CN109020541A - A kind of high-performance environment-friendly capacitor dielectric and preparation method thereof - Google Patents
A kind of high-performance environment-friendly capacitor dielectric and preparation method thereof Download PDFInfo
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- CN109020541A CN109020541A CN201810797027.6A CN201810797027A CN109020541A CN 109020541 A CN109020541 A CN 109020541A CN 201810797027 A CN201810797027 A CN 201810797027A CN 109020541 A CN109020541 A CN 109020541A
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- 239000003990 capacitor Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000000919 ceramic Substances 0.000 claims abstract description 75
- 238000005245 sintering Methods 0.000 claims abstract description 40
- 239000000843 powder Substances 0.000 claims abstract description 33
- 238000000498 ball milling Methods 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 14
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- 238000005498 polishing Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 7
- GZTGGEGYVQCSER-UHFFFAOYSA-N samarium scandium Chemical compound [Sc][Sm] GZTGGEGYVQCSER-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 6
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 5
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 9
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 6
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 6
- 238000005516 engineering process Methods 0.000 claims description 6
- 238000007731 hot pressing Methods 0.000 claims description 6
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims description 6
- 238000004544 sputter deposition Methods 0.000 claims description 6
- DQMUQFUTDWISTM-UHFFFAOYSA-N O.[O-2].[Fe+2].[Fe+2].[O-2] Chemical compound O.[O-2].[Fe+2].[Fe+2].[O-2] DQMUQFUTDWISTM-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 230000005621 ferroelectricity Effects 0.000 claims description 4
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium oxide Chemical compound O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 claims description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 3
- 238000004146 energy storage Methods 0.000 abstract description 16
- 238000000034 method Methods 0.000 abstract description 13
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- 235000013312 flour Nutrition 0.000 abstract 1
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 16
- 239000010439 graphite Substances 0.000 description 12
- 229910002804 graphite Inorganic materials 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 238000011160 research Methods 0.000 description 5
- 229910052706 scandium Inorganic materials 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 4
- 229910052737 gold Inorganic materials 0.000 description 4
- 239000010931 gold Substances 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 229910052772 Samarium Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 229910052573 porcelain Inorganic materials 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 2
- 229910002113 barium titanate Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
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- 230000036541 health Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 244000137852 Petrea volubilis Species 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052620 chrysotile Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
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- 238000005336 cracking Methods 0.000 description 1
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- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
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- 229910052742 iron Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000006101 laboratory sample Substances 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- XMFOQHDPRMAJNU-UHFFFAOYSA-N lead(ii,iv) oxide Chemical compound O1[Pb]O[Pb]11O[Pb]O1 XMFOQHDPRMAJNU-UHFFFAOYSA-N 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- CWBIFDGMOSWLRQ-UHFFFAOYSA-N trimagnesium;hydroxy(trioxido)silane;hydrate Chemical compound O.[Mg+2].[Mg+2].[Mg+2].O[Si]([O-])([O-])[O-].O[Si]([O-])([O-])[O-] CWBIFDGMOSWLRQ-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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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
- C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
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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
- C04B35/622—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
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/6261—Milling
- C04B35/62615—High energy or reactive ball milling
-
- 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
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3272—Iron oxides or oxide forming salts thereof, e.g. hematite, magnetite
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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
- C04B2235/3298—Bismuth oxides, bismuthates or oxide forming salts thereof, e.g. zinc bismuthate
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/95—Products characterised by their size, e.g. microceramics
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Abstract
The present invention relates to a kind of high-performance environment-friendly capacitor dielectric and preparation method thereof, the high-performance environment-friendly capacitor dielectric is made of ferroelectric material hot pressed sintering, and the ferroelectric material is that samarium scandium is co-doped with bismuth ferrite, chemical composition Bi0.83Sm0.17Fe0.95Sc0.05O3.The preparation method comprises the following steps: being co-doped with BiFeO with ball-milling method preparation Sm, Sc3Powder；It after drying and abrasive flour, is pre-sintered, after pre-burning, carries out secondary ball milling；Then it carries out hot pressed sintering and obtains Bi0.83Sm0.17Fe0.95Sc0.05O3Ceramics obtain high-performance environment-friendly capacitor dielectric after cutting sanding and polishing.High-performance environment-friendly capacitor dielectric of the invention effectively improves pure BiFeO3Resistance to pressure is poor, the big disadvantage of leakage current, and greatly improving capable of storing up for capacitor dielectric density and can store up efficiency, and can store up density and can store up efficiency is respectively 2.21J/cm3, 76%, performance is better than other unleaded BiFeO3Base energy storage material, preparation method have the advantages that simple process, high production efficiency, easily controllable.
Description
Technical field
The present invention relates to capacitor areas more particularly to a kind of high-performance environment-friendly capacitor dielectric and preparation method thereof.
Background technique
Energy storage material plays a significant role in hyundai electronics and electrical system, is widely used in various energy storage components, such as
Dielectric capacitor, electrochemical capacitor, battery (lithium ion battery, fuel cell) etc..These three types of elements differ from one another, such as electricity
Pond has highest energy storage density but charge/discharge speed is slow and power density is minimum, suitable for providing setting for lasting stability electric energy
It is standby；Dielectric capacitor have in three maximum power density, can momentary charge, be suitable for pulse high-power power equipment；Electricity
Chemical capacitor then falls between.However, the energy storage material that uses of Current commercial mostly with lead-containing compounds (such as: zirconium metatitanic acid
Lead, abbreviation PZT) based on, and raw material lead monoxide (or lead orthoplumbate) used in this kind of material accounts for about the total matter of raw material
Amount 70%, they are readily volatilized during high temperature production, and lead in atmosphere the raising of " lead " content, high risks people
The health of class and the environment depended on for existence.Research and develop unleaded dielectric functional material already become instantly global scientist,
Engineers focus of attention.The research of novel lead-free dielectric substance not only contributes to environmental protection, and is conducive to promote electric Jie
The energy storage density of material, and it is resistant to higher voltage, to realize the miniaturization and facilitation of capacitor, it is expanded using model
It encloses.
In recent years, the research of novel lead-free capacitor material is a lot of, and main includes doping BaTiO3(BT) ceramics of base and
Thick film research, unleaded BiFeO3The research of based solid solution relaxation ferroelectric dielectric, but respectively have its own limitation.Wherein, with
BaTiO3(BT) for the ceramics of base, the highest energy storage density that such material is reported at present is only 1.2J/cm3, efficiency is not also high,
Resistance to pressure is the bottleneck that it develops with that can store up efficiency.
Summary of the invention
Based on this, the purpose of the present invention is to overcome the shortcomings of the existing technology, Optimizing Technical, response green life number
It calls together, provides a kind of high-performance environment-friendly capacitor dielectric and preparation method thereof, the high-performance environment-friendly capacitor dielectric has
Density can be stored up and can store up high-efficient, resistance to pressure is good, and leakage current is small, and performance is better than other unleaded BiFeO3Base energy storage material it is excellent
Point, the preparation method have the advantages that simple process, high production efficiency, easily controllable.
The technical solution adopted by the present invention is as follows:
A kind of high-performance environment-friendly capacitor dielectric, is made of ferroelectric material hot pressed sintering, and the ferroelectric material is samarium scandium
It is co-doped with bismuth ferrite, chemical composition Bi0.83Sm0.17Fe0.95Sc0.05O3。
High-performance environment-friendly capacitor dielectric of the invention is by ferroelectric material bismuth ferrite (BiFeO3) by mixing rare earth member
Plain Sm samarium (Sm) and scandium (Sc) hot pressed sintering are made.Using the pure bismuth ferrite of Sm and Sc doping vario-property, it is allowed to contain with rare earth element
The increase of amount, slowly from apparent ferroelectricity to close to paraelectric phase transition, and para-electric has the performance of high pressure resistance, and suitable
Electric layer plays the role of that charge is isolated, so as to obtain big breakdown strength.The BiFeO of unleaded high-performance environment-friendly of the invention3
Based capacitor dielectric substance effectively improves pure BiFeO3Resistance to pressure is poor, and the big disadvantage of leakage current greatly improves capacitor
Device is dielectric to be stored up density and can store up efficiency, and can store up density and can store up efficiency is respectively 2.21J/cm3, 76%, performance is excellent
In other unleaded BiFeO3Base energy storage material.
The preparation method of the high-performance environment-friendly capacitor dielectric, comprising the following steps:
Step 1, with bismuth oxide (Bi2O3), samarium sesquioxide (Sm2O3), di-iron trioxide (Fe2O3) and three oxidations
Two scandium (Sc2O3) it is raw material, Bi is made by ball milling0.83Sm0.17Fe0.95Sc0.05O3Powder；
Step 2 carries out secondary ball by powder pre-burning 5 minutes at 860 DEG C obtained by step 1, then to the powder after pre-burning
Mill；
Step 3 obtains powder hot pressed sintering 5 minutes at 820~860 DEG C obtained by step 2
Bi0.83Sm0.17Fe0.95Sc0.05O3Then ceramics obtain high-performance environment-friendly capacitor dielectric by cutting, sanding and polishing.
In the preparation step, step 1 prepares Bi by ball milling0.83Sm0.17Fe0.95Sc0.05O3Powder, simple process, easily
In realization；Step 2 to the powder secondary ball milling after pre-burning can obtain component more evenly, the thinner target powder of particle, be conducive to
Promote the pressure-resistant performance and optimization microstructure of subsequent ceramics；During the rapid thermal pressed sintering of the step 3,820~
Keeping the temperature five minutes at 860 DEG C can make ceramics well at phase and discharge internal stress.
Compared to conventional solid sintering and fast performance liquid sintering, preparation method of the present invention passes through rapid thermal pressed sintering
The ceramics of method sintering, structure is finer and close, component is more uniform, while generating substantially without miscellaneous phase, so there is very excellent relaxation
Ferroelectric properties and pressure-resistant property, so that obtaining bigger can store up density, and simple process, high production efficiency, easily controllable pottery
The generation of porcelain structure.
Further, step 1 specifically: according to the ratio by bismuth oxide, samarium sesquioxide, di-iron trioxide and three oxygen
Change two scandiums to be added in ball grinder, and zirconium oxide balls be added as abrasive media, addition alcohol as abrasive solvents, then with
300~500 revs/min of revolving speed carries out ball milling 12~36 hours, obtains Bi0.83Sm0.17Fe0.95Sc0.05O3Powder.
Further, step 2 specifically: after the drying of powder obtained by step 1, then ground, be then fed into tubular type
In furnace at 860 DEG C pre-burning 5 minutes, then regrind, then carry out secondary ball milling, dried, ground again after secondary ball milling.
By multiple ball milling and the grinding after drying every time, can obtain component more evenly, the thinner target powder of particle, advantageously ensure that
Finally obtain that ceramic structure is finer and close, component is more uniform.
Further, step 3 specifically: powder obtained by step 2 is fitted into hot pressing die, in 0.8 megapascal of pressure, temperature
Rapid thermal pressed sintering is carried out under conditions of 860 DEG C of degree, heat preservation obtains Bi after five minutes0.83Sm0.17Fe0.95Sc0.05O3Ceramics, then
High-performance environment-friendly capacitor dielectric is obtained by cutting, sanding and polishing.By being sintered under the pressure of 0.8 megapascal so that material
Structure is very fine and close, basic to exist without cavity, while the clear size of crystal grain is uniform, so that the ceramics of excellent are obtained, with
Ceramic performance made from 860 DEG C of sintering temperatures is optimal.
Further, it during the rapid thermal pressed sintering of step 3, is rapidly heated with 200 DEG C of rate per minute to 860
℃.It is rapidly heated with the heating rate, is avoided that during hot pressed sintering, generating miscellaneous phase influences ceramic performance.
Further, in step 3, the cutting is to be obtained with cutting machine from hot pressed sintering
Bi0.83Sm0.17Fe0.95Sc0.05O3Ceramic middle section interception is less than or equal to the thin slice of 1mm thickness, and the sanding and polishing is with gold
Phase sand paper chooses thin slice sanding and polishing to the ceramic sheet of 0.1~0.5mm thickness, the thickness of ceramic sheet according to actual needs.
Further, further include step 4: being plated respectively using the two sides of sputtering technology ceramic sheet obtained by step 3
Hearth electrode and top electrode.
In order to better understand and implement, the invention will now be described in detail with reference to the accompanying drawings.
Detailed description of the invention
Fig. 1 is the XRD diffraction comparison diagram of BSFSO ceramics sample and pure BFO ceramics sample；
Fig. 2 is the section the SEM phenogram of BSFSO ceramics sample；
Fig. 3 is ferroelectric hysteresis loop of the BSFSO ceramics sample under different voltages and can store up performance map；
Wherein, Fig. 3 (a) is ferroelectric hysteresis loop figure of the BSFSO ceramics sample under different voltages, and Fig. 3 (b) is BSFSO ceramics
Sample can store up performance map under different voltages；
Fig. 4 is the ferroelectric hysteresis loop of BSFSO ceramics sample at different temperatures and can store up performance map；
Wherein, Fig. 4 (a) is the ferroelectric hysteresis loop figure of BSFSO ceramics sample at different temperatures, and Fig. 4 (b) is BSFSO ceramics
Sample at different temperatures can store up performance map；
Fig. 5 is the ferroelectric hysteresis loop of BSFSO sample at different frequencies and can store up performance map；
Wherein, Fig. 5 (a) is the ferroelectric hysteresis loop figure of BSFSO ceramics sample at different frequencies, and Fig. 5 (b) is BSFSO ceramics
Sample at different frequencies can store up performance map；
Fig. 6 is the ferroelectric hysteresis loop for the BSFSO ceramics sample that different sintering temperatures obtain and can store up performance comparison figure；
Wherein, Fig. 6 (a) is the ferroelectric hysteresis loop figure for the BSFSO ceramics sample that different sintering temperatures obtain, and Fig. 6 (b) is different
The BSFSO ceramics sample that sintering temperature obtains can store up performance comparison figure；
Fig. 7 is the EDS map and data of BSFSO ceramics sample；
Wherein, left figure is the EDS map of BSFSO ceramics sample, and right table is the atomicity of tetra- kinds of elements of Bi, Sm, Fe, Sc, O
The experiment value and theoretical value of percentage；
Fig. 8 is dielectric constant, loss and the leakage data of BSFSO ceramics sample；
Wherein, Fig. 8 (a) is the curve graph that changes with test frequency of dielectric constant of BSFSO ceramics sample, and Fig. 8 (b) is
The curve graph that the loss of BSFSO ceramics sample changes with test frequency, Fig. 8 (c) be BSFSO ceramics sample leakage current value with
The curve graph of electric field strength variation.
Specific embodiment
Embodiment 1
Steps are as follows for the preparation method of the high-performance environment-friendly capacitor dielectric of the present embodiment:
Step 1: preparation Bi0.83Sm0.17Fe0.95Sc0.05O3(BSFSO) powder.
In the present embodiment, gained BSFSO powder total amount is 0.08mol, then BSFSO powder to prepare raw material as shown in table 1:
1 BSFSO powder of table prepares raw material
| Nomenclature of drug | Molecular weight | Drug purity | Experiment proportion | Stoichiometric number | Weigh quality |
| Bismuth oxide | 465.96 | 0.9999 | 1 | 0.83 | 15.4714g |
| Samarium sesquioxide | 348.7 | 0.9999 | 1 | 0.17 | 2.3714g |
| Di-iron trioxide | 159.69 | 0.999 | 1 | 0.95 | 6.0742g |
| Scandium oxide | 137.91 | 0.999 | 1 | 0.05 | 0.2760g |
Specific step is as follows:
1) each raw material is weighed according to the weighing quality in table 1；
2) load weighted raw material is added in nylon ball grinder, and zirconium oxide balls is added as abrasive media, wine is added
Essence is used as abrasive solvents, carries out mixing and first ball milling.Wherein, the control of the mass ratio of abrasive media and raw material is in 1:1 or so；It grinds
The Gradation Control of abrading-ball used in grinding media is big: in: small=1:2:3 or so；The revolving speed of ball mill is 418 revs/min, when ball milling
Between be 24 hours.
Step 2: pre-burning.Specific step is as follows:
1) after the first ball milling of step 1, gained powder is poured in culture dish, baking oven is put into and is dried, until
Alcohol is all until drying.Powder after drying is scraped in agate mortar with spoon, is ground 30 minutes with agate bar, then will
Powder is sent into tube furnace pre-burning 5 minutes at 860 DEG C, is then added in agate mortar and is ground 20 minutes with agate bar again,
In case secondary ball milling.
2) powder of pre-burning is subjected to secondary ball milling, after secondary ball milling, gained powder is poured in culture dish,
It is put into baking oven to be dried, until alcohol all drying, then uses powder in the agate mortar the grinding of agate bar more equal
It is even, thinner, BSFSO target powder is obtained, is sealed against being stored in Muffle furnace.The condition of the secondary ball milling and step 1
The condition of first ball milling is identical.
Step 3: preparation Bi0.83Sm0.17Fe0.95Sc0.05O3(BSFSO) ceramic.Specific step is as follows:
1) the BSFSO powder about 4.5g for weighing step 2 preparation is fitted into the graphite jig for hot pressed sintering, with painting
There is the high temperature resistant carbon paper of boron nitride to keep apart the upper lower gasket of powder and graphite jig, it is therefore intended that prevent in graphite jig
Carbon penetrates into laboratory sample, to influence the performance of sample.It is needed in graphite jig for the cylindrical cavity of setting-out product
It is wrapped up with one layer of high temperature resistant carbon paper, mitigates carbon in graphite grinding tool and permeated to sample area.
2) it will be coated outside the graphite jig equipped with BSFSO powder with the asbestos of one layer of high temperature resistant heat insulation, mitigate graphite mo(u)ld
Have the loss in high temperature hot pressing sintering process, can recycle and be used for multiple times.The top of graphite jig also to pad one layer it is resistance to
Then graphite jig is put into fast-speed direct current hot press by high chrysotile, to its upper and lower graphite plate plus-pressure to 0.8 megapascal.
3) recirculated cooling water for opening fast-speed direct current hot press, because big calorimetric can be generated in high temperature hot pressing sintering process
Amount, needs to cool down in time；Open the ventilating system in laboratory, it is therefore intended that be discharged from the dust generated in experimentation, avoid hurting
The health of evil experimenter；By in the aperture for being used to measure sintering temperature of thermocouple insertion graphite jig, opening temperature is aobvious
Display screen, convenient sample temperature check at any time guarantee the preciseness and correctness of experiment.After preparation before carrying out test, i.e.,
Hot pressed sintering test can formally be carried out.
4) in order to which guarantee test is gone on smoothly, two laboratory technicians is needed to cooperate to complete.One people is responsible for controlling fast-speed direct current hot pressing
The heating instrument board of machine, while the registration of electric thermo-couple temperature display screen is kept a close eye on, avoiding sintering temperature is more than the predetermined temperature of test
Degree.An other people is responsible for controlling the pressure that autoclave test is added in sample both ends, because in high-temperature sintering process, after sample calcination
Pressure be will lead to lower than scheduled pressure value, at this moment just need to pressurize to sample in time, pressure is made to maintain 0.8 megapascal always.This
The cooperation for passing through two laboratory technicians in experimentation is first fast with 200 DEG C of heating rate per minute under the pressure of 0.8 megapascal
Sintering temperature is risen to 860 DEG C by speed, is then kept the temperature 5 minutes, is facilitated the release of sample interior stress.It, will be hot after the completion of heat preservation
Press is closed, and allows sample Temperature fall, and it is 0.8 that the pressure for being added in sample both ends is still kept before its temperature drops to 600 DEG C
Megapascal prevents it from cracking in temperature-fall period and stomata.
5) when sample temperature is down to room temperature, it is taken out from graphite jig, obtains the cylindrical BSFSO pottery of thick 4mm
Tile then with cutting machine from the thin slice of potsherd middle section interception about 0.6mm thickness, then is polished to thin slice with abrasive paper for metallograph and is thrown
Light to 0.17mm thickness BSFSO ceramic sheet, so that next plated electrode does dependence test.
Step 4: top electrode is plated respectively on the two sides of BSFSO ceramic sheet.Specific step is as follows:
1) hearth electrode is plated for BSFSO ceramic sheet, hearth electrode is face electrode.Potsherd is put into small ion sputter
In, after installing gold target material to small ion sputter, power supply is opened, is evacuated to 2 × 10-3Pa and it is following after, start to instrument
High-purity (99.99%) argon gas is passed through as ionization medium.Before starting sputtering, it is ensured that electric current (can lead between 6~8mA
The needle-valve for crossing instrument is adjusted) because excessively high electric current may damage instrument.Each sputtering time is 40s, repetitive operation 4
Secondary, every minor tick 20s first closes the air valve for being passed through argon gas after the completion, turns off instrument power source, begin to speak to sample.After taking out sample,
It is toasted 6 minutes or so for 90 DEG C on warm table, the gold electrode in sputtering is allowed preferably to be adhered to potsherd bottom surface.
2) top electrode is plated for BSFSO ceramic sheet, top electrode is point electrode.Potsherd is put into small ion sputter
In, one piece of mask plate is covered above, and the diameter in hole is 1.5mm on mask plate.The technique of top electrode is plated with the step in step 4
1) after, taking out sample, it is toasted 6 minutes or so for 90 DEG C on warm table, the gold electrode in sputtering is allowed preferably to be adhered to pottery
Tile surface.Obtain having plated the BSFSO potsherd of hearth electrode and top electrode, as high-performance environment-friendly capacitor dielectric as a result,.
Embodiment 2
The preparation method of the high-performance environment-friendly capacitor dielectric of the present embodiment is substantially the same manner as Example 1, difference
It is following two points:
1., by the cooperation of two laboratory technicians, first sintering temperature is distinguished during the step 4) hot pressed sintering of step 3
860 DEG C, 840 DEG C, 820 DEG C of three kinds of different temperatures are risen to, then keep the temperature 5 minutes respectively, three parts of different sintering temperature are obtained after cooling
BSFSO ceramics sample made of spending.
2. the step 2) of step 4 plates top electrode, the diameter in hole is 1mm on the mask plate that uses.
Embodiment 3
To high-performance environment-friendly capacitor dielectric made from embodiment 1 and embodiment 2, i.e. (samarium scandium is co-doped with BSFSO ceramics
BFO ceramics) performance tested and characterized:
(1) XRD diffraction is tested
Referring to Fig. 1, it is the XRD diffraction comparison diagram of BSFSO ceramics sample and pure BFO ceramics sample, the curve 1 in figure
For the XRD diffraction pattern of BSFSO ceramics, curve 2 is the XRD diffraction pattern of pure BFO ceramics.The test result passes through X-ray diffractometer
(X ' Pert PRO, PANalytical) obtains BSFSO ceramic test made from embodiment 1.From figure 1 it appears that
BSFSO ceramic energy is independent at phase, and no other miscellaneous phases generate.
(2) section SEM characterizes
Referring to Fig. 2, it is the section the SEM phenogram and partial enlarged view of BSFSO ceramics sample, the test result is logical
Overscanning electron microscope (ZEISS Gemini500) obtains BSFSO ceramic test made from embodiment 1.It can be with from Fig. 2
Find out that BSFSO ceramic structure is very fine and close, crystal phase is obvious, exists without hole, defect and impurity generates.
(3) ferroelectric hysteresis loop and performance evaluation can be stored up
By ferroelectricity tester (Radiant Technology Ferroelectric Tester) to embodiment 1 and in fact
It applies step 4 in example 2 and has plated the BSFSO ceramics progress electrical testing after bottom, top electrode.
Test result is as seen in figures 3-6, wherein Fig. 3 (a), Fig. 4 (a), Fig. 5 (a) are 1 gained BSFSO of embodiment pottery respectively
Ferroelectric hysteresis loop figure of the porcelain sample under different voltages, different temperatures and different frequency；Fig. 3 (b), 4 (b) and 5 (b) are to implement respectively
Energy storage value and energy storage efficiency comparison of the 1 gained BSFSO ceramics sample of example under different voltages, different temperatures and different frequency
Scheme, two curves in each figure enclose ordinate pointed by arrow by its ellipse, correspond respectively to energy storage value or energy storage effect
Rate curve；Fig. 6 (a) is the ferroelectric hysteresis loop figure for the BSFSO ceramics sample that embodiment 2 is obtained in different sintering temperatures, and Fig. 6 (b) is
The energy storage value and energy storage efficiency comparison diagram for the BSFSO ceramics sample that embodiment 2 is obtained in different sintering temperatures.
As seen from Figure 3, the resistance to electric field strength of BSFSO ceramics is up to 230kV/cm, and the shape of ferroelectric hysteresis loop is thinner
Long, corresponding energy storage value and efficiency are respectively 2.21J/cm3With 76%, better than the 1.66J/cm reported at present3Can store up it is close
Degree and 75% can store up efficiency.
As seen from Figure 4, BSFSO ceramics have good temperature stability, in 120 DEG C of acquirement optimum performances.
As seen from Figure 5, BSFSO ceramics have excellent frequency stability, obtain optimal performance in 1Hz.
As seen from Figure 6, BSFSO ceramics have top performance under 860 DEG C of hot pressing conditions.
Above-mentioned good characteristic shows that BSFSO ceramics (samarium scandium is co-doped with BFO ceramics) can apply to high speed, high temperature energy density
Dielectric capacitor.
(4) EDS data is analyzed
Referring to Fig. 7, it is the EDS data of BSFSO ceramics sample.The test result passes through Flied emission scanning electron microscopy
Mirror (ZEISS Gemini500) obtains BSFSO ceramic test made from embodiment 1.It can be seen from figure 7 that all elements
Experiment value it is almost the same with theoretical value, show that Sm and Sc codope and rapid thermal pressed sintering method can inhibit Bi element
Volatilization.
(5) Dielectric behavior and leakage current analysis
Referring to Fig. 8, it is dielectric constant, loss and the leakage data of BSFSO ceramics sample, these test results
It is made pottery as ferroelectricity tester (Radiant Technology Ferroelectric Tester) to BSFSO made from embodiment 1
Porcelain is tested to obtain.As can be seen that the dielectric constant of the BSFSO ceramics sample subtracts with the increase of test frequency from Fig. 8 (a)
Few, numerical value illustrates BSFSO ceramics sample good properties between 200 to 260, while as can see from Figure 8, dielectric damage
Consumption and leakage current value all very littles, illustrate that the insulating properties of sample is very good, and the above-mentioned related data tested out is its characteristic value,
Test result science is reliable.
Compared with the existing technology, the samarium scandium that the present invention is sintered by rapid thermal pressed sintering method is co-doped with BFO ceramics
(BSFSO), compared to conventional solid sintering and fast performance liquid sintering, can it is finer and close, component is more uniform, while substantially without miscellaneous phase
It generates, so have very excellent relaxor ferroelectric performance and pressure-resistant property, so that obtaining bigger can store up density.The above experimental result
Illustrate that the BSFSO ceramics of high-performance environment-friendly of the invention effectively improve that BFO resistance to pressure is poor, the big disadvantage of leakage current is promoted
Capacitor dielectric can store up density and can store up efficiency.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.
Claims (8)
1. a kind of high-performance environment-friendly capacitor dielectric, it is characterised in that: be made of ferroelectric material hot pressed sintering, the ferroelectricity material
Material is that samarium scandium is co-doped with bismuth ferrite, chemical composition Bi0.83Sm0.17Fe0.95Sc0.05O3。
2. the preparation method of high-performance environment-friendly capacitor dielectric described in claim 1, it is characterised in that: including following step
It is rapid:
Step 1 is made using bismuth oxide, samarium sesquioxide, di-iron trioxide and scandium oxide as raw material by ball milling
Bi0.83Sm0.17Fe0.95Sc0.05O3Powder；
Step 2 carries out secondary ball milling by powder pre-burning 5 minutes at 860 DEG C obtained by step 1, then to the powder after pre-burning；
Step 3 obtains powder hot pressed sintering 5 minutes at 820~860 DEG C obtained by step 2
Bi0.83Sm0.17Fe0.95Sc0.05O3Then ceramics obtain high-performance environment-friendly capacitor dielectric by cutting, sanding and polishing.
3. the preparation method of high-performance environment-friendly capacitor dielectric according to claim 2, it is characterised in that: step 1 tool
Body are as follows: bismuth oxide, samarium sesquioxide, di-iron trioxide and scandium oxide are added in ball grinder according to the ratio, and are added
Zirconium oxide balls are added alcohol as abrasive solvents, then carry out ball with 300~500 revs/min of revolving speed as abrasive media
Mill 12~36 hours, obtains Bi0.83Sm0.17Fe0.95Sc0.05O3Powder.
4. the preparation method of high-performance environment-friendly capacitor dielectric according to claim 2, it is characterised in that: step 2 tool
Body are as follows: after the drying of powder obtained by step 1, then ground, be then fed into tube furnace pre-burning 5 minutes at 860 DEG C, so
After regrind, then carry out secondary ball milling, dried, ground again after secondary ball milling.
5. the preparation method of high-performance environment-friendly capacitor dielectric according to claim 2, it is characterised in that: step 3 tool
Body are as follows: powder obtained by step 2 is fitted into hot pressing die, carries out fast speed heat under conditions of 0.8 megapascal of pressure, 860 DEG C of temperature
Pressure sintering, heat preservation obtain Bi after five minutes0.83Sm0.17Fe0.95Sc0.05O3Then ceramics obtain high property by cutting, sanding and polishing
It can environmentally friendly capacitor dielectric.
6. the preparation method of high-performance environment-friendly capacitor dielectric according to claim 5, it is characterised in that: step 3
During rapid thermal pressed sintering, it is rapidly heated with 200 DEG C of rate per minute to 860 DEG C.
7. the preparation method of high-performance environment-friendly capacitor dielectric according to claim 5, it is characterised in that: step 3
In, the cutting is the Bi obtained with cutting machine from hot pressed sintering0.83Sm0.17Fe0.95Sc0.05O3Ceramic middle section interception is less than
Or the thin slice equal to 1mm thickness, the sanding and polishing are the ceramics with abrasive paper for metallograph to thin slice sanding and polishing to 0.1~0.5mm thickness
Thin slice.
8. the preparation method of high-performance environment-friendly capacitor dielectric according to claim 7, it is characterised in that: further include step
Rapid four: hearth electrode and top electrode are plated using the two sides of sputtering technology ceramic sheet obtained by step 3 respectively.
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