CN1532166A - Method for producing high dielectric constant ceramic powder and ceramic capacitor - Google Patents

Method for producing high dielectric constant ceramic powder and ceramic capacitor Download PDF

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Publication number
CN1532166A
CN1532166A CNA03113971XA CN03113971A CN1532166A CN 1532166 A CN1532166 A CN 1532166A CN A03113971X A CNA03113971X A CN A03113971XA CN 03113971 A CN03113971 A CN 03113971A CN 1532166 A CN1532166 A CN 1532166A
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ceramic
weight percentage
batio
ceramic powder
dielectric
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王作华
李明
司留启
彭道华
冯兆泉
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Guangdong Fenghua High New Science & Technology Group Co Ltd
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Guangdong Fenghua High New Science & Technology Group Co Ltd
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Abstract

The present invention relates to the production process of high dielectric constant ceramic powder with 2B4 characteristic and ceramic capacitor. The high dielectric constant ceramic powder contains BaTiO3 in 93-99.5 wt% as the main component and one or several of MgCO3, CaO, Sb2O3, MnO2, ZnO, Nb2O5, SiO2, SnO2, Ni2O3, Sm2O3 and CuO as the subsidiary components. The circular chip capacitor of the ceramic powder has 2B4 characteristic and X7R characteristic, and the ceramic powder may be used to replace SrTiO3-PbTiO3-Bi2O3.nTiO2 2B4 ceramic to raise environment performance and lower production cost.

Description

The manufacture method of high-dielectric-constant ceramics powder and ceramic condenser
Technical field
The present invention relates to a kind of high-dielectric-constant ceramics powder and utilize the prepared ceramic condenser of this high-dielectric-constant ceramics powder, particularly relate to and have 2B 4The high-dielectric-constant ceramics powder of characteristic and X7R characteristic and utilize the prepared ceramic condenser of this high-dielectric-constant ceramics powder.
The invention still further relates to and a kind ofly utilize above-mentioned high-dielectric-constant ceramics powder to prepare the method for ceramic condenser.
Background technology
Along with in the world environmental protection consciousness being strengthened day by day, the material that contains elements such as lead, bismuth, cadmium, arsenic will be eliminated gradually.Be applied in the electrical condenser in mesohigh electronic circuit and power equipment such as colour television set, laser apparatus, electric power block device, microwave oven, static compounding machine, the electric billy etc. at present, contain elements such as lead, bismuth, cadmium, arsenic in the employed electron ceramic material of its electrical condenser, can produce environment during use and pollute.For example, has 2B at present 4Characteristic (so-called 2B 4Characteristic is meant-25 ℃～+ 85 ℃
Figure A0311397100042
) the high-k electron ceramic material mainly be SrTiO 3-PbTiO 3-Bi 2O 3NTiO 2The porcelain of system, and the specific inductivity of this porcelain system (20 ℃, 1kHz) :≤4200, dielectric loss (20 ℃, 1kHz) :≤50 * 10 -4, insulating property:＞10 10, dielectric strength:＞6kv/mm, temperature profile :-25 ℃～+ 85 ℃ Sintering characteristic: T S=1280 ± 15 ℃.But contain elements such as lead, bismuth in the above-mentioned materials, and produce the used starting material SrTiO of this material 3, PbTiO 3, Bi 2O 3, TiO 2Deng cost, compare BaTiO 3The BaCO of system 3, TiO 2High several times, elements such as lead, bismuth have hot volatility simultaneously, can produce environment during use and pollute; And its production technique is heterogeneous mixing synthesis technique, and is more loaded down with trivial details, complicated.
Summary of the invention
At above-mentioned the deficiencies in the prior art, the invention provides a kind of high-dielectric-constant ceramics powder, this high-dielectric-constant ceramics powder is a kind of 2B that both had 4Characteristic has the X7R characteristic again, the high-k electronic ceramic powder of elements such as simultaneously not leaded, bismuth, cadmium, arsenic.
On the other hand, the present invention also provides by the ceramic condenser of above-mentioned high-dielectric-constant ceramics powder manufacturing and the method for preparing this ceramic condenser.
The high-dielectric-constant ceramics powder that is used to prepare ceramic condenser disclosed in this invention, by following formulated:
(1) adopts BaTiO 3As the main ingredient of this high-dielectric-constant ceramics powder, its content is 93.0%～99.5% by weight percentage, and wherein the scope of Ba, Ti mol ratio is 0.98～1.03;
(2) from MgCO 3, CaO, Sb 2O 3, MnO 2, ZnO, Nb 2O 5, SiO 2, SnO 2, Ni 2O 3, Sm 2O 3, select one or more materials among the CuO, as the accessory constituent of this high-dielectric-constant ceramics powder, its content is 0.5%～7.0% by weight percentage.
Preferably, above-mentioned main ingredient BaTiO 3Weight percentage in the high-dielectric-constant ceramics powder is 95～99%; The above-mentioned MgCO that is selected from 3, CaO, Sb 2O 3, MnO 2, ZnO, Nb 2O 5, SiO 2, SnO 2, Ni 2O 3, Sm 2O 3, the accessory constituent of one or more materials among the CuO, the weight percentage in the high-dielectric-constant ceramics powder is 0.8～5%.
The present invention also provides a kind of ceramic condenser, and this ceramic condenser is by comprising that the following high-dielectric-constant ceramics powder of forming makes:
BaTiO 3????????????????????????????????????????93.0～99.5wt％
Be selected from MgCO 3, CaO, Sb 2O 3, MnO 2, ZnO, Nb 2O 5, SiO 2,
SnO 2, Ni 2O 3, Sm 2O 3, one or more the 0.5～7.0wt% among the CuO
Preferably, in above-mentioned ceramic condenser, described BaTiO 3In the mol ratio of Ba, Ti be 0.98～1.03.
Further preferably, in above-mentioned ceramic condenser, described BaTiO 3Weight percentage be 95～99%; Described one or more are selected from MgCO 3, CaO, Sb 2O 3, MnO 2, ZnO, Nb 2O 5, SiO 2, SnO 2, Ni 2O 3, Sm 2O 3, the component among the CuO weight percentage be 0.8～5%.
Above-mentioned ceramic condenser both can be the wafer capacitance device, also can be the electrical condenser of other form; Its preparation method mainly is to adopt dry-pressing, push or roll method such as film to make green compact, then through lamination, sintering, ultrasonic cleaning, sorting, Yin Yin, reduction, test, seal, test, obtain the electrical condenser that can on complete machine, use at last.
The every performance index of wafer capacitance device of making of ceramic powder of the present invention all meet 2B 4Group GB standard also has the X7R characteristic, compliance with environmental protection requirements, and production cost is reduced greatly, complete alternative SrTiO 3-PbTiO 3-Bi 2O 3NTiO 2The 2B of system 4The group porcelain.Principal character parameter by its electrical condenser that makes is:
Specific inductivity (20 ℃, 1kHz): 3500～5000
Dielectric loss (20 ℃, 1kHz) :≤150 * 10 -4
Insulating property:＞10 10
Dielectric strength: V DC〉=6kv/mm V AC〉=3.0kv/mm
Temperature profile :-55 ℃～+ 125 ℃
Figure A0311397100061
Sintering temperature: T S=1300 ± 30 ℃
Among the present invention, term 2B 4Characteristic is meant-25 ℃～+ 85 ℃
Figure A0311397100062
Term X7R be meant temperature-55 ℃ to+125 ℃ volume change rate between positive and negative 15%.
By embodiment the present invention is further detailed below, but scope of the present invention is not limited to following embodiment.
Embodiment
Choose electronic-grade or technical grade BaCO earlier 3And TiO 2As starting material, then with BaCO 3And TiO 2Powder weighing also mixes, and obtains with Formula B aTiO 3The raw material of the main ingredient of expression.With BaTiO 3Place ball mill to carry out wet-milling, the temperature with 1200 ℃ was calcined 1～3 hour in air subsequently, thereby obtained the main ingredient powder after the calcining, can adopt following two kinds of methods to obtain ceramic condenser then:
1, with the BaTiO after the above-mentioned calcining 3Powder and MgCO 3, CaO, Sb 2O 3, MnO 2, ZnO, Nb 2O 5, SiO 2, SnO 2, Ni 2O 3, Sm 2O 3, CuO etc. 1～10 weighs and mixes by filling a prescription in the table 1.Place ball mill or sand mill to carry out wet-milling in mixture, temperature with 250 ℃ is dried in air subsequently, the porcelain that obtains is adapted to use extruding or rolls membrane method and make wafer capacitance device green compact, pass through lamination, kiln sintering, ultrasonic cleaning, sorting, Yin Yin, reduction again, test, seal, test, obtain the ceramic condenser that on complete machine, to use at last, record in performance such as the table 2 1～10.
2, with the main ingredient BaTiO after the above-mentioned calcining 3And MgCO 3, CaO, Sb 2O 3, MnO 2, ZnO, Nb 2O 5, SiO 2, SnO 2, Ni 2O 3, Sm 2O 3, powder such as CuO is by 11～20 weighing and mix in the table 1.Place ball mill or sand mill to carry out wet-milling in mixture, adopt then by weight 20.0% adding 5.0%～30.0%PVA (2.0%～8.0%) glue solution of dry powder and an amount of dispersion agent, defoamer, remover etc., carry out drying-granulating with granulating and drying machine, dry-pressing formed and make wafer capacitance device green compact at press, pass through lamination, kiln sintering, ultrasonic cleaning, sorting, Yin Yin, reduction again, test, seal, test, obtain the ceramic condenser that on complete machine, to use at last, record in performance such as the table 2 11～20.
Various material prescriptions and performance index are shown in table 1, table 2:
Table 1
Material number ??BaTiO 3 ????Nb 2O 5 ????Sm 2O 3 ???Ni 2O 3 ???MnO 2 ???MnCO 3 ??ZnO ??MgCO 3 ??CaO ?Sb 2O 3 ??SnO 2 ??SiO 2
????1 ????95 ????1.0 ????0.3 ????0.7 ????0.2 ????0.4 ??0.6 ??0.05 ??0.4 ??0.6
????2 ????95 ????0.2 ????0.5 ????0.3 ????0.4 ??0.6 ??0.1
????3 ????95 ????1.3 ????0.4 ????0.1 ??0.2 ??0.1 ??0.2 ??0.3
????4 ????95 ????1.2 ????0.2 ??0.3 ??0.1 ??0.2 ??0.5 ??0.4
????5 ????96 ????0.1 ????0.2 ??0.4 ??0.2 ??0.1
????6 ????96 ????1.3 ????0.2 ????0.4 ??0.1 ??0.2 ??0.3
????7 ????96 ????1.1 ????0.25 ????0.7 ??0.2 ??0.5 ??0.4
????8 ????96 ????1.2 ????0.7 ????0.5 ??0.4 ??0.5 ??0.4
????9 ????97 ????1.3 ????0.4 ??0.4 ??0.4 ??0.3 ??0.4
????10 ????97 ????0.2 ????0.2 ??0.1 ??0.2 ??0.1
????11 ????97 ????1.3 ????0.5 ??0.2 ??0.1
????12 ????97 ????1.2 ??0.1 ??0.2 ??0.2 ??0.2
????13 ????98 ????1.3 ????0.4 ????0.5 ??0.1 ??0.2
????14 ????98 ????1.3 ????0.2 ??0.1 ??0.3
????15 ????98 ????1.4 ????0.2 ??0.1 ??0.3 ??0.3 ??0.1
????16 ????98 ????1.5 ????0.3 ??0.2 ??0.2 ??0.1 ??0.2
????17 ????99 ????0.1 ????1.5 ??0.2 ??0.3
????18 ????99 ????0.2 ????1.4 ??0.3 ??0.2
????19 ????99 ????0.3 ????1.3 ??0.1 ??0.1
????20 ????99 ????0.4 ????1.2 ??0.1 ??0.1
Table 2
Sample number into spectrum Sintering temperature (℃) DIELECTRIC CONSTANT ??tanδ ??(×10 -4) ????????????????????ΔC/C 20℃(％) ??B·D·V ??(DC)KV/mm ??B·D·V ??(AC)KV/mm Insulation resistance (* 10 10Ω)
??-55℃ ??-25℃ ??85℃ ??125℃
????1 ??1285 ??3650 ??132 ??-8.9 ??-5.4 ??-65 ??-8.7 ????7.1 ????3.5 ????5
????2 ??1295 ??3590 ??123 ??-85 ??-4.9 ??-5.0 ??-7.6 ????7.2 ????3.6 ????6
????3 ??1305 ??3670 ??145 ??-9.1 ??-3.2 ??-4.0 ??-7.4 ????7.4 ????3.6 ????5
????4 ??1315 ??3650 ??132 ??-8.0 ??-3.2 ??-4.1 ??-8.7 ????7.9 ????3.7 ????5
????5 ??1285 ??3800 ??101 ??-7.7 ??-4.5 ??-4.5 ??-8.0 ????7.4 ????3.8 ????5
????6 ??1295 ??3950 ??103 ??-9.2 ??-6.1 ??-5.6 ??-7.9 ????7.5 ????3.9 ????3
????7 ??1305 ??3904 ??104 ??-8.2 ??-5.1 ??-5.0 ??-9.1 ????7.6 ????4.0 ????6
????8 ??1315 ??3980 ??123 ??-7.8 ??-4.1 ??-5.1 ??-8.0 ????7.1 ????3.5 ????5
????9 ??1285 ??4102 ??134 ??-8.6 ??-4.4 ??-5.4 ??-7.0 ????8.0 ????3.5 ????5
????10 ??1295 ??4150 ??125 ??-9.2 ??-1.2 ??-3.1 ??-7.4 ????7.4 ????3.6 ????4
????11 ??1305 ??4520 ??136 ??-9.4 ??-2.4 ??-3.4 ??-7.9 ????7.3 ????3.7 ????6
????12 ??1315 ??4563 ??140 ??-9.0 ??-3.2 ??-3.5 ??-8.4 ????7.0 ????3.5 ????3
????13 ??1285 ??3800 ??148 ??-9.1 ??-3.1 ??-4.1 ??-7.4 ????7.1 ????4.0 ????6
????14 ??1295 ??3720 ??99 ??-9.1 ??-3.4 ??-3.6 ??-8.0 ????7.2 ????4.0 ????6
????15 ??1305 ??3920 ??95 ??-8.4 ??-4.0 ??-3.4 ??-9.1 ????7.3 ????3.9 ????5
????16 ??1315 ??4102 ??97 ??7.8 ??-4.2 ??3.4 ??-9.4 ????7.1 ????4.0 ????5
????17 ??1285 ??4200 ??102 ??-8.0 ??-4.5 ??-5.0 ??-9.8 ????7.4 ????3.7 ????4
????18 ??1295 ??4300 ??109 ??-8.1 ??-4.2 ??-5.0 ??-8.7 ????7.4 ????3.6 ????3
????19 ??1305 ??4600 ??104 ??-8.0 ??-4.5 ??-4.2 ??-9.0 ????7.5 ????3.7 ????4
????20 ??1315 ??4805 ??110 ??-8.1 ??-5.0 ??-4.1 ??-9.1 ????7.6 ????3.8 ????1
In acetoacetic ester 115 grams, obtain the phenoxy resin solution of 30 weight %.
As silicone, in being 12 aqueous ethanolic solution, 20 ℃ of pH values that methyltrimethoxy silane joined with 300 rev/mins of stirrings make its hydrolysis, condensation, and the storage elasticity rate that makes 25 ℃ is 8MPa, and median size is spherical particle of 2 μ m.
To contain phenoxy resin solution (with solid-state weight ratio phenoxy resin 45 grams) silicone micropartical 30 grams, liquid epoxies (the epoxy equivalent (weight) 185 of microcapsule-type potentiality solidifying agent, Asahi Chemical Industry Co., Ltd's system, ノ バ キ ュ ァ HX--3941) 20 grams, bisphenol A type epoxy resin (epoxy equivalent (weight) 180) 50 grams mix, and (diameter: 5 μ m) thereby conducting particles of surface formation Au layer is dispersed in 6 volume % and wherein makes thin film coated solution will to examine core at polystyrene.Subsequently, with coating unit this solution being coated to thickness is that the single face of the film of 50 μ m carries out on surface-treated PET (polyethylene terephthalate, body material film, the separator) film, through 70 ℃ of warm air dryings 10 minutes, obtaining adhesive layer thickness was the film like binding agent of 45 μ m.About this binding agent, to the reaction time opening, the reaction concluding time, 60% and 80% end temp of curing reaction, the thermal value of the DSC that finishes up to 80% of curing reaction, and thermal value and the spring rate of the DSC that finishes fully up to curing reaction measure, it the results are shown in table 1.
Secondly, use the film like binding agent of gained will be with golden flange (area 80 * 80 μ m as shown below, interval 30 μ m, height 15 μ m, flange several 288) chip (10 * 10mm, thickness 500 μ m) is connected with having with the Cu circuit printing plate of the plating Ni/Au of the corresponding circuit electrode of electrode of chip.
With the film like binding agent (12 * 12mm) at 80 ℃, 1.0MPa (10 kgfs/centimetre 2) pressure under stick on the Cu circuit printing plate (electrode height 20mm, thickness 0.8mm) of plating Ni/Au, the peel separation device coincide the position of the Cu circuit printing plate (thickness 0.8mm) of the flange of chip and plating Ni/Au.Subsequently, at 180 ℃, 75 gram/each flange are heated, are pressurizeed by the chip top under 20 seconds the condition, thereby realize this connection.
The deflection of this connection back chip is 1 μ m (to the deflection of chip direction projection).In addition, the connection impedance after this connection, each flange is the highest 15M Ω, average out to 8M Ω, insulation impedance is 18 8More than the Ω.Even these values are carrying out-1000 circular treatment of heat shock resistance test of 55--125 ℃, and PCT test (121 ℃, 0.2MPa (2 normal atmosphere)) 200 hours, dipping did not change after 10 seconds yet during 260 ℃ of solderings were bathed, and showed the connection reliability that it is good.

Claims (9)

1, a kind of high-dielectric-constant ceramics powder, it comprises that weight percentage is 93.0～99.5% BaTiO 3, and weight percentage be 0.5～7.0%, one or more are selected from MgCO 3, CaO, Sb 2O 3, MnO 2, ZnO, Nb 2O 5, SiO 2, SnO 2, Ni 2O 3, Sm 2O 3, the component among the CuO.
2, ceramic powder according to claim 1 is characterized in that, described BaTiO 3The mol ratio of middle Ba, Ti is 0.98～1.03.
3, ceramic powder according to claim 1 and 2 is characterized in that, described BaTiO 3Weight percentage be 95～99%.
4, ceramic powder according to claim 1 and 2 is characterized in that, described one or more are selected from MgCO 3, CaO, Sb 2O 3, MnO 2, ZnO, Nb 2O 5, SiO 2, SnO 2, Ni 2O 3, Sm 2O 3, the component among the CuO weight percentage be 0.8～5%.
5, a kind of ceramic condenser of being made by the high-dielectric-constant ceramics powder is characterized in that, described high-dielectric-constant ceramics powder comprises that weight percentage is 93.0～99.5% BaTiO 3, and weight percentage be 0.5～7.0%, one or more are selected from MgCO 3, CaO, Sb 2O 3, MnO 2, ZnO, Nb 2O 5, SiO 2, SnO 2, Ni 2O 3, Sm 2O 3, the component among the CuO.
6, ceramic condenser according to claim 5 is characterized in that, described BaTiO 3The mol ratio of middle Ba, Ti is 0.98～1.03.
7, ceramic condenser according to claim 5 is characterized in that, described BaTiO 3Weight percentage be 95～99%.
8, ceramic condenser according to claim 5 is characterized in that, described one or more are selected from MgCO 3, CaO, Sb 2O 3, MnO 2, ZnO, Nb 2O 5, SiO 2, SnO 2, Ni 2O 3, Sm 2O 3, the component among the CuO weight percentage be 0.8～5%.
9, a kind of preparation comprises: the described ceramic powder of one of claim 1-4 is carried out dry-pressing, pushes or roll film make green compact as the method for one of claim 5-8 described ceramic condenser; Carry out lamination, sintering, ultrasonic cleaning then successively; Carry out sorting, Yin Yin, reduction at last, test, seal.
CNA03113971XA 2003-03-21 2003-03-21 Method for producing high dielectric constant ceramic powder and ceramic capacitor Pending CN1532166A (en)

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CN1295188C (en) * 2005-03-10 2007-01-17 中国科学院青海盐湖研究所 Method for high temperature quick synthesizing titanate ceramic powder
CN100345799C (en) * 2006-06-22 2007-10-31 西安交通大学 Bismuth zinc niobate / barium strontium titanate composite dielectric adjustable thick film preparation method
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CN103864415A (en) * 2014-01-29 2014-06-18 河南科技大学 Zinc Stannate-doped barium titanate high-dielectric ceramic and preparation method thereof
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CN1295188C (en) * 2005-03-10 2007-01-17 中国科学院青海盐湖研究所 Method for high temperature quick synthesizing titanate ceramic powder
CN100358835C (en) * 2005-03-10 2008-01-02 中国科学院青海盐湖研究所 Method for high temperature quick synthesizing blender or compound titanate ceramic powder
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CN101937771B (en) * 2009-06-30 2013-05-01 广东风华高新科技股份有限公司 Preparation method of high voltage multilayer ceramic capacitor
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CN102086121A (en) * 2009-11-20 2011-06-08 株式会社村田制作所 Dielectric ceramic and laminated ceramic capacitor
CN102060523B (en) * 2010-11-12 2013-03-20 陕西科技大学 Composite material with high dielectric constant and preparation method thereof
CN102060523A (en) * 2010-11-12 2011-05-18 陕西科技大学 Composite material with high dielectric constant and preparation method thereof
CN102173785A (en) * 2011-01-21 2011-09-07 天津大学 Method for preparing wide-working-temperature-zone thermostabilization composite dielectric ceramic
CN103224388A (en) * 2012-01-27 2013-07-31 Tdk株式会社 Dielectric ceramic composition and electronic component
CN103224388B (en) * 2012-01-27 2014-12-10 Tdk株式会社 Dielectric ceramic composition and electronic component
CN103864415A (en) * 2014-01-29 2014-06-18 河南科技大学 Zinc Stannate-doped barium titanate high-dielectric ceramic and preparation method thereof
CN103864415B (en) * 2014-01-29 2016-03-30 河南科技大学 Barium titanate high dielectric ceramic of a kind of zinc doping and preparation method thereof
CN104591727A (en) * 2015-02-05 2015-05-06 中国科学院上海硅酸盐研究所 High-voltage-resistant ceramic material and preparation method thereof
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CN111056837A (en) * 2019-12-30 2020-04-24 西南大学 Preparation method of barium titanate ferroelectric ceramic material with high electric field strength and product thereof

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