, Co
2O
30.3-0.7%, Bi
2Sn
2O
76-8%.
4. a kind of low temperature sintering high stable according to claim 1, high-voltage ceramic condenser medium is characterized in that said medium prescription representes to comprise with percentage by weight: BaTiO
370-84%, SrTiO
32-19%, CaZrO
35-8%, Nb
2O
50.5-0.8%, Y
2O
30.3-0.6%, Co
2O
30.5-0.7%, Bi
2Sn
2O
710-20%.
5. according to claim 1,2,3 or 4 described a kind of low temperature sintering high stables, high-voltage ceramic condenser medium, it is characterized in that: Bi
2Sn
2O
7The preparation method be: with the chemical raw material Bi of routine
2O
3And SnO
2By 1: 2 molar ratio ingredient, put into alumina crucible in 1000 ℃ of insulations 600 minutes after ground and mixed is even, solid phase reaction is synthesized Bi
2Sn
2O
7, ground 200 mesh sieves, subsequent use.
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|---|---|---|---|
| CN2008101550569A CN101386534B (en) | 2008-10-24 | 2008-10-24 | High performance middle and low temperature sintered high-voltage ceramic capacitor medium |
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|---|---|---|---|
| CN2008101550569A CN101386534B (en) | 2008-10-24 | 2008-10-24 | High performance middle and low temperature sintered high-voltage ceramic capacitor medium |
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| Publication Number | Publication Date |
|---|---|
| CN101386534A CN101386534A (en) | 2009-03-18 |
| CN101386534B true CN101386534B (en) | 2012-07-04 |
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|---|---|---|---|
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101792312A (en) * | 2010-03-10 | 2010-08-04 | 天津大学 | SrTiO3 ceramic dielectric material and preparation method of capacitor thereof |
| CN102354599B (en) * | 2011-06-30 | 2013-05-01 | 广东风华高新科技股份有限公司 | Preparation method for temperature compensation type multi-layer ceramic chip capacitor |
| CN103113100B (en) * | 2013-03-01 | 2014-10-29 | 江苏大学 | High-temperature stabilization ceramic capacitor dielectric |
| CN103408302B (en) * | 2013-07-19 | 2015-02-04 | 江苏大学 | High permittivity and high temperature stability ceramic capacitor medium and its preparation method |
| CN103664163B (en) * | 2013-10-08 | 2015-07-08 | 江苏大学 | Medium for highly-dielectric grain boundary layer ceramic capacitor and preparation method thereof |
| CN104628378B (en) * | 2015-02-05 | 2017-02-22 | 汕头高新区松田实业有限公司 | Medium for copper electrode ceramic capacitor and preparation method thereof |
| CN105645952B (en) * | 2015-12-30 | 2017-03-15 | 北京七星飞行电子有限公司 | A kind of little loss super-pressure ceramic capacitor dielectric material |
| CN106587988B (en) * | 2016-11-14 | 2019-10-01 | 江苏大学 | A kind of High-temperature stabilization ceramic capacitor dielectric |
| CN106565238B (en) * | 2016-11-16 | 2019-10-01 | 江苏大学 | A kind of low-temperature sintering high-voltage ceramic condenser medium |
| CN114133238B (en) * | 2021-11-02 | 2022-09-16 | 广东省先进陶瓷材料科技有限公司 | Ceramic dielectric material and preparation method and application thereof |
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|---|---|---|---|---|
| CN1619726A (en) * | 2004-09-03 | 2005-05-25 | 江苏大学 | Medium low temperature sintered high voltage ceramic capacitor medium |
| CN101048345A (en) * | 2004-08-31 | 2007-10-03 | 昭和电工株式会社 | Barium titanate and its manufacturing method as well as capacitor |
| CN101131894A (en) * | 2007-09-26 | 2008-02-27 | 江苏大学 | Medium for high-voltage ceramic capacitor |
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2008
- 2008-10-24 CN CN2008101550569A patent/CN101386534B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101048345A (en) * | 2004-08-31 | 2007-10-03 | 昭和电工株式会社 | Barium titanate and its manufacturing method as well as capacitor |
| CN1619726A (en) * | 2004-09-03 | 2005-05-25 | 江苏大学 | Medium low temperature sintered high voltage ceramic capacitor medium |
| CN101131894A (en) * | 2007-09-26 | 2008-02-27 | 江苏大学 | Medium for high-voltage ceramic capacitor |
Non-Patent Citations (2)
| Title |
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| JP平4-26545A 1992.01.29 |
| JP特开2005-268712A 2005.09.29 |
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