CN102557672A - Additive and application thereof to reduce sintering temperature of barium-strontium titanate capacitor ceramic - Google Patents
Additive and application thereof to reduce sintering temperature of barium-strontium titanate capacitor ceramic Download PDFInfo
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- CN102557672A CN102557672A CN2012100011670A CN201210001167A CN102557672A CN 102557672 A CN102557672 A CN 102557672A CN 2012100011670 A CN2012100011670 A CN 2012100011670A CN 201210001167 A CN201210001167 A CN 201210001167A CN 102557672 A CN102557672 A CN 102557672A
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- additive
- sintering temperature
- libio
- barium strontium
- glass powder
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention relates to the technical field of inorganic non-metal materials, in particular to an additive and application thereof to reduce the sintering temperature of barium-strontium titanate capacitor ceramic. The additive is characterized in that the adding amount of the additive for reducing the sintering temperature is 1 to 8 mass percent; the additive comprises 44 to 65 mass percent of LiBiO2, 0.5 to 20 mass percent of CuO and 25 to 45 mass percent of Li2O-B2O3-ZnO glass powder. According to the low-temperature sintering capacitor ceramic prepared by adding the additive, the sintering temperature is low and between 900 and 920 DEG C; high voltage can be resisted and can reach more than 10 kV/mm (direct current voltage, DC) and 4 kV/mm (alternating voltage, AC); the dielectric constant is high and can reach about 3,000; the capacitance temperature change ratio is small and accords with the requirement of X7R characteristic; the dielectric loss is less than 1.5 percent; and during the using process, performance stability and safety are high and environmental pollution is avoided.
Description
Technical field
The present invention relates to technical field of inorganic nonmetallic materials, refer in particular to the purposes of a kind of additive and reduction barium strontium condenser ceramics sintering temperature thereof, adopt special additive LiBiO
2+ CuO+ Li
2O-B
2O
3-ZnO glass powder reduces the sintering temperature of condenser ceramics; Obtain low-temperature sintering (900 ~ 920 ℃) barium strontium high voltage capacitor ceramic dielectic; This medium is suitable for preparing monolithic ceramic capacitor and multiple-layer sheet ceramic capacitor; The cost of ceramic condenser can be reduced greatly, the range of application of proof voltage can be improved simultaneously with the expansion ceramic condenser, and free from environmental pollution in preparation and use.
Background technology
Fields such as colour TV, computer, communication, aerospace, guided missile, navigation press for the voltage breakdown height, temperature stability is good, safety is high, miniaturized, jumbo ceramic condenser; The sintering temperature of general single-chip high voltage ceramic capacitor dielectric is 1300 ~ 1400 ℃; And the high-voltage ceramic condenser medium sintering temperature of utilizing additive of the present invention to obtain is 900 ~ 920 ℃; Can reduce the cost of high voltage ceramic capacitor so greatly; Can adopt high Pd/Ag alloy of Ag or Ag content etc. as interior electrode, reduce the cost of laminated ceramic capacitor greatly; The not leaded and cadmium of capacitor ceramic dielectric of the additive of the reduction sintering temperature of this patent acquisition simultaneously, condenser ceramics is free from environmental pollution in preparation and use; In addition, utilize the specific inductivity of the condenser ceramics that additive of the present invention obtains higher, the capacity and the miniaturized that can improve ceramic condenser like this, sintering temperature is low, meets the development trend of ceramic condenser, can reduce the cost of ceramic condenser greatly.
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 detrimentally affect.
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), and sintering temperature is 1260-1400 ℃, and is high more a lot of than this patent; Specific inductivity is lower than this patent, and sintering temperature is high.
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 plumbiferous, and does not relate to proof voltage, and sintering temperature is minimum to be 1080 ℃, and higher than this patent, the low-temperature sintering additive that is adopted also is 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 " inquired into BaTiO in the literary composition
3Base porcelain intermediate sintering temperature mechanism has been analyzed intermediate sintering temperature BaTiO
3The composition of base porcelain and uneven texture distribute to the influence of specific inductivity and temperature profile; Used BaTiO
3Raw material is to adopt the method for chemical coprecipitation to prepare, and can increase the cost of ceramic condenser like this, and the used BaTiO of this patent
3, SrTiO
3, CaZrO
3Be to adopt conventional chemical feedstocks synthetic, form and be different from this patent that contain a certain amount of lead in the component, and do not relate to proof voltage, sintering temperature is minimum to be 1050 ℃, higher than this patent respectively 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
3Sosoloid adds an amount of boron-lead-zinc-copper glass agglutinant, makes porcelain at intermediate sintering temperature, and its performance is: specific inductivity is more than or equal to 16000, and withstand voltage is 700V/mm; Though this patent specific inductivity is high, the material of being reported withstand voltage too poor is merely 700V/mm; Its component contains a certain amount of lead in addition; This patent sintering temperature is 1080-1140 ℃, and higher than this patent, the low-temperature sintering additive that is adopted also is different from patent of the present invention.
Other has patent " method of manufacture of high-voltage ceramic condenser medium " (patent No. 91101958.8); It adopts unconventional prepared medium; Be the flow casting molding film, laminated medium body then, with the multilayered medium body carry out the even pressure of heating under vacuum, punching, then carry out binder removal, burn till and get; The shortcoming of this patent is preparation technology's method complicacy, causes cost of goods manifactured to increase that the sintering temperature of this patented medium is 1080-1330 ℃, than the height of this patent.
(number of patent application: 97117287.0), it adopts unique prescription (weight percent) (BaTiO to also have Chinese patent " high-performance intermediate sintering temperature chip multilayer ceramic capacitor porcelain "
393 ~ 96%+Nb
2O
50.8 ~ 1.5%+Bi
2O
31.0 ~ 2.2%+ fusing assistant 1.8 ~ 3.5%+ properties-correcting agent 0.25 ~ 1.0%) obtain the condenser ceramics that satisfies following performance of intermediate sintering temperature: specific inductivity is 3000, and dielectric loss is less than 1.5%, and withstand voltage is 860V/mm; The fusing assistant of this patent contains a certain amount of lead, and the proof voltage of this patent is too poor, and specific inductivity is low simultaneously, and less than this patent, the sintering temperature of this medium is 1100-1140 ℃, and than the height of this patent, the low-temperature sintering additive that is adopted also is different from patent of the present invention.
(number of patent application: 200410041863.x), it adopts unique prescription (weight percent) (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 sosoloid 0.05-10%) obtain the condenser ceramics that satisfies following performance of intermediate sintering temperature: specific inductivity is 2000 ~ 3000, and proof voltage is more than the 6kV/mm, and the additive that reduces sintering temperature is a bismuth lithium sosoloid; The specific inductivity of this patent and proof voltage are high less than this patent; The condenser ceramics sintering temperature that this patent is announced is 1100-1150 ℃, and is higher than this patent, and the additive that this patent is used to reduce sintering temperature is different from this patent.
Summary of the invention
The additive and the add-on thereof that the purpose of this invention is to provide the high voltage capacitor ceramic sintering temperature of reduction barium strontium-Niobium Pentxoxide-cobalt sesquioxide basic recipe system.
The objective of the invention is to realize like this:
With barium strontium-Niobium Pentxoxide-cobalt sesquioxide is basic recipe system (Ba
0.71Sr
0.29TiO
3+ 0.5% (quality) Nb
2O
5+ 0.3% (quality) Co
2O
3), to calculate by mass percentage, the amount of additive is 1～8% of a basic recipe system, the component in the additive is in mass percent: LiBiO
244 ~ 65%, CuO0.5 ~ 20%, Li
2O-B
2O
3-ZnO glass powder 25 ~ 45%.
The present invention adopts conventional high-voltage ceramic condenser medium preparation technology, promptly at first adopts conventional chemical feedstocks with the synthetic respectively BaTiO of solid phase method
3, SrTiO
3, LiBiO
2, Li
2O-B
2O
3-ZnO glass powder mixes the admixtion ball mill pulverizing by the prescription batching, after drying then; Add the tackiness agent granulation, be pressed into green sheet again, in air, carry out binder removal and sintering then; Behind insulation and naturally cooling, obtain ceramic capacitor dielectric, on medium, surveyed performance and get final product by electrode.
Above-mentioned additive and add-on thereof of falling barium strontium high voltage capacitor ceramic sintering temperature preferably adopts following three kinds of schemes (mass percent):
(1) amount of additive is 1～8% of a basic recipe system, (quality): LiBiO in the additive
244 ~ 65%, CuO0.5 ~ 20%, Li
2O-B
2O
3-ZnO glass powder 25 ~ 45%.
(2) amount of additive is 2～7% of a basic recipe system, (quality): LiBiO in the additive
246 ~ 63%, CuO2 ~ 18%, Li
2O-B
2O
3-ZnO glass powder 27 ~ 43%.
(3) amount of additive is 3～6% of a basic recipe system, (quality): LiBiO in the additive
247 ~ 60%, CuO5 ~ 16%, Li
2O-B
2O
3-ZnO glass powder 28 ~ 40%.
The present invention compared with prior art has following advantage:
1, utilizing the medium of the additive acquisition of this patent is low-temperature sintering (sintering temperature is 900 ~ 920 ℃) barium strontium based capacitor pottery; Can reduce the cost of high voltage ceramic capacitor so greatly; Not leaded and cadmium in the media components of this patent, environmentally safe.
2, utilizing the specific inductivity of the medium that the additive of this patent obtains higher, is about 3000; Proof voltage is high, the direct current proof voltage can reach that 10kV/mm is above, 4kV/mm (voltage of alternating current, AC) more than; Dielectric loss is little, less than 1.5%.The specific inductivity of this medium is higher, can realize the miniaturized and the large vol of ceramic condenser, can reduce cost equally.
3, utilize the percentage of capacitance variation with temperature of the medium that the additive of this patent obtains little, meet the requirement of X7R characteristic.Dielectric loss is less than 1.5%, and stability is good in the use, and is safe.
4, utilize the main raw material of the medium that the additive of this patent obtains to adopt that the ceramic condenser level is pure can to produce capacitor ceramic dielectric.
5, utilize the capacitor ceramic dielectric of the additive acquisition of this patent to adopt conventional solid phase method ceramic capacitor dielectric preparation technology to prepare.
Embodiment
Combine embodiment that the present invention is done further description now.
With barium strontium-Niobium Pentxoxide-cobalt sesquioxide is the basic recipe system, and barium strontium is Ba
0.71Sr
0.29TiO
3, the Niobium Pentxoxide add-on is Ba
0.71Sr
0.29TiO
30.5% of weight, cobalt sesquioxide add-on are Ba
0.71Sr
0.29TiO
30.3% of weight, basic recipe system are 100g.
Table 1,2 provides 6 prescriptions of two groups of embodiment of the present invention, and the main raw material of 6 prescriptions of two groups of embodiment adopts the ceramic condenser level pure, at first adopts conventional chemical feedstocks with the synthetic respectively BaTiO of solid phase method in the preparation
3, SrTiO
3, LiBiO
2, Li
2O-B
2O
3-ZnO glass powder then by the prescription batching, adopts the planetary ball mill ball mill mixing with the material for preparing with zero(ppm) 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 the concentration account for its weight 8 ~ 10% and be 10% polyvinyl alcohol solution, carry out granulation, mix and grind the back and cross 40 mesh sieves; Under 20 ~ 30Mpa 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 900 ~ 920 ℃ then, were incubated 15 minutes down at 780 ~ 800 ℃ again and carried out silver ink firing; Form silver electrode, solder taul is sealed again; Promptly get ceramic condenser, test its dielectric properties, above-mentioned dielectric properties of respectively filling a prescription sample are listed in table 3.
Can find out that from table 3 prepared condenser ceramics proof voltage is high, can reach 10kV/mm (volts DS, DC) above, 4kV/mm (voltage of alternating current, AC) more than; Specific inductivity is about 3000; Dielectric loss is less than 1.5%; Percentage of capacitance variation with temperature is little, meets the requirement of X7R characteristic.
LiBiO
2The preparation process following: with Bi
2O
3And Li
2CO
3With the material mixed grinding mixing of the molar ratio of 1:1, compound is placed in the corundum crucible at 800 ℃ to 820 ℃ insulation preparation in 30 minutes LiBiO down
2, grind up to crossing 200 mesh sieves the cooling back, stays with subsequent use.
Li
2O-B
2O
3The preparation process of-ZnO glass powder is following: with Li
2CO
3: B
2O
3: ZnO is with the material mixed grinding mixing of the molar ratio of 1:3:1, and compound is placed in the corundum crucible and is incubated 40 minutes down at 810 ℃ to 840 ℃, pours quenching in the cold water subsequently into, grinds up to crossing 200 mesh sieves after the drying, stays with subsequent use.
The add-on of table 1 additive and composition
The add-on of table 2 additive and composition
Respectively the fill a prescription dielectric properties of sample of table 3
Claims (10)
1. additive, it is characterized in that: the component in the additive is in mass percent: LiBiO
244 ~ 65%, CuO0.5 ~ 20%, Li
2O-B
2O
3-ZnO glass powder 25 ~ 45%.
2. a kind of additive as claimed in claim 1 is characterized in that: the component in the additive is in mass percent: LiBiO
246 ~ 63%, CuO2 ~ 18%, Li
2O-B
2O
3-ZnO glass powder 27 ~ 43%.
3. a kind of additive as claimed in claim 1 is characterized in that: the component in the additive is in mass percent:: LiBiO
247 ~ 60%, CuO5 ~ 16%, Li
2O-B
2O
3-ZnO glass powder 28 ~ 40%.
4. like claim 1,2 or 3 described a kind of additives, it is characterized in that: LiBiO
2The preparation process following: with Bi
2O
3And Li
2CO
3With the material mixed grinding mixing of the molar ratio of 1:1, compound is placed in the corundum crucible at 800 ℃ to 820 ℃ insulation preparation in 30 minutes LiBiO down
2, grind up to crossing 200 mesh sieves the cooling back, stays with subsequent use.
5. like claim 1,2 or 3 described a kind of additives, it is characterized in that: Li
2O-B
2O
3The preparation process of-ZnO glass powder is following: with Li
2CO
3: B
2O
3: ZnO is with the material mixed grinding mixing of the molar ratio of 1:3:1, and compound is placed in the corundum crucible and is incubated 40 minutes down at 810 ℃ to 840 ℃, and to going into quenching in the cold water, the dry grinding later on up to crossing 200 mesh sieves stayed with subsequent use subsequently.
6. a kind of additive as claimed in claim 1 is in the purposes that reduces barium strontium condenser ceramics sintering temperature, and it is characterized in that: with barium strontium-Niobium Pentxoxide-cobalt sesquioxide is the basic recipe system, calculates by mass percentage; The amount of additive is 1～8% of a basic recipe system; By the prescription batching admixtion ball mill pulverizing is mixed, after drying, add the tackiness agent granulation; Be pressed into green sheet again; In air, carry out binder removal and sintering then, behind insulation and naturally cooling, obtain condenser ceramics.
7. a kind of additive as claimed in claim 6 is in the purposes that reduces barium strontium condenser ceramics sintering temperature, and it is characterized in that: said basic recipe system is Ba
0.71Sr
0.29TiO
3+ Ba
0.71Sr
0.29TiO
30.5% Nb of weight
2O
5+ Ba
0.71Sr
0.29TiO
30.3% Co of weight
2O
3
8. a kind of additive as claimed in claim 6 is characterized in that in the purposes that reduces barium strontium condenser ceramics sintering temperature: calculate by mass percentage, additive is 2～7% of a basic recipe system.
9. a kind of additive as claimed in claim 6 is characterized in that in the purposes that reduces barium strontium condenser ceramics sintering temperature: calculate by mass percentage, additive is 3～6% of a basic recipe system.
10. a kind of additive as claimed in claim 6 is characterized in that in the purposes that reduces barium strontium condenser ceramics sintering temperature: at first adopt conventional chemical feedstocks with the synthetic respectively BaTiO of solid phase method in the preparation
3, SrTiO
3, LiBiO
2, Li
2O-B
2O
3-ZnO glass powder then by the prescription batching, adopts the planetary ball mill ball mill mixing with the material for preparing with zero(ppm) 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 the concentration account for its weight 8 ~ 10% and be 10% polyvinyl alcohol solution; Carry out granulation, 40 mesh sieves are crossed in the mixed back of grinding, and under 20 ~ 30Mpa pressure, carry out dry-pressing again and become green sheet; Insulation was carried out binder removal and sintering in 1 ~ 4 hour under temperature is 900 ~ 920 ℃ then, promptly got condenser ceramics.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210001167.0A CN102557672B (en) | 2012-01-05 | 2012-01-05 | Additive and application thereof to reduce sintering temperature of barium-strontium titanate capacitor ceramic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210001167.0A CN102557672B (en) | 2012-01-05 | 2012-01-05 | Additive and application thereof to reduce sintering temperature of barium-strontium titanate capacitor ceramic |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102557672A true CN102557672A (en) | 2012-07-11 |
| CN102557672B CN102557672B (en) | 2014-05-28 |
Family
ID=46404460
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210001167.0A Expired - Fee Related CN102557672B (en) | 2012-01-05 | 2012-01-05 | Additive and application thereof to reduce sintering temperature of barium-strontium titanate capacitor ceramic |
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|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103664163A (en) * | 2013-10-08 | 2014-03-26 | 江苏大学 | Medium for highly-dielectric grain boundary layer ceramic capacitor and preparation method thereof |
| CN108191428A (en) * | 2018-02-02 | 2018-06-22 | 天津大学 | It is a kind of to prepare SrTiO3The method of base huge dielectric constant medium ceramic material |
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|---|---|---|---|---|
| CN1326203A (en) * | 1996-07-05 | 2001-12-12 | 株式会社村田制作所 | Stacked ceramic capacitor with dielectric ceramic composition |
| CN1350312A (en) * | 2000-10-24 | 2002-05-22 | 株式会社村田制作所 | Insulating ceramic and its preparation method, and multi-layer ceramic capacitor |
| CN1619726A (en) * | 2004-09-03 | 2005-05-25 | 江苏大学 | Medium low temperature sintered high voltage ceramic capacitor medium |
| CN101348369A (en) * | 2008-09-06 | 2009-01-21 | 广东风华高新科技股份有限公司 | Barium titanate ceramic dielectric material |
| CN101805183A (en) * | 2010-03-02 | 2010-08-18 | 中国科学院上海硅酸盐研究所 | A low-temperature sintered Pb (Ni1/3Nb2/3) O3-Pb (Zr, ti) O3ceramic powder and its prepn |
-
2012
- 2012-01-05 CN CN201210001167.0A patent/CN102557672B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1326203A (en) * | 1996-07-05 | 2001-12-12 | 株式会社村田制作所 | Stacked ceramic capacitor with dielectric ceramic composition |
| CN1350312A (en) * | 2000-10-24 | 2002-05-22 | 株式会社村田制作所 | Insulating ceramic and its preparation method, and multi-layer ceramic capacitor |
| CN1619726A (en) * | 2004-09-03 | 2005-05-25 | 江苏大学 | Medium low temperature sintered high voltage ceramic capacitor medium |
| CN101348369A (en) * | 2008-09-06 | 2009-01-21 | 广东风华高新科技股份有限公司 | Barium titanate ceramic dielectric material |
| CN101805183A (en) * | 2010-03-02 | 2010-08-18 | 中国科学院上海硅酸盐研究所 | A low-temperature sintered Pb (Ni1/3Nb2/3) O3-Pb (Zr, ti) O3ceramic powder and its prepn |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103664163A (en) * | 2013-10-08 | 2014-03-26 | 江苏大学 | Medium for highly-dielectric grain boundary layer ceramic capacitor and preparation method thereof |
| CN108191428A (en) * | 2018-02-02 | 2018-06-22 | 天津大学 | It is a kind of to prepare SrTiO3The method of base huge dielectric constant medium ceramic material |
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| Publication number | Publication date |
|---|---|
| CN102557672B (en) | 2014-05-28 |
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