CN102810400A - Composite solid electrolytic capacitor electrode plate and manufacturing method thereof - Google Patents
Composite solid electrolytic capacitor electrode plate and manufacturing method thereof Download PDFInfo
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Abstract
The invention belongs to the field of capacitor electrodes and discloses a composite solid electrolytic capacitor electrode plate and a manufacturing method thereof. The composite solid electrolytic capacitor electrode plate is aluminum/aluminum oxide-titanium dioxide/graphene. By the composite solid electrolytic capacitor electrode plate, the traditional conductive polymer electrolyte material is replaced by the graphene, so that the composite solid electrolytic capacitor electrode plate has excellent stability and consistency; and moreover, the electrode plate is simple in manufacturing process, low in cost and suitable for 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-titanium dioxide/Graphene, the conductivity of this composite solid electrolytic capacitor sheet is 55000～100000s/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 immersed fill in the container of titanium tetrachloride solution, repeated multiple times places air with said aluminium foil or aluminium net then, makes titanium tetrachloride fully and water reacted titanium dioxide, makes the titanium deoxid film layer at aluminium foil or aluminium net surface subsequently;
S2, with in the water-soluble solution of graphene oxide, add carbonic hydroammonium or urea subsequently, make electrolyte; Wherein, the molar concentration of graphene oxide is 1～3mol/L;
The aluminium foil of S3, titanium dioxide coated that step S1 is made or aluminium net immerse 1～72h in the electrolyte that S2 makes, and toast 1～72h in the vacuum environment subsequently, obtain aluminium/titanium dioxide/graphene oxide electrode slice;
S4, aluminium/titanium dioxide/graphene oxide electrode slice that step S3 is made place atmosphere of inert gases under 100～1000 ℃, to feed hydrazine steam, carry out redox reaction, after having reacted, make aluminium/titanium dioxide/Graphene electrodes sheet;
S5, employing anode oxidation method; On aluminium/titanium dioxide/Graphene electrodes sheet that step S4 obtains, pass through direct voltage; After being 0.5～2h conduction time; Alumina changes into alundum (Al, and making structure is the said composite solid electrolytic capacitor sheet of aluminium/alundum (Al-titanium dioxide/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-titanium dioxide/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-titanium dioxide/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-titanium dioxide/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-titanium dioxide/Graphene, the conductivity of this composite solid electrolytic capacitor sheet is 5500～100000s/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 immersed fill in the container of titanium tetrachloride solution, repeated multiple times places air with said aluminium foil or aluminium net then, makes titanium tetrachloride fully and water reacted titanium dioxide, makes the titanium deoxid film layer at aluminium foil or aluminium net surface subsequently;
S2, with in the water-soluble solution of graphene oxide, add the carbonic hydroammonium or the urea of the effect play reducing agent subsequently, make electrolyte; Wherein, the molar concentration of graphene oxide is 1～3mol/L;
The aluminium foil of S3, titanium dioxide coated that step S1 is made or aluminium net immerse 1～72h in the electrolyte that S2 makes, and toast 1～72h in the vacuum environment subsequently, obtain aluminium/titanium dioxide/graphene oxide electrode slice;
S4, aluminium/titanium dioxide/graphene oxide electrode slice that step S3 is made place atmosphere of inert gases under 100～1000 ℃, to feed hydrazine steam, carry out redox reaction, after having reacted, make aluminium/titanium dioxide/Graphene electrodes sheet;
S5, employing anode oxidation method; On aluminium/titanium dioxide/Graphene electrodes sheet that step S4 obtains, pass through direct voltage; After being 0.5～2h conduction time; Aluminaization obtains alundum (Al, and making structure is the said composite solid electrolytic capacitor sheet of aluminium/alundum (Al-titanium dioxide/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) the aluminium foil immersion is filled in the container of titanium tetrachloride solution, repeated multiple times places air with said aluminium foil then, makes the abundant and water reacted titanium dioxide of titanium tetrachloride, makes the titanium deoxid film layer at aluminium foil surface subsequently;
(3) graphene oxide that (1) is prepared is dissolved in the water, and adds carbonic hydroammonium then, and forming molar concentration is the graphene oxide electrolyte of 1mol/L;
The aluminium foil of the titanium dioxide coated that (4) (2) is made immerses 1h in the electrolyte that (2) make, and toasts 24h in the vacuum environment subsequently, obtains aluminium/titanium dioxide/graphene oxide electrode slice;
(5) aluminium/titanium dioxide that (4) is made/graphene oxide electrode slice places atmosphere of inert gases under 100 ℃, to feed hydrazine steam, carries out redox reaction, after having reacted, makes aluminium/titanium dioxide/Graphene electrodes sheet;
(6) aluminium/titanium dioxide that (5) is obtained/Graphene electrodes sheet carries out roller compaction to be handled;
(7) aluminium/titanium dioxide 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-titanium dioxide/Graphene, and the conductivity of this electrode slice is 100000s/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) immersion of aluminium net is filled in the container of titanium tetrachloride solution, repeated multiple times places air with said aluminium net then, makes the abundant and water reacted titanium dioxide of titanium tetrachloride, makes the titanium deoxid film layer at the aluminium net surface subsequently;
(3) graphene oxide that (1) is prepared is dissolved in the water, and adds urea then, and forming molar concentration is the graphene oxide electrolyte of 1mol/L;
The aluminium net of the titanium dioxide coated that (4) (2) is made immerses 24h in the electrolyte that (2) make, and toasts 36h in the vacuum environment subsequently, obtains aluminium/titanium dioxide/graphene oxide electrode slice;
(5) aluminium/titanium dioxide that (4) is made/graphene oxide electrode slice places atmosphere of inert gases under 1000 ℃, to feed hydrazine steam, carries out redox reaction, after having reacted, makes aluminium/titanium dioxide/Graphene electrodes sheet;
(6) aluminium/titanium dioxide that (5) is obtained/Graphene electrodes sheet carries out roller compaction to be handled;
(7) aluminium/titanium dioxide 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-titanium dioxide/Graphene, and the conductivity of this electrode slice is 75000s/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) the aluminium foil immersion is filled in the container of titanium tetrachloride solution, repeated multiple times places air with said aluminium foil then, makes the abundant and water reacted titanium dioxide of titanium tetrachloride, makes the titanium deoxid film layer at aluminium foil surface subsequently;
(3) graphene oxide that (1) is prepared is dissolved in the water, and adds urea then, and forming molar concentration is the graphene oxide electrolyte of 2mol/L;
The aluminium foil of the titanium dioxide coated that (4) (2) is made immerses 36h in the electrolyte that (2) make, and toasts 72h in the vacuum environment subsequently, obtains aluminium/titanium dioxide/graphene oxide electrode slice;
(5) aluminium/titanium dioxide that (4) is made/graphene oxide electrode slice places atmosphere of inert gases under 500 ℃, to feed hydrazine steam, carries out redox reaction, after having reacted, makes aluminium/titanium dioxide/Graphene electrodes sheet;
(6) aluminium/titanium dioxide that (5) is obtained/Graphene electrodes sheet carries out roller compaction to be handled;
(7) aluminium/titanium dioxide 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-titanium dioxide/Graphene, and the conductivity of this electrode slice is 65000s/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) the aluminium foil immersion is filled in the container of titanium tetrachloride solution, repeated multiple times places air with said aluminium foil then, makes the abundant and water reacted titanium dioxide of titanium tetrachloride, makes the titanium deoxid film layer at aluminium foil surface subsequently;
(3) graphene oxide that (1) is prepared is dissolved in the water, and adds carbonic hydroammonium then, and forming molar concentration is the graphene oxide electrolyte of 3mol/L;
The aluminium foil of the titanium dioxide coated that (4) (2) is made immerses 72h in the electrolyte that (2) make, and toasts 1h in the vacuum environment subsequently, obtains aluminium/titanium dioxide/graphene oxide electrode slice;
(5) aluminium/titanium dioxide that (4) is made/graphene oxide electrode slice places atmosphere of inert gases under 800 ℃, to feed hydrazine steam, carries out redox reaction, after having reacted, makes aluminium/titanium dioxide/Graphene electrodes sheet;
(6) aluminium/titanium dioxide that (5) is obtained/Graphene electrodes sheet carries out roller compaction to be handled;
(7) aluminium/titanium dioxide 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-titanium dioxide/Graphene, and the conductivity of this electrode slice is 550000s/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-titanium dioxide/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 55000～100000s/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 immersed fill in the container of titanium tetrachloride solution, repeated multiple times places air with said aluminium foil or aluminium net then, makes the titanium deoxid film layer at aluminium foil or aluminium net surface subsequently;
S2, with in the water-soluble solution of graphene oxide, add carbonic hydroammonium or urea subsequently, make electrolyte;
The aluminium foil of S3, titanium dioxide coated that step S1 is made or aluminium net immerse 1～72h in the electrolyte that S2 makes, and toast 1～72h in the vacuum environment subsequently, obtain aluminium/titanium dioxide/graphene oxide electrode slice;
S4, aluminium/titanium dioxide/graphene oxide electrode slice that step S3 is made place 100～1000 ℃ of following and feeding hydrazine steam, carry out redox reaction, after having reacted, make aluminium/titanium dioxide/Graphene electrodes sheet;
S5, employing anode oxidation method; On aluminium/titanium dioxide/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-titanium dioxide/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 S2, in the said electrolyte, the molar concentration of 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 55000～100000s/m.
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| CN105174381A (en) * | 2015-09-21 | 2015-12-23 | 清华大学 | Method for making Ti-graphene electrode through oxidized graphene in assistive mode |
| CN107794556A (en) * | 2017-10-09 | 2018-03-13 | 上海电力学院 | A kind of surface modifying method of used in proton exchange membrane fuel cell aluminium alloy bipolar plates |
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