CN106495687B - A kind of existing fringing field, dielectric ceramic of high-energy density and preparation method thereof - Google Patents
A kind of existing fringing field, dielectric ceramic of high-energy density and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims description 93
- 238000001035 drying Methods 0.000 claims description 49
- 238000000498 ball milling Methods 0.000 claims description 38
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 20
- 239000012254 powdered material Substances 0.000 claims description 20
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 16
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 12
- 239000000853 adhesive Substances 0.000 claims description 10
- 230000001070 adhesive effect Effects 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 238000005498 polishing Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000010792 warming Methods 0.000 claims description 10
- 239000012856 weighed raw material Substances 0.000 claims description 10
- 230000005684 electric field Effects 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims description 9
- 239000010935 stainless steel Substances 0.000 claims description 9
- 238000003825 pressing Methods 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims 2
- 229910002929 BaSnO3 Inorganic materials 0.000 claims 1
- 238000005453 pelletization Methods 0.000 claims 1
- 238000004146 energy storage Methods 0.000 abstract description 21
- 239000004615 ingredient Substances 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 230000010354 integration Effects 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000004570 mortar (masonry) Substances 0.000 description 21
- 238000005469 granulation Methods 0.000 description 16
- 230000003179 granulation Effects 0.000 description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 14
- 229960000935 dehydrated alcohol Drugs 0.000 description 14
- 239000000203 mixture Substances 0.000 description 14
- 239000003990 capacitor Substances 0.000 description 11
- 238000000034 method Methods 0.000 description 8
- 230000010287 polarization Effects 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 239000011230 binding agent Substances 0.000 description 7
- 238000000643 oven drying Methods 0.000 description 7
- 239000002904 solvent Substances 0.000 description 7
- 230000005621 ferroelectricity Effects 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- 239000011232 storage material Substances 0.000 description 5
- 229910002113 barium titanate Inorganic materials 0.000 description 3
- 239000003985 ceramic capacitor Substances 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 3
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000010425 computer drawing Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229920002545 silicone oil Polymers 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- MTZOKGSUOABQEO-UHFFFAOYSA-L barium(2+);phthalate Chemical compound [Ba+2].[O-]C(=O)C1=CC=CC=C1C([O-])=O MTZOKGSUOABQEO-UHFFFAOYSA-L 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229940071182 stannate Drugs 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
- C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
- C04B35/465—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates
- C04B35/468—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates
- C04B35/4682—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates based on BaTiO3 perovskite phase
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
- C04B41/5116—Ag or Au
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/88—Metals
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/08—Inorganic dielectrics
- H01G4/12—Ceramic dielectrics
- H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The invention discloses a kind of existing fringing field, the dielectric ceramic of high-energy density and preparation method thereof, the chemical formula of the dielectric ceramic is (1-x) BaTiO3‑xBaSnO3, x is molar percentage, wherein 0.03≤x≤0.15, the present invention uses the preparation method of synthesis in solid state, has obtained the dielectric ceramic with energy-storage property high under existing fringing field, ingredient of the invention and processing step are simple, easily operated, reproducible;It is mainly used in the fields such as the portable and wearable electronic of high integration miniaturization.
Description
Technical field
The invention belongs to field of electronic ceramic materials, and in particular to a kind of existing fringing field, high-energy density dielectric ceramic and
Preparation method.
Background technique
In the environment of fossil energy worsening shortages and global warming, energy storage is a Xiang Guanjian of reasonable energy utilization
Technology.In modern industry and social life, electric energy is main energetic medium, and the weight that storage is effective use of energy sources is carried out to it
Want method.In electric energy storage method, common energy storage device has rechargeable battery, supercapacitor, fuel cell etc., these set
It is standby that there is very high energy density, but the charge and discharge time is slow.In comparison, energy-storage capacitor has the spy of fast charging and discharging
Point, therefore have huge application prospect in hybrid vehicle, pulse-power apparatus etc..
Currently, most of energy-storage capacitor is applied in the area high electric field (6000kV/cm), this is strong to the breakdown of dielectric substance
Degree proposes very high request, while proposing very high dielectric strength requirement to the insulation system of capacitor.Especially Highgrade integration,
There is biggish application to limit in the portable or wearable device of miniaturization.So high-energy of the development and application in existing fringing field intensity
The novel energy-storing material of density is very urgent.
Summary of the invention
The purpose of the present invention is to provide a kind of existing fringing field, the dielectric ceramic of high-energy density and preparation method thereof, with gram
The problems of the above-mentioned prior art is taken, the method that the present invention is modulated by ingredient lures in barium phthalate base binary material system
Critical effect is issued, so that the capacitivity of system be significantly increased, has been made in existing fringing field intensity (10kV/cm), higher
Energy density (31mJ/cm3) dielectric ceramic.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
The dielectric ceramic of a kind of existing fringing field, high-energy density, the chemical formula of the dielectric ceramic are (1-x) BaTiO3-
xBaSnO3, wherein 0.03≤x≤0.15, x are mole percent.
Further, the chemical formula of the dielectric ceramic is (1-x) BaTiO3-xBaSnO3, wherein x=0.105, x are mole
Percentage.
A kind of existing fringing field, high-energy density dielectric ceramic preparation method, comprising the following steps:
(1) chemical formula (1-x) BaTiO is pressed3-xBaSnO3The proportion of middle each element weighs raw material BaCO3、TiO2And SnO2,
In 0.03≤x≤0.15, x is mole percent;
(2) ball milling, drying and grinding are successively carried out after mixing weighed raw material, 60 meshes is then crossed and obtains powder;
(3) by powder pre-burning in air, room temperature is naturally cooled to, preburning powdered material is obtained;
(4) secondary ball milling is carried out after grinding preburning powdered material, obtains dry powder after drying;
(5) be added and adhesive and be uniformly mixed after grinding dry powder, then filter out partial size be 0.15mm extremely
The granulation powder of 0.28mm;
(6) pressing mold forms to obtain cylindrical blank after being granulated powder drying;
(7) adhesive of cylindrical blank is discharged, is then sintered 3-5 hours, obtains burned at 1425~1475 DEG C
Potsherd;
(8) conductive silver paste is coated after polishing smooth burned potsherd upper and lower surface, burning Electrode treatment is then carried out and obtains
To existing fringing field, the dielectric ceramic of high-energy density.
Further, Ball-milling Time is 4 hours in step (2), and revolving speed is 40-50 revs/min, and drying temperature is 80 DEG C, when
Between be 3 hours;The secondary ball milling time is 8 hours in step (4), and revolving speed is 40-50 revs/min, and drying temperature is 80 DEG C, and the time is
3 hours.
Further, calcined temperature is 1350 DEG C in step (3), keeps the temperature 4 hours.
Further, adhesive is PVA in step (5), and additional amount is the 5-10% for drying powder quality.
Further, drying temperature is 80 DEG C in step (6), and drying time is 5-10 minutes;Pressing mold molding specifically: will
Granulation powder after drying pours into the stainless steel mould that diameter is 10mm, is shaped to cylinder within pressure maintaining 90 seconds under 30MPa pressure
Shape blank.
Further, cylindrical blank is kept the temperature 2 hours in 600 DEG C adhesive is discharged in step (7).
Further, Electrode treatment is burnt in step (8) specifically: be warming up to 800 DEG C in air after coating conductive silver paste
And 20 minutes are kept the temperature, then cooled to room temperature.
Compared with prior art, the invention has the following beneficial technical effects:
A kind of dielectric ceramic of novel existing fringing field high-energy density has been made in the present invention, which has phase under existing fringing field
To higher energy storage density.The method that the method for the present invention uses synthesis in solid state, with barium titanate (BT) for matrix, doping Sn obtains titanium
Sour barium-barium stannate (BT-BS), obtains the dielectric ceramic of high-dielectric constant, existing fringing field high energy storage density.Ingredient and technique of the invention
Step is simple, easily operated, reproducible, high yield rate.It obtains by gradient experiment in x=0.105, i.e. 0.89BaTiO3-
0.105BaSnO3Locating capacitor energy storage density has peak, is 31mJ/cm at existing fringing field (10kV/cm)3, the parameter values
Capacitive energy storage material is commonly used considerably beyond other.
Detailed description of the invention
Fig. 1 is the polarization intensity for the dielectric ceramic that embodiment 1 obtains and the relationship of electric field;
Fig. 2 is comparison of the different materials energy storage density of embodiment 2 under same electric field.
Specific embodiment
Below with reference to the invention will be described in further detail:
The dielectric ceramic of a kind of existing fringing field, high-energy density, the chemical formula of the dielectric ceramic are (1-x) BaTiO3-
xBaSnO3, x is molar percentage, wherein 0.03≤x≤0.15, preferred x=0.105.
A kind of existing fringing field, high-energy density dielectric ceramic preparation method, comprising the following steps:
(1) chemical formula (1-x) BaTiO is pressed3-xBaSnO3The proportion of middle each element weighs raw material BaCO3、TiO2And SnO2,
In 0.03≤x≤0.15;
(2) it is put into ball grinder after mixing weighed raw material, ball milling solvent dehydrated alcohol and agate ball, ball milling 4 is added
Hour, rotational speed of ball-mill is 40-50 revs/min, then mixture is put into baking oven and is dried 3 hours for 80 DEG C, it places into mortar and grinds,
Then 60 meshes are crossed and obtain powder;
(3) powder that step (2) obtains is put into crucible, is compacted, covered;In 1350 DEG C of pre-burnings in Muffle furnace, protect
Temperature 4 hours, naturally cools to room temperature, comes out of the stove, obtain preburning powdered material;
(4) preburning powdered material that step (3) obtains is ground into mortar fine powder, be fitted into ball grinder, ball milling is added and is situated between
Matter dehydrated alcohol carries out secondary ball milling, and revolving speed is 40-50 revs/min, continues 8 hours, and mixture is put into 80 DEG C of drying in baking oven
Obtain within 3 hours drying powder;
(5) the drying powder that step (4) obtains is ground in mortar, binder PVA is added, and PVA accounts for drying powder
The 5-10% of quality is uniformly mixed, and crosses the granulation powder for filtering out that partial size is 0.15mm to 0.28mm;
(6) the granulation powder that step (5) obtains is put into baking oven drying 5-10 minutes at a temperature of 80 DEG C, powder is taken to fall
In the stainless steel mould for entering diameter 10mm, it is shaped to cylindrical blank within pressure maintaining 90 seconds under 30MPa pressure;
(7) the cylindrical blank that step (6) obtains is put into Muffle furnace, temperature rises to 600 DEG C, keeps the temperature 2 hours, discharge
PVA;
(8) sample after dumping in step (7) is put into crucible, buries material with similar powder and buries burning, 1425~
It is sintered in 1475 DEG C, keeps the temperature 4 hours, with furnace cooled to room temperature, obtain burned potsherd.
(9) conductive silver paste is coated after polishing smooth potsherd upper and lower surface obtained, is warming up to 800 DEG C of guarantors in air
Temperature cooled to room temperature after twenty minutes obtains the dielectric ceramic of a kind of existing fringing field, high-energy density.
The energy storage characteristic of the ceramic capacitor is measured using ferroelectricity work station (Radiant technology).By ceramic electrical
Container is placed into the fixture of ferroelectricity work station two-electrode system, connection work station voltage source and capacitor upper/lower electrode.Entirely
Two-electrode system, which is immersed in methyl-silicone oil, prevents air flashover.Voltage source is controlled using ferroelectricity work station, in ceramic capacitor
The upper unipolar triangle voltage waveform E for applying 10Hz, a 10kV/cm.The survey of work station is used while application voltage
Quantity collection system measures the polarization intensity P of capacitor, and the relation curve of polarization intensity and electric field strength is gone out by computer drawing
(ferroelectric hysteresis loop).The definition of energy is stored according to capacitor it is found that calculating electric field strength to the integral of polarization intensity by curve
Capacitor energy storage density U can be obtained multiplied by a constante。
Present invention discover that in (1-x) BaTiO3-xBaSnO3Three Near The Critical Points of ferroelectric ceramics, ceramic material is in existing fringing field
Under have biggish energy density.This is because ferroelectric ceramics domain wall free energy minimization at three critical points, the pole under electric field action
Easily deflection polarization, and store electric energy.The present invention passes through in BaTiO3Middle doping Sn is in material by the method that ingredient is modulated
Three Near The Critical Points, the energy storage density of material can reach 31mJ/cm at existing fringing field (10kV/cm) at that point3.It therefore can be with
The material is applied to portable and wearable electronic equipment etc. to require on the energy-storage travelling wave tube in the equipment of low-voltage-grade.
Below with reference to embodiment, the invention will be described in further detail:
Embodiment 1
(1) chemical formula (1-x) BaTiO is pressed3-xBaSnO3The proportion of middle each element weighs raw material BaCO3、TiO2And SnO2,
Middle x=0.03;
(2) it is put into ball grinder after mixing weighed raw material, ball milling solvent dehydrated alcohol and agate ball, ball milling 4 is added
Hour, rotational speed of ball-mill is 40 revs/min, then mixture is put into baking oven and is dried 3 hours for 80 DEG C, places into mortar and grinds, so
60 meshes are crossed afterwards obtains powder;
(3) powder that step (2) obtains is put into crucible, is compacted, covered;In 1350 DEG C of pre-burnings in Muffle furnace, protect
Temperature 4 hours, naturally cools to room temperature, comes out of the stove, obtain preburning powdered material;
(4) preburning powdered material that step (3) obtains is ground into mortar fine powder, be fitted into ball grinder, ball milling is added and is situated between
Matter dehydrated alcohol carries out secondary ball milling, and revolving speed is 40 revs/min, continues 8 hours, and it is small that mixture is put into 80 DEG C of drying 3 in baking oven
When obtain drying powder;
(5) the drying powder that step (4) obtains is ground in mortar, binder PVA is added, and PVA accounts for drying powder
The 5% of quality is uniformly mixed, and crosses the granulation powder for filtering out that partial size is 0.15mm to 0.28mm;
(6) the granulation powder that step (5) obtains is put into baking oven drying 5 minutes at a temperature of 80 DEG C, powder is taken to pour into
In the stainless steel mould of diameter 10mm, it is shaped to cylindrical blank within pressure maintaining 90 seconds under 30MPa pressure;
(7) the cylindrical blank that step (6) obtains is put into Muffle furnace, temperature rises to 600 DEG C, keeps the temperature 2 hours, discharge
PVA;
(8) sample after dumping in step (7) is put into crucible, buries material with similar powder and bury burning, in 1425 DEG C
Sintering keeps the temperature 4 hours, with furnace cooled to room temperature, obtains burned potsherd.
(9) conductive silver paste is coated after polishing smooth potsherd upper and lower surface obtained, is warming up to 800 DEG C of guarantors in air
Temperature cooled to room temperature after twenty minutes obtains the dielectric ceramic of a kind of existing fringing field, high-energy density.
Embodiment 2
(1) chemical formula (1-x) BaTiO is pressed3-xBaSnO3The proportion of middle each element weighs raw material BaCO3、TiO2And SnO2,
Middle x=0.09;
(2) it is put into ball grinder after mixing weighed raw material, ball milling solvent dehydrated alcohol and agate ball, ball milling 4 is added
Hour, rotational speed of ball-mill is 45 revs/min, then mixture is put into baking oven and is dried 3 hours for 80 DEG C, places into mortar and grinds, so
60 meshes are crossed afterwards obtains powder;
(3) powder that step (2) obtains is put into crucible, is compacted, covered;In 1350 DEG C of pre-burnings in Muffle furnace, protect
Temperature 4 hours, naturally cools to room temperature, comes out of the stove, obtain preburning powdered material;
(4) preburning powdered material that step (3) obtains is ground into mortar fine powder, be fitted into ball grinder, ball milling is added and is situated between
Matter dehydrated alcohol carries out secondary ball milling, and revolving speed is 45 revs/min, continues 8 hours, and it is small that mixture is put into 80 DEG C of drying 3 in baking oven
When obtain drying powder;
(5) the drying powder that step (4) obtains is ground in mortar, binder PVA is added, and PVA accounts for drying powder
The 6% of quality is uniformly mixed, and crosses the granulation powder for filtering out that partial size is 0.15mm to 0.28mm;
(6) the granulation powder that step (5) obtains is put into baking oven drying 7 minutes at a temperature of 80 DEG C, powder is taken to pour into
In the stainless steel mould of diameter 10mm, it is shaped to cylindrical blank within pressure maintaining 90 seconds under 30MPa pressure;
(7) the cylindrical blank that step (6) obtains is put into Muffle furnace, temperature rises to 600 DEG C, keeps the temperature 2 hours, discharge
PVA;
(8) sample after dumping in step (7) is put into crucible, buries material with similar powder and bury burning, in 1450 DEG C
Sintering keeps the temperature 4 hours, with furnace cooled to room temperature, obtains burned potsherd.
(9) conductive silver paste is coated after polishing smooth potsherd upper and lower surface obtained, is warming up to 800 DEG C of guarantors in air
Temperature cooled to room temperature after twenty minutes obtains the dielectric ceramic of a kind of existing fringing field, high-energy density.
Embodiment 3
(1) chemical formula (1-x) BaTiO is pressed3-xBaSnO3The proportion of middle each element weighs raw material BaCO3、TiO2And SnO2,
Middle x=0.1;
(2) it is put into ball grinder after mixing weighed raw material, ball milling solvent dehydrated alcohol and agate ball, ball milling 4 is added
Hour, rotational speed of ball-mill is 50 revs/min, then mixture is put into baking oven and is dried 3 hours for 80 DEG C, places into mortar and grinds, so
60 meshes are crossed afterwards obtains powder;
(3) powder that step (2) obtains is put into crucible, is compacted, covered;In 1350 DEG C of pre-burnings in Muffle furnace, protect
Temperature 4 hours, naturally cools to room temperature, comes out of the stove, obtain preburning powdered material;
(4) preburning powdered material that step (3) obtains is ground into mortar fine powder, be fitted into ball grinder, ball milling is added and is situated between
Matter dehydrated alcohol carries out secondary ball milling, and revolving speed is 50 revs/min, continues 8 hours, and it is small that mixture is put into 80 DEG C of drying 3 in baking oven
When obtain drying powder;
(5) the drying powder that step (4) obtains is ground in mortar, binder PVA is added, and PVA accounts for drying powder
The 10% of quality is uniformly mixed, and crosses the granulation powder for filtering out that partial size is 0.15mm to 0.28mm;
(6) the granulation powder that step (5) obtains is put into baking oven drying 8 minutes at a temperature of 80 DEG C, powder is taken to pour into
In the stainless steel mould of diameter 10mm, it is shaped to cylindrical blank within pressure maintaining 90 seconds under 30MPa pressure;
(7) the cylindrical blank that step (6) obtains is put into Muffle furnace, temperature rises to 600 DEG C, keeps the temperature 2 hours, discharge
PVA;
(8) sample after dumping in step (7) is put into crucible, buries material with similar powder and bury burning, in 1475 DEG C
Sintering keeps the temperature 4 hours, with furnace cooled to room temperature, obtains burned potsherd.
(9) conductive silver paste is coated after polishing smooth potsherd upper and lower surface obtained, is warming up to 800 DEG C of guarantors in air
Temperature cooled to room temperature after twenty minutes obtains the dielectric ceramic of a kind of existing fringing field, high-energy density.
Embodiment 4
(1) chemical formula (1-x) BaTiO is pressed3-xBaSnO3The proportion of middle each element weighs raw material BaCO3、TiO2And SnO2,
Middle x=0.105;
(2) it is put into ball grinder after mixing weighed raw material, ball milling solvent dehydrated alcohol and agate ball, ball milling 4 is added
Hour, rotational speed of ball-mill is 40 revs/min, then mixture is put into baking oven and is dried 3 hours for 80 DEG C, places into mortar and grinds, so
60 meshes are crossed afterwards obtains powder;
(3) powder that step (2) obtains is put into crucible, is compacted, covered;In 1350 DEG C of pre-burnings in Muffle furnace, protect
Temperature 4 hours, naturally cools to room temperature, comes out of the stove, obtain preburning powdered material;
(4) preburning powdered material that step (3) obtains is ground into mortar fine powder, be fitted into ball grinder, ball milling is added and is situated between
Matter dehydrated alcohol carries out secondary ball milling, and revolving speed is 40 revs/min, continues 8 hours, and it is small that mixture is put into 80 DEG C of drying 3 in baking oven
When obtain drying powder;
(5) the drying powder that step (4) obtains is ground in mortar, binder PVA is added, and PVA accounts for drying powder
The 8% of quality is uniformly mixed, and crosses the granulation powder for filtering out that partial size is 0.15mm to 0.28mm;
(6) the granulation powder that step (5) obtains is put into baking oven drying 5 to 10 minutes at a temperature of 80 DEG C, takes powder
It pours into the stainless steel mould of diameter 10mm, is shaped to cylindrical blank within pressure maintaining 90 seconds under 30MPa pressure;
(7) the cylindrical blank that step (6) obtains is put into Muffle furnace, temperature rises to 600 DEG C, keeps the temperature 2 hours, discharge
PVA;
(8) sample after dumping in step (7) is put into crucible, buries material with similar powder and bury burning, in 1465 DEG C
Sintering keeps the temperature 4 hours, with furnace cooled to room temperature, obtains burned potsherd.
(9) conductive silver paste is coated after polishing smooth potsherd upper and lower surface obtained, is warming up to 800 DEG C of guarantors in air
Temperature cooled to room temperature after twenty minutes obtains the dielectric ceramic of a kind of existing fringing field, high-energy density.
Embodiment 5
(1) chemical formula (1-x) BaTiO is pressed3-xBaSnO3The proportion of middle each element weighs raw material BaCO3、TiO2And SnO2,
Middle x=0.12;
(2) it is put into ball grinder after mixing weighed raw material, ball milling solvent dehydrated alcohol and agate ball, ball milling 4 is added
Hour, rotational speed of ball-mill is 45 revs/min, then mixture is put into baking oven and is dried 3 hours for 80 DEG C, places into mortar and grinds, so
60 meshes are crossed afterwards obtains powder;
(3) powder that step (2) obtains is put into crucible, is compacted, covered;In 1350 DEG C of pre-burnings in Muffle furnace, protect
Temperature 4 hours, naturally cools to room temperature, comes out of the stove, obtain preburning powdered material;
(4) preburning powdered material that step (3) obtains is ground into mortar fine powder, be fitted into ball grinder, ball milling is added and is situated between
Matter dehydrated alcohol carries out secondary ball milling, and revolving speed is 45 revs/min, continues 8 hours, and it is small that mixture is put into 80 DEG C of drying 3 in baking oven
When obtain drying powder;
(5) the drying powder that step (4) obtains is ground in mortar, binder PVA is added, and PVA accounts for drying powder
The 10% of quality is uniformly mixed, and crosses the granulation powder for filtering out that partial size is 0.15mm to 0.28mm;
(6) the granulation powder that step (5) obtains is put into baking oven drying 6 minutes at a temperature of 80 DEG C, powder is taken to pour into
In the stainless steel mould of diameter 10mm, it is shaped to cylindrical blank within pressure maintaining 90 seconds under 30MPa pressure;
(7) the cylindrical blank that step (6) obtains is put into Muffle furnace, temperature rises to 600 DEG C, keeps the temperature 2 hours, discharge
PVA;
(8) sample after dumping in step (7) is put into crucible, buries material with similar powder and bury burning, in 1445 DEG C
Sintering keeps the temperature 4 hours, with furnace cooled to room temperature, obtains burned potsherd.
(9) conductive silver paste is coated after polishing smooth potsherd upper and lower surface obtained, is warming up to 800 DEG C of guarantors in air
Temperature cooled to room temperature after twenty minutes obtains the dielectric ceramic of a kind of existing fringing field, high-energy density.
Embodiment 6
(1) chemical formula (1-x) BaTiO is pressed3-xBaSnO3The proportion of middle each element weighs raw material BaCO3、TiO2And SnO2,
Middle x=0.15;
(2) it is put into ball grinder after mixing weighed raw material, ball milling solvent dehydrated alcohol and agate ball, ball milling 4 is added
Hour, rotational speed of ball-mill is 40 revs/min, then mixture is put into baking oven and is dried 3 hours for 80 DEG C, places into mortar and grinds, so
60 meshes are crossed afterwards obtains powder;
(3) powder that step (2) obtains is put into crucible, is compacted, covered;In 1350 DEG C of pre-burnings in Muffle furnace, protect
Temperature 4 hours, naturally cools to room temperature, comes out of the stove, obtain preburning powdered material;
(4) preburning powdered material that step (3) obtains is ground into mortar fine powder, be fitted into ball grinder, ball milling is added and is situated between
Matter dehydrated alcohol carries out secondary ball milling, and revolving speed is 50 revs/min, continues 8 hours, and it is small that mixture is put into 80 DEG C of drying 3 in baking oven
When obtain drying powder;
(5) the drying powder that step (4) obtains is ground in mortar, binder PVA is added, and PVA accounts for drying powder
The 5% of quality is uniformly mixed, and crosses the granulation powder for filtering out that partial size is 0.15mm to 0.28mm;
(6) the granulation powder that step (5) obtains is put into baking oven drying 5 minutes at a temperature of 80 DEG C, powder is taken to pour into
In the stainless steel mould of diameter 10mm, it is shaped to cylindrical blank within pressure maintaining 90 seconds under 30MPa pressure;
(7) the cylindrical blank that step (6) obtains is put into Muffle furnace, temperature rises to 600 DEG C, keeps the temperature 2 hours, discharge
PVA;
(8) sample after dumping in step (7) is put into crucible, buries material with similar powder and bury burning, in 1450 DEG C
Sintering keeps the temperature 4 hours, with furnace cooled to room temperature, obtains burned potsherd.
(9) conductive silver paste is coated after polishing smooth potsherd upper and lower surface obtained, is warming up to 800 DEG C of guarantors in air
Temperature cooled to room temperature after twenty minutes obtains the dielectric ceramic of a kind of existing fringing field, high-energy density.
Select dielectric ceramic 0.91BaTiO made from the embodiment of the present invention 2 and embodiment 43-0.09BaSnO3With
0.895BaTiO3-0.105BaSnO3, and comparison capacitive energy storage material is lead zirconate titanate (PZT), lead magnesium niobate-lead titanate
(PMNPT) and Kynoar-chlorotrifluoroethylene (P (VDF-CTFE)) metal-insulator-gold, is made in above-mentioned a variety of materials
Belong to structure capacitance, energy storage characteristic and the progress of each capacitor are measured using ferroelectricity work station (Radiant technology)
Comparison.Each capacitor is placed into respectively in the fixture of ferroelectricity work station two-electrode system, connection work station voltage source and electricity
Container upper/lower electrode.Entire two-electrode system, which is immersed in methyl-silicone oil, prevents air flashover.Electricity is controlled using ferroelectricity work station
Potential source applies unipolar triangle voltage waveform E of 10Hz, a 10kV/cm on ceramic capacitor.It applies alive same
When using work station measurement acquisition system measurement capacitor polarization intensity P, by computer drawing go out polarization intensity and electricity
The relation curve of field intensity, as shown in Figure 1, the dielectric ceramic that the present invention obtains is at room temperature, the phase at existing fringing field (10kV/cm)
Than there are highest polarization intensity (10 μ C/cm in other common energy storage materials2), while there is minimum loss.
Dielectric ceramic 0.91BaTiO made from the selection embodiment of the present invention 2, embodiment 3, embodiment 4 and embodiment 53-
0.09BaSnO3、0.9BaTiO3-0.1BaSnO3、0.895BaTiO3-0.105BaSnO3And 0.88BaTiO3-
0.12BaSnO3, selecting comparison energy storage material is PZT, PMNPT and P (VDF-CTFE), calculates above-mentioned each material sample in room
Under temperature, the data obtained is depicted as histogram, as shown in Fig. 2, can see by energy density under the electric field of 10Hz, 10kV/cm
Out, dielectric ceramic prepared by the present invention has relatively highest energy storage (31mJ/cm3), it is twice of other common energy storage materials
More than.
Claims (7)
1. the dielectric ceramic of a kind of existing fringing field, high-energy density, which is characterized in that the chemical formula of the dielectric ceramic is (1-x)
BaTiO3-xBaSnO3, wherein x=0.105, x are mole percent;
The preparation method of the dielectric ceramic, comprising the following steps:
(1) chemical formula (1-x) BaTiO is pressed3-xBaSnO3The proportion of middle each element weighs raw material BaCO3、TiO2And SnO2, wherein x=
0.105, x is mole percent;
(2) ball milling, drying and grinding are successively carried out after mixing weighed raw material, 60 meshes is then crossed and obtains powder;
(3) by powder pre-burning in air, room temperature is naturally cooled to, preburning powdered material is obtained;
(4) secondary ball milling is carried out after grinding preburning powdered material, obtains dry powder after drying;
(5) adhesive is added after grinding dry powder and is uniformly mixed, then filtering out partial size is 0.15mm to 0.28mm's
It is granulated powder;
(6) pressing mold forms to obtain cylindrical blank after being granulated powder drying;
(7) adhesive of cylindrical blank is discharged, is then sintered 3-5 hours at 1425~1475 DEG C, obtains burned pottery
Tile;
(8) coat conductive silver paste after polishing smooth burned potsherd upper and lower surface, then carry out burn Electrode treatment obtain it is low
The dielectric ceramic of electric field, high-energy density;
Pre-burning mode is to heat in Muffle furnace to powder described in step (3) in air, and calcined temperature is 1350 DEG C, heat preservation 4
Hour.
2. a kind of preparation method of the dielectric ceramic of existing fringing field, high-energy density, which comprises the following steps:
(1) chemical formula (1-x) BaTiO is pressed3-xBaSnO3The proportion of middle each element weighs raw material BaCO3、TiO2And SnO2, wherein x
=0.105, x are mole percent;
(2) ball milling, drying and grinding are successively carried out after mixing weighed raw material, 60 meshes is then crossed and obtains powder;
(3) by powder pre-burning in air, room temperature is naturally cooled to, preburning powdered material is obtained;
(4) secondary ball milling is carried out after grinding preburning powdered material, obtains dry powder after drying;
(5) adhesive is added after grinding dry powder and is uniformly mixed, then filtering out partial size is 0.15mm to 0.28mm's
It is granulated powder;
(6) pressing mold forms to obtain cylindrical blank after being granulated powder drying;
(7) adhesive of cylindrical blank is discharged, is then sintered 3-5 hours at 1425~1475 DEG C, obtains burned pottery
Tile;
(8) coat conductive silver paste after polishing smooth burned potsherd upper and lower surface, then carry out burn Electrode treatment obtain it is low
The dielectric ceramic of electric field, high-energy density;
Pre-burning mode is to heat in Muffle furnace to powder described in step (3) in air, and calcined temperature is 1350 DEG C, heat preservation 4
Hour.
3. the preparation method of the dielectric ceramic of a kind of existing fringing field according to claim 2, high-energy density, feature exist
In Ball-milling Time is 4 hours in step (2), and revolving speed is 40-50 revs/min, and drying temperature is 80 DEG C, and the time is 3 hours;Step
(4) the secondary ball milling time is 8 hours in, and revolving speed is 40-50 revs/min, and drying temperature is 80 DEG C, and the time is 3 hours.
4. the preparation method of the dielectric ceramic of a kind of existing fringing field according to claim 2, high-energy density, feature exist
In adhesive is PVA in step (5), and additional amount is the 5-10% for drying powder quality.
5. the preparation method of the dielectric ceramic of a kind of existing fringing field according to claim 2, high-energy density, feature exist
In drying temperature is 80 DEG C in step (6), and drying time is 5-10 minutes;Pressing mold molding specifically: by the pelletizing after drying
Material pours into the stainless steel mould that diameter is 10mm, is shaped to cylindrical blank within pressure maintaining 90 seconds under 30MPa pressure.
6. the preparation method of the dielectric ceramic of a kind of existing fringing field according to claim 2, high-energy density, feature exist
In, in step (7) by cylindrical blank in 600 DEG C keep the temperature 2 hours adhesive is discharged.
7. the preparation method of the dielectric ceramic of a kind of existing fringing field according to claim 2, high-energy density, feature exist
In burning Electrode treatment in step (8) specifically: be warming up to 800 DEG C in air after coating conductive silver paste and keep the temperature 20 minutes, so
Cooled to room temperature afterwards.
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