CN106045498A - BME ceramic dielectric capacitor ceramic material and preparation method thereof - Google Patents
BME ceramic dielectric capacitor ceramic material and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 29
- 239000000919 ceramic Substances 0.000 title abstract description 3
- 239000003990 capacitor Substances 0.000 title abstract 2
- 238000000498 ball milling Methods 0.000 claims abstract description 52
- 238000005245 sintering Methods 0.000 claims abstract description 37
- 238000001035 drying Methods 0.000 claims abstract description 28
- 229910007562 Li2SiO3 Inorganic materials 0.000 claims abstract description 21
- 238000009413 insulation Methods 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 17
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 15
- 229910002976 CaZrO3 Inorganic materials 0.000 claims abstract description 14
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 14
- 238000005516 engineering process Methods 0.000 claims abstract description 12
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 claims abstract description 5
- JYTUFVYWTIKZGR-UHFFFAOYSA-N holmium oxide Inorganic materials [O][Ho]O[Ho][O] JYTUFVYWTIKZGR-UHFFFAOYSA-N 0.000 claims abstract description 5
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 5
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims abstract description 5
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 claims abstract description 5
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000003825 pressing Methods 0.000 claims abstract description 4
- 239000003985 ceramic capacitor Substances 0.000 claims description 30
- 238000001354 calcination Methods 0.000 claims description 21
- 239000000126 substance Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 229910020489 SiO3 Inorganic materials 0.000 claims description 11
- 238000012546 transfer Methods 0.000 claims description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 7
- 229910052681 coesite Inorganic materials 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 229910052906 cristobalite Inorganic materials 0.000 claims description 7
- 125000001967 indiganyl group Chemical group [H][In]([H])[*] 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 229910052682 stishovite Inorganic materials 0.000 claims description 7
- 229910052905 tridymite Inorganic materials 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 201000005505 Measles Diseases 0.000 claims description 3
- 238000009826 distribution Methods 0.000 claims description 3
- 239000012188 paraffin wax Substances 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 3
- 229910052691 Erbium Inorganic materials 0.000 claims description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000001027 hydrothermal synthesis Methods 0.000 claims 1
- 239000002689 soil Substances 0.000 claims 1
- 238000003786 synthesis reaction Methods 0.000 claims 1
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 abstract description 5
- 238000013461 design Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 abstract 2
- 238000007599 discharging Methods 0.000 abstract 1
- 239000005416 organic matter Substances 0.000 abstract 1
- 239000010953 base metal Substances 0.000 description 22
- 238000002156 mixing Methods 0.000 description 16
- 229910052709 silver Inorganic materials 0.000 description 11
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 10
- 239000004332 silver Substances 0.000 description 10
- 238000010304 firing Methods 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- VKJLWXGJGDEGSO-UHFFFAOYSA-N barium(2+);oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[O-2].[Ti+4].[Ba+2] VKJLWXGJGDEGSO-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005553 drilling Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
A BME ceramic dielectric capacitor ceramic material is prepared from BaTiO3, CaZrO3, rare earth oxide, Er2O3, MnO2, BaCO3, Co2O3, ZnB2O4 and Li2SiO3, the materials are matched in a certain proportion and subjected to ball milling, drying, prilling, circular slice green body pressing, organic matter discharging, sintering and the like. The rare earth oxide is one or several of Yb2O3, Ho2O3, Dy2O3, Sm2O3 and Y2O3. An X7R type MLCC material with excellent performance can be sintered at the reducing atmosphere, the preparation technology is simple, the formula design is simple and adjustable, the sintering technology is easy to control, the material is suitable for large-scale production, the uniformity of the material is good, the material has a high dielectric constant, a low dielectric loss and good high-temperature insulation resistance and insulation strength, the production cost of MLCC can be effectively reduced, and the application range of the material is enlarged.
Description
Technical field
The present invention relates to technical field of functional ceramics, particularly a kind of BME ceramic capacitor ceramic material and preparation side thereof
Method.
Background technology
Along with polytype electronic equipment, such as digital camera, mobile phone, notebook computer, GPS, satellite reception
The fast development of the mobile electronic devices such as machine, on electronic circuit, miniaturization and the lightness of device are inexorable trends, to adapt to electricity
The surface mounting technology (SMD) of sub-components and parts needs.SMD requires that components and parts are chip components and parts.And multilayer ceramic capacitor
(MLCC) it is a most widely used class in electronic circuit as chip components and parts.Meanwhile, in terms of device miniaturization, it is desirable to
There is high dielectric constant.Under the conditions of equivalent capability, dielectric constant is the biggest, and device is the least.
It addition, along with science and techniques of defence and auto industry, the demand of drilling technique and development, in automobile, oil drilling, defend
In the major fields such as star navigation, mobile communication, it is desirable to ceramic capacitor can be suitably used for harsher working environment, and this is just
The work ceiling temperature requiring ceramic capacitor constantly extends, therefore can meet X7R standard (operating temperature is-55～+125 DEG C,
Δ C/C20 DEG C≤± 15%) barium titanate based dielectric pottery obtain extensive concern and research practical.
With the MLCC material that Barium metatitanate. is main base material, the when that it sintering in air atmosphere, need to use noble metal such as
The precious metals such as Ag, Pt, Pd or its alloy, as interior electrode, occupy MLCC and produce significant cost, thus due to height
High cost, limits the extensive application of MLCC.Consideration based on cost, uses electrodes in base metal (BME) conducts such as Ni, Cu
The interior electrode of MLCC, can effectively be greatly lowered the production cost of MLCC.But, owing to using BME, it is desirable to MLCC is in inertia
Or reducing atmosphere (predominantly H2、N2Sintering under), otherwise BME will be oxidized in sintering process, interior electrode lose electric action and
MLCC is caused to lose efficacy.Therefore, exploitation one can sinter under reducing atmosphere, uses the MLCC material of BME to be particularly important, can
Effectively to reduce MLCC production cost, expand its range of application.
At present, the multilayer ceramic capacitor technology of base metal X7R mainly rests in a few developed country, especially beautiful
The major industrial country such as state, Japan, now widely used X7R type MLCC product, mainly use in civil area, there is also
The deficiency of the aspects such as such as dielectric constant is the highest, dielectric loss is big, high volume resistivity is little or dielectric strength is low, limits it
Application in higher field such as Aero-Space, weaponry.
Summary of the invention
The main object of the present invention is the shortcoming overcoming prior art, it is provided that a kind of preparation technology is easy, formula design letter
Single the most adjustable, sintering process is easy to control, have high dielectric constant, low dielectric loss and good high-temperature insulation resistance and
Dielectric strength, can effectively reduce MLCC production cost, expand its range of application, the BME porcelain dielectric that can sinter under reducing atmosphere
Container ceramic material and preparation method thereof.
The present invention adopts the following technical scheme that
A kind of BME ceramic capacitor ceramic material, by the BaTiO of 100 weight portions3, 0.5～4 CaZrO of weight portion3、0.5
～2.0 rare earth oxide, 0.03～0.15% Er of weight portion of weight portion2O3, 0.1～0.4% MnO of weight portion2, 0.5～
The BaCO of 2.5% weight portion3, 0.01～0.1 Co of weight portion2O3, 0.15～1.5 ZnB of weight portion2O4And 0.15～1.5 weights
The Li of amount part2SiO3Being prepared from, described rare earth oxide uses Yb2O3、Ho2O3、Dy2O3、Sm2O3、Y2O3In one or several
Kind.
Further, described BaTiO3For water heat transfer, granularity is below 0.8 μm.
The preparation method of a kind of BME ceramic capacitor ceramic material, comprises the following steps:
Prepare CaZrO the most respectively3、ZnB2O4And Li2SiO3；
2. with the BaTiO of 100 weight portions3It is main base material, adds the CaZrO of 0.5～4.0 weight portions3, 0.5～2.0 weight
Part rare earth oxide, 0.03～0.15 Er of weight portion2O3, 0.1～0.4 MnO of weight portion2, 0.5～2.5 weight portions
BaCO3, 0.01～0.1 Co of weight portion2O3, 0.15～1.5 ZnB of weight portion2O4And 0.15～1.5 Li of weight portion2SiO3,
Described rare earth oxide uses Yb2O3、Ho2O3、Dy2O3、Sm2O3、Y2O3In one or more, after carrying out dispensing, use deionization
Water, as disperse medium, carries out ball milling, dries and pelletize；
3. the powder pressing after pelletize is become disk green compact, at a temperature of 350～450 DEG C, arrange Organic substance；
4. by the disk green compact after row's Organic substance at N2/H2Atmosphere furnace sinters, sintering temperature 1250 DEG C～1340 DEG C, protect
Temperature 3h, furnace cooling after insulation, i.e. prepare low-loss BME ceramic capacitor ceramic material.
Further, described step 1. in, prepare CaZrO3Time, first by CaO or CaCO3And ZrO2Carry out proportioning, weighing,
Mixing, ball milling, sieve, and in 1150～1200 DEG C of temperature lower calcinations, then ball milling, drying, CaZrO can be obtained3。
Further, described step 1. in, prepare ZnB2O4Time, first by ZnO and H3BO3Carry out proportioning, weigh, mix, ball
Grind, sieve, and in 550～700 DEG C of temperature lower calcinations, then ball milling, drying, ZnB can be obtained2O4。
Further, described step 1. in, prepare Li2SiO3Time, first by Li2CO3And SiO2Carry out proportioning, weigh, mix,
Ball milling, sieve, and in 550～700 DEG C of temperature lower calcinations, then ball milling, drying, Li can be obtained2SiO3。
Further, described BaTiO3For water heat transfer.
Further, described step 2. in, ball-milling technology uses SC-Mi l l ultra micro measle grinding machine, after grinding distribution, logical
Crossing drying cupboard to dry slurry, then crush drying block material, 80 mesh standard sieves crossed by the powder after crushing, then add
Enter the paraffin of 7～9 weight portions to make binding agent and jointly bakee pelletize, the most again cross 80 mesh standard sieves.
Further, described step 3. in, the powder after pelletize is pressed into disk green compact under 8～10MPa, 350～
450 DEG C of row Organic substance 6h.
Further, described step 4. in, disk green compact are at N2/H2In atmosphere furnace sintering time, temperature reach 600 DEG C it
Before, atmosphere furnace is passed through N2, air pressure controls at more than 1.05atm；Temperature reaches 600 DEG C later to sintering temperature and insulation rank thereof
Section, stops being passed through N2, change into being passed through H2；After sintering temperature insulation terminates, stop being passed through H2, then change into being passed through N2, air pressure is reduced to
1.01～1.03atm；Then 1000 DEG C are cooled the temperature to certain rate of temperature fall, temperature fall time 3h, and it is incubated 5h, insulation knot
Shu Hou, keeps atmosphere furnace atmosphere and pressure constant, lowers the temperature with stove.
From the above-mentioned description of this invention, compared with prior art, the invention has the beneficial effects as follows:
Pass through CaZrO3, rare earth oxide improve BaTiO3Resistance to reduction, make Ti4+In the reducing atmosphere of high temperature not
It is prone to be reduced to Ti3+, and the temperature characterisitic of dielectric material can be effectively improved；Pass through MnO2Doping make BaTiO3Medium damage
Consumption reduces, and improves resistance to reduction the most further simultaneously；Pass through Er2O3Improve the insulation resistance of Barium metatitanate., especially 125 DEG C exhausted
Edge resistance；Pass through ZnB2O4And Li2SiO3Regulate BaTiO3Sintering temperature, be allowed to densified sintering product at a certain temperature, improve
Its resistance to breakdown strength, and temperature characterisitic can be improved further；BaCO3Incorporation can change the Ba/Ti value in material system,
Thus change and surround and watch structure, it is possible to improve resistance to reduction energy further, the X7R type of excellent performance can be sintered out under reducing atmosphere
MLCC material, preparation technology is easy, and formula design is the most adjustable, sintering process is easy to control, it is adaptable to large-scale production, and material
Uniformity good, there is high dielectric constant, low dielectric loss and good high-temperature insulation resistance and dielectric strength, energy
Effectively reduce MLCC production cost, expand its range of application.
Detailed description of the invention
Below by way of detailed description of the invention, the invention will be further described.
Embodiment one
The preparation method of a kind of BME ceramic capacitor ceramic material of the present invention, comprises the following steps:
Prepare CaZrO the most respectively3、ZnB2O4And Li2SiO3；
Preparation CaZrO3: weigh analytically pure CaCO respectively310g、ZrO212.32g, mixing, ball milling, sieves, and in
1150～1200 DEG C of temperature lower calcinations, then ball milling, drying, can obtain CaZrO3；
Preparation ZnB2O4: weigh 8.14g ZnO and 12.37g H respectively3BO3, mixing, ball milling, sieve, and in 550～700
DEG C temperature lower calcination, then ball milling, drying, can obtain ZnB2O4；
Preparation Li2SiO3: weigh 7.39g Li respectively2CO3With 6.0g SiO2, mixing, ball milling, sieve, and in 550～700
DEG C temperature lower calcination, then ball milling, drying, can obtain Li2SiO3。
Weigh the BaTiO of 100g water heat transfer the most respectively3, the CaZrO of 0.5g3, the rare earth oxide Yb of 0.6g2O3、
The Er of 0.05g2O3, the MnO of 0.1g2, the BaCO of 0.5g3, the Co of 0.01g2O3, the ZnB of 0.15g2O4And the Li of 0.15g2SiO3,
Described BaTiO3Granularity is below 0.8 μm, to guarantee that granularity, crystal structure c/a value, Ba/Ti value meet the requirements.Carry out dispensing
After, with deionized water as disperse medium, carry out ball milling, dry and pelletize.
3. the powder after pelletize is pressed under 8～10MPa disk green compact, at a temperature of 350～450 DEG C, arranges Organic substance
6h。
4. by the disk green compact after row's Organic substance at N2/H2Atmosphere furnace sinters, sintering temperature 1340 DEG C, be incubated 3h；Disk
Green compact are at N2/H2In atmosphere furnace during sintering, before temperature reaches 600 DEG C, atmosphere furnace is passed through N2, air pressure controls at 1.05atm
Above；Temperature reaches 600 DEG C later to sintering temperature 1340 DEG C and holding stage thereof, stops being passed through N2, change into being passed through H2；Sintering
After temperature terminates, stop being passed through H2, then change into being passed through N2, air pressure reduces to 1.01～1.03atm；Then with certain cooling
Speed cools the temperature to 1000 DEG C, temperature fall time 3h, and is incubated 5h, after insulation terminates, keeps atmosphere furnace atmosphere and pressure not
Become, lower the temperature with stove, i.e. prepare low-loss BME ceramic capacitor ceramic material.Brush silver on disk the most after firing,
640 DEG C are burnt 30min, prepare silver electrode, test every electrical property.
Embodiment two
The preparation method of a kind of BME ceramic capacitor ceramic material of the present invention, comprises the following steps:
Prepare CaZrO the most respectively3、ZnB2O4And Li2SiO3；
Preparation CaZrO3: weigh analytically pure CaCO respectively310g、ZrO212.32g, mixing, ball milling, sieves, and in
1150～1200 DEG C of temperature lower calcinations, then ball milling, drying, can obtain CaZrO3；
Preparation ZnB2O4: weigh 8.14g ZnO and 12.37g H respectively3BO3, mixing, ball milling, sieve, and in 550～700
DEG C temperature lower calcination, then ball milling, drying, can obtain ZnB2O4；
Preparation Li2SiO3: weigh 7.39g Li respectively2CO3With 6.0g SiO2, mixing, ball milling, sieve, and in 550～700
DEG C temperature lower calcination, then ball milling, drying, can obtain Li2SiO3。
Weigh the BaTiO of 100g water heat transfer the most respectively3, the CaZrO of 0.5g3, the rare earth oxide Ho of 1.0g2O3、
The Er of 0.05g2O3, the MnO of 0.1g2, the BaCO of 0.5g3, the Co of 0.01g2O3, the ZnB of 0.5g2O4And the Li of 0.5g2SiO3, institute
State BaTiO3Granularity is below 0.8 μm, to guarantee that granularity, crystal structure c/a value, Ba/Ti value meet the requirements.After carrying out dispensing,
With deionized water as disperse medium, carry out ball milling, dry and pelletize.
3. the powder after pelletize is pressed under 8～10MPa disk green compact, at a temperature of 350～450 DEG C, arranges Organic substance
6h。
4. by the disk green compact after row's Organic substance at N2/H2Atmosphere furnace sinters, sintering temperature 1300 DEG C, be incubated 3h；Disk
Green compact are at N2/H2In atmosphere furnace during sintering, before temperature reaches 600 DEG C, atmosphere furnace is passed through N2, air pressure controls at 1.05atm
Above；Temperature reaches 600 DEG C later to sintering temperature 1300 DEG C and holding stage thereof, stops being passed through N2, change into being passed through H2；Sintering
After temperature terminates, stop being passed through H2, then change into being passed through N2, air pressure reduces to 1.01～1.03atm；Then with certain cooling
Speed cools the temperature to 1000 DEG C, temperature fall time 3h, and is incubated 5h, after insulation terminates, keeps atmosphere furnace atmosphere and pressure not
Become, lower the temperature with stove, i.e. prepare low-loss BME ceramic capacitor ceramic material.Brush silver on disk the most after firing,
640 DEG C are burnt 30min, prepare silver electrode, test every electrical property.
Embodiment three
The preparation method of a kind of BME ceramic capacitor ceramic material of the present invention, comprises the following steps:
Prepare CaZrO the most respectively3、ZnB2O4And Li2SiO3；
Preparation CaZrO3: weigh analytically pure CaCO respectively310g、ZrO212.32g, mixing, ball milling, sieves, and in
1150～1200 DEG C of temperature lower calcinations, then ball milling, drying, can obtain CaZrO3；
Preparation ZnB2O4: weigh 8.14g ZnO and 12.37g H respectively3BO3, mixing, ball milling, sieve, and in 550～700
DEG C temperature lower calcination, then ball milling, drying, can obtain ZnB2O4；
Preparation Li2SiO3: weigh 7.39g Li respectively2CO3With 6.0g SiO2, mixing, ball milling, sieve, and in 550～700
DEG C temperature lower calcination, then ball milling, drying, can obtain Li2SiO3。
Weigh the BaTiO of 100g water heat transfer the most respectively3, the CaZrO of 2.0g3, the rare earth oxide Sm of 1.2g2O3、
The Er of 0.05g2O3, the MnO of 0.1g2, the BaCO of 1.0g3, the Co of 0.01g2O3, the ZnB of 0.5g2O4And the Li of 0.2g2SiO3, institute
State BaTiO3Granularity is below 0.8 μm, to guarantee that granularity, crystal structure c/a value, Ba/Ti value meet the requirements.After carrying out dispensing,
With deionized water as disperse medium, carry out ball milling, dry and pelletize.
3. the powder after pelletize is pressed under 8～10MPa disk green compact, at a temperature of 350～450 DEG C, arranges Organic substance
6h。
4. by the disk green compact after row's Organic substance at N2/H2Atmosphere furnace sinters, sintering temperature 1320 DEG C, be incubated 3h；Disk
Green compact are at N2/H2In atmosphere furnace during sintering, before temperature reaches 600 DEG C, atmosphere furnace is passed through N2, air pressure controls at 1.05atm
Above；Temperature reaches 600 DEG C later to sintering temperature 1320 DEG C and holding stage thereof, stops being passed through N2, change into being passed through H2；Sintering
After temperature terminates, stop being passed through H2, then change into being passed through N2, air pressure reduces to 1.01～1.03atm；Then with certain cooling
Speed cools the temperature to 1000 DEG C, temperature fall time 3h, and is incubated 5h, after insulation terminates, keeps atmosphere furnace atmosphere and pressure not
Become, lower the temperature with stove, i.e. prepare low-loss BME ceramic capacitor ceramic material.Brush silver on disk the most after firing,
640 DEG C are burnt 30min, prepare silver electrode, test every electrical property.
Embodiment four
The preparation method of a kind of BME ceramic capacitor ceramic material of the present invention, comprises the following steps:
Prepare CaZrO the most respectively3、ZnB2O4And Li2SiO3；
Preparation CaZrO3: weigh analytically pure CaCO respectively310g、ZrO212.32g, mixing, ball milling, sieves, and in
1150～1200 DEG C of temperature lower calcinations, then ball milling, drying, can obtain CaZrO3；
Preparation ZnB2O4: weigh 8.14g ZnO and 12.37g H respectively3BO3, mixing, ball milling, sieve, and in 550～700
DEG C temperature lower calcination, then ball milling, drying, can obtain ZnB2O4；
Preparation Li2SiO3: weigh 7.39g Li respectively2CO3With 6.0g SiO2, mixing, ball milling, sieve, and in 550～700
DEG C temperature lower calcination, then ball milling, drying, can obtain Li2SiO3。
Weigh the BaTiO of 100g water heat transfer the most respectively3, the CaZrO of 3.0g3, the rare earth oxide Dy of 2.0g2O3、
The Er of 0.01g2O3, the MnO of 0.1g2, the BaCO of 0.75g3, the Co of 0.01g2O3, the ZnB of 1.0g2O4And the Li of 1.0g2SiO3, institute
State BaTiO3Granularity is below 0.8 μm, to guarantee that granularity, crystal structure c/a value, Ba/Ti value meet the requirements.After carrying out dispensing,
With deionized water as disperse medium, carry out ball milling, dry and pelletize.
3. the powder after pelletize is pressed under 8～10MPa disk green compact, at a temperature of 350～450 DEG C, arranges Organic substance
6h。
4. by the disk green compact after row's Organic substance at N2/H2Atmosphere furnace sinters, sintering temperature 1270 DEG C, be incubated 3h；Disk
Green compact are at N2/H2In atmosphere furnace during sintering, before temperature reaches 600 DEG C, atmosphere furnace is passed through N2, air pressure controls at 1.05atm
Above；Temperature reaches 600 DEG C later to sintering temperature 1270 DEG C and holding stage thereof, stops being passed through N2, change into being passed through H2；Sintering
After temperature terminates, stop being passed through H2, then change into being passed through N2, air pressure reduces to 1.01～1.03atm；Then with certain cooling
Speed cools the temperature to 1000 DEG C, temperature fall time 3h, and is incubated 5h, after insulation terminates, keeps atmosphere furnace atmosphere and pressure not
Become, lower the temperature with stove, i.e. prepare low-loss BME ceramic capacitor ceramic material.Brush silver on disk the most after firing,
640 DEG C are burnt 30min, prepare silver electrode, test every electrical property.
Embodiment five
The preparation method of a kind of BME ceramic capacitor ceramic material of the present invention, comprises the following steps:
Prepare CaZrO the most respectively3、ZnB2O4And Li2SiO3；
Preparation CaZrO3: weigh analytically pure CaCO respectively310g、ZrO212.32g, mixing, ball milling, sieves, and in
1150～1200 DEG C of temperature lower calcinations, then ball milling, drying, can obtain CaZrO3；
Preparation ZnB2O4: weigh 8.14g ZnO and 12.37g H respectively3BO3, mixing, ball milling, sieve, and in 550～700
DEG C temperature lower calcination, then ball milling, drying, can obtain ZnB2O4；
Preparation Li2SiO3: weigh 7.39g Li respectively2CO3With 6.0g SiO2, mixing, ball milling, sieve, and in 550～700
DEG C temperature lower calcination, then ball milling, drying, can obtain Li2SiO3。
Weigh the BaTiO of 100g water heat transfer the most respectively3, the CaZrO of 4.0g3, the rare earth oxide Y of 1.2g2O3、
The Er of 0.06g2O3, the MnO of 0.2g2, the BaCO of 1.5g3, the Co of 0.01g2O3, the ZnB of 0.8g2O4And the Li of 0.4g2SiO3, institute
State BaTiO3Granularity is below 0.8 μm, to guarantee that granularity, crystal structure c/a value, Ba/Ti value meet the requirements.After carrying out dispensing,
With deionized water as disperse medium, carry out ball milling, dry and pelletize.
3. the powder after pelletize is pressed under 8～10MPa disk green compact, at a temperature of 350～450 DEG C, arranges Organic substance
6h。
4. by the disk green compact after row's Organic substance at N2/H2Atmosphere furnace sinters, sintering temperature 1300 DEG C, be incubated 3h；Disk
Green compact are at N2/H2In atmosphere furnace during sintering, before temperature reaches 600 DEG C, atmosphere furnace is passed through N2, air pressure controls at 1.05atm
Above；Temperature reaches 600 DEG C later to sintering temperature 1300 DEG C and holding stage thereof, stops being passed through N2, change into being passed through H2；Sintering
After temperature terminates, stop being passed through H2, then change into being passed through N2, air pressure reduces to 1.01～1.03atm；Then with certain cooling
Speed cools the temperature to 1000 DEG C, temperature fall time 3h, and is incubated 5h, after insulation terminates, keeps atmosphere furnace atmosphere and pressure not
Become, lower the temperature with stove, i.e. prepare low-loss BME ceramic capacitor ceramic material.Brush silver on disk the most after firing,
640 DEG C are burnt 30min, prepare silver electrode, test every electrical property.
In above-mentioned five embodiments, step 2. in described ball-milling technology use SC-Mi l l ultra micro measle grinding machine, coordinate
The Dispersing Technology of Double shaft stirring, its concrete technology parameter such as following table (as a example by 10kg level powder):
After grinding distribution, by drying cupboard, slurry is dried, then drying block material is crushed, after crushing
80 mesh standard sieves crossed by powder, add the paraffin of 7～9 weight portions and make binding agent and jointly bakee pelletize, the most again cross 80 targets
Quasi-sieve.
Above-mentioned five embodiments are in burning till step, and 9, the dry-pressing disk green compact that can respectively take different formulations enter to burn, and finally make
The 5 groups of different formulations obtained and 15 styles of firing temperature, its performance parameter is listed in the table below, wherein Max | Δ c/c25℃| (%) value
Temperature range: 55 DEG C～+1250 DEG C.
Above are only five detailed description of the invention of the present invention, but the design concept of the present invention is not limited thereto, all profits
With this design, the present invention is carried out the change of unsubstantiality, the behavior invading scope all should be belonged to.
Claims (10)
1. a BME ceramic capacitor ceramic material, it is characterised in that: by the BaTiO of 100 weight portions3, 0.5～4 weight portions
CaZrO3, 0.5～2.0 rare earth oxide, 0.03～0.15% Er of weight portion of weight portion2O3, 0.1～0.4% weight portion
MnO2, 0.5～2.5% BaCO of weight portion3, 0.01～0.1 Co of weight portion2O3, 0.15～1.5 ZnB of weight portion2O4And
The Li of 0.15～1.5 weight portions2SiO3Being prepared from, described rare earth oxide uses Yb2O3、Ho2O3、Dy2O3、Sm2O3、Y2O3In
One or more.
2. a kind of BME ceramic capacitor ceramic material as claimed in claim 1, it is characterised in that: described BaTiO3For hydro-thermal method
Synthesis, granularity is below 0.8 μm.
3. the preparation method of a BME ceramic capacitor ceramic material, it is characterised in that: comprise the following steps:
Prepare CaZrO the most respectively3、ZnB2O4And Li2SiO3；
2. with the BaTiO of 100 weight portions3It is main base material, adds the CaZrO of 0.5～4.0 weight portions3, 0.5～2.0 weight portions
Rare earth oxide, 0.03～0.15 Er of weight portion2O3, 0.1～0.4 MnO of weight portion2, 0.5～2.5 BaCO of weight portion3、
The Co of 0.01～0.1 weight portion2O3, 0.15～1.5 ZnB of weight portion2O4And 0.15～1.5 Li of weight portion2SiO3, described dilute
Soil oxide uses Yb2O3、Ho2O3、Dy2O3、Sm2O3、Y2O3In one or more, after carrying out dispensing, use deionized water conduct
Disperse medium, carries out ball milling, dries and pelletize；
3. the powder pressing after pelletize is become disk green compact, at a temperature of 350～450 DEG C, arrange Organic substance；
4. by the disk green compact after row's Organic substance at N2/H2Atmosphere furnace sinters, sintering temperature 1250 DEG C～1340 DEG C, is incubated 3h,
Furnace cooling after insulation, i.e. prepares low-loss BME ceramic capacitor ceramic material.
The preparation method of a kind of BME ceramic capacitor ceramic material the most as claimed in claim 3, it is characterised in that: described step
The most 1., in, CaZrO is prepared3Time, first by CaO or CaCO3And ZrO2Carry out proportioning, weigh, mix, ball milling, sieve, and in 1150
～1200 DEG C of temperature lower calcinations, then ball milling, drying, CaZrO can be obtained3。
The preparation method of a kind of BME ceramic capacitor ceramic material the most as claimed in claim 3, it is characterised in that: described step
The most 1., in, ZnB is prepared2O4Time, first by ZnO and H3BO3Carry out proportioning, weigh, mix, ball milling, sieve, and in 550～700 DEG C
Temperature lower calcination, then ball milling, drying, can obtain ZnB2O4。
The preparation method of a kind of BME ceramic capacitor ceramic material the most as claimed in claim 3, it is characterised in that: described step
The most 1., in, Li is prepared2SiO3Time, first by Li2CO3And SiO2Carry out proportioning, weigh, mix, ball milling, sieve, and in 550～700
DEG C temperature lower calcination, then ball milling, drying, can obtain Li2SiO3。
The preparation method of a kind of BME ceramic capacitor ceramic material the most as claimed in claim 3, it is characterised in that: described
BaTiO3For water heat transfer.
The preparation method of a kind of BME ceramic capacitor ceramic material the most as claimed in claim 3, it is characterised in that: described step
The most 2., in, ball-milling technology uses SC-Mill ultra micro measle grinding machine, after grinding distribution, is dried slurry by drying cupboard, so
Crushing drying block material afterwards, 80 mesh standard sieves crossed by the powder after crushing, and the paraffin adding 7～9 weight portions bonds
Agent bakees pelletize jointly, the most again crosses 80 mesh standard sieves.
The preparation method of a kind of BME ceramic capacitor ceramic material the most as claimed in claim 3, it is characterised in that: described step
The most 3. in, the powder after pelletize is pressed into disk green compact under 8～10MPa, arranges Organic substance 6h at 350～450 DEG C.
The preparation method of a kind of BME ceramic capacitor ceramic material the most as claimed in claim 3, it is characterised in that: described step
The most 4., in, disk green compact are at N2/H2In atmosphere furnace during sintering, before temperature reaches 600 DEG C, atmosphere furnace is passed through N2, air pressure control
System is at more than 1.05atm；Temperature reaches 600 DEG C later to sintering temperature and holding stage thereof, stops being passed through N2, change into being passed through H2；
After sintering temperature insulation terminates, stop being passed through H2, then change into being passed through N2, air pressure reduces to 1.01～1.03atm；Then with certain
Rate of temperature fall cools the temperature to 1000 DEG C, temperature fall time 3h, and is incubated 5h, after insulation terminates, keeps atmosphere furnace atmosphere and pressure
Power is constant, lowers the temperature with stove.
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| CN112645708A (en) * | 2020-12-24 | 2021-04-13 | 福建火炬电子科技股份有限公司 | Anti-reduction BME ceramic dielectric capacitor and ceramic material for capacitor |
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