CN104200997B - Composite current collector and preparation method thereof - Google Patents
Composite current collector and preparation method thereof Download PDFInfo
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- CN104200997B CN104200997B CN201410459651.7A CN201410459651A CN104200997B CN 104200997 B CN104200997 B CN 104200997B CN 201410459651 A CN201410459651 A CN 201410459651A CN 104200997 B CN104200997 B CN 104200997B
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of composite current collector and preparation method thereof, comprise the following steps：In the mixture that surface coated with nano Carbon Materials, Nano metal powder, metallic catalyst, binding resin and an organic solvent of light paper tinsel are formed, roll-in crimps to form conductive coating after drying；Under vacuum or protective gas atmosphere, high temperature carbonization treatment is carried out to conductive coating, obtain composite current collector.The preparation method of this composite current collector on light paper tinsel by forming the conductive coating that carbon nano-material, Nano metal powder, metallic catalyst and binding resin mix, binding resin is carbonized under the catalysis of metallic catalyst under high temperature, formed Nano metal powder, carbon nano-material interconnect be bundled together and with the carbon filament of the compact crystal whisker-shaped of light paper tinsel.The preparation method of this composite current collector need not use magnetron sputtering apparatus, high equipment investment be eliminated, while without methane atmosphere, reducing the danger in production process.
Description
Technical field
The present invention relates to energy storage device field, more particularly to a kind of composite current collector and preparation method thereof.
Background technology
Conducting polymer solid capacitor, with outstanding high frequency low-resistance characteristic, application field more comes wide in types of applications,
With the reduction of cost, there is the trend for progressively replacing original liquid electrolyte electric capacity.But in its superior impedance operator and life-span
Under characteristic, solid capacitor compares traditional liquid electrochemical capacitor, also there is obvious inferior position.Its main drawback is：Leakage current is big,
Usual product electric leakage is in 100 μ A~300 μ A scopes, and the electric leakage of liquid electric capacity is usual all in below 1 μ A, and the two is very different；
Secondly voltage endurance capability is not high, is only used for below 35v products mostly at present, and the product of higher voltage is due to the sheet of conducting polymer
Body feature, it is difficult to accomplish the product of more than 100v.Again, its capacity extraction rate is lower than liquid electric capacity.
As solid capacitance is in the extensive use of electronic applications, traditional electrolyte electric capacity is progressively substituted, at past 3 years
In evolution, realize that the encapsulation volume of the convoluted solid capacitor of regulation capacitance and ESR is less and less, price is also more come just
Preferably, therefore while its every electrical property is ensured production cost Shi Ge companies focus of attention how is reduced to greatest extent.
And the company for producing solid capacitor makes great progress in the in-situ polymerization process aspect of conducting polymer so that anode foils
Capacity extraction rate improve constantly, in terms of the product of low-voltage miniature, the extraction rate of anode has reached more than 80%, polymerization work
The improved space of skill aspect is few.Further to improve content volume ratio, it is necessary to start with Cathode Foil capacity from improving.Mesh
Before, the low voltage product for below 10V wants to accomplish the generally accepted size in market, it is necessary to use special cathode with high specific volume
Paper tinsel could be realized.This foil of cathode with high specific volume is only produced for two companies of Japan, and the country there is no the product that can be substituted, price
Costly, a price higher and is maintained over several years, has become one of most important cost of solid capacitor.
From unlike traditional Cathode Foil, this kind of foil of cathode with high specific volume is not to increase Cathode Foil by electrochemical corrosion
Surface area so as to obtain specific volume higher, it is but heavy above with coating, chemical vapor deposition or physical vapor in light paper tinsel
Long-pending means form the material of a thin layer high connductivity, such as：Carbon black, aluminium powder, aluminium carbide, titanium carbide, titanium carbonitride, carbon Nanowire
Dimension etc., these high connductivity material self-conductive performances very well, there is good stability to chemical substance, oxygen and high temperature, and
And because its special production technology, the conductive materials of growth are similar to " thick grass " in threadiness, penetrate aluminium foil surface passivation layer
(aluminum oxide), is taken root on the matrix of aluminium foil, and actual conducting state is formed between collector.On the one hand due to aluminium foil table
Fibre morphology on face high connductivity material is microcosmic, is conducive to PEDOT to permeate thereon, in-situ polymerization and close attachment, drops significantly
Contact resistance between low conducting polymer and Cathode Foil.On the other hand, because high connductivity " fiber " penetrates aluminium foil surface oxidation
Film, is directly combined with underlying metal, is directly drawn by collector equivalent to cathode current, and the capacity of Cathode Foil is " infinite
Greatly ".Therefore this Cathode Foil is used, using same polymeric technique and production method, the impedance of product can be not only greatly reduced,
Due also to its negative electrode is the effect for getting collected current, itself does not exist capacity, so can to greatest extent by positive pole
Capacity is brought into play, so that reduce the volume of product, even if being far above conventional cathode paper tinsel in the current foil of cathode with high specific volume price
In the case of, still can greatly reduce the cost of raw materials used of product.
The process route of the Fabrication of High Specific Capacitance solid capacitor Cathode Foil of existing ripe application mainly has two kinds：In corrosive aluminum foil or light
Paper tinsel surface is deposited with one layer of charcoal, titanium, titanium nitride or nitrogen titanium aluminide, titanium carbonitride by way of magnetron sputtering or vacuum evaporation, from
And the specific surface of aluminium foil is drastically increased, compared with former paper tinsel surface, its specific capacity increases in several times.As solid capacitance
Negative electrode, capacity extraction rate can be greatly improved, and reduce impedance and the DF value of electric capacity.Current JCC has a Fabrication of High Specific Capacitance charcoal
Paper tinsel is exactly to be made of this technique.
The charcoal aluminium foil that covers of Japan's aluminium is to be coated with one layer by the good slurry of powdered carbon, aluminium powder and mixed with resin on light paper tinsel surface, is dried
The coating of 1~3 μ m thick is formed after dry, then in methane atmosphere, by the method for chemical vapor deposition, organic carbon source is existed
Cracked under high temperature, and be attached to nano level carbon fiber, the carbon fiber of growth are grown on the micro catalytic metal center in paper tinsel face
Many cogongrass are similar to take root on the oxide-film of aluminium foil or on aluminum metal substrate.Because carbon fiber is in growth course, break
It is broken partial oxide film directly to be turned on metallic matrix, the appearance that Cathode Foil is shown by the natural oxide film of its Surface Creation
Amount is disappeared, and is directly led out equivalent to conductive polymer cathode, and cathode capacities are embodied " infinity ".
This two charcoal paper tinsel of the ripe application of existing market, can greatly improve capacity extraction rate, reduce solid capacitor
Internal resistance.The charcoal paper tinsel of JCC, be on light paper tinsel by way of magnetron sputtering by carbon deposit on base material, equipment used is too held high
It is expensive.The carbon paper tinsel of Japan's aluminium is then utilized in being coated with one layer of aluminium powder and powdered carbon on aluminium foil, then under carbon source atmosphere, high temperature cabonization,
Carbonization al whisker is formed, is connected between face coat and base material.This processing procedure, has methane atmosphere, causes production cost
Improve, have requirement higher to the body of heater material of high-temperature firing, and have certain danger.
The content of the invention
Based on this, it is necessary to provide a kind of production cost relatively low while producing dangerous relatively low composite current collector and its system
Preparation Method.
A kind of preparation method of composite current collector, comprises the following steps：
Light paper tinsel is provided；
Electrocondution slurry is coated on a surface of the smooth paper tinsel, roll-in crimps to form conductive coating after drying, the conduction
Slurry is the mixture that carbon nano-material, Nano metal powder, metallic catalyst, binding resin and organic solvent are formed；
Under vacuum or protective gas atmosphere, the described smooth paper tinsel to being formed with conductive coating carries out high temperature carbonization treatment, obtains
To the composite current collector.
In one embodiment, the smooth paper tinsel is aluminium foil, corrosive aluminum foil, Copper Foil or corrosion Copper Foil.
In one embodiment, the electrocondution slurry according to the carbon nano-material that mass fraction is 5~15 parts, 15~25 parts
Nano metal powder, 0.2~0.8 part of metallic catalyst, 5~15 parts of binding resin and 80~120 parts of organic solvent shape
Into mixture.
In one embodiment, the thickness of the conductive coating is 1 μm~5 μm.
In one embodiment, the carbon nano-material is graphene powder, conductive black, CNT, carbon fiber, second
Acetylene black, active carbon powder or graphite powder, the particle diameter of the carbon nano-material is 40nm~60nm；
The Nano metal powder is nanometer aluminium powder, nano-nickel powder, nano-silver powder, nano titanium powder, nanometer manganese powder, nanometer Mg powder
Or nanometer potassium powder, the particle diameter of the Nano metal powder is 80nm~120nm.
In one embodiment, the metallic catalyst is the nickel of nickel salicylates complex or salicylic acid ethylenediamine schiff bases
Complex.
In one embodiment, the binding resin is novolac epoxy resin, and the organic solvent is butanone.
In one embodiment, the protective gas atmosphere is nitrogen atmosphere, helium atmosphere, neon atmosphere, argon atmosphere
Or Krypton atmosphere.
In one embodiment, the temperature of the high temperature carbonization treatment is 450 DEG C~650 DEG C, the high temperature carbonization treatment
Time be 4h~8h.
A kind of composite current collector, is prepared using the preparation method of above-mentioned composite current collector；
Being formed with the described smooth paper tinsel of conductive coating carries out high temperature carbonization treatment, and the binding resin is in the metallic catalyst
Catalysis under charing form the carbon filament of crystal whisker-shaped, the carbon filament of the crystal whisker-shaped is by the carbon nano-material and the Nano metal powder
Interconnection is bundled together and is combined closely with the smooth paper tinsel.
The preparation method of this composite current collector is urged by forming carbon nano-material, Nano metal powder, metal on light paper tinsel
Agent and binding resin mixing conductive coating, roll-in crimping after under vacuum or inert gas atmosphere high temperature carbonization, bond
Resin is carbonized under the catalysis of metallic catalyst, forms the carbon filament of crystal whisker-shaped, and the carbon filament of crystal whisker-shaped is Nano metal powder, Nano carbon
Material interconnects and is bundled together and is tightly combined with light paper tinsel, and obtained composite current collector has capacity extraction rate high and low
ESR.
The preparation method of this composite current collector need not use magnetron sputtering apparatus, eliminate high equipment investment,
Methane atmosphere need not be used simultaneously, reduce the danger in production process.Relative to the preparation side of traditional composite current collector
Method, the preparation method production cost of this composite current collector is relatively low while producing dangerous relatively low.
Brief description of the drawings
Fig. 1 is the flow chart of the preparation method of the collector of an implementation method.
Specific embodiment
To enable the above objects, features and advantages of the present invention more obvious understandable, below in conjunction with the accompanying drawings to the present invention
Specific embodiment be described in detail.Elaborate many details in order to fully understand this hair in the following description
It is bright.But the present invention can be implemented with being much different from other manner described here, and those skilled in the art can be not
Similar improvement is done in the case of running counter to intension of the present invention, therefore the present invention is not limited by following public specific implementation.
The preparation method of the composite current collector of an implementation method as shown in Figure 1, comprises the following steps：
S10, offer light paper tinsel.
Light paper tinsel can be aluminium foil, corrosive aluminum foil, Copper Foil or corrosion Copper Foil.
One surface coating electrocondution slurry of S20, the light paper tinsel obtained in S10, roll-in crimps to form conductive coating after drying.
Electrocondution slurry is the mixed of carbon nano-material, Nano metal powder, metallic catalyst, binding resin and organic solvent formation
Compound.
In one preferably embodiment, electrocondution slurry is according to the carbon nano-material that mass fraction is 5~15 parts, 15~25
Part Nano metal powder, 0.2~0.8 part of metallic catalyst, 5~15 parts of binding resin and 80~120 parts of organic solvent
The mixture of formation.
The thickness of conductive coating can be 1 μm~5 μm.
Carbon nano-material can be active carbon powder, graphene powder, conductive black, CNT, carbon fiber, acetylene black
Or graphite powder, the particle diameter of carbon nano-material is 40nm~60nm.
Nano metal powder can be nanometer aluminium powder, nano-nickel powder, nano-silver powder, nano titanium powder, nanometer manganese powder, nanometer Mg powder
Or nanometer potassium powder, the particle diameter of Nano metal powder is 80nm~120nm.
In one preferably embodiment, the particle diameter of carbon nano-material is 50nm, and Nano metal powder is that particle diameter is 100nm's
Nanometer aluminium powder.
Metallic catalyst can be nickel salicylates complex, the nickel complex of salicylic acid ethylenediamine schiff bases.
Binding resin can be novolac epoxy resin.
Organic solvent can be butanone.
S30, under vacuum or protective gas atmosphere, the light paper tinsel that the formation obtained to S20 has conductive coating carries out pyrocarbon
Change is processed, and obtains composite current collector.
Vacuum under vacuum condition is 1 × 10-3Pa~1 × 10-5Pa。
Protective gas atmosphere can be nitrogen atmosphere, helium atmosphere, neon atmosphere, argon atmosphere or Krypton atmosphere.
In S30, the temperature of high temperature carbonization treatment is 450 DEG C~650 DEG C, and the time of high temperature carbonization treatment is 4h~8h.
The preparation method of this composite current collector is urged by forming carbon nano-material, Nano metal powder, metal on light paper tinsel
Agent and binding resin mixing conductive coating, roll-in crimping after under vacuum or inert gas atmosphere high temperature carbonization, bond
Resin is carbonized under the catalysis of metallic catalyst, forms the carbon filament of crystal whisker-shaped, and the carbon filament of crystal whisker-shaped is Nano metal powder, Nano carbon
Material interconnects and is bundled together and is tightly combined with light paper tinsel, and obtained composite current collector has capacity extraction rate high and low
ESR.
The preparation method of this composite current collector need not use magnetron sputtering apparatus, eliminate high equipment investment,
Methane atmosphere need not be used simultaneously, reduce the danger in production process.Relative to the preparation side of traditional composite current collector
Method, the preparation method production cost of this composite current collector is relatively low while producing dangerous relatively low.
The composite current collector that a kind of preparation method using above-mentioned composite current collector is prepared, is formed with conductive coating
Described smooth paper tinsel carry out high temperature carbonization after, binding resin carbonizes the charcoal for forming crystal whisker-shaped under the catalysis of the metallic catalyst
Be connected with each other for carbon nano-material and Nano metal powder and be bundled together and combined closely with light paper tinsel by silk, the carbon filament of crystal whisker-shaped.
This composite current collector has capacity extraction rate and low ESR high, suitable with existing commercially available charcoal paper tinsel performance.
This composite current collector can be as the collector of solid-state capacitor, ultracapacitor and lithium ion battery etc..
It is below specific embodiment.
Embodiment 1
According to mass fraction, by conductive black 1g, 100 nanometers of aluminium powder 2g, epoxy novolac that average grain diameter is 50 nanometers
Resin 1g, nickel salicylates complex 0.05g, is scattered in 10g butanone, forms the good electrocondution slurry of degree of scatter, coats
Roll-in crimping is crossed on aluminium foil, after drying, the conductive coating of 2 μ m thicks is formed.It is last in a vacuum furnace, 1 × 10-3The condition of Pa
Under, the aluminium foil to being formed with conductive coating carries out high temperature carbonization treatment, and the temperature of high temperature carbonization treatment is 550 DEG C, pyrocarbon
The time for changing treatment is 6h, obtains required composite current collector.
Embodiment 2
According to mass fraction, by active carbon powder 0.5g, 120 nanometers of nickel powder 1.5g, phenol that average grain diameter is 40 nanometers
Formaldehyde epoxy resin 0.5g, nickel salicylates complex 0.02g, is scattered in 8g butanone, forms the good electrocondution slurry of degree of scatter,
Coat on corrosive aluminum foil, roll-in crimping is crossed after drying, form the conductive coating of 1 μ m thick.It is last in a vacuum furnace, blanket of nitrogen
Under enclosing, the aluminium foil to being formed with conductive coating carries out high temperature carbonization treatment, and the temperature of high temperature carbonization treatment is 450 DEG C, high temperature
The time of charing process is 8h, obtains required composite current collector.
Embodiment 3
According to mass fraction, by CNT 1.5g, 80 nanometers of silver powder 2.5g, phenolic aldehyde ring that average grain diameter is 60 nanometers
Oxygen tree fat 1.5g, nickel salicylates complex 0.08g, is scattered in 12g butanone, forms the good electrocondution slurry of degree of scatter, applies
It is distributed on Copper Foil, the conductive coating of 5 μ m thicks is formed after drying.It is last in a vacuum furnace, 1 × 10-5Under conditions of Pa, to being formed
The aluminium foil for having conductive coating carries out high temperature carbonization treatment, and the temperature of high temperature carbonization treatment is 650 DEG C, high temperature carbonization treatment when
Between be 4h, obtain required composite current collector.
Embodiment 4
According to mass fraction, by graphene powder 1.2g, 90 nanometers of manganese powder 2g, phenolic aldehyde ring that average grain diameter is 55 nanometers
Oxygen tree fat 1.2g, is scattered in 12g butanone, forms the good electrocondution slurry of degree of scatter, coats on corrosion Copper Foil, after drying
Roll-in crimping is crossed, the conductive coating of 4 μ m thicks is formed.It is last in a vacuum furnace, under helium atmosphere, to being formed with conductive coating
Aluminium foil carries out high temperature carbonization treatment, and the temperature of high temperature carbonization treatment is 500 DEG C, and the time of high temperature carbonization treatment is 5.5h, is obtained
To required composite current collector.
The composite current collector prepared to embodiment 1~4, the adhesive force of conductive coating is detected using 3M adhesive tapes, and is pressed
The electric capacity of 2.5v-820 μ F is prepared according to existing method, the testing result for obtaining is as shown in table 1 below.
Table 1：The performance comparison of the composite current collector that embodiment 1~4 is prepared.
As can be seen from Table 1, the composite current collector that embodiment 1~4 is prepared has capacity extraction rate high and low
ESR is suitable with existing commercially available charcoal paper tinsel performance.
Embodiment described above only expresses several embodiments of the invention, and its description is more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Shield scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (9)
1. a kind of preparation method of composite current collector, it is characterised in that comprise the following steps：
Light paper tinsel is provided；
Electrocondution slurry is coated on a surface of the smooth paper tinsel, roll-in crimps to form conductive coating after drying, the electrocondution slurry
It is the mixture that carbon nano-material, Nano metal powder, metallic catalyst, binding resin and organic solvent are formed, wherein, the gold
Metal catalyst is the nickel complex of nickel salicylates complex or salicylic acid ethylenediamine schiff bases；
Under vacuum or protective gas atmosphere, the described smooth paper tinsel to being formed with conductive coating carries out high temperature carbonization treatment, obtains institute
State composite current collector.
2. the preparation method of composite current collector according to claim 1, it is characterised in that the smooth paper tinsel is aluminium foil, corrosion
Aluminium foil, Copper Foil or corrosion Copper Foil.
3. the preparation method of composite current collector according to claim 1, it is characterised in that the electrocondution slurry is according to quality
Number be 5~15 parts carbon nano-material, 15~25 parts of Nano metal powder, 0.2~0.8 part of metallic catalyst, 5~15 parts
Binding resin and 80~120 parts organic solvent formed mixture.
4. the preparation method of composite current collector according to claim 1, it is characterised in that the thickness of the conductive coating is
1 μm~5 μm.
5. the preparation method of composite current collector according to claim 1, it is characterised in that the carbon nano-material is graphite
Alkene powder, conductive black, CNT, carbon fiber, acetylene black, active carbon powder or graphite powder, the grain of the carbon nano-material
Footpath is 40nm~60nm；
The Nano metal powder is nanometer aluminium powder, nano-nickel powder, nano-silver powder, nano titanium powder, nanometer manganese powder, nanometer Mg powder or receives
Rice potassium powder, the particle diameter of the Nano metal powder is 80nm~120nm.
6. the preparation method of composite current collector according to claim 1, it is characterised in that the binding resin is phenolic aldehyde ring
Oxygen tree fat, the organic solvent is butanone.
7. the preparation method of composite current collector according to claim 1, it is characterised in that the protective gas atmosphere is nitrogen
Atmosphere is enclosed, helium atmosphere, neon atmosphere, argon atmosphere or Krypton atmosphere.
8. the preparation method of composite current collector according to claim 1, it is characterised in that the temperature of the high temperature carbonization treatment
It is 450 DEG C~650 DEG C to spend, and the time of the high temperature carbonization treatment is 4h~8h.
9. a kind of composite current collector, it is characterised in that the composite current collector is using described in any one in claim 1~8
The preparation method of composite current collector prepare；
Being formed with the described smooth paper tinsel of conductive coating carries out high temperature carbonization treatment, and the binding resin is urged the metallic catalyst
Change the carbon filament that lower charing forms crystal whisker-shaped, the carbon filament of the crystal whisker-shaped is mutual by the carbon nano-material and the Nano metal powder
Connection is bundled together and is combined closely with the smooth paper tinsel.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106082693A (en) * | 2016-06-24 | 2016-11-09 | 成都天航智虹企业管理咨询有限公司 | A kind of method preparing transparent graphene conductive film |
| CN106024200A (en) * | 2016-06-24 | 2016-10-12 | 成都天航智虹企业管理咨询有限公司 | Method for preparing graphene conductive thin film |
| CN107579256B (en) * | 2016-07-05 | 2021-02-05 | 江苏天奈科技股份有限公司 | Conductive slurry and method for forming net-shaped carbon heat-conducting and electric-conducting network current collector by using same |
| CN107863487B (en) * | 2017-08-23 | 2020-07-17 | 中航锂电（洛阳）有限公司 | Lithium-sulfur battery positive electrode and preparation method thereof, lithium-sulfur battery cell and lithium-sulfur battery |
| CN108899476B (en) * | 2018-07-17 | 2020-07-28 | 大同新成新材料股份有限公司 | Preparation process of lithium battery graphene-based composite negative electrode material |
| CN111105932B (en) * | 2018-10-26 | 2021-11-02 | 南通宇华新材料科技有限公司 | Solid-state capacitance carbon foil nano conductive carbon paste and preparation method thereof |
| CN111105933B (en) * | 2018-10-26 | 2021-08-20 | 南通宇华新材料科技有限公司 | High-compactness, acid-resistant and oxidation-resistant solid capacitor carbon foil production process |
| CN109888296B (en) * | 2019-03-19 | 2020-11-10 | 合肥国轩高科动力能源有限公司 | Preparation method of carbon-coated current collector for positive electrode of lithium ion battery |
| CN109929230A (en) * | 2019-04-08 | 2019-06-25 | 安徽律正科技信息服务有限公司 | A kind of high temperature-resistant polymer conducing composite material |
| CN110783112B (en) * | 2019-12-12 | 2021-11-26 | 广东风华高新科技股份有限公司 | Super capacitor pole piece with Ag transition layer and preparation method thereof |
| CN116246890A (en) * | 2023-02-13 | 2023-06-09 | 北海星石碳材料科技有限责任公司 | Graphene reinforced aluminum-based supercapacitor current collector and preparation method thereof |
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