CN102557672B - 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 PDF

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CN102557672B
CN102557672B CN201210001167.0A CN201210001167A CN102557672B CN 102557672 B CN102557672 B CN 102557672B CN 201210001167 A CN201210001167 A CN 201210001167A CN 102557672 B CN102557672 B CN 102557672B
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additive
sintering temperature
libio
mass percent
condenser ceramics
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CN102557672A (en
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黄新友
高春华
李言
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Jiangsu University
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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

The purposes of a kind of additive and reduction barium strontium condenser ceramics sintering temperature thereof
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 dust reduces the sintering temperature of condenser ceramics, obtain low-temperature sintering (900 ~ 920 ℃) barium strontium high-voltage capacitor ceramic dielectric, this medium is suitable for preparing monolithic ceramic capacitor and multiple-layer sheet ceramic capacitor, can greatly 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 fields such as colour TV, computer, communication, Aero-Space, guided missile, navigation are high in the urgent need to puncture voltage, temperature stability good, reliability is high, miniaturization, jumbo ceramic capacitor; 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 greatly reduce like this cost of high voltage ceramic capacitor, can adopt Pd/Ag alloy that Ag or Ag content are high etc. as interior electrode, reduce greatly the cost of multilayer ceramic capacitor; The not leaded and cadmium of capacitor ceramic dielectric that simultaneously additive of the reduction sintering temperature of this patent obtains, condenser ceramics is free from environmental pollution in preparation and use procedure; In addition, utilize the dielectric constant of the condenser ceramics that additive of the present invention obtains higher, capacity and the miniaturization that can improve like this ceramic capacitor, sintering temperature is low, meets the development trend of ceramic capacitor, can greatly reduce the cost of ceramic capacitor.
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 harmful effect.
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 10kV/mm above (direct current), sintering temperature is 1260-1400 ℃, high more a lot of than this patent, dielectric constant 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 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 lead borosilicate low-melting glass, and medium is leaded, and does not relate to proof voltage, and sintering temperature is minimum is 1080 ℃, higher than this patent, and the low-temperature sintering additive adopting 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, has analyzed intermediate sintering temperature BaTiO 3the impact on dielectric constant and temperature characterisitic that distributes of the composition of base porcelain and uneven texture; BaTiO used 3raw material is to adopt the method for chemical coprecipitation to prepare, and can increase like this cost of ceramic capacitor, and this patent BaTiO used 3, SrTiO 3, CaZrO 3be respectively to adopt conventional chemical raw material synthetic with solid phase method, composition is different from this patent, contains a certain amount of lead, and do not relate to proof voltage in component, and sintering temperature is minimum is 1050 ℃, higher than this patent.
Separately there is patent " high Jie's high-performance medium temp. sintered chip multilayer ceramic capacitor porcelain " (number of patent application: 97117286.2), it is to adopt the 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 appropriate 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 withstand voltage is 700V/mm; Although this patent dielectric constant is high, the material of reporting withstand voltage too poor, is only 700V/mm, its component contains a certain amount of lead in addition, this patent sintering temperature is 1080-1140 ℃, higher than this patent, and the low-temperature sintering additive adopting is also different from patent of the present invention.
Separately there is patent " manufacture method of high-voltage ceramic condenser medium " (patent No. 91101958.8), it adopts unconventional technique to prepare medium, it is flow casting molding film, then laminated medium body, carries out multilayer dielectricity body the even pressure of heating in vacuum, punching, then carries out binder removal, burns till and obtain; The shortcoming of this patent is process of preparing complexity, cause cost of goods manufactured to increase, and the sintering temperature of this patented medium is 1080-1330 ℃, than the height of this patent.
Also has Chinese patent " high-performance medium temp. sintered chip multilayer ceramic capacitor porcelain " (number of patent application: 97117287.0), it adopts unique formula (percentage by weight) (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 meets 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 low simultaneously, is less than this patent, and the sintering temperature of this medium is 1100-1140 ℃, and than the height of this patent, the low-temperature sintering additive adopting is also different from patent of the present invention.
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 that meets following performance of intermediate sintering temperature: dielectric constant is 2000 ~ 3000, proof voltage is more than 6kV/mm, the additive that reduces sintering temperature is bismuth lithium solid solution, dielectric constant and the proof voltage of this patent are high less than this patent, the condenser ceramics sintering temperature that this patent is announced is 1100-1150 ℃, and higher than this patent, this patent is different from this patent for reducing the additive of sintering temperature.
Summary of the invention
The object of this invention is to provide additive and the addition thereof of the high-voltage capacitor ceramic sintering temperature of reduction barium strontium-niobium pentaoxide-cobalt sesquioxide basic recipe system.
The object of the present invention is achieved like this:
Take barium strontium-niobium pentaoxide-cobalt sesquioxide as 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 basic recipe system, the component in additive is calculated in mass percent: LiBiO 244 ~ 65%, CuO0.5 ~ 20%, Li 2o-B 2o 3-ZnO glass dust 25 ~ 45%.
The present invention adopts conventional high-voltage ceramic condenser medium preparation technology, first adopts conventional chemical raw material solid phase method synthetic BaTiO respectively 3, SrTiO 3, LiBiO 2, Li 2o-B 2o 3-ZnO glass dust, then mixes batch ball mill grinding by formula batching, after drying, add adhesive granulation, then be pressed into green sheet, then in air, carry out binder removal and sintering, after insulation is also naturally cooling, obtain ceramic capacitor dielectric, on medium, surveyed performance by electrode.
Above-mentioned additive and addition 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 basic recipe system, (quality): LiBiO in additive 244 ~ 65%, CuO0.5 ~ 20%, Li 2o-B 2o 3-ZnO glass dust 25 ~ 45%.
(2) amount of additive is 2～7% of basic recipe system, (quality): LiBiO in additive 246 ~ 63%, CuO2 ~ 18%, Li 2o-B 2o 3-ZnO glass dust 27 ~ 43%.
(3) amount of additive is 3～6% of basic recipe system, (quality): LiBiO in additive 247 ~ 60%, CuO5 ~ 16%, Li 2o-B 2o 3-ZnO glass dust 28 ~ 40%.
Compared with prior art, tool has the following advantages in the present invention:
1, the medium that utilizes the additive of this patent to obtain is low-temperature sintering (sintering temperature is 900 ~ 920 ℃) Titanium acid 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 dielectric constant of medium that utilizes the additive of this patent to obtain is higher, is 3000 left and right; Proof voltage is high, more than direct current proof voltage can reach 10kV/mm, more than 4kV/mm (alternating voltage, AC); Dielectric loss is little, is less than 1.5%.The dielectric constant of this medium is higher, can realize miniaturization and the large capacity of ceramic capacitor, can reduce costs equally.
3, the percentage of capacitance variation with temperature of medium that utilizes the additive of this patent to obtain is little, meets the requirement of X7R characteristic.Dielectric loss is less than 1.5%, and use procedure performance good stability is safe.
4, utilize the primary raw material of the medium that the additive of this patent obtains to adopt that ceramic capacitor level is pure can produce capacitor ceramic dielectric.
5, the capacitor ceramic dielectric that utilizes the additive of this patent to obtain 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.
Take barium strontium-niobium pentaoxide-cobalt sesquioxide as basic recipe system, barium strontium is Ba 0.71sr 0.29tiO 3, niobium pentaoxide addition is Ba 0.71sr 0.29tiO 30.5% of weight, cobalt sesquioxide addition is Ba 0.71sr 0.29tiO 30.3% of weight, basic recipe system is 100g.
Table 1,2 provides 6 formulas of two groups of embodiment of the present invention, and the primary raw material of 6 formulas of two groups of embodiment adopts ceramic capacitor level pure, first adopts in the preparation conventional chemical raw material solid phase method synthetic BaTiO respectively 3, SrTiO 3, LiBiO 2, Li 2o-B 2o 3-ZnO glass dust, then by formula batching, adopt planetary ball mill ball milling to mix with distilled water or deionized water in the material preparing, material: ball: water=1:3:(0.6 ~ 1.0), after ball milling 4 ~ 8 hours, dry to obtain dry mash, in dry mash, add and account for the poly-vinyl alcohol solution that the concentration of its weight 8 ~ 10% is 10%, carry out granulation, mixed rear mistake 40 mesh sieves, under 20 ~ 30Mpa pressure, carry out again dry-pressing and become green sheet, then be at 900 ~ 920 ℃, to be incubated 1 ~ 4 hour to carry out binder removal and sintering in temperature, at 780 ~ 800 ℃, be incubated 15 minutes again and carry out silver ink firing, form silver electrode, solder taul again, seal, obtain ceramic capacitor, test its dielectric property, the dielectric property of above-mentioned each formula sample are listed in table 3.
Prepared condenser ceramics proof voltage is high as can be seen from Table 3, more than can reaching 10kV/mm (direct voltage, DC), more than 4kV/mm (alternating voltage, AC); Dielectric constant is 3000 left and right; Dielectric loss is less than 1.5%; Percentage of capacitance variation with temperature is little, meets the requirement of X7R characteristic.
LiBiO 2preparation process as follows: by Bi 2o 3and Li 2cO 3material mixed grinding with the molar ratio of 1:1 mixes, and compound is placed on and in corundum crucible, at 800 ℃ to 820 ℃, is incubated 30 minutes preparation LiBiO 2, cooling rear grinding until can cross 200 mesh sieves, is stayed with for subsequent use.
Li 2o-B 2o 3the preparation process of-ZnO glass dust is as follows: by Li 2cO 3: B 2o 3: ZnO mixes with the material mixed grinding of the molar ratio of 1:3:1, and compound is placed in corundum crucible and is incubated 40 minutes at 810 ℃ to 840 ℃, pours subsequently quenching in cold water into, is dried grinding later until can cross 200 mesh sieves, stays with for subsequent use.
The addition of table 1 additive and composition
Figure 466656DEST_PATH_IMAGE001
。
The addition of table 2 additive and composition
Figure 509391DEST_PATH_IMAGE002
。
The dielectric property of the each formula of table 3 sample
Figure 269537DEST_PATH_IMAGE003

Claims (7)

1. the additive that can reduce condenser ceramics sintering temperature, is characterized in that: the component in additive is calculated in mass percent: LiBiO 244 ~ 65%, CuO0.5 ~ 20%, Li 2o-B 2o 3-ZnO glass dust 25 ~ 45%;
Described LiBiO 2preparation process as follows: by Bi 2o 3and Li 2cO 3material mixed grinding with the molar ratio of 1:1 mixes, and compound is placed on and in corundum crucible, at 800 ℃ to 820 ℃, is incubated 30 minutes preparation LiBiO 2, cooling rear grinding until can cross 200 mesh sieves, stay with for subsequent use;
Described Li 2o-B 2o 3the preparation process of-ZnO glass dust is as follows: by Li 2cO 3: B 2o 3: ZnO mixes with the material mixed grinding of the molar ratio of 1:3:1, and compound is placed in corundum crucible and is incubated 40 minutes at 810 ℃ to 840 ℃, subsequently to entering quenching in cold water, is dried grinding later until can cross 200 mesh sieves, stays with for subsequent use;
Take barium strontium-niobium pentaoxide-cobalt sesquioxide as basic recipe system, calculate by mass percentage, the amount of additive is 1～8% of basic recipe system, by formula batching, batch ball mill grinding is mixed, after drying, add adhesive granulation, be pressed into again green sheet, then in air, carry out binder removal and sintering, after insulation is also naturally cooling, obtain condenser ceramics.
2. a kind of additive that can reduce condenser ceramics sintering temperature as claimed in claim 1, is characterized in that: the component in additive is calculated in mass percent: LiBiO 246 ~ 63%, CuO2 ~ 18%, Li 2o-B 2o 3-ZnO glass dust 27 ~ 43%.
3. a kind of additive that can reduce condenser ceramics sintering temperature as claimed in claim 1, is characterized in that: the component in additive is calculated in mass percent:: LiBiO 247 ~ 60%, CuO5 ~ 16%, Li 2o-B 2o 3-ZnO glass dust 28 ~ 40%.
4. a kind of additive that can reduce condenser ceramics sintering temperature as claimed in claim 1, is characterized in that: described 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.
5. a kind of additive that can reduce condenser ceramics sintering temperature as claimed in claim 1, is characterized in that: calculate by mass percentage, additive is 2～7% of basic recipe system.
6. a kind of additive that can reduce condenser ceramics sintering temperature as claimed in claim 5, is characterized in that: calculate by mass percentage, additive is 3～6% of basic recipe system.
7. a kind of additive that can reduce condenser ceramics sintering temperature as claimed in claim 1, is characterized in that: first adopt in the preparation conventional chemical raw material solid phase method synthetic BaTiO respectively 3, SrTiO 3, LiBiO 2, Li 2o-B 2o 3-ZnO glass dust, then by formula batching, adopt planetary ball mill ball milling to mix with distilled water or deionized water in the material preparing, material: ball: water=1:3:(0.6 ~ 1.0), after ball milling 4 ~ 8 hours, dry to obtain dry mash, in dry mash, add and account for the poly-vinyl alcohol solution that the concentration of its weight 8 ~ 10% is 10%, carry out granulation, mixed rear mistake 40 mesh sieves, under 20 ~ 30MPa pressure, carrying out dry-pressing again and become green sheet, is then at 900 ~ 920 ℃, to be incubated 1 ~ 4 hour to carry out binder removal and sintering in temperature, obtains condenser ceramics.
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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
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

Citations (5)

* Cited by examiner, † Cited by third party
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

Patent Citations (5)

* Cited by examiner, † Cited by third party
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

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