CN106495687A - 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 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims description 85
- 238000001035 drying Methods 0.000 claims description 40
- 238000000498 ball milling Methods 0.000 claims description 36
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 18
- 239000012254 powdered material Substances 0.000 claims description 18
- 239000002994 raw material Substances 0.000 claims description 18
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 16
- 239000011230 binding agent Substances 0.000 claims description 15
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 11
- 238000010792 warming Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims description 9
- 239000010935 stainless steel Substances 0.000 claims description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 9
- 230000005684 electric field Effects 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 238000005453 pelletization Methods 0.000 claims 1
- 229910052573 porcelain Inorganic materials 0.000 claims 1
- 238000004146 energy storage Methods 0.000 abstract description 20
- 230000010354 integration Effects 0.000 abstract description 3
- 238000010532 solid phase synthesis reaction Methods 0.000 abstract description 2
- 239000004570 mortar (masonry) Substances 0.000 description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 14
- 150000001875 compounds Chemical class 0.000 description 14
- 229960000935 dehydrated alcohol Drugs 0.000 description 14
- 239000003990 capacitor Substances 0.000 description 10
- 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
- 238000001914 filtration 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
- 238000005516 engineering process Methods 0.000 description 4
- 239000003985 ceramic capacitor Substances 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000010425 computer drawing Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 229920002545 silicone oil Polymers 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 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 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
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram 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
- 238000005259 measurement Methods 0.000 description 1
- 229940071182 stannate Drugs 0.000 description 1
- 238000003860 storage Methods 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
- H01G4/1218—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates
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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 dielectric ceramic of a kind of existing fringing field, 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, preparation method of the present invention using solid phase synthesis, has obtained the dielectric ceramic with high energy-storage property under existing fringing field, and the composition and processing step of the present invention is 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, the dielectric ceramic of high-energy-density and
Its preparation method.
Background technology
In the environment of fossil energy worsening shortages and global warming, energy storage is a key of reasonable energy utilization
Technology.In modern industry and social life, electric energy is main energetic medium, and it is the weight of effective use of energy sources which is carried out storing
Want method.In electrical power storage method, conventional energy storage device has rechargeable battery, ultracapacitor, fuel cell etc., and these set
Getting everything ready has very high energy density, but the discharge and recharge time is slow.Comparatively speaking, energy-storage capacitor has the spy of fast charging and discharging
Point, therefore has huge application prospect in hybrid vehicle, pulse-power apparatus etc..
At present, most of energy-storage capacitor is applied in high electric field (6000kV/cm) area, and this is strong to puncturing for dielectric substance
Degree proposes very high request, while the insulation system to electric capacity proposes very high dielectric strength requirement.Particularly Highgrade integration,
There is larger application limitation 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.
Content of the invention
It is an object of the invention to provide dielectric ceramic of a kind of existing fringing field, high-energy-density and preparation method thereof, with gram
The defect that above-mentioned prior art is present is taken, the method that the present invention is modulated by composition is lured in barium phthalate base binary material system
Critical effect is sent, so as to the dielectric constant of system has been significantly increased, has been obtained in existing fringing field intensity (10kV/cm), higher
Energy density (31mJ/cm3) dielectric ceramic.
For reaching above-mentioned purpose, the present invention is adopted the following technical scheme that：
A kind of existing fringing field, the dielectric ceramic of high-energy-density, the chemical formula of the dielectric ceramic is (1-x) BaTiO3-
xBaSnO3, wherein 0.03≤x≤0.15, x is mole percent.
Further, the chemical formula of the dielectric ceramic is (1-x) BaTiO3-xBaSnO3, wherein x=0.105, x for mole
Percent.
A kind of existing fringing field, the preparation method of the dielectric ceramic of high-energy-density, comprise the following steps：
(1) chemical formula (1-x) BaTiO is pressed3-xBaSnO3The proportioning of middle each element weighs raw material BaCO3、TiO2And SnO2, its
In 0.03≤x≤0.15, x is mole percent；
(2) ball milling, drying and grinding will be carried out successively after the raw material for weighing mixing, then crosses 60 mesh sieves and obtain powder；
(3) by powder pre-burning in atmosphere, room temperature is naturally cooled to, preburning powdered material is obtained；
(4) secondary ball milling is carried out after grind preburning powdered material, obtain dry powder after drying；
(5) binding agent mix homogeneously are added after grind dry powder, particle diameter is then filtered out for 0.15mm extremely
The pelletize powder of 0.28mm；
(6) pressing mold molding after the drying of pelletize powder is obtained cylindrical blank；
(7) binding agent of cylindrical blank is discharged, then at 1425～1475 DEG C, sinters 3-5 hours, obtain burned
Potsherd；
(8) conductive silver paste is coated after polish smooth burned potsherd upper and lower surface, then carry out burning Electrode treatment and obtain
Arrive existing fringing field, the dielectric ceramic of high-energy-density.
Further, in step (2), Ball-milling Time is 4 hours, and rotating speed is 40-50 rev/min, and drying temperature is 80 DEG C, when
Between be 3 hours；In step (4), the secondary ball milling time is 8 hours, and rotating speed is 40-50 rev/min, and drying temperature is 80 DEG C, and the time is
3 hours.
Further, in step (3), calcined temperature is 1350 DEG C, is incubated 4 hours.
Further, in step (5), binding agent is PVA, and addition is the 5-10% for drying powder quality.
Further, in step (6), drying temperature is 80 DEG C, and drying time is 5-10 minutes；Pressing mold molding is specially：Will
Pelletize powder after drying is poured in the stainless steel mould of a diameter of 10mm, and pressurize under 30MPa pressure is shaped to cylinder in 90 seconds
Shape blank.
Further, cylindrical blank is incubated 2 hours to discharge binding agent in 600 DEG C in step (7).
Further, burn Electrode treatment to be specially in step (8)：800 DEG C are warming up to after coating conductive silver paste in atmosphere
And 20 minutes are incubated, then naturally cool to room temperature.
Compared with prior art, the present invention has following beneficial technique effect：
The present invention has been obtained a kind of dielectric ceramic of new existing fringing field high-energy-density, and the pottery has phase under existing fringing field
To higher energy storage density.Method of the inventive method using solid phase synthesis, based on Barium metatitanate. (BT), doping Sn obtains titanium
Sour barium-barium stannate (BT-BS), obtains high-dielectric constant, the dielectric ceramic of existing fringing field high energy storage density.The composition of the present invention and technique
Step is simple, easily operated, reproducible, high yield rate.Obtain in x=0.105 through gradient experiment, i.e. 0.89BaTiO3-
0.105BaSnO3Place's capacitor energy storage density has peak, is 31mJ/cm under existing fringing field (10kV/cm)3, the parameter values
Considerably beyond other conventional capacitance energy storage materials.
Description of the drawings
Fig. 1 is the relation of the polarization intensity with electric field of the dielectric ceramic that embodiment 1 is obtained；
Fig. 2 is contrast of the different materials energy storage density of embodiment 2 under same electric field.
Specific embodiment
With reference to being described in further detail to the present invention：
A kind of existing fringing field, the dielectric ceramic of high-energy-density, the chemical formula of the dielectric ceramic is (1-x) BaTiO3-
xBaSnO3, x is molar percentage, wherein 0.03≤x≤0.15, preferred x=0.105.
A kind of existing fringing field, the preparation method of the dielectric ceramic of high-energy-density, comprise the following steps：
(1) chemical formula (1-x) BaTiO is pressed3-xBaSnO3The proportioning of middle each element weighs raw material BaCO3、TiO2And SnO2, its
In 0.03≤x≤0.15；
(2) will be put in ball grinder after the raw material for weighing mixing, add ball milling solvent dehydrated alcohol and agate ball, ball milling 4
Hour, rotational speed of ball-mill is 40-50 rev/min, then compound is put in baking oven 80 DEG C dries 3 hours, places in mortar and grinds,
Then 60 mesh sieves are crossed and obtains powder；
(3) powder that step (2) is obtained is put in crucible, is compacted, adds a cover；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) is obtained is ground to form fine powder in mortar, is loaded in ball grinder, add ball milling to be situated between
Matter dehydrated alcohol, carries out secondary ball milling, and rotating speed is 40-50 rev/min, continues 8 hours, and compound is put into 80 DEG C of drying in baking oven
Obtain within 3 hours drying powder；
(5) the drying powder that step (4) is obtained is ground in mortar, adds binder PVA, and PVA accounts for drying powder
The 5-10% of quality, mix homogeneously cross the pelletize powder for filtering out that particle diameter is 0.15mm to 0.28mm；
(6) the pelletize powder that step (5) is obtained is put in baking oven and 5-10 minutes is dried at a temperature of 80 DEG C, take powder and fall
Enter in the stainless steel mould of diameter 10mm, pressurize under 30MPa pressure is shaped to cylindrical blank in 90 seconds；
(7) the cylindrical blank that step (6) is obtained is put in Muffle furnace, temperature rises to 600 DEG C, is incubated 2 hours, discharged
PVA；
(8) sample after dumping in step (7) is put in crucible, material is buried with similar powder and bury burning, 1425～
Sinter in 1475 DEG C, be incubated 4 hours, room temperature naturally cooled to stove, obtain burned potsherd.
(9) conductive silver paste is coated after polish smooth obtained potsherd upper and lower surface, be warming up to 800 DEG C of guarantors in atmosphere
Temperature naturally cooled to room temperature after 20 minutes, obtained the dielectric ceramic of a kind of existing fringing field, high-energy-density.
The energy storage characteristic that the ceramic capacitor is measured using ferroelectricity work station (Radiant technology).By ceramic electrical
Container is placed in the fixture of ferroelectricity work station two-electrode system, UNICOM work station voltage source and capacitor upper/lower electrode.Entirely
Two-electrode system is immersed in methyl-silicone oil prevents air flashover.Using ferroelectricity work station control voltage source, in ceramic capacitor
Upper unipolar triangle voltage waveform E for applying 10Hz, a 10kV/cm.While applied voltage using work station survey
Quantity collection system measures polarization intensity P of capacitor, the relation curve for going out polarization intensity and electric field intensity by computer drawing
(ferroelectric hysteresis loop).According to the definition that capacitor stores energy, integration of the electric field intensity to polarization intensity is calculated by curve
It is multiplied by a constant again and can obtains capacitor energy storage density Ue.
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 larger energy density.This be due to ferroelectric ceramics at three critical points domain wall free energy minimization, 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 composition is modulated
Three Near The Critical Points, at that point the energy storage density of material can reach 31mJ/cm under existing fringing field (10kV/cm)3.Therefore can be with
By on energy-storage travelling wave tube of the materials application in the equipment that portable He wearable electronic equipment etc. requires low-voltage-grade.
The present invention is described in further detail with reference to embodiment：
Embodiment 1
(1) chemical formula (1-x) BaTiO is pressed3-xBaSnO3The proportioning of middle each element weighs raw material BaCO3、TiO2And SnO2, its
Middle x=0.03；
(2) will be put in ball grinder after the raw material for weighing mixing, add ball milling solvent dehydrated alcohol and agate ball, ball milling 4
Hour, rotational speed of ball-mill is 40 revs/min, then compound is put in baking oven 80 DEG C dries 3 hours, places in mortar and grinds, so
Cross 60 mesh sieves afterwards and obtain powder；
(3) powder that step (2) is obtained is put in crucible, is compacted, adds a cover；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) is obtained is ground to form fine powder in mortar, is loaded in ball grinder, add ball milling to be situated between
Matter dehydrated alcohol, carries out secondary ball milling, and rotating speed is 40 revs/min, continues 8 hours, compound is put into 80 DEG C of drying 3 in baking oven little
When obtain dry powder；
(5) the drying powder that step (4) is obtained is ground in mortar, adds binder PVA, and PVA accounts for drying powder
The 5% of quality, mix homogeneously cross the pelletize powder for filtering out that particle diameter is 0.15mm to 0.28mm；
(6) the pelletize powder that step (5) is obtained is put in baking oven and is dried 5 minutes at a temperature of 80 DEG C, taken powder and pour into
In the stainless steel mould of diameter 10mm, pressurize under 30MPa pressure is shaped to cylindrical blank in 90 seconds；
(7) the cylindrical blank that step (6) is obtained is put in Muffle furnace, temperature rises to 600 DEG C, is incubated 2 hours, discharged
PVA；
(8) sample after dumping in step (7) is put in crucible, material is buried with similar powder and bury burning, in 1425 DEG C
Sintering, is incubated 4 hours, naturally cools to room temperature with stove, obtain burned potsherd.
(9) conductive silver paste is coated after polish smooth obtained potsherd upper and lower surface, be warming up to 800 DEG C of guarantors in atmosphere
Temperature naturally cooled to room temperature after 20 minutes, obtained the dielectric ceramic of a kind of existing fringing field, high-energy-density.
Embodiment 2
(1) chemical formula (1-x) BaTiO is pressed3-xBaSnO3The proportioning of middle each element weighs raw material BaCO3、TiO2And SnO2, its
Middle x=0.09；
(2) will be put in ball grinder after the raw material for weighing mixing, add ball milling solvent dehydrated alcohol and agate ball, ball milling 4
Hour, rotational speed of ball-mill is 45 revs/min, then compound is put in baking oven 80 DEG C dries 3 hours, places in mortar and grinds, so
Cross 60 mesh sieves afterwards and obtain powder；
(3) powder that step (2) is obtained is put in crucible, is compacted, adds a cover；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) is obtained is ground to form fine powder in mortar, is loaded in ball grinder, add ball milling to be situated between
Matter dehydrated alcohol, carries out secondary ball milling, and rotating speed is 45 revs/min, continues 8 hours, compound is put into 80 DEG C of drying 3 in baking oven little
When obtain dry powder；
(5) the drying powder that step (4) is obtained is ground in mortar, adds binder PVA, and PVA accounts for drying powder
The 6% of quality, mix homogeneously cross the pelletize powder for filtering out that particle diameter is 0.15mm to 0.28mm；
(6) the pelletize powder that step (5) is obtained is put in baking oven and is dried 7 minutes at a temperature of 80 DEG C, taken powder and pour into
In the stainless steel mould of diameter 10mm, pressurize under 30MPa pressure is shaped to cylindrical blank in 90 seconds；
(7) the cylindrical blank that step (6) is obtained is put in Muffle furnace, temperature rises to 600 DEG C, is incubated 2 hours, discharged
PVA；
(8) sample after dumping in step (7) is put in crucible, material is buried with similar powder and bury burning, in 1450 DEG C
Sintering, is incubated 4 hours, naturally cools to room temperature with stove, obtain burned potsherd.
(9) conductive silver paste is coated after polish smooth obtained potsherd upper and lower surface, be warming up to 800 DEG C of guarantors in atmosphere
Temperature naturally cooled to room temperature after 20 minutes, obtained the dielectric ceramic of a kind of existing fringing field, high-energy-density.
Embodiment 3
(1) chemical formula (1-x) BaTiO is pressed3-xBaSnO3The proportioning of middle each element weighs raw material BaCO3、TiO2And SnO2, its
Middle x=0.1；
(2) will be put in ball grinder after the raw material for weighing mixing, add ball milling solvent dehydrated alcohol and agate ball, ball milling 4
Hour, rotational speed of ball-mill is 50 revs/min, then compound is put in baking oven 80 DEG C dries 3 hours, places in mortar and grinds, so
Cross 60 mesh sieves afterwards and obtain powder；
(3) powder that step (2) is obtained is put in crucible, is compacted, adds a cover；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) is obtained is ground to form fine powder in mortar, is loaded in ball grinder, add ball milling to be situated between
Matter dehydrated alcohol, carries out secondary ball milling, and rotating speed is 50 revs/min, continues 8 hours, compound is put into 80 DEG C of drying 3 in baking oven little
When obtain dry powder；
(5) the drying powder that step (4) is obtained is ground in mortar, adds binder PVA, and PVA accounts for drying powder
The 10% of quality, mix homogeneously cross the pelletize powder for filtering out that particle diameter is 0.15mm to 0.28mm；
(6) the pelletize powder that step (5) is obtained is put in baking oven and is dried 8 minutes at a temperature of 80 DEG C, taken powder and pour into
In the stainless steel mould of diameter 10mm, pressurize under 30MPa pressure is shaped to cylindrical blank in 90 seconds；
(7) the cylindrical blank that step (6) is obtained is put in Muffle furnace, temperature rises to 600 DEG C, is incubated 2 hours, discharged
PVA；
(8) sample after dumping in step (7) is put in crucible, material is buried with similar powder and bury burning, in 1475 DEG C
Sintering, is incubated 4 hours, naturally cools to room temperature with stove, obtain burned potsherd.
(9) conductive silver paste is coated after polish smooth obtained potsherd upper and lower surface, be warming up to 800 DEG C of guarantors in atmosphere
Temperature naturally cooled to room temperature after 20 minutes, obtained the dielectric ceramic of a kind of existing fringing field, high-energy-density.
Embodiment 4
(1) chemical formula (1-x) BaTiO is pressed3-xBaSnO3The proportioning of middle each element weighs raw material BaCO3、TiO2And SnO2, its
Middle x=0.105；
(2) will be put in ball grinder after the raw material for weighing mixing, add ball milling solvent dehydrated alcohol and agate ball, ball milling 4
Hour, rotational speed of ball-mill is 40 revs/min, then compound is put in baking oven 80 DEG C dries 3 hours, places in mortar and grinds, so
Cross 60 mesh sieves afterwards and obtain powder；
(3) powder that step (2) is obtained is put in crucible, is compacted, adds a cover；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) is obtained is ground to form fine powder in mortar, is loaded in ball grinder, add ball milling to be situated between
Matter dehydrated alcohol, carries out secondary ball milling, and rotating speed is 40 revs/min, continues 8 hours, compound is put into 80 DEG C of drying 3 in baking oven little
When obtain dry powder；
(5) the drying powder that step (4) is obtained is ground in mortar, adds binder PVA, and PVA accounts for drying powder
The 8% of quality, mix homogeneously cross the pelletize powder for filtering out that particle diameter is 0.15mm to 0.28mm；
(6) the pelletize powder that step (5) is obtained is put in baking oven and is dried 5 to 10 minutes at a temperature of 80 DEG C, take powder
Pour in the stainless steel mould of diameter 10mm, pressurize under 30MPa pressure is shaped to cylindrical blank in 90 seconds；
(7) the cylindrical blank that step (6) is obtained is put in Muffle furnace, temperature rises to 600 DEG C, is incubated 2 hours, discharged
PVA；
(8) sample after dumping in step (7) is put in crucible, material is buried with similar powder and bury burning, in 1465 DEG C
Sintering, is incubated 4 hours, naturally cools to room temperature with stove, obtain burned potsherd.
(9) conductive silver paste is coated after polish smooth obtained potsherd upper and lower surface, be warming up to 800 DEG C of guarantors in atmosphere
Temperature naturally cooled to room temperature after 20 minutes, obtained the dielectric ceramic of a kind of existing fringing field, high-energy-density.
Embodiment 5
(1) chemical formula (1-x) BaTiO is pressed3-xBaSnO3The proportioning of middle each element weighs raw material BaCO3、TiO2And SnO2, its
Middle x=0.12；
(2) will be put in ball grinder after the raw material for weighing mixing, add ball milling solvent dehydrated alcohol and agate ball, ball milling 4
Hour, rotational speed of ball-mill is 45 revs/min, then compound is put in baking oven 80 DEG C dries 3 hours, places in mortar and grinds, so
Cross 60 mesh sieves afterwards and obtain powder；
(3) powder that step (2) is obtained is put in crucible, is compacted, adds a cover；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) is obtained is ground to form fine powder in mortar, is loaded in ball grinder, add ball milling to be situated between
Matter dehydrated alcohol, carries out secondary ball milling, and rotating speed is 45 revs/min, continues 8 hours, compound is put into 80 DEG C of drying 3 in baking oven little
When obtain dry powder；
(5) the drying powder that step (4) is obtained is ground in mortar, adds binder PVA, and PVA accounts for drying powder
The 10% of quality, mix homogeneously cross the pelletize powder for filtering out that particle diameter is 0.15mm to 0.28mm；
(6) the pelletize powder that step (5) is obtained is put in baking oven and is dried 6 minutes at a temperature of 80 DEG C, taken powder and pour into
In the stainless steel mould of diameter 10mm, pressurize under 30MPa pressure is shaped to cylindrical blank in 90 seconds；
(7) the cylindrical blank that step (6) is obtained is put in Muffle furnace, temperature rises to 600 DEG C, is incubated 2 hours, discharged
PVA；
(8) sample after dumping in step (7) is put in crucible, material is buried with similar powder and bury burning, in 1445 DEG C
Sintering, is incubated 4 hours, naturally cools to room temperature with stove, obtain burned potsherd.
(9) conductive silver paste is coated after polish smooth obtained potsherd upper and lower surface, be warming up to 800 DEG C of guarantors in atmosphere
Temperature naturally cooled to room temperature after 20 minutes, obtained the dielectric ceramic of a kind of existing fringing field, high-energy-density.
Embodiment 6
(1) chemical formula (1-x) BaTiO is pressed3-xBaSnO3The proportioning of middle each element weighs raw material BaCO3、TiO2And SnO2, its
Middle x=0.15；
(2) will be put in ball grinder after the raw material for weighing mixing, add ball milling solvent dehydrated alcohol and agate ball, ball milling 4
Hour, rotational speed of ball-mill is 40 revs/min, then compound is put in baking oven 80 DEG C dries 3 hours, places in mortar and grinds, so
Cross 60 mesh sieves afterwards and obtain powder；
(3) powder that step (2) is obtained is put in crucible, is compacted, adds a cover；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) is obtained is ground to form fine powder in mortar, is loaded in ball grinder, add ball milling to be situated between
Matter dehydrated alcohol, carries out secondary ball milling, and rotating speed is 50 revs/min, continues 8 hours, compound is put into 80 DEG C of drying 3 in baking oven little
When obtain dry powder；
(5) the drying powder that step (4) is obtained is ground in mortar, adds binder PVA, and PVA accounts for drying powder
The 5% of quality, mix homogeneously cross the pelletize powder for filtering out that particle diameter is 0.15mm to 0.28mm；
(6) the pelletize powder that step (5) is obtained is put in baking oven and is dried 5 minutes at a temperature of 80 DEG C, taken powder and pour into
In the stainless steel mould of diameter 10mm, pressurize under 30MPa pressure is shaped to cylindrical blank in 90 seconds；
(7) the cylindrical blank that step (6) is obtained is put in Muffle furnace, temperature rises to 600 DEG C, is incubated 2 hours, discharged
PVA；
(8) sample after dumping in step (7) is put in crucible, material is buried with similar powder and bury burning, in 1450 DEG C
Sintering, is incubated 4 hours, naturally cools to room temperature with stove, obtain burned potsherd.
(9) conductive silver paste is coated after polish smooth obtained potsherd upper and lower surface, be warming up to 800 DEG C of guarantors in atmosphere
Temperature naturally cooled to room temperature after 20 minutes, obtained the dielectric ceramic of a kind of existing fringing field, high-energy-density.
From the embodiment of the present invention 2 and dielectric ceramic 0.91BaTiO obtained in embodiment 43-0.09BaSnO3With
0.895BaTiO3-0.105BaSnO3, and capacitance energy storage material is contrasted for lead zirconate titanate (PZT), PMN-PT
(PMNPT) above-mentioned various materials are made metal-insulator-gold and Kynoar-CTFE (P (VDF-CTFE)),
Category structure capacitance, measures the energy storage characteristic of each capacitor using ferroelectricity work station (Radiant technology) and carries out
Contrast.Respectively each capacitor is placed in the fixture of ferroelectricity work station two-electrode system, work station voltage source is connected with electricity
Container upper/lower electrode.Whole two-electrode system is immersed in methyl-silicone oil and prevents air flashover.Using ferroelectricity work stand control electricity
Potential source, applies unipolar triangle voltage waveform E of 10Hz, a 10kV/cm on ceramic capacitor.Applied voltage same
When using work station measurement acquisition system measure capacitor polarization intensity P, by computer drawing go out polarization intensity with electricity
The relation curve of field intensity, as shown in figure 1, the dielectric ceramic that the present invention is obtained is at room temperature, phase under existing fringing field (10kV/cm)
Than there are highest polarization intensity (10 μ C/cm in other conventional energy storage materials2), while with minimum loss.
From the embodiment of the present invention 2, embodiment 3, embodiment 4 and dielectric ceramic 0.91BaTiO obtained in embodiment 53-
0.09BaSnO3、0.9BaTiO3-0.1BaSnO3、0.895BaTiO3-0.105BaSnO3And 0.88BaTiO3-
0.12BaSnO3, be PZT, PMNPT and P (VDF-CTFE) from contrast energy storage material, each material sample above-mentioned is calculated in room
Under temperature, the data obtained is depicted as block diagram, as shown in Fig. 2 can see by energy density under the electric field of 10Hz, 10kV/cm
Go out, dielectric ceramic prepared by the present invention has relative highest energy storage (31mJ/cm3), it is the twice of other conventional energy storage materials
More than.
Claims (9)
1. the dielectric ceramic of a kind of existing fringing field, high-energy-density, it is characterised in that the chemical formula of the dielectric ceramic is (1-x)
BaTiO3-xBaSnO3, wherein 0.03≤x≤0.15, x is mole percent.
2. a kind of existing fringing field according to claim 1, the dielectric ceramic of high-energy-density, it is characterised in that dielectric pottery
The chemical formula of porcelain is (1-x) BaTiO3-xBaSnO3, wherein x=0.105, x are mole percent.
3. a kind of existing fringing field, the preparation method of the dielectric ceramic of high-energy-density, it is characterised in that comprise the following steps：
(1) chemical formula (1-x) BaTiO is pressed3-xBaSnO3The proportioning of middle each element weighs raw material BaCO3、TiO2And SnO2, wherein
0.03≤x≤0.15, x are mole percent；
(2) ball milling, drying and grinding will be carried out successively after the raw material for weighing mixing, then crosses 60 mesh sieves and obtain powder；
(3) by powder pre-burning in atmosphere, room temperature is naturally cooled to, preburning powdered material is obtained；
(4) secondary ball milling is carried out after grind preburning powdered material, obtain dry powder after drying；
(5) binding agent mix homogeneously is added after grind dry powder, then filters out particle diameter for 0.15mm's to 0.28mm
Pelletize powder；
(6) pressing mold molding after the drying of pelletize powder is obtained cylindrical blank；
(7) binding agent of cylindrical blank is discharged, then at 1425～1475 DEG C, sinters 3-5 hours, obtain burned pottery
Ceramics；
(8) coat conductive silver paste after polish smooth burned potsherd upper and lower surface, then carry out burn Electrode treatment obtain low
Electric field, the dielectric ceramic of high-energy-density.
4. a kind of existing fringing field according to claim 3, the preparation method of the dielectric ceramic of high-energy-density, its feature exist
In in step (2), Ball-milling Time is 4 hours, and rotating speed is 40-50 rev/min, and drying temperature is 80 DEG C, and the time is 3 hours；Step
(4) in, the secondary ball milling time is 8 hours, and rotating speed is 40-50 rev/min, and drying temperature is 80 DEG C, and the time is 3 hours.
5. a kind of existing fringing field according to claim 3, the preparation method of the dielectric ceramic of high-energy-density, its feature exist
In in step (3), calcined temperature is 1350 DEG C, is incubated 4 hours.
6. a kind of existing fringing field according to claim 3, the preparation method of the dielectric ceramic of high-energy-density, its feature exist
In in step (5), binding agent is PVA, and addition is the 5-10% for drying powder quality.
7. a kind of existing fringing field according to claim 3, the preparation method of the dielectric ceramic of high-energy-density, its feature exist
In in step (6), drying temperature is 80 DEG C, and drying time is 5-10 minutes；Pressing mold molding is specially：Pelletizing after by drying
Material is poured in the stainless steel mould of a diameter of 10mm, and pressurize under 30MPa pressure is shaped to cylindrical blank in 90 seconds.
8. a kind of existing fringing field according to claim 3, the preparation method of the dielectric ceramic of high-energy-density, its feature exist
In cylindrical blank is incubated 2 hours discharging binding agent in 600 DEG C in step (7).
9. a kind of existing fringing field according to claim 3, the preparation method of the dielectric ceramic of high-energy-density, its feature exist
In in step (8), burning Electrode treatment is specially：It is warming up to 800 DEG C after coating conductive silver paste in atmosphere and is incubated 20 minutes, so
After naturally cool to room temperature.
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| CN107500753A (en) * | 2017-09-06 | 2017-12-22 | 天津大学 | A kind of low-loss titanium barium stannate dielectric material |
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| CN108610040A (en) * | 2018-04-27 | 2018-10-02 | 天津大学 | A method of reducing titanium barium stannate system dielectric loss under reducing atmosphere |
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| CN107162583A (en) * | 2017-07-05 | 2017-09-15 | 西安交通大学 | The method that barium titanate based ceramic dielectric-temperature stability is improved based on component gradient |
| CN107162583B (en) * | 2017-07-05 | 2020-05-22 | 西安交通大学 | Method for improving dielectric temperature stability of barium titanate-based ceramic based on component gradient |
| CN107382308A (en) * | 2017-07-17 | 2017-11-24 | 天津大学 | A kind of anti-reduced form dielectric material of high-k |
| CN107500753A (en) * | 2017-09-06 | 2017-12-22 | 天津大学 | A kind of low-loss titanium barium stannate dielectric material |
| CN108610041A (en) * | 2018-04-27 | 2018-10-02 | 天津大学 | A method of improving titanium barium stannate dielectric properties under reducing atmosphere |
| CN108610040A (en) * | 2018-04-27 | 2018-10-02 | 天津大学 | A method of reducing titanium barium stannate system dielectric loss under reducing atmosphere |
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| CN116082032A (en) * | 2022-04-26 | 2023-05-09 | 西安交通大学 | Electric card refrigeration ceramic and preparation method thereof |
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