CN106542821A - A kind of Bi2O3‑B2O3ZnO glass adds Ba0.4Sr0.6TiO3Base energy storage ceramic and preparation method thereof - Google Patents
A kind of Bi2O3‑B2O3ZnO glass adds Ba0.4Sr0.6TiO3Base energy storage ceramic and preparation method thereof Download PDFInfo
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- 239000011521 glass Substances 0.000 title claims abstract description 51
- 239000000919 ceramic Substances 0.000 title claims abstract description 48
- 238000004146 energy storage Methods 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 229910010252 TiO3 Inorganic materials 0.000 claims abstract description 75
- 238000001035 drying Methods 0.000 claims abstract description 26
- 238000009413 insulation Methods 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 17
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 17
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 17
- 238000000498 ball milling Methods 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 229910000018 strontium carbonate Inorganic materials 0.000 claims abstract description 10
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 claims abstract description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims description 38
- 239000000203 mixture Substances 0.000 claims description 33
- 238000010792 warming Methods 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 21
- 238000000137 annealing Methods 0.000 claims description 18
- 238000005469 granulation Methods 0.000 claims description 18
- 230000003179 granulation Effects 0.000 claims description 18
- 238000005520 cutting process Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000005498 polishing Methods 0.000 claims description 8
- 229910052709 silver Inorganic materials 0.000 claims description 8
- 239000004332 silver Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 6
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 4
- 239000000428 dust Substances 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 claims description 2
- 230000001070 adhesive effect Effects 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 239000002003 electrode paste Substances 0.000 claims 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 239000002002 slurry Substances 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 18
- 238000009825 accumulation Methods 0.000 description 15
- 239000012071 phase Substances 0.000 description 14
- 239000003989 dielectric material Substances 0.000 description 8
- 229910010293 ceramic material Inorganic materials 0.000 description 7
- 239000011267 electrode slurry Substances 0.000 description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- 238000003723 Smelting Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000002131 composite material Substances 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- 229910052593 corundum Inorganic materials 0.000 description 6
- 239000010431 corundum Substances 0.000 description 6
- 239000000156 glass melt Substances 0.000 description 6
- 239000004570 mortar (masonry) Substances 0.000 description 6
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 6
- 238000005491 wire drawing Methods 0.000 description 6
- 229910001928 zirconium oxide Inorganic materials 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 229910002370 SrTiO3 Inorganic materials 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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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
- C04B35/01—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
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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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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Abstract
The invention discloses a kind of Bi2O3‑B2O3ZnO glass adds Ba0.4Sr0.6TiO3Base energy storage ceramic and preparation method thereof, including main component SrCO3、TiO2And BaCO3, auxiliary element Bi2O3‑B2O3ZnO glass.Its preparation method is：By SrCO3、TiO2And BaCO3Weigh according to certain stoichiometric proportion for raw material, ball milling, discharge post-drying, and at 1150 DEG C, pre-burning 2h, obtains Ba0.4Sr0.6TiO3Powder body.According to (100 x) wt%Ba0.4Sr0.6TiO3+ xwt%Bi2O3‑B2O3ZnO quality proportionings mixs with zirconium ballstone and deionized water after weighing, carry out successively ball milling, drying, pelletize, sieve after be pressed into sample, sinter within 2 hours in 1250～1350 DEG C of insulations in atmosphere and make, furnace cooling, last electrode coated slurry.Unleaded dielectric substance prepared by the inventive method meets topmost three features in terms of energy storage ceramic dielectric properties：High dielectric constant, low dielectric loss, high disruptive field intensity and big energy storage density, preparation process is simple are inexpensive, environmental protection.
Description
Technical field
The present invention relates to ceramic dielectric material field, and in particular to a kind of Bi2O3-B2O3- ZnO glass adds
Ba0.4Sr0.6TiO3Base energy storage ceramic and preparation method thereof.
Background technology
In recent years, with the rise of new technology revolution, economic fast development, its demand to the energy are also continuously increased.Newly
The exploitation of the energy, become the effective way for solving current energy crisis.Research and development new forms of energy so as to replace traditional energy
Source, reduces the pollution to environment, it is to avoid the exhaustion of traditional energy, is the final energy demand prediction for meeting human social development.New
In the exploitation of the energy, need for unidirectional current to be changed into the use of alternating current supply load, this is completed using contravariant equipment generally
One transformation, and condenser ceramics is the of paramount importance element of energy conversion in contravariant equipment.Under electric field action, condenser ceramics
(media ceramic) can produce polarization, can store and discharge electric charge, what capacitor was exactly fabricated by using this characteristic.
Ba1-xSrxTiO3Ceramics combine BaTiO3Ceramics and SrTiO3The premium properties of ceramics, becomes energy-storing dielectric ceramic
The study hotspot in field.However, Ba1-xSrxTiO3The crystal grain and crystal boundary of abnormal growth, space, impurity etc. are there is in ceramics no
Uniform microstructure, while Ba1-xSrxTiO3The dielectric loss and electrostriction effect of ceramics, can cause material to be made in electric field
Occurs micro-crack with, the factor such as uneven microstructure and micro-crack makes Ba1-xSrxTiO3Ceramics will under compared with existing fringing field
It is breakdown.How to improve the micro-property of ceramics, reduce dielectric loss, improve disruptive field intensity, so as to the energy storage for improving ceramics is close
Degree, becomes the focus of Recent study.
The content of the invention
It is an object of the invention to provide a kind of Bi2O3-B2O3- ZnO glass adds Ba0.4Sr0.6TiO3Base energy storage ceramic and
Its preparation method, with the defect for overcoming above-mentioned prior art to exist, by accumulation energy type ceramic dielectric obtained in the inventive method
Material, not only preparation process is simple, the cost of material is low, and with higher dielectric constant, low dielectric loss, high puncture
Voltage and high energy storage density, it is possible to become replacement Ba0.4Sr0.6TiO3The unleaded accumulation energy type ceramic material of base is in technology and economy
Upper and excellent important candidate material.
To reach above-mentioned purpose, the present invention is adopted the following technical scheme that：
A kind of Bi2O3-B2O3- ZnO glass adds Ba0.4Sr0.6TiO3Base energy storage ceramic, formula are (100-x)
Ba0.4Sr0.6TiO3+x Bi2O3-B2O3- ZnO, wherein x=1～9wt%, x are mass percent.
Further, x=1wt%, 3wt%, 5wt%, 7wt% or 9wt%.
A kind of Bi2O3-B2O3- ZnO glass adds Ba0.4Sr0.6TiO3The preparation method of base energy storage ceramic, including following step
Suddenly：
Step one：According to mol ratio 0.6:1:0.4 weighs SrCO3、TiO2And BaCO3It is mixed to form mixture A；Will mixing
Thing A carries out ball milling, drying, after briquetting, is incubated 1.5～2 hours in 1120～1150 DEG C, forms the Ba of pure phase0.4Sr0.6TiO3Powder
Body, it is standby；
Step 2：According to Bi2O3：B2O3：ZnO=6:3:1 mol ratio weighs raw material, adds after being fully ground stirring and evenly mixing
Heat, is incubated 1.5～2h and obtains high-temperature fusant after being warming up to 1200～1300 DEG C, then by high-temperature fusant first one-step forming, treat preliminary
Made annealing treatment after molding, cut after annealing, the sample of well cutting is carried out into Crystallizing treatment, Bi after cooling, is obtained2O3-
B2O3- ZnO glass dust；
Step 3：By the Ba for obtaining0.4Sr0.6TiO3Powder body and Bi2O3-B2O3- ZnO glass dust is according to (100-x)
Ba0.4Sr0.6TiO3+xBi2O3-B2O3- ZnO is mixed to get mixture B, take after mixture B is mixed with zirconium ballstone and deionized water according to
It is secondary to carry out ball milling, drying, pelletize, sieve, granulation material is formed, wherein x=1～9wt%, x are mass percent；
Step 4：Granulation material obtained by step 3 is made into sample under the pressure of 110～120MPa, then with 2 DEG C/min
500 DEG C of insulation 60min are warming up to, and are incubated 2～3 hours, afterwards, with 5 DEG C/min when 1250～1350 DEG C are warming up to 5 DEG C/min
After being cooled to 500 DEG C, room temperature is cooled to the furnace；
Step 5：After the sample that polishing, cleaning step four are sintered, silver electrode slurry is uniformly coated in sample tow sides
Material, sinters 20～30 minutes in 600 DEG C, obtains Bi2O3-B2O3- ZnO glass adds Ba0.4Sr0.6TiO3Base energy storage ceramic.
Further, in step 2, annealing is specially：Anneal in 500 DEG C of annealing furnace is warming up in advance 2h；Move back
The size of 10.0mm × 10.0mm × 2.0mm is cut to after fire.
Further, in step 2, Crystallizing treatment is specially：The sample of well cutting is placed on stove heat in Muffle furnace,
4h is incubated after 700 DEG C～750 are risen to the heating rate of 10 DEG C/min.
Further, step one, Ball-milling Time is 4～6 hours in three.
Further, take in step 3 carried out after mixture B is mixed with zirconium ballstone and deionized water successively ball milling, drying after
Drying material is obtained, binding agent is added into drying material carries out pelletize, binding agent accounts for 8～10%, Ran Houfen of drying material quality
Do not cross 40 mesh and 80 mesh sieves take middle material and obtain granulation material.
Further, described adhesive is polyvinyl alcohol water solution.
Further, the mass concentration of binding agent is 4～6%.
Compared with prior art, the present invention has following beneficial technique effect：
The present invention is prepared using conventional solid-state method, technical maturity, is adapted to industrialization production, is employed Bi in addition2O3-B2O3-
ZnO glass, is acted on using the liquid-phase sintering of glass phase, improves Ba0.4Sr0.6TiO3The microstructure of ceramics and dielectric properties, this
Unleaded accumulation energy type ceramic dielectric material not only preparation process is simple prepared by inventive method, the cost of material is low, and with compared with
High dielectric constant, low dielectric loss, high breakdown voltage and high energy storage density, it is intended to improve Ba0.4Sr0.6TiO3Ceramics
Microstructure and improve its energy storage density.
Description of the drawings
Fig. 1 is comparative example and embodiment 1-5Ba0.4Sr0.6TiO3Ceramics sample and Bi2O3-B2O3The XRD figure of-ZnO glass,
Wherein (a) is Ba0.4Sr0.6TiO3The XRD figure of ceramics sample；B () is Bi2O3-B2O3The XRD figure of-ZnO glass；
Fig. 2 is comparative example and embodiment 1-5 addition Bi2O3-B2O3The Ba of-ZnO glass0.4Sr0.6TiO3The SEM of ceramics sample
Figure：(a) x=0；(b) x=1；(c) x=3；(d) x=5；(e) x=7；(f) x=9；
Fig. 3 is comparative example and embodiment 1-5 addition Bi2O3-B2O3The Ba of-ZnO glass0.4Sr0.6TiO3Jie of ceramics sample
The characteristic curve that electric constant and dielectric loss change with frequency；
Fig. 4 is comparative example and embodiment 1-5 addition Bi2O3-B2O3The Ba of-ZnO glass0.4Sr0.6TiO3The prestige of ceramics sample
Boolean's scattergram；
Fig. 5 is comparative example and embodiment 1-5 addition Bi2O3-B2O3The Ba of-ZnO glass0.4Sr0.6TiO3The electricity of ceramics sample
Hysteresis curves and dielectric constant, average disruptive field intensity and energy storage density with the variation diagram of glass addition, wherein (a) is electric hysteresis
Loop line；B () is dielectric constant, average disruptive field intensity and energy storage density with the variation diagram of glass addition.
Specific embodiment
Below in conjunction with the accompanying drawings and embodiment is described in further detail to the present invention：
Comparative example
Ba of the present invention0.4Sr0.6TiO3The unleaded accumulation energy type ceramic dielectric material of base, its formula are (100-x) wt%
Ba0.4Sr0.6TiO3+ xwt%Bi2O3-B2O3- ZnO, wherein x=0.
Step one：Prepare Ba0.4Sr0.6TiO3Powder is standby.According to mol ratio 0.6:1:0.4 weighs SrCO3、TiO2And BaCO3
It is mixed to form mixture.
Step 2：Mixture and zirconium ballstone and deionized water are taken, is 1 according to mass ratio:1:Ball is carried out successively after 1 mixing
Mill, drying, after briquetting, be placed in batch-type furnace and 2 hours be incubated in 1150 DEG C, form the Ba of pure phase0.4Sr0.6TiO3Powder body, it is standby；
Step 3：By glass composite according to 60Bi2O3-30B2O3The mol ratio of -10ZnO (mol%) weighs raw material, in
Pour into after stirring and evenly mixing is fully ground in mortar in corundum crucible, be placed in high temperature resistance furnace and heat.According to the intensification speed of setting
Rate is warming up to 1300 DEG C, insulation 2h after, by wire drawing judge glass melt whether found well, without it was observed that bubble and
Calculus, and high-temperature fusant has good ductility, shows that glass smelting is complete.Crucible can be taken out rapidly now and by high temperature melting
Body is quickly poured on pre-heated copper coin.After vitreous humour just one-step forming, it is quickly placed to be warming up to 500 DEG C of annealing in advance
The process of annealing 2h is carried out in stove, it is therefore intended that eliminate the residual stress in glass.Sample is taken out after furnace cooling, cut
Process is cut, after sample is cut to the size of 10.0mm × 10.0mm × 2.0mm, prepares follow-up Crystallizing treatment.By the sample of well cutting
Product place Muffle furnace in stove heat, rise to 700 DEG C with the heating rate of 10 DEG C/min, insulation 4h carry out Crystallizing treatment, treat with
After stove cooling, that is, complete the preparation of sample.
Step 4：With pure phase Ba0.4Sr0.6TiO3, 0wt%Bi2O3-B2O3- ZnO, forms mixture, according to quality after mixing
Percentage composition weighs to form full dispensing, standby；
Step 5：Full dispensing and zirconium ballstone and deionized water that step 4 is obtained are taken respectively, are 1 according to mass ratio:1:1 mixes
Carry out ball milling, drying after conjunction successively, pelletize, sieve, form granulation material；
Step 6：Granulation material obtained by step 5 is made into sample under the pressure of 120MPa, then, is placed in and with zirconium oxide is
In the aluminium oxide saggar of backing plate in high temperature box furnace, 500 DEG C of insulation 60min are warming up to 2 DEG C/min, are heated up with 5 DEG C/min
2 hours are incubated to when 1350 DEG C, afterwards, are cooled to after 500 DEG C with 5 DEG C/min, are cooled to room temperature with the furnace；
Step 7：After the sample that polishing, cleaning step five are sintered, silver electrode slurry is uniformly coated in sample tow sides
Material, sinters 20 minutes in 600 DEG C, obtains Ba0.4Sr0.6TiO3The unleaded accumulation energy type ceramic material sample of base.
Embodiment 1
Ba of the present invention0.4Sr0.6TiO3The unleaded accumulation energy type ceramic dielectric material of base, its formula are (100-x) wt%
Ba0.4Sr0.6TiO3+ xwt%Bi2O3-B2O3- ZnO, wherein x=1.
Step one：Prepare Ba0.4Sr0.6TiO3Powder is standby.According to mol ratio 0.6:1:0.4 weighs SrCO3、TiO2And BaCO3
It is mixed to form mixture.
Step 2：Mixture and zirconium ballstone and deionized water are taken, is 1 according to mass ratio:1:Ball is carried out successively after 1 mixing
Mill, drying, after briquetting, be placed in batch-type furnace and 2 hours be incubated in 1120 DEG C, form the Ba of pure phase0.4Sr0.6TiO3Powder body, it is standby；
Step 3：By glass composite according to 60Bi2O3-30B2O3The mol ratio of -10ZnO (mol%) weighs raw material, in
Pour into after stirring and evenly mixing is fully ground in mortar in corundum crucible, be placed in high temperature resistance furnace and heat.According to the intensification speed of setting
Rate is warming up to 1200 DEG C, after insulation 1.5h, judges whether glass melt is founded well by wire drawing, without it was observed that bubble
And calculus, and high-temperature fusant has good ductility, shows that glass smelting is complete.Crucible can be taken out rapidly now and by high temperature
Melt is quickly poured on pre-heated copper coin.After vitreous humour just one-step forming, it is quickly placed to be warming up in advance 500 DEG C and moves back
The process of annealing 2h is carried out in stove, it is therefore intended that eliminate the residual stress in glass.Sample is taken out after furnace cooling, carried out
Cutting process, prepares follow-up Crystallizing treatment after sample is cut to the size of 10.0mm × 10.0mm × 2.0mm.By well cutting
With stove heat in sample placement Muffle furnace, 700 DEG C are risen to the heating rate of 10 DEG C/min, insulation 4h carries out Crystallizing treatment, treats
After furnace cooling, that is, complete the preparation of sample.
Step 4：With pure phase 99wt%Ba0.4Sr0.6TiO3, 1wt%Bi2O3-B2O3- ZnO, forms mixture, presses after mixing
Weigh to form full dispensing according to weight/mass percentage composition, it is standby；
Step 5：Full dispensing and zirconium ballstone and deionized water that step 4 is obtained are taken respectively, are 1 according to mass ratio:1:1 mixes
Carry out ball milling, drying after conjunction successively, pelletize, sieve, form granulation material；
Step 6：Granulation material obtained by step 5 is made into sample under the pressure of 120MPa, then, is placed in and with zirconium oxide is
In the aluminium oxide saggar of backing plate in high temperature box furnace, 500 DEG C of insulation 60min are warming up to 2 DEG C/min, are heated up with 5 DEG C/min
2 hours are incubated to when 1250 DEG C, afterwards, are cooled to after 500 DEG C with 5 DEG C/min, are cooled to room temperature with the furnace；
Step 7：After the sample that polishing, cleaning step five are sintered, silver electrode slurry is uniformly coated in sample tow sides
Material, sinters 20 minutes in 600 DEG C, obtains Ba0.4Sr0.6TiO3The unleaded accumulation energy type ceramic material sample of base.
Embodiment 2
Ba of the present invention0.4Sr0.6TiO3The unleaded accumulation energy type ceramic dielectric material of base, its formula are (100-x) wt%
Ba0.4Sr0.6TiO3+ xwt%Bi2O3-B2O3- ZnO, wherein x=3.
Step one：Prepare Ba0.4Sr0.6TiO3Powder is standby.According to mol ratio 0.6:1:0.4 weighs SrCO3、TiO2And BaCO3
It is mixed to form mixture.
Step 2：Mixture and zirconium ballstone and deionized water are taken, is 1 according to mass ratio:1:Ball is carried out successively after 1 mixing
Mill, drying, after briquetting, be placed in batch-type furnace and 1.5 hours be incubated in 1150 DEG C, form the Ba of pure phase0.4Sr0.6TiO3Powder body, it is standby
With；
Step 3：By glass composite according to 60Bi2O3-30B2O3The mol ratio of -10ZnO (mol%) weighs raw material, in
Pour into after stirring and evenly mixing is fully ground in mortar in corundum crucible, be placed in high temperature resistance furnace and heat.According to the intensification speed of setting
Rate is warming up to 1250 DEG C, insulation 2h after, by wire drawing judge glass melt whether found well, without it was observed that bubble and
Calculus, and high-temperature fusant has good ductility, shows that glass smelting is complete.Crucible can be taken out rapidly now and by high temperature melting
Body is quickly poured on pre-heated copper coin.After vitreous humour just one-step forming, it is quickly placed to be warming up to 500 DEG C of annealing in advance
The process of annealing 2h is carried out in stove, it is therefore intended that eliminate the residual stress in glass.Sample is taken out after furnace cooling, cut
Process is cut, after sample is cut to the size of 10.0mm × 10.0mm × 2.0mm, prepares follow-up Crystallizing treatment.By the sample of well cutting
Product place Muffle furnace in stove heat, rise to 750 DEG C with the heating rate of 10 DEG C/min, insulation 4h carry out Crystallizing treatment, treat with
After stove cooling, that is, complete the preparation of sample.
Step 4：With pure phase 97wt%Ba0.4Sr0.6TiO3, 3wt%Bi2O3-B2O3- ZnO, forms mixture, presses after mixing
Weigh to form full dispensing according to weight/mass percentage composition, it is standby；
Step 5：Full dispensing and zirconium ballstone and deionized water that step 4 is obtained are taken respectively, are 1 according to mass ratio:1:1 mixes
Carry out ball milling, drying after conjunction successively, pelletize, sieve, form granulation material；
Step 6：Granulation material obtained by step 5 is made into sample under the pressure of 110MPa, then, is placed in and with zirconium oxide is
In the aluminium oxide saggar of backing plate in high temperature box furnace, 500 DEG C of insulation 60min are warming up to 2 DEG C/min, are heated up with 5 DEG C/min
3 hours are incubated to when 1280 DEG C, afterwards, are cooled to after 500 DEG C with 5 DEG C/min, are cooled to room temperature with the furnace；
Step 7：After the sample that polishing, cleaning step five are sintered, silver electrode slurry is uniformly coated in sample tow sides
Material, sinters 20 minutes in 600 DEG C, obtains Ba0.4Sr0.6TiO3The unleaded accumulation energy type ceramic material sample of base.
Embodiment 3
Ba of the present invention0.4Sr0.6TiO3The unleaded accumulation energy type ceramic dielectric material of base, its formula are (100-x) wt%
Ba0.4Sr0.6TiO3+ xwt%Bi2O3-B2O3- ZnO, wherein x=5.
Step one：Prepare Ba0.4Sr0.6TiO3Powder is standby.According to mol ratio 0.6:1:0.4 weighs SrCO3、TiO2And BaCO3
It is mixed to form mixture.
Step 2：Mixture and zirconium ballstone and deionized water are taken, is 1 according to mass ratio:1:Ball is carried out successively after 1 mixing
Mill, drying, after briquetting, be placed in batch-type furnace and 2 hours be incubated in 1150 DEG C, form the Ba of pure phase0.4Sr0.6TiO3Powder body, it is standby；
Step 3：By glass composite according to 60Bi2O3-30B2O3The mol ratio of -10ZnO (mol%) weighs raw material, in
Pour into after stirring and evenly mixing is fully ground in mortar in corundum crucible, be placed in high temperature resistance furnace and heat.According to the intensification speed of setting
Rate is warming up to 1260 DEG C, after insulation 1.5h, judges whether glass melt is founded well by wire drawing, without it was observed that bubble
And calculus, and high-temperature fusant has good ductility, shows that glass smelting is complete.Crucible can be taken out rapidly now and by high temperature
Melt is quickly poured on pre-heated copper coin.After vitreous humour just one-step forming, it is quickly placed to be warming up in advance 500 DEG C and moves back
The process of annealing 2h is carried out in stove, it is therefore intended that eliminate the residual stress in glass.Sample is taken out after furnace cooling, carried out
Cutting process, prepares follow-up Crystallizing treatment after sample is cut to the size of 10.0mm × 10.0mm × 2.0mm.By well cutting
With stove heat in sample placement Muffle furnace, 700 DEG C are risen to the heating rate of 10 DEG C/min, insulation 4h carries out Crystallizing treatment, treats
After furnace cooling, that is, complete the preparation of sample.
Step 4：With pure phase 95wt%Ba0.4Sr0.6TiO3, 5wt%Bi2O3-B2O3- ZnO, forms mixture, presses after mixing
Weigh to form full dispensing according to weight/mass percentage composition, it is standby；
Step 5：Full dispensing and zirconium ballstone and deionized water that step 4 is obtained are taken respectively, are 1 according to mass ratio:1:1 mixes
Carry out ball milling, drying after conjunction successively, pelletize, sieve, form granulation material；
Step 6：Granulation material obtained by step 5 is made into sample under the pressure of 120MPa, then, is placed in and with zirconium oxide is
In the aluminium oxide saggar of backing plate in high temperature box furnace, 500 DEG C of insulation 60min are warming up to 2 DEG C/min, are heated up with 5 DEG C/min
2 hours are incubated to when 1290 DEG C, afterwards, are cooled to after 500 DEG C with 5 DEG C/min, are cooled to room temperature with the furnace；
Step 7：After the sample that polishing, cleaning step five are sintered, silver electrode slurry is uniformly coated in sample tow sides
Material, sinters 30 minutes in 600 DEG C, obtains Ba0.4Sr0.6TiO3The unleaded accumulation energy type ceramic material sample of base.
Embodiment 4
Ba of the present invention0.4Sr0.6TiO3The unleaded accumulation energy type ceramic dielectric material of base, its formula are (100-x) wt%
Ba0.4Sr0.6TiO3+ xwt%Bi2O3-B2O3- ZnO, wherein x=7.
Step one：Prepare Ba0.4Sr0.6TiO3Powder is standby.According to mol ratio 0.6:1:0.4 weighs SrCO3、TiO2And BaCO3
It is mixed to form mixture.
Step 2：Mixture and zirconium ballstone and deionized water are taken, is 1 according to mass ratio:1:Ball is carried out successively after 1 mixing
Mill, drying, after briquetting, be placed in batch-type furnace and 1.5 hours be incubated in 1150 DEG C, form the Ba of pure phase0.4Sr0.6TiO3Powder body, it is standby
With；
Step 3：By glass composite according to 60Bi2O3-30B2O3The mol ratio of -10ZnO (mol%) weighs raw material, in
Pour into after stirring and evenly mixing is fully ground in mortar in corundum crucible, be placed in high temperature resistance furnace and heat.According to the intensification speed of setting
Rate is warming up to 1280 DEG C, insulation 2h after, by wire drawing judge glass melt whether found well, without it was observed that bubble and
Calculus, and high-temperature fusant has good ductility, shows that glass smelting is complete.Crucible can be taken out rapidly now and by high temperature melting
Body is quickly poured on pre-heated copper coin.After vitreous humour just one-step forming, it is quickly placed to be warming up to 500 DEG C of annealing in advance
The process of annealing 2h is carried out in stove, it is therefore intended that eliminate the residual stress in glass.Sample is taken out after furnace cooling, cut
Process is cut, after sample is cut to the size of 10.0mm × 10.0mm × 2.0mm, prepares follow-up Crystallizing treatment.By the sample of well cutting
Product place Muffle furnace in stove heat, rise to 750 DEG C with the heating rate of 10 DEG C/min, insulation 4h carry out Crystallizing treatment, treat with
After stove cooling, that is, complete the preparation of sample.
Step 4：With pure phase 93wt%Ba0.4Sr0.6TiO3, 7wt%Bi2O3-B2O3- ZnO, forms mixture, presses after mixing
Weigh to form full dispensing according to weight/mass percentage composition, it is standby；
Step 5：Full dispensing and zirconium ballstone and deionized water that step 4 is obtained are taken respectively, are 1 according to mass ratio:1:1 mixes
Carry out ball milling, drying after conjunction successively, pelletize, sieve, form granulation material；
Step 6：Granulation material obtained by step 5 is made into sample under the pressure of 110MPa, then, is placed in and with zirconium oxide is
In the aluminium oxide saggar of backing plate in high temperature box furnace, 500 DEG C of insulation 60min are warming up to 2 DEG C/min, are heated up with 5 DEG C/min
2.5 hours are incubated to when 1300 DEG C, afterwards, are cooled to after 500 DEG C with 5 DEG C/min, are cooled to room temperature with the furnace；
Step 7：After the sample that polishing, cleaning step five are sintered, silver electrode slurry is uniformly coated in sample tow sides
Material, sinters 20 minutes in 600 DEG C, obtains Ba0.4Sr0.6TiO3The unleaded accumulation energy type ceramic material sample of base.
Embodiment 5
Ba of the present invention0.4Sr0.6TiO3The unleaded accumulation energy type ceramic dielectric material of base, its formula are (100-x) wt%
Ba0.4Sr0.6TiO3+ xwt%Bi2O3-B2O3- ZnO, wherein x=9.
Step one：Prepare Ba0.4Sr0.6TiO3Powder is standby.According to mol ratio 0.6:1:0.4 weighs SrCO3、TiO2And BaCO3
It is mixed to form mixture.
Step 2：Mixture and zirconium ballstone and deionized water are taken, is 1 according to mass ratio:1:Ball is carried out successively after 1 mixing
Mill, drying, after briquetting, be placed in batch-type furnace and 2 hours be incubated in 1150 DEG C, form the Ba of pure phase0.4Sr0.6TiO3Powder body, it is standby；
Step 3：By glass composite according to 60Bi2O3-30B2O3The mol ratio of -10ZnO (mol%) weighs raw material, in
Pour into after stirring and evenly mixing is fully ground in mortar in corundum crucible, be placed in high temperature resistance furnace and heat.According to the intensification speed of setting
Rate is warming up to 1300 DEG C, after insulation 1.5h, judges whether glass melt is founded well by wire drawing, without it was observed that bubble
And calculus, and high-temperature fusant has good ductility, shows that glass smelting is complete.Crucible can be taken out rapidly now and by high temperature
Melt is quickly poured on pre-heated copper coin.After vitreous humour just one-step forming, it is quickly placed to be warming up in advance 500 DEG C and moves back
The process of annealing 2h is carried out in stove, it is therefore intended that eliminate the residual stress in glass.Sample is taken out after furnace cooling, carried out
Cutting process, prepares follow-up Crystallizing treatment after sample is cut to the size of 10.0mm × 10.0mm × 2.0mm.By well cutting
With stove heat in sample placement Muffle furnace, 700 DEG C are risen to the heating rate of 10 DEG C/min, insulation 4h carries out Crystallizing treatment, treats
After furnace cooling, that is, complete the preparation of sample.
Step 4：With pure phase 91wt%Ba0.4Sr0.6TiO3, 9wt%Bi2O3-B2O3- ZnO, forms mixture, presses after mixing
Weigh to form full dispensing according to weight/mass percentage composition, it is standby；
Step 5：Full dispensing and zirconium ballstone and deionized water that step 4 is obtained are taken respectively, are 1 according to mass ratio:1:1 mixes
Carry out ball milling, drying after conjunction successively, pelletize, sieve, form granulation material；
Step 6：Granulation material obtained by step 5 is made into sample under the pressure of 120MPa, then, is placed in and with zirconium oxide is
In the aluminium oxide saggar of backing plate in high temperature box furnace, 500 DEG C of insulation 60min are warming up to 2 DEG C/min, are heated up with 5 DEG C/min
3 hours are incubated to when 1350 DEG C, afterwards, are cooled to after 500 DEG C with 5 DEG C/min, are cooled to room temperature with the furnace；
Step 7：After the sample that polishing, cleaning step five are sintered, silver electrode slurry is uniformly coated in sample tow sides
Material, sinters 25 minutes in 600 DEG C, obtains Ba0.4Sr0.6TiO3The unleaded accumulation energy type ceramic material sample of base.
Claims (9)
1. a kind of Bi2O3-B2O3- ZnO glass adds Ba0.4Sr0.6TiO3Base energy storage ceramic, it is characterised in that formula is (100-x)
Ba0.4Sr0.6TiO3+x Bi2O3-B2O3- ZnO, wherein x=1～9wt%, x are mass percent.
2. a kind of Bi according to claim 12O3-B2O3- ZnO glass adds Ba0.4Sr0.6TiO3Base energy storage ceramic, which is special
Levy and be, x=1wt%, 3wt%, 5wt%, 7wt% or 9wt%.
3. a kind of Bi2O3-B2O3- ZnO glass adds Ba0.4Sr0.6TiO3The preparation method of base energy storage ceramic, it is characterised in that bag
Include following steps：
Step one：According to mol ratio 0.6:1:0.4 weighs SrCO3、TiO2And BaCO3It is mixed to form mixture A；Mixture A is entered
Row ball milling, drying, after briquetting, 1.5～2 hours are incubated in 1120～1150 DEG C, form the Ba of pure phase0.4Sr0.6TiO3Powder body, it is standby
With；
Step 2：According to Bi2O3：B2O3：ZnO=6:3:1 mol ratio weighs raw material, is fully ground stirring and evenly mixing post-heating, rises
Temperature is incubated 1.5～2h to after 1200～1300 DEG C and obtains high-temperature fusant, then by high-temperature fusant first one-step forming, after just one-step forming
Made annealing treatment, cut after annealing, the sample of well cutting is carried out into Crystallizing treatment, Bi after cooling, is obtained2O3-B2O3-ZnO
Glass dust；
Step 3：By the Ba for obtaining0.4Sr0.6TiO3Powder body and Bi2O3-B2O3- ZnO glass dust is according to (100-x)
Ba0.4Sr0.6TiO3+xBi2O3-B2O3- ZnO is mixed to get mixture B, take after mixture B is mixed with zirconium ballstone and deionized water according to
It is secondary to carry out ball milling, drying, pelletize, sieve, granulation material is formed, wherein x=1～9wt%, x are mass percent；
Step 4：Granulation material obtained by step 3 is made into sample under the pressure of 110～120MPa, is then heated up with 2 DEG C/min
To 500 DEG C of insulation 60min, be incubated 2～3 hours when 1250～1350 DEG C are warming up to 5 DEG C/min, afterwards, lowered the temperature with 5 DEG C/min
To after 500 DEG C, room temperature is cooled to the furnace；
Step 5：After the sample that polishing, cleaning step four are sintered, silver electrode paste is uniformly coated in sample tow sides, in
600 DEG C sinter 20～30 minutes, obtain Bi2O3-B2O3- ZnO glass adds Ba0.4Sr0.6TiO3Base energy storage ceramic.
4. a kind of Bi according to claim 32O3-B2O3- ZnO glass adds Ba0.4Sr0.6TiO3The preparation of base energy storage ceramic
Method, it is characterised in that annealing is specially in step 2：Anneal in 500 DEG C of annealing furnace is warming up in advance 2h；Annealing
The size of 10.0mm × 10.0mm × 2.0mm is cut to afterwards.
5. a kind of Bi according to claim 32O3-B2O3- ZnO glass adds Ba0.4Sr0.6TiO3The preparation of base energy storage ceramic
Method, it is characterised in that Crystallizing treatment is specially in step 2：The sample of well cutting is placed on stove heat in Muffle furnace,
4h is incubated after 700 DEG C～750 are risen to the heating rate of 10 DEG C/min.
6. a kind of Bi according to claim 32O3-B2O3- ZnO glass adds Ba0.4Sr0.6TiO3The preparation of base energy storage ceramic
Method, it is characterised in that step one, Ball-milling Time is 4～6 hours in three.
7. a kind of Bi according to claim 32O3-B2O3- ZnO glass adds Ba0.4Sr0.6TiO3The preparation of base energy storage ceramic
Method, it is characterised in that take in step 3 carried out after mixture B is mixed with zirconium ballstone and deionized water successively ball milling, drying after
Drying material is obtained, binding agent is added into drying material carries out pelletize, binding agent accounts for 8～10%, Ran Houfen of drying material quality
Do not cross 40 mesh and 80 mesh sieves take middle material and obtain granulation material.
8. a kind of Bi according to claim 72O3-B2O3- ZnO glass adds Ba0.4Sr0.6TiO3The preparation of base energy storage ceramic
Method, it is characterised in that described adhesive is polyvinyl alcohol water solution.
9. a kind of Bi according to claim 72O3-B2O3- ZnO glass adds Ba0.4Sr0.6TiO3The preparation of base energy storage ceramic
Method, it is characterised in that the mass concentration of binding agent is 4～6%.
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Application publication date: 20170329 |