CN102810401A - Composite type solid electrolytic capacitor electrode slice and preparation method thereof - Google Patents
Composite type solid electrolytic capacitor electrode slice and preparation method thereof Download PDFInfo
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- CN102810401A CN102810401A CN2011101447131A CN201110144713A CN102810401A CN 102810401 A CN102810401 A CN 102810401A CN 2011101447131 A CN2011101447131 A CN 2011101447131A CN 201110144713 A CN201110144713 A CN 201110144713A CN 102810401 A CN102810401 A CN 102810401A
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Abstract
The invention discloses a composite type solid electrolytic capacitor electrode slice and a preparation method thereof, belonging to the field of capacitor electrodes. The composite solid electrolytic capacitor electrode slice is structurally made of aluminum/aluminum oxide-barium titanate/graphene. As the graphene is used for taking the place of a conductive macromolecule electrolyte material, the composite solid electrolytic capacitor electrode slice provided by the invention has excellent stability and consistency; and moreover the electrode slice is simple in preparation process, low in cost and is applicable to industrial production.
Description
Technical field
The present invention relates to a kind of electrode slice, relate in particular to a kind of composite solid electrolytic capacitor sheet and preparation method.
Background technology
Solid capacitor mainly is divided into solid organic polymer capacitors such as organic molecules such as manganese dioxide, TCNQ and PEDOT.In electrochemical capacitor, traditional alminium electrolytic condenser by be with electrolyte as dielectric material, this capacitor does not break away from because physical characteristic and expanded by heating, the dangerous phenomenon of leakage occurs, lets aluminium electrolytic capacitor face outstanding unprecedented pressure and challenge; In addition, the conventional aluminum electrochemical capacitor adopts manganese dioxide as cathode material, except the danger that occurs easily burning owing to voltage problem, more because environmental issue makes the future market significantly limited.
Organic semiconductor TCNQ is a kind of cyanide, when high temperature, volatilizes the dicyanogen of severe toxicity easily, therefore, has also just limited the TCNQ application.Macromolecule product PEDOT is as the solid capacitor of cathode material, and its production cost is high, has also just limited the application of PEDOT.
Summary of the invention
The object of the present invention is to provide a kind of security performance good, nontoxic, and the low composite solid electrolytic capacitor sheet of production cost
Technical scheme of the present invention is following:
A kind of composite solid electrolytic capacitor sheet, its structure is aluminium/alundum (Al-barium titanate/Graphene, the conductivity of this composite solid electrolytic capacitor sheet is 15000～50000s/m; Wherein, in the composite solid electrolytic capacitor sheet, the thickness of alundum (Al is 720～900nm.
Another object of the present invention is to provide the preparation method of composite solid electrolytic capacitor sheet, its step is following:
S1, aluminium foil or aluminium net are immersed in the container of the suspension that fills Barium Titanate nano-powder, then under the vacuum in 500-700 ℃ of heat treatment 0.5-12h, obtain applying the aluminium foil or the aluminium net of barium titanate;
S2, with in the water-soluble solution of graphene oxide, make electrolyte; Wherein, the molar concentration of graphene oxide is 1～3mol/L;
In the electrolyte that the aluminium foil of S3, coating barium titanate that step S1 is made or aluminium net make as electrode inserting step S2, and on electrode, pass to the direct current of 1～10mA, be 1～24h conduction time, obtains aluminium/barium titanate/graphene oxide electrode slice;
S4, aluminium/barium titanate/graphene oxide electrode slice that step S3 is made place vacuum, 80～300 ℃ of following baking 2～24h, make aluminium/barium titanate/Graphene electrodes sheet;
S5, employing anode oxidation method; On aluminium/barium titanate/Graphene electrodes sheet that step S4 obtains, pass through direct voltage; After being 0.5～2h conduction time; Aluminium is direct oxidation into alundum (Al, and making structure is the said composite solid electrolytic capacitor sheet of aluminium/alundum (Al-barium titanate/Graphene; Wherein, the magnitude of voltage of said direct voltage is 135～200% of a solid electrolytic capacitor load voltage value, i.e. the voltage of the about every volt formation of the thickness of alundum (Al is 1.2～1.5nm, and the thickness of this alundum (Al is about 720～900nm.
Among the above-mentioned preparation method, among the step S2, said graphite oxide adopts following step to make:
S21,2: 1: 1 graphite powder of mass ratio, potassium peroxydisulfate, phosphorus pentoxide are added in the concentrated sulfuric acid, stir, cool off subsequently, filter, and washing filter thing is to neutrality, drying, subsequent use;
In S22, the concentrated sulfuric acid, add potassium permanganate subsequently, stir 0 ℃ of the dried filter thing adding of step S21; Then add deionized water and mass concentration successively and be 30% hydrogen peroxide solution, mix and be mixed solution; Wherein, the quality of potassium permanganate is 3 times of graphite powder quality;
The mixed solution of S23, filtration step S22, and to use mass concentration be 10% salt acid elution, suction filtration, dry filter thing, obtains graphene oxide at last.
Composite solid electrolytic capacitor sheet provided by the invention replaces traditional conductive polyelectrolyte material with Graphene, can well improve the stability and the consistency of product; And this electrode slice preparation technology is simple, with low cost, be fit to suitability for industrialized production.
Description of drawings
Fig. 1 is the SEM figure of aluminium/alundum (Al of the present invention-barium titanate/Graphene electrodes sheet; Wherein, surface sweeping Electronic Speculum model: FESEM, Hitachi S-4300; Accelerating voltage: 10-15KV;
Fig. 2 is the section S EM figure of aluminium/alundum (Al of the present invention-barium titanate/Graphene electrodes sheet; Wherein, surface sweeping Electronic Speculum model: FESEM, Hitachi S-4300; Accelerating voltage: 10-15KV;
Fig. 3 is preparation technology's flow chart of aluminium/alundum (Al of the present invention-barium titanate/Graphene electrodes sheet.
Embodiment
A kind of composite solid electrolytic capacitor sheet provided by the invention, as illustrated in fig. 1 and 2, its structure is aluminium/alundum (Al-barium titanate/Graphene, the conductivity of this composite solid electrolytic capacitor sheet is 15000-50000s/m; Wherein, the thickness of alundum (Al is 720～900nm.
The preparation method of above-mentioned composite solid electrolytic capacitor sheet provided by the invention, its step is following:
S1, aluminium foil or aluminium net are immersed in the container of the suspension that fills Barium Titanate nano-powder, then under the vacuum in 500-700 ℃ of heat treatment 0.5-12h, obtain applying the aluminium foil or the aluminium net of barium titanate;
S2, with in the water-soluble solution of graphene oxide, make electrolyte; Wherein, the molar concentration of graphene oxide is 1～3mol/L;
In the electrolyte that the aluminium foil of S3, coating barium titanate that step S1 is made or aluminium net make as electrode inserting step S2, and on electrode, pass to the direct current of 1～10mA, be 1～24h conduction time, obtains aluminium/barium titanate/graphene oxide electrode slice;
S4, aluminium/barium titanate/graphene oxide electrode slice that step S3 is made place vacuum, 80～300 ℃ of following baking 2～24h, make aluminium/barium titanate/Graphene electrodes sheet;
S5, adopt anode oxidation method, on aluminium/barium titanate/Graphene electrodes sheet that step S4 obtains through direct voltage, be 0.5～2h conduction time after, aluminium (Al) is direct oxidation into alundum (Al (Al
2O
3), making structure is the said composite solid electrolytic capacitor sheet of aluminium/alundum (Al-barium titanate/Graphene; Wherein, the magnitude of voltage of said direct voltage is 135～200% of a solid electrolytic capacitor load voltage value, i.e. the voltage of the about every volt formation of the thickness of alundum (Al is 1.2～1.5nm, and the thickness of this alundum (Al is about 720～900nm.
Among the above-mentioned preparation method, among the step S2, said graphite oxide adopts following step to make:
S21,2: 1: 1 graphite powder of mass ratio, potassium peroxydisulfate, phosphorus pentoxide added in 80 ℃ the concentrated sulfuric acid, stir, cool off subsequently more than the 6h, filter, and washing filter thing is to neutral, drying, subsequent use;
In S22, the concentrated sulfuric acid, add potassium permanganate subsequently, stir 0 ℃ of the dried filter thing adding of step S21; Then add deionized water and mass concentration successively and be 30% hydrogen peroxide solution, mix and be mixed solution; Wherein, the quality of potassium permanganate is 3 times of graphite powder quality;
The mixed solution of S23, filtration step S22, and to use mass concentration be salt acid elution, suction filtration, 60 ℃ of following vacuumizes filter thing 48h of 10%, obtains graphene oxide at last.
Below in conjunction with accompanying drawing, further explain is done in preferred embodiment of the present invention.
Embodiment 1
The preparation method of composite solid electrolytic capacitor sheet is following:
(1) graphite oxide: with 20g purity is that 99.5% 50 order graphite powders, 10g potassium peroxydisulfate and 10g phosphorus pentoxide add in 80 ℃ the concentrated sulfuric acid, stirs, and more than the cooling 6h, washing is to neutral, drying; In the concentrated sulfuric acid with 0 ℃ of dried sample adding, 230mL, add 60g potassium permanganate again, the temperature of mixture remains on below 20 ℃, in 35 ℃ oil bath, behind the maintenance 2h, slowly adds the 920mL deionized water then; Behind the 15min; Add 2.8L deionized water and 50mL mass concentration more successively and be 30% hydrogen peroxide solution; The mixture color becomes glassy yellow afterwards, and suction filtration while hot uses that 5L concentration is that 10% hydrochloric acid washs again, suction filtration, promptly obtains graphite oxide at 60 ℃ of vacuumize 48h;
(2) aluminium foil is immersed in the container of the suspension fill Barium Titanate nano-powder, then under the vacuum, 500 ℃ of heat treatment 12h obtain applying the aluminium foil of barium titanate;
(3) graphene oxide that (1) is prepared is dissolved in the container that fills water, and forming molar concentration is the graphene oxide electrolyte of 1mol/L;
The aluminium foil of the coating barium titanate that (4) (2) is made inserts in the electrolyte that (3) make as electrode, and on electrode, passes to the direct current of 1mA, and be 1h conduction time, obtains aluminium/barium titanate/Graphene electrodes sheet;
(5); Aluminium/barium titanate/graphene oxide electrode slice that step (4) is made places vacuum, 120 ℃ of following baking 12h, makes aluminium/barium titanate/Graphene electrodes sheet;
(6) aluminium/barium titanate that (5) is obtained/Graphene electrodes sheet carries out roller compaction to be handled;
(7) aluminium/barium titanate through compaction treatment that (6) is obtained/Graphene electrodes sheet is through direct voltage, and this voltage is 135% of final capacitor rated voltage, and be 0.5h conduction time; After intact, obtaining structure is the said composite solid electrolytic capacitor sheet of aluminium/alundum (Al-barium titanate/Graphene, and the conductivity of this electrode slice is 15000s/m; Wherein, the thickness of alundum (Al is greatly about 720nm.
Embodiment 2
The preparation method of composite solid electrolytic capacitor sheet is following:
(1) graphite oxide: with 20g purity is that 99.5% 50 order graphite powders, 10g potassium peroxydisulfate and 10g phosphorus pentoxide add in 80 ℃ the concentrated sulfuric acid, stirs, and more than the cooling 6h, washing is to neutral, drying; In the concentrated sulfuric acid with 0 ℃ of dried sample adding, 230mL, add 60g potassium permanganate again, the temperature of mixture remains on below 20 ℃, in 35 ℃ oil bath, behind the maintenance 2h, slowly adds the 920mL deionized water then; Behind the 15min; Add 2.8L deionized water and 50mL mass concentration more successively and be 30% hydrogen peroxide solution; The mixture color becomes glassy yellow afterwards, and suction filtration while hot uses that 5L concentration is that 10% hydrochloric acid washs again, suction filtration, promptly obtains graphite oxide at 60 ℃ of vacuumize 48h;
(2) aluminium foil is immersed in the container of the suspension fill Barium Titanate nano-powder, then under the vacuum, 550 ℃ of heat treatment 8h obtain applying the aluminium net of barium titanate;
(3) graphene oxide that (1) is prepared is dissolved in the container that fills water, and forming molar concentration is the graphene oxide electrolyte of 1.5mol/L;
The aluminium net of the coating barium titanate that (4) (2) is made inserts in the electrolyte that (3) make as electrode, and on electrode, passes to the direct current of 1mA, and be 24h conduction time, obtains aluminium/barium titanate/Graphene electrodes sheet;
(5); Aluminium/barium titanate/graphene oxide electrode slice that step (4) is made places vacuum, 300 ℃ of following baking 24h, makes aluminium/barium titanate/Graphene electrodes sheet;
(6) aluminium/barium titanate that (5) is obtained/Graphene electrodes sheet carries out roller compaction to be handled;
(7) aluminium/barium titanate through compaction treatment that (6) is obtained/Graphene electrodes sheet is through direct voltage, and this voltage is 150% of final capacitor rated voltage, and be 1h conduction time; After intact, obtaining structure is the said composite solid electrolytic capacitor sheet of aluminium/alundum (Al-barium titanate/Graphene, and the conductivity of this electrode slice is 30000s/m; Wherein, the thickness of alundum (Al is greatly about 800nm.
Embodiment 3
The preparation method of composite solid electrolytic capacitor sheet is following:
(1) graphite oxide: with 20g purity is that 99.5% 50 order graphite powders, 10g potassium peroxydisulfate and 10g phosphorus pentoxide add in 80 ℃ the concentrated sulfuric acid, stirs, and more than the cooling 6h, washing is to neutral, drying; In the concentrated sulfuric acid with 0 ℃ of dried sample adding, 230mL, add 60g potassium permanganate again, the temperature of mixture remains on below 20 ℃, in 35 ℃ oil bath, behind the maintenance 2h, slowly adds the 920mL deionized water then; Behind the 15min; Add 2.8L deionized water and 50mL mass concentration more successively and be 30% hydrogen peroxide solution; The mixture color becomes glassy yellow afterwards, and suction filtration while hot uses that 5L concentration is that 10% hydrochloric acid washs again, suction filtration, promptly obtains graphite oxide at 60 ℃ of vacuumize 48h;
(2) aluminium foil is immersed in the container of the suspension fill Barium Titanate nano-powder, then under the vacuum, 600 ℃ of heat treatment 4h obtain applying the aluminium foil of barium titanate;
(3) graphene oxide that (1) is prepared is dissolved in the container that fills water, and forming molar concentration is the graphene oxide electrolyte of 3mol/L;
The aluminium foil of the coating barium titanate that (4) (2) is made inserts in the electrolyte that (3) make as electrode, and on electrode, passes to the direct current of 10mA, and be 1h conduction time, obtains aluminium/barium titanate/Graphene electrodes sheet;
(5); Aluminium/barium titanate/graphene oxide electrode slice that step (4) is made places vacuum, 80 ℃ of following baking 2h, makes aluminium/barium titanate/Graphene electrodes sheet;
(6) aluminium/barium titanate that (5) is obtained/Graphene electrodes sheet carries out roller compaction to be handled;
(7) aluminium/barium titanate through compaction treatment that (6) is obtained/Graphene electrodes sheet is through direct voltage, and this voltage is 180% of final capacitor rated voltage, and be 1.5h conduction time; After intact, obtaining structure is the said composite solid electrolytic capacitor sheet of aluminium/alundum (Al-barium titanate/Graphene, and the conductivity of this electrode slice is 40000s/m; Wherein, the thickness of alundum (Al is greatly about 830nm.
Embodiment 4
The preparation method of composite solid electrolytic capacitor sheet is following:
(1) graphite oxide: with 20g purity is that 99.5% 50 order graphite powders, 10g potassium peroxydisulfate and 10g phosphorus pentoxide add in 80 ℃ the concentrated sulfuric acid, stirs, and more than the cooling 6h, washing is to neutral, drying; In the concentrated sulfuric acid with 0 ℃ of dried sample adding, 230mL, add 60g potassium permanganate again, the temperature of mixture remains on below 20 ℃, in 35 ℃ oil bath, behind the maintenance 2h, slowly adds the 920mL deionized water then; Behind the 15min; Add 2.8L deionized water and 50mL mass concentration more successively and be 30% hydrogen peroxide solution; The mixture color becomes glassy yellow afterwards, and suction filtration while hot uses that 5L concentration is that 10% hydrochloric acid washs again, suction filtration, promptly obtains graphite oxide at 60 ℃ of vacuumize 48h;
(2) aluminium foil is immersed in the container of the suspension fill Barium Titanate nano-powder, then under the vacuum, 700 ℃ of heat treatment 0.5h obtain applying the aluminium foil of barium titanate;
(3) graphene oxide that (1) is prepared is dissolved in the container that fills water, and forming molar concentration is the graphene oxide electrolyte of 2mol/L;
The aluminium foil of the coating barium titanate that (4) (2) is made inserts in the electrolyte that (3) make as electrode, and on electrode, passes to the direct current of 2mA, and be 5h conduction time, obtains aluminium/barium titanate/Graphene electrodes sheet;
(5); Aluminium/barium titanate/graphene oxide electrode slice that step (4) is made places vacuum, 300 ℃ of following baking 12h, makes aluminium/barium titanate/Graphene electrodes sheet;
(6) aluminium/barium titanate that (5) is obtained/Graphene electrodes sheet carries out roller compaction to be handled;
(7) aluminium/barium titanate through compaction treatment that (6) is obtained/Graphene electrodes sheet is through direct voltage, and this voltage is 200% of final capacitor rated voltage, and be 2h conduction time; After intact, obtaining structure is the said composite solid electrolytic capacitor sheet of aluminium/alundum (Al-barium titanate/Graphene, and the conductivity of this electrode slice is 50000s/m; Wherein, the thickness of alundum (Al is greatly about 900nm.。
Should be understood that above-mentioned statement to preferred embodiment of the present invention is comparatively detailed, can not therefore think the restriction to scope of patent protection of the present invention, scope of patent protection of the present invention should be as the criterion with accompanying claims.
Claims (10)
1. a composite solid electrolytic capacitor sheet is characterized in that, the structure of this composite solid electrolytic capacitor sheet is aluminium/alundum (Al-barium titanate/Graphene.
2. composite solid electrolytic capacitor sheet according to claim 1 is characterized in that the thickness of said alundum (Al is 720～900nm.
3. composite solid electrolytic capacitor sheet according to claim 1 and 2 is characterized in that the conductivity of said composite solid electrolytic capacitor sheet is 15000～50000s/m.
4. the preparation method of a composite solid electrolytic capacitor sheet is characterized in that, comprises the steps:
S1, aluminium foil or aluminium net are immersed in the container of the suspension that fills Barium Titanate nano-powder, then under the vacuum in 500-700 ℃ of heat treatment 0.5-12h, obtain applying the aluminium foil or the aluminium net of barium titanate;
S2, with in the water-soluble solution of graphene oxide, make electrolyte;
In the electrolyte that the aluminium foil of S3, coating barium titanate that step S1 is made or aluminium net make as electrode inserting step S2, and on electrode, pass to the direct current of 1～10mA, be 1～24h conduction time, obtains aluminium/barium titanate/graphene oxide electrode slice;
S4, aluminium/barium titanate/graphene oxide electrode slice that step S3 is made place vacuum, 80～300 ℃ of following baking 2～24h, make aluminium/barium titanate/Graphene electrodes sheet;
S5, employing anode oxidation method; On aluminium/barium titanate/Graphene electrodes sheet that step S4 obtains, pass through direct voltage; After being 0.5～2h conduction time, making structure is the said composite solid electrolytic capacitor sheet of aluminium/alundum (Al-barium titanate/Graphene; Wherein, the magnitude of voltage of said direct voltage is 135～200% of a solid electrolytic capacitor load voltage value.
5. preparation method according to claim 4 is characterized in that, among the step S2, said graphite oxide adopts following step to make:
S21,2: 1: 1 graphite powder of mass ratio, potassium peroxydisulfate, phosphorus pentoxide are added in the concentrated sulfuric acid, stir, cool off subsequently, filter, and washing filter thing is to neutrality, drying, subsequent use;
In S22, the concentrated sulfuric acid, add potassium permanganate subsequently, stir 0 ℃ of the dried filter thing adding of step S21; Then add deionized water and mass concentration successively and be 30% hydrogen peroxide solution, mix and be mixed solution;
The mixed solution of S23, filtration step S22, and to use mass concentration be 10% salt acid elution, suction filtration, dry filter thing, obtains graphene oxide at last.
6. preparation method according to claim 5 is characterized in that, among the step S22, the quality of potassium permanganate is 3 times of graphite powder quality.
7. preparation method according to claim 5 is characterized in that, among the step S22, the volume number of said hydrogen peroxide solution is 50ml.
8. preparation method according to claim 4 is characterized in that, among the step S1, the molar concentration of said graphene oxide is 1～3mol/L.
9. preparation method according to claim 4 is characterized in that, among the step S5, the thickness of said alundum (Al is 720～900nm.
10. according to the arbitrary described preparation method of claim 4 to 9, it is characterized in that the conductivity of said composite solid electrolytic capacitor sheet is 15000-50000s/m.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108010725A (en) * | 2016-10-27 | 2018-05-08 | 株式会社东金 | Solid electrolyte capacitators |
| CN109942893A (en) * | 2019-04-03 | 2019-06-28 | 大连大学 | A kind of barium titanate-graphene oxide composite nano-grade sheet and preparation method thereof |
| CN109942997A (en) * | 2019-04-03 | 2019-06-28 | 大连大学 | A kind of graphene oxide-barium titanate dielectric composite film and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1438662A (en) * | 2003-03-05 | 2003-08-27 | 西安交通大学 | Technology for preparing ande foil of aluminium electrolytic capacitor |
| US20110090621A1 (en) * | 2009-05-21 | 2011-04-21 | Antony Chacko | Solid electrolytic capacitors with improved reliability |
-
2011
- 2011-05-31 CN CN201110144713.1A patent/CN102810401B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1438662A (en) * | 2003-03-05 | 2003-08-27 | 西安交通大学 | Technology for preparing ande foil of aluminium electrolytic capacitor |
| US20110090621A1 (en) * | 2009-05-21 | 2011-04-21 | Antony Chacko | Solid electrolytic capacitors with improved reliability |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108010725A (en) * | 2016-10-27 | 2018-05-08 | 株式会社东金 | Solid electrolyte capacitators |
| CN109942893A (en) * | 2019-04-03 | 2019-06-28 | 大连大学 | A kind of barium titanate-graphene oxide composite nano-grade sheet and preparation method thereof |
| CN109942997A (en) * | 2019-04-03 | 2019-06-28 | 大连大学 | A kind of graphene oxide-barium titanate dielectric composite film and preparation method thereof |
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