CN107154313B - A method of preparing ultracapacitor based on coating transfer techniques - Google Patents
A method of preparing ultracapacitor based on coating transfer techniques Download PDFInfo
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- CN107154313B CN107154313B CN201610836864.6A CN201610836864A CN107154313B CN 107154313 B CN107154313 B CN 107154313B CN 201610836864 A CN201610836864 A CN 201610836864A CN 107154313 B CN107154313 B CN 107154313B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/13—Energy storage using capacitors
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Abstract
The invention discloses a kind of methods preparing ultracapacitor based on coating transfer techniques；By the binder and active material mixed slurry of preparation, electrode plates are prepared into based on coating arts techniques, are then transferred to foamed nickel current collector by pressure transfer techniques, in conjunction with diaphragm and electrolyte or ionic liquid, are assembled into ultracapacitor；The coating transfer techniques preparation method of the ultracapacitor rapidly and efficiently, have excellent performance, be reproducible, is at low cost, be with a wide range of applications.
Description
Technical field
The present invention relates to a kind of methods prepared by ultracapacitor, belong to ultracapacitor manufacturing technology field.
Background technology
Ultracapacitor is a kind of a kind of novel green energy storage device between plate condenser and battery, with tradition
Capacitor compared with battery, ultracapacitor has that power density and energy density are high, have extended cycle life, operational temperature model
Enclose the advantages that wide, safe and reliable, at low cost.Especially ultracapacitor can carry out the fast charging and discharging of high current density, such as
Identical energy is stored, several hours may be needed for battery, and ultracapacitor only needs several seconds time.
Thus ultracapacitor is widely used in energy storage, electric vehicle, mobile communication equipment, health care, military equipment, industry life
Produce equipment etc..
In the existing technology for preparing ultracapacitor, knife coating is a kind of common methods for preparing electrode of super capacitor.
Collector is generally done using metal foil in knife coating, then the mixture paste that active material and binder are formed by a certain percentage
It scratches in metal foil, preformed electrode is formed after dry.However there is active material distributions for the electrode prepared of this method
Uneven, active material quality is difficult to control and has the shortcomings that certain pollution, limits carrying for performance of the supercapacitor
It is high.In addition, if by metal foil directly as collector, the specific capacity of untreated metal foil meeting restricted activity substance is led
Sending a telegraph pole cannot be infiltrated by electrolyte well, and effective rate of utilization is low.Based on this, the present invention for the problems of above-mentioned,
A kind of method that coating transfer techniques prepare ultracapacitor is proposed, above-mentioned problem has not only been well solved, and
And also adapt to serialization, large-scale production process process.
Invention content
The method of the present invention for preparing ultracapacitor based on coating transfer techniques, is based on binder and active material
The slurry of preparation is prepared into electrode plates by coating arts techniques, then cuts into the pole piece to be transferred of suitable dimension, and leads to
Excess pressure is transferred in the foamed nickel current collector of identical size, is assembled into ultracapacitor.
The method of the present invention for preparing ultracapacitor based on coating transfer techniques, the binder is polyvinylidene fluoride
Alkene (PVDF), it is first that PVDF powder is dry in 80 degree to 100 degree of baking oven in technology of preparing to claim after 4 hours to 6 hours
Amount is then dissolved in the PVDF solution for forming that mass concentration is 2% to 5% in N-Methyl pyrrolidone (NMP), under air-proof condition
Magnetic agitation 8 hours to 10 hours, keeps its fully dispersed.
The method of the present invention for preparing ultracapacitor based on coating transfer techniques, the active material are activity
Charcoal, lithium titanate, graphene, carbon nanotube, specific surface area 1500m2/ g to 3000m2Between/g, active material is set using preceding
Processing is dried in 80 degree to 100 degree of baking oven, forms floccule after avoiding binder PVDF from meeting water, influences caking property
Energy.
The method of the present invention for preparing ultracapacitor based on coating transfer techniques, the slurry of the preparation will be active
PVDF solution is added in substance, and it is 5 to form mass ratio with PVDF:1 to 12:1 mixed solution, then magnetic agitation 2 under room temperature
Hour was by 5 hours.
The method of the present invention for preparing ultracapacitor based on coating transfer techniques, the coating are using blade coating skill
Art or slot coating technique, in metal aluminum foil or copper foil or polyethylene terephthalate (PET) or poly- naphthalenedicarboxylic acid second two
On alcohol ester (PEN) or polyimides (PI) substrate, it is coated, can be formed with the speed between 1 m/min to 120 ms/min
The active layer thickness of thickness between 1 micron to 15 microns is then placed into 80 degree to 100 degree baking ovens and is dried.
The method of the present invention for preparing ultracapacitor based on coating transfer techniques, the identical size bubbles nickel are
It is identical as pole piece size to be transferred to refer to nickel foam, and nickel foam is using isopropanol, ethyl alcohol, deionized water ultrasound respectively before
Cleaning is subsequently placed in 80 degree to 100 degree of drying box and dries for use.
The method of the present invention for preparing ultracapacitor based on coating transfer techniques, the pressure transfer are will first to apply
The electrode plates of cloth and foamed nickel current collector are compound, then hydraulic press are used to apply the pressure between 2MPa to 20MPa, will be active
Substance is completely transferred to from metal aluminum foil or copper foil or PET or PEN or PI substrates in foamed nickel current collector.
The method of the present invention for preparing ultracapacitor based on coating transfer techniques, the assembling ultracapacitor
Diaphragm polyethylene (PE) or polypropylene (PP) or high density polyethylene (HDPE) (HDPE) or ultra-high molecular weight polyethylene are added in the process
(UHMWPE) and a concentration of 0.5 mol/L to 1.5 mol/Ls sodium sulphate electrolyte or BF4 ionic liquids or PF6 ionic liquids
Body is assembled into button-shaped ultracapacitor or winding type super capacitor symmetrically or non-symmetrically.
Description of the drawings
【Fig. 1】It is coated with transfer techniques schematic diagram.
【Fig. 2】Scanning electron microscope shape appearance figure of the activated carbon being coated with before transfer on aluminium foil.
【Fig. 3】The quality of activated carbon of coating and the linear relationship of wet-film thickness.
【Fig. 4】Scanning electron microscope shape appearance figure of the activated carbon in nickel foam after transfer.
【Fig. 5】The ultracapacitor chemical property prepared based on coating transfer techniques：A figures are charging and discharging curve, and b figures are
Cyclic voltammetry curve under different scanning speed, c figures are AC impedance curve, and d figures are the specific capacity after 5000 cycles
Retention rate.
【Fig. 6】Charging and discharging curve of 4 ultracapacitors based on coating transfer techniques preparation at 1A/g.
Specific implementation mode and embodiment
Following implementation and embodiment are the further instructions to the content of present invention, rather than limit the guarantor of the present invention
Protect range.
Embodiment 1
Detailed technology of preparing such as Fig. 1 of this embodiment.
Selected active material is to use relatively broad activated carbon, specific surface area 2000m in this embodiment2/ g,
1 hour of processing is dried using preceding activated carbon is placed in 90 degree of baking oven；
Binder making：PVDF powder is weighed in 80 degree of oven dryings after 6 hours, is dissolved in NMP and is configured to 2%
PVDF solution, magnetic agitation 10 hours after sealing, keeps its fully dispersed；
Slurry preparation：The mass ratio of activated carbon and PVDF are 9:1 is mixed, after sealing bottleneck, magnetic force at normal temperatures
Stir 2 hours；
Coating technique：The slurry prepared is scratched onto aluminium foil with blade coating equipment, edge of a knife spacing is 150 microns, coating
Speed is set as 15 ms/min, and coated pole piece is placed in 80 degree of vacuum drying chambers dry, 10 microns of thick porous actives of formation
Film, as shown in Figure 2；And during doctor blade technique, it can establish between active layer quality and the wet-film thickness of coating
Relationship, active layer film quality (milligram)=0.04 × wet-film thickness (micron)+7.49, as shown in Figure 3；
Cut pole piece and diaphragm：Dried pole piece is cut into circular pole piece to be transferred using sheet-punching machine, is cut simultaneously
Diaphragm, and the diameter of diaphragm is bigger than pole piece, and short circuit occurs to prevent the ultracapacitor of assembling；
Cut nickel foam：Nickel foam is cut into size identical with pole piece to be transferred, uses isopropanol, anhydrous second respectively
Alcohol, deionized water are cleaned by ultrasonic 30 minutes, are subsequently placed in for use after being dried in 90 degree of vacuum drying chambers；
Active layer shifts：The electrode plates cut and foamed nickel current collector are compound, with hydraulic press with the pressure of 5MPa
Pressure, foamed nickel current collector is completely transferred to by active material, and the active layer film morphology after shifting is substantially previous with transfer
Sample keeps porous structure, as shown in Figure 4；
Ultracapacitor assembles：Two panels symmetry electrode pole piece is aligned as possible, diaphragm PE is added, implantation concentration rubs for 1.0
You/liter sodium sulphate electrolyte, symmetrical button-shaped ultracapacitor is assembled into, using CHI660e electrochemical workstations to group
The symmetrical button-shaped ultracapacitor of dress is tested and is characterized, and detailed results are as shown in figure 5, the performance detail parameters counted
Stablize with reference to table 1, and by performance of the supercapacitor prepared by this method, favorable repeatability, 4 super electricity as shown in Figure 6
The performance parameter of container.
Embodiment 2
Selected active material is lithium titanate, specific surface area 1800m in this embodiment2/ g, using preceding by lithium titanate
It is placed in 90 degree of baking oven and 1 hour of processing is dried；
Binder making：PVDF powder is weighed in 80 degree of oven dryings after 6 hours, is dissolved in NMP and is configured to 2%
PVDF solution, magnetic agitation 10 hours after sealing, keeps its fully dispersed；
Slurry preparation：The mass ratio of lithium titanate, conductive black and PVDF is 8:1:1 is mixed, after sealing bottleneck,
2 hours of magnetic agitation under room temperature；
Coating technique：The slurry prepared is scratched onto aluminium foil with blade coating equipment, edge of a knife spacing is 180 microns, coating
Speed is set as 10 ms/min, and coated pole piece is placed in 80 degree of vacuum drying chambers dry, 10 microns of thick active layers of formation；
Cut pole piece and diaphragm：Dried pole piece is cut into circular pole piece to be transferred using sheet-punching machine, is cut simultaneously
Diaphragm, and the diameter of diaphragm is bigger than pole piece, and short circuit occurs to prevent the ultracapacitor of assembling；
Cut nickel foam：Nickel foam is cut into size identical with pole piece to be transferred, uses isopropanol, anhydrous second respectively
Alcohol, deionized water are cleaned by ultrasonic 30 minutes, are subsequently placed in for use after being dried in 90 degree of vacuum drying chambers；
Active layer shifts：The electrode plates cut and foamed nickel current collector are compound, with hydraulic press with the pressure of 5MPa
Pressure, active material is completely transferred in foamed nickel current collector；
Ultracapacitor assembles：Two panels symmetry electrode pole piece is aligned as possible, diaphragm PE is added, implantation concentration rubs for 1.0
You/liter sodium sulphate electrolyte, symmetrical button-shaped ultracapacitor is assembled into, using CHI660e electrochemical workstations to group
The symmetrical button-shaped ultracapacitor of dress is tested and is characterized, and under the current density of 1A/g, obtains the specific volume of 56F/g
Amount.
The ultracapacitor detail parameters that table 1 is prepared based on coating transfer techniques
Embodiment 3
Selected active material is graphene, specific surface area 2600m in this embodiment2/ g, using preceding by graphene
It is placed in 90 degree of baking oven and 1 hour of processing is dried；
Binder making：PVDF powder is weighed in 80 degree of oven dryings after 6 hours, is dissolved in NMP and is configured to 2%
PVDF solution, magnetic agitation 10 hours after sealing, keeps its fully dispersed；
Slurry preparation：The mass ratio of graphene and PVDF are 8:1 is mixed, after sealing bottleneck, magnetic force at normal temperatures
Stir 2 hours；
Coating technique：The slurry prepared is applied in PET base with slot coated equipment, spacer thickness is 20 micro-
Rice, coating speed are set as 15 ms/min, and coated pole piece is placed in drying in 80 degree of vacuum drying chambers, forms 12 microns thick
Active layer；
Cut pole piece and diaphragm：Dried pole piece is cut into circular pole piece to be transferred using sheet-punching machine, is cut simultaneously
Diaphragm, and the diameter of diaphragm is bigger than pole piece, and short circuit occurs to prevent the ultracapacitor of assembling；
Cut nickel foam：Nickel foam is cut into size identical with pole piece to be transferred, uses isopropanol, anhydrous second respectively
Alcohol, deionized water are cleaned by ultrasonic 30 minutes, are subsequently placed in for use after being dried in 90 degree of vacuum drying chambers；
Active layer shifts：The electrode plates cut and foamed nickel current collector are compound, with hydraulic press with the pressure of 10MPa
Pressure, active material is completely transferred in foamed nickel current collector；
Ultracapacitor assembles：Two panels symmetry electrode pole piece is aligned as possible, diaphragm PE is added, injects BF4 ionic liquids,
It is assembled into symmetrical button-shaped ultracapacitor, using CHI660e electrochemical workstations to the symmetrical button-shaped super of assembling
Capacitor is tested and is characterized, and under the current density of 1A/g, obtains the specific capacity of 230F/g.
Claims (7)
1. a kind of method preparing ultracapacitor based on coating transfer techniques, feature is as follows, is based on binder and active matter
The slurry that matter is prepared, is prepared into electrode plates by coating arts techniques, then cuts into the pole piece to be transferred of suitable dimension, and
It is transferred to by pressure in the foamed nickel current collector of identical size, is then assembled into ultracapacitor；The pressure transfer is first
The electrode plates of coating and foamed nickel current collector are compound, then hydraulic press is used to apply the pressure between 2MPa to 20MPa, it will
Active material is from metal aluminum foil or copper foil or polyethylene terephthalate (PET) or polyethylene naphthalate (PEN)
Or it is completely transferred in foamed nickel current collector in polyimides (PI) substrate.
2. a kind of method preparing ultracapacitor based on coating transfer techniques as described in claim 1, which is characterized in that described
Binder is Kynoar (PVDF), first dries PVDF powder 6 hours in 80 degree to 100 degree of baking oven in technology of preparing
After weigh, the PVDF solution for forming that mass concentration is 2% to 5% in N-Methyl pyrrolidone (NMP) is then dissolved in, in sealing strip
Magnetic agitation 8 hours to 10 hours under part, keep its fully dispersed.
3. a kind of method preparing ultracapacitor based on coating transfer techniques as described in claim 1, which is characterized in that described
Active material is activated carbon, lithium titanate, graphene, carbon nanotube, specific surface area 1500m2/ g to 3000m2Between/g, use
Processing is dried in preceding active material is placed in 80 degree to 100 degree of baking oven, is formed after avoiding binder PVDF from meeting water cotton-shaped
Object influences adhesive property.
4. a kind of method preparing ultracapacitor based on coating transfer techniques as described in claim 1, which is characterized in that described
PVDF solution is added in active material by the slurry of preparation, and it is 5 to form mass ratio with PVDF:1 to 12:1 mixed solution, then
Magnetic agitation 2 hours to 5 hours under room temperature.
5. a kind of method preparing ultracapacitor based on coating transfer techniques as described in claim 1, which is characterized in that described
Coating be use doctor blade technique or slot coating technique, on metal aluminum foil or copper foil or PET or PEN or PI substrates, with 1 meter/
It minute is coated to the speed between 120 ms/min, the active layer thickness of thickness between 1 micron to 15 microns can be formed, then
It is positioned in 80 degree to 100 degree baking ovens and is dried.
6. a kind of method preparing ultracapacitor based on coating transfer techniques as described in claim 1, which is characterized in that described
Identical size bubbles nickel refers to that nickel foam is identical as pole piece size to be transferred, and nickel foam using it is preceding respectively with isopropanol,
Ethyl alcohol, deionized water are cleaned by ultrasonic, and are subsequently placed in 80 degree to 100 degree of drying box and dry for use.
7. a kind of method preparing ultracapacitor based on coating transfer techniques as described in claim 1, which is characterized in that described
Diaphragm polyethylene (PE) or polypropylene (PP) or high density polyethylene (HDPE) (HDPE) or super are added during assembling ultracapacitor
The sodium sulphate electrolyte or BF of High molecular weight polyethylene (UHMWPE) and a concentration of 0.5 mol/L to 1.5 mol/Ls4Ionic liquid
Body or PF6Ionic liquid is assembled into button-shaped ultracapacitor or winding type super capacitor symmetrically or non-symmetrically.
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|---|---|---|---|---|
| CN101178979A (en) * | 2007-11-21 | 2008-05-14 | 中南大学 | Flexible packing super capacitor and its manufacture process |
| CN102723211A (en) * | 2012-05-08 | 2012-10-10 | 海博瑞恩电子科技无锡有限公司 | High performance super capacitor and manufacturing process thereof |
| CN103151183A (en) * | 2013-03-04 | 2013-06-12 | 成都芝田高分子材料有限公司 | Methods for manufacturing electrode and energy storage device, and energy storage device |
| CN105374985A (en) * | 2014-08-26 | 2016-03-02 | 万星光电子(东莞)有限公司 | Electrode slice preparation apparatus and electrode slice preparation method |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101178979A (en) * | 2007-11-21 | 2008-05-14 | 中南大学 | Flexible packing super capacitor and its manufacture process |
| CN102723211A (en) * | 2012-05-08 | 2012-10-10 | 海博瑞恩电子科技无锡有限公司 | High performance super capacitor and manufacturing process thereof |
| CN103151183A (en) * | 2013-03-04 | 2013-06-12 | 成都芝田高分子材料有限公司 | Methods for manufacturing electrode and energy storage device, and energy storage device |
| CN105374985A (en) * | 2014-08-26 | 2016-03-02 | 万星光电子(东莞)有限公司 | Electrode slice preparation apparatus and electrode slice preparation method |
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