CN105152646A - X8R type double-doped barium titanate ceramic dielectric material with smooth and stable dielectric temperature and preparation method thereof - Google Patents
X8R type double-doped barium titanate ceramic dielectric material with smooth and stable dielectric temperature and preparation method thereof Download PDFInfo
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- CN105152646A CN105152646A CN201510358439.6A CN201510358439A CN105152646A CN 105152646 A CN105152646 A CN 105152646A CN 201510358439 A CN201510358439 A CN 201510358439A CN 105152646 A CN105152646 A CN 105152646A
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Abstract
The invention provides a leadless BaTiO<3>-based ceramic capacitor dielectric material meeting X8R indexes. The chemical composition of the dielectric material is as described in (Ba<1-x>Dy<x>)(Ti<1-x/2>Ca<x/2>)O<3>, wherein x is no less than 10 mol% and no more than 15 mol%. The performance of the ceramic dielectric material prepared in the invention reaches the following indexes: dielectric temperature is smooth and stable; a crystal size is small; single-phase ceramic is obtained; a main perovskite structure expressed by the chemical formula ABO3 is obtained, wherein the main component of a main base material is BaTiO<3>, and the content of BaTiO<3> is no less than 77 mol; the average crystal size of the material can be controlled to be no more than 1.2 [mu] m; a room temperature dielectric constant is in a range of 1500 to 1800; a temperature coefficient of capacitance is in a range of +15% to -15%; and room temperature dielectric loss is no more than 2.3%.
Description
Technical field
The present invention relates to a kind of barium titanate ceramic dielectric material, particularly relate to a kind of dielectric smooth steady X8R type codope barium titanate ceramic dielectric material and preparation method thereof.
Background technology
For adapting to the demand of the field of electric control such as national defence, space flight, automotive industry and shock resistance system, in recent years, investigator conducted extensive research the X8R type capacitor dielectric material can applied under extreme harsh operating conditions.Wherein with environmentally friendly BaTiO
3the MLCC obtained for matrix is subject to the common concern of people because its excellent property stablizes.According to International Electro TIA EIA(ElectronicIndustriesAssociation) standard, X8R type refers to the capacitance of 25 DEG C as benchmark, 8 and X represent lower work temperature respectively and be limited to+150 DEG C and-55 DEG C, R represents temperature coefficient of capacitance between+15% ~-15%.The electrical condenser use temperature of this specification is wider, top temperature scope can extend to 150 DEG C, and capacitance change presents smooth variation feature in wide temperature range, high to the control overflow of material, development is difficulty relatively, is a kind of typical low frequency thermostable element.Further, with traditional X7R type BaTiO with nucleocapsid structure
3-base ceramic material is compared, (the Ba that the present invention relates to
1-xdy
x) (Ti
1-x/2ca
x/2) O
3stupalith (is called for short: BDTC) have two large advantages: 1, preparation condition is more prone to control; 2, Dy/Ca codoped higher level (10mol%≤x≤15mol%) can realize preparing dielectric temperature stable form X8R size ceramic dielectric material.
At present, in disclosed barium titanate capacito device patent, most of X8R type dielectric materials realizes by forming " core-shell structure copolymer " structure, this " core-shell structure copolymer " structure is owing to adding specific additive (as: niobium and cobalt are mixed altogether, magnesium and holmium mix altogether), cause the uneven of material structure and composition, cause ferroelectrics Curie peak stretching, finally form the ferroelectric ceramic material that dielectric temperature is stablized, temperature coefficient of capacitance is less.As: Chinese patent (publication number CN103204677A) and Chinese patent (publication number CN102718477A) they are form " core-shell structure copolymer " structure obtain X8R type capacitor dielectric material by adding appropriate bismuth zirconium mixture and niobium cobalt mixture respectively.And the formation of " core-shell structure copolymer " structure needs strict to control following condition: 1, the content of doped element is close to the stoicheiometry in semiconductor region; 2, suitable sintering condition is selected; 3, the rare earth element of correct radial is selected.But, obtain " core-shell structure copolymer " structure by control sintering condition and the diffusion of control binder component and still there is shortcoming: with the carrying out of sintering, binder component excess diffusion.Therefore, meet above condition completely and prepare specific inductivity to lower " core-shell structure copolymer " structure of temperature dependency relatively not easily, in the present invention, we adopt rare earth element and alkali earth metal pair to mix the ceramic medium material prepared and had dielectric temperature stable form X8R specification, and this material does not have " core-shell structure copolymer " structure diffuseed to form by binder component.This invention doping Easy dosing, preparation technology are easy to operate.
Summary of the invention
The invention provides a kind of dysprosium doping (Dy) and alkaline earth elements ca (Ca) codope dielectric smooth steady X8R type barium titanate ceramics material.The X8R type ceramic capacitor material rare earth utilization ratio high (10mol%≤x≤15mol%) prepared by the present invention, has stable specific inductivity (~ 1500-1900; 2000-2800) and lower dielectric loss (tan
δ≤ 0.03), two rare earth can be substituted and three-rare earth doping barium titanate becomes the important medium candidate material of laminated ceramic capacitor.
By doping with rare-earth ions Dy in unique formula in B position of A position and a kind of alkaline-earth metal ions Ca and preparation technology, the X8R ceramic capacitor material of dielectric smooth steady type is successfully realized.
The chemical general formula of X8R ceramic capacitor material of the present invention meets: (Ba
1-xdy
x) (Ti
1-x/2ca
x/2) O
3(10mol%≤x≤15mol%).Wherein, barium titanate is as major ingredient, and its content is >=95mol%; Rare earth element Dy and alkali earth metal Ca is respectively as A position and B position additive, and content is≤15mol%.Raw materials used is the BaCO of purity 99% and above chemical pure industrial chemicals
3, TiO
2, CaCO
3and Dy
2o
3.
The technical process of preparation dielectric smooth steady X8R type codope barium titanate ceramics material (solid phase method cold pressing ceramic technology) adopts the operation steps of patent CN101328061A, is specially:
1, weigh, mixing, grinding: get analytically pure barium carbonate (BaCO
3), titanium dioxide (TiO
2), Dysprosium trioxide (Dy
2o
3) and calcium carbonate (CaCO
3) powder is according to nominal molecular formula (Ba
1-xdy
x) (Ti
1-x/2ca
x/2) O
3correct amount, mixes, ball milling 40min in agate mortar;
2, pre-burning carbon elimination: the said mixture of drying is calcined 5 hours carbon eliminations in the air of 1100 DEG C, and partial synthesis has the solid solution mixture of perovskite structure;
3, the pulverizing of preburning powdered material: the powder regrind 20min after pre-burning is carried out the powder that thinning processing acquisition particle size is less than 1 μm;
4, PVA tackiness agent is added: the polyvinyl alcohol (PVA organic binder bond) adding 10Wt% in the powder after regrind carries out granulation, binder dosage added by each sample, consider interpolation according to the formula of different sample and calcining temperature, guarantee that in powder, PVA content is at below 1Wt%.Join glue to carry out in agate mortar, join in glue process and constantly grind, make glue and sample even.
5, compression molding: use hydropress compression molding, pressure is 100 ~ 200MPa, pressure duration 1 ~ 2min, and compression mold internal diameter is Φ 12mm.After what every sheet was shaping add glue, powder weight control is at 0.8 – 1.0g.
6, pyroceramicization sintering: forming ceramic sheet is put into high temperature resistance furnace, and in atmosphere with the temperature rise rate temperature programming to 1400 DEG C of 100 DEG C/1h, constant temperature, after 12 hours, is down to 700 DEG C with the rate of temperature fall of 100 DEG C/1h, is naturally down to room temperature afterwards.After sintering, the radial shrinkage of sample is Φ 10.2 ~ Φ 10.5mm, to make thick be the ceramic plate of 1.5 ~ 2.5mm.
7, dielectric piece is prepared in polishing: the ceramic plate be fired into is carried out water mill polished finish on metallographic polisher lapper, makes the thickness of sample close to about 0.8mm.Sample after polishing needs constant temperature 2h at 500 DEG C to carry out oven dry thermal treatment; Then coupons is placed in mould top and bottom to plate one deck gold and make electrode (5 × 5mm
2) strengthen electroconductibility, more coating one deck silver paste, be placed in tin stove and dry and make dielectric piece.
The invention has the beneficial effects as follows:
1, this invention is by obtaining the capacitor material with dielectric smooth steady at A position design rare earth ion with in the mode of B position design alkaline-earth metal ions codoped respectively.This design has important value in the macroscopic dielectric temperature stability improving material;
2, rear-earth-dopedly reach These parameters by adulterated alkaline-earth metal ion substitution is two, make the rear-earth-doped amount of A position control at (≤15mol%), namely rear-earth-doped utilization ratio significantly improves;
3, CaCO is adopted
3and Dy
2o
3carry out codoped, the nominal molecular formula of design charge compensation is conducive to the diffuse phase transition realizing barium titanate ceramics;
4, the formula of this X8R type ceramic condenser is simple, is easy to realize;
5, conventional solid-state method technique is simple, and production cost is low, technology maturation, processing ease;
6, average crystallite granularity≤1.2 μm of pottery, reach close grain yardstick;
7, temperature stability is good, dielectric loss is low, body resistivity is large.
Accompanying drawing explanation
Fig. 1 is the room temperature powder X-ray RD diffraction spectrogram of embodiment 1 sample;
Fig. 2 is the glazed surface pattern micro-structure diagram of embodiment 1 sample;
Fig. 3 is the dielectric thermogram of embodiment 1 sample under direct current (DC) bias;
Fig. 4 is the room temperature powder X-ray RD diffraction spectrogram of embodiment 2 sample;
Fig. 5 is the glazed surface pattern micro-structure diagram of embodiment 2 sample;
Fig. 6 is the dielectric thermogram of embodiment 2 sample under direct current (DC) bias;
Fig. 7 is the room temperature powder X-ray RD diffraction spectrogram of embodiment 3 sample;
Fig. 8 is the glazed surface pattern micro-structure diagram of embodiment 3 sample;
Fig. 9 is the dielectric thermogram of embodiment 3 sample under direct current (DC) bias.
Embodiment
Below in conjunction with the drawings and specific embodiments the present invention made and describing in detail further.
Specific embodiment is as follows:
embodiment 1, first get analytically pure BaCO
3, TiO
2, CaCO
3and Dy
2o
3powder is according to nominal molecular formula (Ba
1-xdy
x) (Ti
1-x/2ca
x/2) O
3correct amount 6.8378g, 2.9223g, 0.1927g and 0.718g, (wherein x=0.10).Grind 40 minutes in agate mortar after fully mixing, then in the air of 1100 DEG C, calcine 5 hours carbon eliminations, the powder regrind after pre-burning is carried out thinning processing in 20 minutes.The polyvinyl alcohol (PVA organic binder bond) adding 10Wt% in powder after regrind carries out granulation, guarantees that in powder, PVA content is at below 1Wt%.Then under 200MPa pressure, 1.0 ~ 1.1g is contained PVA powder compression molding in Φ 12mm mould, put into high temperature resistance furnace again, in atmosphere with the temperature rise rate temperature programming to 1400 DEG C of 100 DEG C/1h, constant temperature is after 12 hours, be down to 700 DEG C with the rate of temperature fall of 100 DEG C/1h, be naturally down to room temperature afterwards.After sintering, the radial shrinkage of sample is Φ 10.2 ~ Φ 10.5mm, to make thick be the ceramic plate of 1.5 ~ 2.5mm.Ceramic plate will be made on metallographic polisher lapper, carry out water mill polished finish, and make the thickness of sample close to about 0.8mm.Sample after polishing needs constant temperature 2h at 500 DEG C to carry out oven dry thermal treatment; Then coupons is placed in mould top and bottom to plate one deck gold and make electrode (5 × 5mm
2) strengthen electroconductibility, more coating one deck silver paste, be placed in tin stove and dry and make dielectric piece.The important electrical performance perameter of sample 1-3 is in table 1.Fig. 1 provides the room temperature powder X-ray RD diffraction spectrogram of the present embodiment sample.Fig. 2 provides the glazed surface pattern micro-structure diagram of the present embodiment sample.Fig. 3 provides the dielectric thermogram of the present embodiment sample under direct current (DC) bias (DC-volt is 11KV/mm).
embodiment 2, first get analytically pure BaCO
3, TiO
2, CaCO
3and Dy
2o
3powder is according to nominal molecular formula (Ba
1-xdy
x) (Ti
1-x/2ca
x/2) O
3correct amount 6.599g, 2.854g, 0.2282g and 0.8504g, (wherein x=0.12).Grind 40 minutes in agate mortar after fully mixing, then in the air of 1100 DEG C, calcine 5 hours carbon eliminations, the powder regrind after pre-burning is carried out thinning processing in 20 minutes.The polyvinyl alcohol (PVA organic binder bond) adding 10Wt% in powder after regrind carries out granulation, guarantees that in powder, PVA content is at below 1Wt%.Then under 200MPa pressure, 1.0 ~ 1.1g is contained PVA powder compression molding in Φ 12mm mould, put into high temperature resistance furnace again, in atmosphere with the temperature rise rate temperature programming to 1400 DEG C of 100 DEG C/1h, constant temperature is after 12 hours, be down to 700 DEG C with the rate of temperature fall of 100 DEG C/1h, be naturally down to room temperature afterwards.After sintering, the radial shrinkage of sample is Φ 10.2 ~ Φ 10.5mm, to make thick be the dielectric ceramic sheet of 1.5 ~ 2.5mm.Ceramic plate will be made on metallographic polisher lapper, carry out water mill polished finish, and make the thickness of sample close to about 0.8mm.Sample after polishing needs constant temperature 2h at 500 DEG C to carry out oven dry thermal treatment; Then coupons is placed in mould top and bottom to plate one deck gold and make electrode (5 × 5mm
2) strengthen electroconductibility, more coating one deck silver paste, be placed in tin stove and dry and make dielectric piece.Important electrical performance perameter is in table 2.Fig. 4 provides the room temperature powder X-ray RD diffraction spectrogram of the present embodiment sample.Fig. 5 provides the glazed surface pattern micro-structure diagram of the present embodiment sample.Fig. 6 provides the dielectric thermogram of the present embodiment sample under direct current (DC) bias (DC-volt is 11KV/mm).
embodiment 3, first get analytically pure BaCO
3, TiO
2, CaCO
3and Dy
2o
3powder is according to nominal molecular formula (Ba
1-xdy
x) (Ti
1-x/2ca
x/2) O
3correct amount 6.4579g, 2.8454g, 0.289g and 1.077g, (wherein x=0.15).Grind 40 minutes in agate mortar after fully mixing, then in the air of 1100 DEG C, calcine 5 hours carbon eliminations, the powder regrind after pre-burning is carried out thinning processing in 20 minutes.The polyvinyl alcohol (PVA organic binder bond) adding 10Wt% in powder after regrind carries out granulation, guarantees that in powder, PVA content is at below 1Wt%.Then under 200MPa pressure, 1.0 ~ 1.1g is contained PVA powder compression molding in Φ 12mm mould, put into high temperature resistance furnace again, in atmosphere with the temperature rise rate temperature programming to 1400 DEG C of 100 DEG C/1h, constant temperature is after 12 hours, be down to 700 DEG C with the rate of temperature fall of 100 DEG C/1h, be naturally down to room temperature afterwards.After sintering, the radial shrinkage of sample is Φ 10.2 ~ Φ 10.5mm, to make thick be the dielectric ceramic sheet of 1.5 ~ 2.5mm.Ceramic plate will be made on metallographic polisher lapper, carry out water mill polished finish, and make the thickness of sample close to about 0.8mm.Sample after polishing needs constant temperature 2h at 500 DEG C to carry out oven dry thermal treatment; Then coupons is placed in mould top and bottom to plate one deck gold and make electrode (5 × 5mm
2) strengthen electroconductibility, more coating one deck silver paste, be placed in tin stove and dry and make dielectric piece.Important electrical performance perameter is in table 3.Fig. 7 provides the room temperature powder X-ray RD diffraction spectrogram of the present embodiment sample.Fig. 8 provides the glazed surface pattern micro-structure diagram of the present embodiment sample.Fig. 9 provides the dielectric thermogram of the present embodiment sample under direct current (DC) bias (DC-volt is 3,7,11KV/mm).
Fig. 1 ~ 9 are for corresponding to the dielectric temperature spectrum under each sample XRD figure sample (adopting CuK α radiation) of embodiment 1 ~ 3, surperficial microstructure and different bias voltage.The temperature-measuring range of specific inductivity is-75 DEG C ~+200 DEG C; DC-volt gets 3,7,11KV/mm respectively; Frequency is 1KHz.
In table 1, the meaning of each parameter representative is as follows:
TCC(-55 DEG C): temperature coefficient of capacitance when-55 DEG C;
ε (25 DEG C): be room temperature dielectric constant;
TCC(150 DEG C): temperature coefficient of capacitance when+150 DEG C;
TCC(T) %=[ε
m(T)-ε (25 DEG C)]/ε (25 DEG C) × 100: the temperature coefficient of capacitance of dielectric peak value;
Tan δ (25 DEG C): room temperature dielectric loss.
Claims (4)
1. a dielectric smooth steady X8R type codope barium titanate based ceramic material, is characterized in that: have by ABO
3the cubic perovskite structure represented, the wherein major ingredient BaTiO of main base-material
3its content is>=77mol%, and two kinds of doped elements are rare earth element and alkali earth metal, and rare earth element is A position additive, and alkali earth metal is B position additive, and the content of two kinds of doping agents is 10mol%≤x≤15mol%.
2. according to codope barium titanate based ceramic material according to claim 1, it is characterized in that: mole number >=85mol%, Ti mole number >=92mol% shared by formula B position that Ba is shared in formula A position, the addition x of two kinds of different doped elements is 10 ~ 15mol%, and rare earth element is dysprosium (Dy), alkali earth metal is calcium (Ca). described material can use following general formula:
(Ba
1-xDy
x)(Ti
1-x/2Ca
x/2)O
3
Rare earth element Dy and alkaline-earth metal Ca addition x preferable range are:
10mol%≤x≤15mol%。
3., according to claim 1 or described codope barium titanate based ceramic material, it is characterized in that, the raw materials used BaCO being chemical pure industrial chemicals
3, TiO
2, CaCO
3and Dy
2o
3.
4. according to the codope barium titanate based ceramic material described in any one of claim 1-3, concrete preparation method is: the preparation method of codope barium titanate dielectric smooth steady type one-component ceramic adopts the operation steps of patent CN101328061A, it is characterized in that: batching, batch mixing, grinding, through 1100 DEG C of pre-burnings, be incubated 2 ~ 5 hours; Fine grinding after being pulverized by sinter, grinds again, adds glue grinding, shaping compressing tablet; Firing temperature is 1400 DEG C, is incubated 12 hours; Be polished to stupalith again.
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Citations (4)
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|---|---|---|---|---|
| US20070138459A1 (en) * | 2005-10-13 | 2007-06-21 | Wong Stanislaus S | Ternary oxide nanostructures and methods of making same |
| CN101328061A (en) * | 2008-07-30 | 2008-12-24 | 吉林化工学院 | High dielectric Y5V type three-rare earth doping barium titanate ceramics material and preparation thereof |
| US20100285316A1 (en) * | 2009-02-27 | 2010-11-11 | Eestor, Inc. | Method of Preparing Ceramic Powders |
| CN102060324A (en) * | 2010-11-11 | 2011-05-18 | 刘秦 | Method for preparing doped barium titanate powder through wet process |
-
2015
- 2015-06-26 CN CN201510358439.6A patent/CN105152646B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070138459A1 (en) * | 2005-10-13 | 2007-06-21 | Wong Stanislaus S | Ternary oxide nanostructures and methods of making same |
| CN101328061A (en) * | 2008-07-30 | 2008-12-24 | 吉林化工学院 | High dielectric Y5V type three-rare earth doping barium titanate ceramics material and preparation thereof |
| US20100285316A1 (en) * | 2009-02-27 | 2010-11-11 | Eestor, Inc. | Method of Preparing Ceramic Powders |
| CN102060324A (en) * | 2010-11-11 | 2011-05-18 | 刘秦 | Method for preparing doped barium titanate powder through wet process |
Non-Patent Citations (2)
| Title |
|---|
| D.-Y. LU 等: "Novel X7R BaTiO3 ceramics co-doped with La3+ and Ca2+ ions", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| 周舟 等: "La3+ 掺杂对钛酸钡陶瓷结构和介电性能的影响", 《中国陶瓷》 * |
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