CN102842437B - The preparation method of polyvinylidene fluoride electrode material and ultracapacitor thereof - Google Patents
The preparation method of polyvinylidene fluoride electrode material and ultracapacitor thereof Download PDFInfo
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Abstract
The present invention relates to a kind of polyvinylidene fluoride button and winding type super capacitor and electrode material preparation method thereof.The method comprises: prepared by (1) Kynoar mixed liquor; (2) poly-vinylidene-fluoride composite film preparation; (3) to composite membrane activation processing, the polyvinylidene fluoride film electrode material of obtained button and winding type super capacitor.Take PVDF membrane material as the electrode of button and winding type super capacitor, be prepared into button ultracapacitor and winding type super capacitor.Electrode material prepared by the present invention, directly need not add active material, its cost is low, charge/discharge rates is fast, technique is simple; Preparation button and winding type super capacitor charge-discharge performance good, have extended cycle life; And electrode material can be processed as arbitrary size, its thickness is approximately 85 ~ 120 μm, meets the requirement of device miniaturization and expands its range of application.
Description
Technical field
The present invention relates to Novel super capacitor preparation and related electrode material, be specifically related to the preparation method of a kind of polyvinylidene fluoride button and winding type super capacitor and electrode material thereof.
Background technology
Ultracapacitor is a kind of novel energy storage device, and because it has, power is high, energy conversion efficiency is high, good cycle, therefore becomes one of focus in mechanism of new electrochemical power sources research.Ultracapacitor is a kind of environmental friendliness between traditional capacitor and rechargeable battery, the novel energy-storing that can not be substituted, energy saver; Compared with traditional capacitor, ultracapacitor had both had the feature of fast charging and discharging, had again the energy storage mechnism of electrochemical cell, but also had the features such as long circulation life, pollution-free, wider operating temperature range, consumption be large.Just because of These characteristics, the application of ultracapacitor in electric automobile, communication, consumption and the field such as recreation electronic, signal monitoring is more and more concerned, as communication apparatus and household electrical appliance etc. such as audio-video equipment, PDA, telephone set, facsimile machine and computers.Special needs to be pointed out is automobile-used ultracapacitor can meet automobile accelerating, start, climbing time high power requirements, to protect main storage battery system, this makes the development of ultracapacitor be thus lifted to a new height.The appearance of ultracapacitor, complies with the requirement of era development just, and it relates to multiple subjects such as material, the energy, chemistry, electronic device, becomes one of focus of cross discipline research, and ultracapacitor is expected to become novel green power supply in this century.
Current, the electrode material of ultracapacitor mainly contains absorbent charcoal material, conducting polymer and composite material thereof and transition metal oxide and combination electrode material thereof.Absorbent charcoal based ultracapacitor research history is longer, and current commercialized degree is higher, and technology is the most ripe, but its complex manufacturing, the production cycle is long, and specific capacity is low; It is reported, conducting polymer ultracapacitor can demonstrate very high power density, but their specific capacity but than carbon/carbon supercapacitor and metal oxide ultracapacitor much lower; Although metal oxide or hydrated metal oxide (as ruthenium-oxide) and carbon nano-tube can produce great energy density and power density, but the ultracapacitor cost manufactured with these materials is higher than other material a lot.Therefore, exploitation have low-cost advantage, properties all has the electrode material being used as button and winding type super capacitor improved more greatly to be necessary.
Summary of the invention
Object of the present invention is exactly the shortcoming and defect existed to overcome existing ultracapacitor electrode used therein material, provides that preparation technology is simple, raw material is easy to get, the preparation method of polyvinylidene fluoride electrode material with low cost; Electrode material prepared by the method directly need not add active material; And electrode material can be processed as arbitrary size, its thickness is approximately 85 ~ 120 μm, meets the requirement of device miniaturization and expands its range of application.Button prepared by the present invention and its charge-discharge performance of winding type super capacitor good, have extended cycle life; And there is very high power density and energy density.
For realizing the object of the invention, the present invention adopts following technical scheme.
The preparation method of polyvinylidene fluoride button provided by the invention and winding type super capacitor electrode material, is characterized in that comprising following processing step:
(1) Kynoar mixed liquor preparation
By polyvinylidene fluoride with after mixing by mass percentage with the additive that polyvinylidene fluoride can produce electrical conductive activities material, dry and be prepared into mixed-powder, then with organic solvent, they are dissolved to obtain mixed liquor;
(2) poly-vinylidene-fluoride composite film preparation
To polyvinylidene fluoride be dissolved with in step (1) and be coated on substrate with its mixed liquor that can produce the additive of electrical conductive activities material, or be poured directly on substrate, then dry and be prepared into poly-vinylidene-fluoride composite film;
(3) activation processing is carried out to poly-vinylidene-fluoride composite film and obtain electrode material
By physical and chemical process, activation processing is carried out to the composite membrane of step (2) gained, thus the electrode material of obtained button and winding type super capacitor.
In such scheme, the described additive that can produce electrical conductive activities material with polyvinylidene fluoride is selected from potash salt or potassium hydroxide.
In such scheme, described polyvinylidene fluoride and it can produce electrical conductive activities material is 99%:1% ~ 50%:50% with the mass percent of additive;
In such scheme, described additive is potash, and polyvinylidene fluoride and its mass percent are 99%:1% ~ 50%:50%; Described additive is potassium hydroxide, and polyvinylidene fluoride and its mass percent are 99%:1% ~ 50%:50%.
In such scheme, described organic solvent to dissolve Kynoar, DMF (DMF) stable relative to additive again or dimethyl sulfoxide (DMSO) (NMP) or 1-METHYLPYRROLIDONE (DMSO).
In such scheme, described substrate is graphite paper, or conductive fibre fabric, or nickel foam, or aluminium foil, or glass.
In such scheme, the described activation processing to poly-vinylidene-fluoride composite film is: the poly-vinylidene-fluoride composite film prepared is distinguished heat treatment 1 ~ 120 minute at 80 ~ 250 DEG C; Maybe the poly-vinylidene-fluoride composite film prepared is soaked 1 ~ 600 minute in potassium hydroxide solution, then heat treatment 1 ~ 120 minute at 80 ~ 250 DEG C.
The preparation method of a kind of polyvinylidene fluoride button of the present invention ultracapacitor, comprises following concrete steps:
(1) Kynoar mixed liquor preparation
By polyvinylidene fluoride with after mixing by mass percentage with the additive that polyvinylidene fluoride can produce electrical conductive activities material, dry and be prepared into mixed-powder, then with organic solvent, they are dissolved to obtain mixed liquor;
(2) poly-vinylidene-fluoride composite film preparation
To polyvinylidene fluoride be dissolved with in step (1) and be coated on substrate with its additives mixed solution that can produce electrical conductive activities material, or be poured on substrate, then dry and be prepared into poly-vinylidene-fluoride composite film;
(3) activation processing is carried out to poly-vinylidene-fluoride composite film and obtain electrode material
Carry out activation processing by the poly-vinylidene-fluoride composite film of physical and chemical process to step (2) gained, thus obtain the electrode material of button ultracapacitor;
(4) button ultracapacitor is prepared
Take poly-vinylidene-fluoride composite film as electrode material, it is cut into a certain size and shape, by electrode material and barrier film, be positioned in button cell shell negative cover according to the order of electrode/barrier film/electrode, and inject electrolyte in battery case negative cover, then battery case positive cover is buckled in negative cover; Button device is encapsulated on cell package machine, i.e. obtained button ultracapacitor.
The button ultracapacitor that the present invention is prepared according to above-mentioned preparation method, it is characterized in that with poly-vinylidene-fluoride composite film electrode material for electrode; The electrolyte adopting the flexible substrate graphite paper of conduction, nickel foam, aluminium foil or conductive fibre fabric to do to inject in collector, its battery case negative cover is inorganic electrolyte liquid or organic electrolyte.
The preparation method of a kind of polyvinylidene fluoride winding type super capacitor of the present invention, comprises following concrete steps:
(1) Kynoar mixed liquor preparation
By polyvinylidene fluoride with after mixing by mass percentage with the additive that polyvinylidene fluoride can produce electrical conductive activities material, dry and be prepared into mixed-powder, then with organic solvent, they are dissolved to obtain mixed liquor;
(2) poly-vinylidene-fluoride composite film preparation
To polyvinylidene fluoride be dissolved with in step (1) and be coated on substrate with its additives mixed solution that can produce electrical conductive activities material, or be poured on substrate, then dry and be prepared into poly-vinylidene-fluoride composite film;
(3) activation processing is carried out to poly-vinylidene-fluoride composite film and obtain electrode material
Carry out activation processing by the poly-vinylidene-fluoride composite film of physical and chemical process to step (2) gained, thus obtain the electrode material of winding type super capacitor;
(4) acquisition of winding type super capacitor blank product
With poly-vinylidene-fluoride composite film electrode material for electrode, it is cut into elongate in shape, by electrode material and barrier film, be positioned between two post-like conductive metal rods according to the order of electrode/barrier film/electrode, reel, make electrode material press close to post-like conductive metal rod closely, obtain blank product;
(5) winding type super capacitor is prepared
By the blank product obtained that reels, be positioned over the interior encapsulation of the encapsulating shell with upper and lower inner cap; , before encapsulation, inject inorganic electrolyte liquid or organic electrolyte; I.e. obtained winding type super capacitor.
The present invention is in order to improve capacity of super capacitor, reduce internal resistance, produce more active materials, therefore, the compound film electrode material prepared is passed through physical and chemical process, or heat treatment certain hour at a certain temperature, then the composite membrane after heat treatment is soaked certain hour in potassium hydroxide solution; Or by utilizing vapour deposition method or sputtering vapor deposition film method deposit metallic material on prepared poly-vinylidene-fluoride composite film; Or utilize electro-plating method deposit metallic material on poly-vinylidene-fluoride composite film, thus the polyvinylidene fluoride membrane electrode material of obtained button and winding type super capacitor.
The present invention makes poly-vinylidene-fluoride composite film produce electrical conductive activities material and is conducive to increasing the loose structure of electrode specific surface area and ion transfer, therefore the compound film electrode material prepared is distinguished heat treatment 1 ~ 120 minute at 80 ~ 250 DEG C; Maybe the poly-vinylidene-fluoride composite film prepared is soaked 1 ~ 600 minute in potassium hydroxide solution, then heat treatment 1 ~ 120 minute at 80 ~ 250 DEG C.
Polyvinylidene fluoride film electrode material prepared by preparation method of the present invention, this electrode material comprises polyvinylidene fluoride and can produce the additive of electrical conductive activities material with polyvinylidene fluoride; Described electrode material size is controlled, and thickness is between 50-150 micron, and its electrochemical AC impedance is 5 ohm.
The button that the present invention makes with polyvinylidene fluoride compound film electrode material and winding type super capacitor, comprise electrode, collector, barrier film, electrolyte; Be characterized in directly with the electrode that polyvinylidene fluoride composite film material is button and winding type super capacitor; Described collector adopts the flexible substrate graphite paper or nickel foam or aluminium foil or conductive fibre fabric that conduct electricity; Also glass can be adopted to make substrate; Described barrier film is the one in pi or polypropylene fibre; Described electrolyte is inorganic electrolyte liquid or organic electrolyte.
The feature that the preparation method of polyvinylidene fluoride electrode material of the present invention and ultracapacitor thereof has and Advantageous Effects:
The preparation method of the electrode material of button provided by the present invention and winding type super capacitor, its main advantage be directly with polyvinylidene fluoride composite film material for electrode material; By physical and chemical process, activation processing is carried out to prepared membrane material, Kynoar itself is made to produce electrical conductive activities material, thus reduce the contact resistance of Kynoar and active material, allow electrical conductive activities material more be evenly distributed in Kynoar.Utilize heating treatment process to make polyvinylidene fluoride composite film material have loose structure simultaneously, so just can increase the specific area of electrode material more simply, improve ultracapacitor electric capacity.Button prepared by the present invention and winding type super capacitor electrode material not only have good flexibility, its thickness also little; The button prepared with this electrode material and winding type super capacitor not only have very high power density and energy density, have extended cycle life; And cost is low, technique simple, be suitable for large-scale production and application.
Accompanying drawing explanation
The cyclic voltammetry result of the button ultracapacitor that Fig. 1 the present invention prepares by embodiment 1
The constant current charge-discharge test result of the button ultracapacitor that Fig. 2 the present invention prepares by embodiment 1;
The cyclic voltammetry result of the winding type super capacitor that Fig. 3 the present invention prepares by embodiment 4;
The constant current charge-discharge test result of the winding type super capacitor that Fig. 4 the present invention prepares by embodiment 4.
Embodiment
The present invention is described in further detail to use specific embodiment and design sketch below, but be not meant to be any restriction to scope.
In the embodiment of the present invention, electronic balance used is the FA-1104N type electronic analytical balance that upper Nereid's tech device Technology Co., Ltd. produces;
Thermostatic drying chamber used is the KXH101-2A type thermostatic drying chamber that Chinese Shanghai Ke Xi laboratory apparatus factory produces;
PVDF used is that in Chengdu, fluorine chemical Co., Ltd produces;
Test result electrochemical workstation used is the CS3500 chem workstation of Wuhan Gastec.
Embodiment 1:
With electronic balance by Kynoar and K
2cO
3be the ratio weighing of 73%:27% by mass percentage, the raw material taken mixed, dries and make powder, then as solvent, the powder mixed fully is dissolved with 10mL DMF, form mixed solution; By mixed solution even application on graphite paper substrate, and to be placed in thermostatic drying chamber 15 hours, after taking-up, graphite paper to form one deck poly-vinylidene-fluoride composite film.By poly-vinylidene-fluoride composite film heat treatment 60 minutes at 220 DEG C of temperature, composite membrane after heat treatment is soaked 30 minutes in saturated potassium hydroxide solution, at 200 DEG C, carry out the activation processing of 60 minutes again, namely prepare the polyvinylidene fluoride membrane electrode material of ultracapacitor.By polyvinylidene fluoride film electrode material, be processed into a certain size disk, barrier film is cut into the shape similar to membrane electrode material, and size is a bit larger tham membrane electrode material; Then disk is packaged in button cell shell negative cover by the form of film/barrier film/film, in encapsulation forward direction battery case negative cover, injects 6mol/L potassium hydroxide solution; Again battery case positive cover is buckled in negative cover; Button device is encapsulated on cell package machine, i.e. obtained polyvinylidene fluoride button ultracapacitor.With electrochemical workstation test button ultracapacitor cyclic voltammetric and constant current charge-discharge, its test result is shown in that, shown in Fig. 1, Fig. 2, electric capacity is about 45mF/cm as can be seen from Figure 2
2.
Embodiment 2:
With electronic balance by Kynoar and K
2cO
3be the ratio weighing of 99%:1% by mass percentage, the raw material taken mixed, dries and make powder, then as solvent, the powder mixed fully is dissolved with 10mL DMF, form mixed solution; By mixed solution even application on conductive fibre fabric substrate, and to be placed in thermostatic drying chamber 15 hours, after taking-up, conductive fibre fabric to form one deck poly-vinylidene-fluoride composite film.By poly-vinylidene-fluoride composite film heat treatment 1 minute at 250 DEG C of temperature, composite membrane after heat treatment is soaked 1 minute in saturated potassium hydroxide solution, at 250 DEG C, carry out the activation processing of 1 minute again, namely prepare the polyvinylidene fluoride membrane electrode material of ultracapacitor.By polyvinylidene fluoride film electrode material, be processed into a certain size disk, barrier film is cut into the shape similar to membrane electrode material, and size is a bit larger tham membrane electrode material; Then disk is packaged in button cell shell negative cover by the form of film/barrier film/film, in encapsulation forward direction battery case negative cover, injects 6mol/L potassium hydroxide solution; Again battery case positive cover is buckled in negative cover; Button device is encapsulated on cell package machine, i.e. obtained polyvinylidene fluoride button ultracapacitor.
Embodiment 3:
With electronic balance by Kynoar and K
2cO
3be the ratio weighing of 50%:50% by mass percentage, the raw material taken mixed, dries and make powder, then as solvent, the powder mixed fully is dissolved with 10mLNMP, form mixed solution; Mixed solution is evenly poured in glass substrate, and is placed in thermostatic drying chamber 15 hours, after taking-up, glass forms one deck poly-vinylidene-fluoride composite film.By poly-vinylidene-fluoride composite film heat treatment 120 minutes at 80 DEG C of temperature, composite membrane after heat treatment is soaked 600 minutes in saturated potassium hydroxide solution, at 80 DEG C, carry out the activation processing of 120 minutes again, namely prepare the polyvinylidene fluoride membrane electrode material of ultracapacitor.By polyvinylidene fluoride film electrode material, be processed into a certain size disk, barrier film is cut into the shape similar to membrane electrode material, and size is a bit larger tham membrane electrode material; Then disk is packaged in button cell shell negative cover by the form of film/barrier film/film, in encapsulation forward direction battery case negative cover, injects 6mol/L potassium hydroxide solution; Again battery case positive cover is buckled in negative cover; Button device is encapsulated on cell package machine, i.e. obtained polyvinylidene fluoride button ultracapacitor.
Embodiment 4:
With electronic balance by Kynoar and K
2cO
3be the ratio weighing of 73%:27% by mass percentage, the raw material taken mixed, dries and make powder, then as solvent, the powder mixed fully is dissolved with 10mLNMP, form mixed solution; By mixed solution even application on nickel foam substrate, and to be placed in thermostatic drying chamber 15 hours, after taking-up, nickel foam to form one deck poly-vinylidene-fluoride composite film.By poly-vinylidene-fluoride composite film heat treatment 60 minutes at 220 DEG C of temperature, composite membrane after heat treatment is soaked 30 minutes in saturated potassium hydroxide solution, at 200 DEG C, carry out the activation processing of 60 minutes again, namely prepare the polyvinylidene fluoride membrane electrode material of ultracapacitor.By polyvinylidene fluoride film electrode material, cut into elongate in shape, by electrode material and barrier film, be positioned between two post-like conductive metal rods according to the order of electrode/barrier film/electrode, reel, make electrode material press close to post-like conductive metal rod closely, obtain blank product; By the blank product that obtains of reeling, be positioned over there is upper and lower inner cap encapsulating shell in, inject 6mol/L potassium hydroxide solution, encapsulation i.e. obtained winding type super capacitor.With electrochemical workstation test winding type super capacitor cyclic voltammetric and constant current charge-discharge, test result is shown in shown in Fig. 3, Fig. 4, and its electric capacity is about 37.5mF/cm as can be seen from Figure 4
2.
Embodiment 5:
With electronic balance by Kynoar and K
2cO
3be the ratio weighing of 99%:1% by mass percentage, the raw material taken mixed, dries and make powder, then as solvent, the powder mixed fully is dissolved with 10mL DMSO, form mixed solution; Mixed solution is evenly poured in glass substrate, and is placed in thermostatic drying chamber 15 hours, after taking-up, glass forms one deck poly-vinylidene-fluoride composite film.By poly-vinylidene-fluoride composite film heat treatment 1 minute at 250 DEG C of temperature, composite membrane after heat treatment is soaked 1 minute in saturated potassium hydroxide solution, at 250 DEG C, carry out the activation processing of 1 minute again, namely prepare the polyvinylidene fluoride membrane electrode material of ultracapacitor.By polyvinylidene fluoride film electrode material, cut into elongate in shape, by electrode material and barrier film, be positioned between two post-like conductive metal rods according to the order of electrode/barrier film/electrode, reel, make electrode material press close to post-like conductive metal rod closely, obtain blank product; By the blank product that obtains of reeling, be positioned over there is upper and lower inner cap encapsulating shell in, inject 6mol/L potassium hydroxide solution, encapsulation i.e. obtained winding type super capacitor.
Embodiment 6:
With electronic balance by Kynoar and K
2cO
3be the ratio weighing of 50%:50% by mass percentage, the raw material taken mixed, dries and make powder, then as solvent, the powder mixed fully is dissolved with 10mL DMSO, form mixed solution; Mixing material is coated in aluminum substrates equably, and is placed in thermostatic drying chamber 15 hours, after taking-up, aluminium foil forms one deck poly-vinylidene-fluoride composite film.By poly-vinylidene-fluoride composite film heat treatment 120 minutes at 80 DEG C of temperature, composite membrane after heat treatment is soaked 600 minutes in saturated potassium hydroxide solution, at 80 DEG C, carry out the activation processing of 120 minutes again, namely prepare the polyvinylidene fluoride membrane electrode material of ultracapacitor.By polyvinylidene fluoride film electrode material, cut into elongate in shape, by electrode material and barrier film, be positioned between two post-like conductive metal rods according to the order of electrode/barrier film/electrode, reel, make electrode material press close to post-like conductive metal rod closely, obtain blank product; By the blank product that obtains of reeling, be positioned over there is upper and lower inner cap encapsulating shell in, inject 6mol/L potassium hydroxide solution, encapsulation i.e. obtained winding type super capacitor.
Claims (8)
1. a preparation method for polyvinylidene fluoride button and winding type super capacitor electrode material, is characterized in that comprising following processing step:
(1) Kynoar mixed liquor preparation
After the ratio of polyvinylidene fluoride and the additive 99%:1% ~ 50%:50% by mass percentage that can produce electrical conductive activities material with polyvinylidene fluoride is mixed, oven dry is prepared into mixed-powder, then with organic solvent, they is dissolved to obtain mixed liquor;
(2) poly-vinylidene-fluoride composite film preparation
To polyvinylidene fluoride be dissolved with in step (1) and be coated on substrate with its additives mixed liquid that can produce electrical conductive activities material, or be poured directly on substrate, then dry and be prepared into poly-vinylidene-fluoride composite film;
(3) activation processing is carried out to poly-vinylidene-fluoride composite film and obtain electrode material
By physical and chemical process, activation processing is carried out to the poly-vinylidene-fluoride composite film of step (2) gained, the poly-vinylidene-fluoride composite film being about to prepare soaks 1 ~ 600 minute in potassium hydroxide solution, then heat treatment 1 ~ 120 minute at 80 ~ 250 DEG C; I.e. obtained polyvinylidene fluoride button and winding type super capacitor electrode material.
2. the preparation method of polyvinylidene fluoride button and winding type super capacitor electrode material according to claim 1, is characterized in that the described additive that can produce electrical conductive activities material with polyvinylidene fluoride is selected from potash salt or potassium hydroxide.
3. the preparation method of polyvinylidene fluoride button and winding type super capacitor electrode material according to claim 1 or 2, it is characterized in that described additive is potash, polyvinylidene fluoride and its mass percent are 99%:1% ~ 50%:50%; Described additive is potassium hydroxide, and polyvinylidene fluoride and its mass percent are 99%:1% ~ 50%:50%.
4. the preparation method of polyvinylidene fluoride button and winding type super capacitor electrode material according to claim 1, it is characterized in that described organic solvent to dissolve Kynoar, DMF (DMF) stable relative to additive again or dimethyl sulfoxide (DMSO) (DMSO) or 1-METHYLPYRROLIDONE (NMP).
5. the preparation method of polyvinylidene fluoride button and winding type super capacitor electrode material according to claim 1, is characterized in that described substrate is graphite paper, or conductive fibre fabric, or glass.
6. the preparation method of a polyvinylidene fluoride button ultracapacitor, it is characterized in that the polyvinylidene fluoride button obtained by any one of claim 1-5 preparation method and winding type super capacitor electrode material, by this electrode material and barrier film, be positioned in button cell shell negative cover according to the order of electrode/barrier film/electrode, and inject electrolyte in battery case negative cover, then battery case positive cover is buckled in negative cover; Button device is encapsulated on cell package machine, i.e. obtained polyvinylidene fluoride button ultracapacitor.
7. the polyvinylidene fluoride button ultracapacitor obtained by preparation method according to claim 6, it is characterized in that with poly-vinylidene-fluoride composite film electrode material for electrode; The electrolyte adopting the flexible substrate graphite paper of conduction or conductive fibre fabric to do to inject in collector, its battery case negative cover is inorganic electrolyte liquid or organic electrolyte.
8. the preparation method of a polyvinylidene fluoride winding type super capacitor, it is characterized in that the polyvinylidene fluoride button obtained by any one of claim 1-5 preparation method and winding type super capacitor electrode material, by this electrode material and barrier film, be positioned between two post-like conductive metal rods according to the order of electrode/barrier film/electrode, reel, make electrode material press close to post-like conductive metal rod closely, obtain blank product; By the blank product obtained that reels, be positioned over the interior encapsulation of the encapsulating shell with upper and lower inner cap; Inorganic electrolyte liquid or organic electrolyte is injected before encapsulation; I.e. obtained polyvinylidene fluoride winding type super capacitor.
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| CN201210310195.0A CN102842437B (en) | 2012-08-28 | 2012-08-28 | The preparation method of polyvinylidene fluoride electrode material and ultracapacitor thereof |
| US14/425,312 US9734955B2 (en) | 2012-08-28 | 2013-01-14 | Electrode material, preparation method thereof and supercapacitor based thereof |
| PCT/CN2013/070430 WO2014032404A1 (en) | 2012-08-28 | 2013-01-14 | Electrode material and preparation method thereof as well as super-capacitor based on the same |
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