CN105932288A - Graphene composite conductive agent and preparation method thereof - Google Patents
Graphene composite conductive agent and preparation method thereof Download PDFInfo
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- CN105932288A CN105932288A CN201610365003.4A CN201610365003A CN105932288A CN 105932288 A CN105932288 A CN 105932288A CN 201610365003 A CN201610365003 A CN 201610365003A CN 105932288 A CN105932288 A CN 105932288A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
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Abstract
The invention relates to a graphene composite conductive agent and a preparation method thereof. The graphene composite conductive agent is prepared from the following components in parts by weight: 70-100 parts of graphene, 20-45 parts of carbon nano-tubes, 30-45 parts of epoxy resin, 10-25 parts of monoethanolamine, 200-300 parts of solvent, 2-3 parts of additives, 7-10 parts of conductive polymer agent, 2-4 parts of glass beads and 3-8 parts of iridium acetylacetonate. According to the conductive agent and the method, the graphene is taken as the master component, the carbon nano-tubes are taken as the secondary component, through utilization of the excellent electric conductivity of the graphene, the capacity of an electrode material is increased, the internal resistance of a battery is reduced, and the cycle life of the battery is prolonged. The 2C rate is improved by 6-10% when a lithium ion battery is prepared, the cost is reduced, and the lithium ion battery is highly competitive.
Description
Technical field
The present invention relates to lithium ion battery, particularly relate to a kind of reduce cost, improve electric conductivity and the Graphene of cycle life
Combined conductive agent.
Background technology
Lithium ion battery has the advantage such as high-energy-density, memory-less effect, gets the favour of people as new forms of energy the most again,
Thus develop rapidly, along with the maturation of technology, people are more and more higher to the requirement of lithium ion battery.
The lithium ion battery of prior art mainly uses electrically conductive graphite, acetylene black and the CNT as conductive agent, acetylene black to be
The chain thing being made up of amorphous carbon particles spherical in shape, is currently used most commonly used conductive agent, cheap, but in order to
Reaching to strengthen the purpose contacted with each other between electrode active material, required addition is relatively big, thus causes the decline of electrode capacity；
CNT is the one-dimensional carbonaceous material in line style, and compared with acetylene black, CNT has more preferably electric conductivity and addition
Few, but current CNT is expensive, and the shortcoming that there is difficulties in dispersion as conductive agent when using.
China Patent Publication No. CN 1529382A, publication date JIUYUE in 2004 15 days, entitled high power plastics lithium ion
The patent of invention of battery, this application case discloses a kind of high-power plastic lithium-ion cell, is situated between including positive plate, negative plate, electricity
Film material, electrolyte material, soft compound package material and cabinet, positive plate include positive electrode, adhesive, DBP,
Carbon black, aluminum net, negative plate includes negative material, adhesive, DBP, carbon black, copper mesh, membrane materials for electrolyte include adhesive,
Silicon dioxide, DBP.Positive plate, negative plate and dielectric film make unit battery core by heating is compound, unit battery core are overlapped,
After using composite film material packaging, form assembled battery, draw lug, make the positive and negative electrode of assembled battery by ear pole material with
Positive and negative electrode terminal connects, and assembled battery is placed in plastics and internal, makes lid be merged by ultrasound wave with box body, formed complete
High-power plastic lithium-ion cell.It is disadvantageous in that, when prior art is in order to prevent high-multiplying power discharge, at battery pole ear and
Battery core caloric value is excessive, shortens cycle performance of battery and increases conductive black content, while reducing caloric value, can reduce electricity
The energy density in pond；In order to increase the battery high rate cyclic life-span, select to increase binder content, the internal resistance of cell can be increased, electricity
Pond caloric value increases.
Summary of the invention
The invention aims to solve the deficiencies in the prior art and provide a kind of and reduce cost, raising electric conductivity and circulation
The graphene composite conductive agent in life-span.
To achieve these goals, the present invention is by the following technical solutions:
A kind of graphene composite conductive agent, the mass fraction of the described each component of graphene composite conductive agent is: 70-100 part Graphene, 20-45
Part CNT, 30-45 part epoxy resin, 10-25 part monoethanolamine, 200-300 part solvent, 2-3 part auxiliary agent, 7-10 part are led
Electricity polymeric agent, 2-4 part glass microballoon and 3-8 part acetylacetone,2,4-pentanedione iridium.In the technical program, the structure of Graphene is appreciated that
For the graphite of monolayer, therefore having the most excellent electric conductivity, wherein the movement velocity of electronics has reached the 1/300 of the light velocity, simultaneously
Two-dimensional nano layer structure and huge specific surface area that Graphene is unique have as conductive agent compared to CNT or white carbon black etc.
There is the most prominent advantage；Selecting epoxy resin and monoethanolamine is then to improve Graphene dispersing uniformity in a solvent,
The problem solving Graphene part difficulties in dispersion；
The selection of glass microballoon, so that Graphene makes it be more easy to dispersion under the influence of a magnetic field, produces with epoxy resin, monoethanolamine
Collaborative peptizaiton, and graphene dispersion is uniformly so that the advantage that graphene conductive agent had both played high electron conduction improves
The transfer rate of ion, can play again huge specific surface area advantage and improve the imbibition liquid-keeping property of active material in course of reaction
And the transmittability of lithium ion.
Adding primarily to improve the stability of battery of acetylacetone,2,4-pentanedione iridium, thus improve the security performance of battery.
As preferably, described solvent is the one in Ketohexamethylene, Ketocyclopentane, ethanol, acetone, hexamethylene or oxolane.
As preferably, described conducting polymer agent is polyacetylene, gathers styrene or polyaniline.
As preferably, Graphene is the black powder that particle diameter is distributed in 10 nanometer-100 microns, is equal by monolayer-1000 layers
Row or the carbonaceous material constituted close to parallel graphene sheet layer, specific surface area is 50-1500/g.
As preferably, auxiliary agent is made up of the raw material of following weight portion: hydroxyethyl cellulose 5-10 part, chitosan 10-15 part,
Algae clay 5-10 part and silane coupler 15-25 part.
A kind of preparation method of graphene composite conductive agent, described preparation method comprises the following steps:
1) Graphene, epoxy resin are mixed with the solvent of half with glass microballoon, at 55-65 DEG C of ultrasonic disperse 10-25min, obtain
Premixed liquid A；
2) CNT, monoethanolamine are mixed with remaining solvent with acetylacetone,2,4-pentanedione iridium, at 78-90 DEG C, stir 30-60min,
To premixed liquid B；
3) by step 1) the premixed liquid A that obtains and step 2) the premixed liquid B stirring that obtains is mixed and added into auxiliary agent and conducting polymer
Agent, carries out good pressure distribution process under pressure 21000PSI, then heats to 150-220 DEG C, stirs 3-6h, grinds after cooling
One-tenth particle diameter is 10-20nm, obtains graphene composite conductive agent.
As preferably, step 1) Graphene is initially charged before combination in acetic acid, is warming up to 90 DEG C, stirs 3h, wash afterwards
Clean and dry.
As preferably, supersonic frequency is 50-65KHz.
Beneficial effects of the present invention:
1) present invention is based on Graphene, is aided with CNT, utilizes the electric conductivity that Graphene is excellent, improves the capacity of electrode material,
Reduce the internal resistance of cell, improve battery cycle life；
2) the graphene conductive agent that prepared by the present invention but improves 6-10% preparing lithium ion battery 2C multiplying power, provides cost savings, makes
Obtain lithium ion battery and have more competitiveness；
3) the conductive agent electronic conduction ability that the present invention prepares is strong and heat conduction uniformly, be doped to inside lithium ion battery to have stronger
Imbibition liquid-keeping property.
Detailed description of the invention
Technical scheme in the embodiment of the present invention will be carried out clear, complete description below, it is clear that described embodiment
It is only a part of embodiment of the present invention rather than whole embodiments.Based on the embodiment in the present invention, the common skill in this area
All other embodiments that art personnel are obtained under not making creative work premise, broadly fall into the scope of protection of the invention.
Graphene used by the present invention is purchased from Ningbo Mo Xi Science and Technology Ltd., and remaining raw material is all commercially available.Graphene is
Particle diameter is distributed in the black powder of 10 nanometer-100 microns, is parallel by monolayer-1000 layers or close to parallel graphene film
The carbonaceous material that layer is constituted, specific surface area is 50-1500/g.
Embodiment 1
A kind of graphene composite conductive agent, the mass fraction of the described each component of graphene composite conductive agent is: 70 parts of Graphenes, 20 parts receive
Rice carbon pipe, 30 parts of epoxy resin, 10 parts of monoethanolamine, 200 parts of solvents, 2 parts of auxiliary agents, 7 parts of conducting polymer agent, 2 parts of glass
Glass microballon and 3 parts of acetylacetone,2,4-pentanedione iridium.
Solvent is Ketohexamethylene.
Conducting polymer agent is polyacetylene.
Auxiliary agent is made up of the raw material of following weight portion: hydroxyethyl cellulose 5 parts, chitosan 10 parts, algae clay 5 parts and silicon
Alkane coupling agent 15 parts.
A kind of preparation method of graphene composite conductive agent, described preparation method comprises the following steps:
1) Graphene is initially charged in acetic acid, is warming up to 90 DEG C, stir 3h, afterwash and dry；By Graphene, epoxy resin
Mix with the solvent of half with glass microballoon, at 55 DEG C of ultrasonic disperse 10min, obtain premixed liquid A；Supersonic frequency is 50KHz；
2) CNT, monoethanolamine are mixed with remaining solvent with acetylacetone,2,4-pentanedione iridium, at 78 DEG C, stir 30min, premixed
Liquid B；
3) by step 1) the premixed liquid A that obtains and step 2) the premixed liquid B stirring that obtains is mixed and added into auxiliary agent and conducting polymer
Agent, carries out good pressure distribution process under pressure 21000PSI, then heats to 150 DEG C, stirs 3h, grinds to form particle diameter after cooling
For 10-20nm, obtain graphene composite conductive agent.
Embodiment 2
A kind of graphene composite conductive agent, the mass fraction of the described each component of graphene composite conductive agent is: 80 parts of Graphenes, 35 parts receive
Rice carbon pipe, 38 parts of epoxy resin, 17 parts of monoethanolamine, 260 parts of solvents, 3 parts of auxiliary agents, 8 parts of conducting polymer agent, 3 parts of glass
Glass microballon and 5 parts of acetylacetone,2,4-pentanedione iridium.
Solvent is ethanol.
Conducting polymer agent is for gathering styrene.
Auxiliary agent is made up of the raw material of following weight portion: hydroxyethyl cellulose 7 parts, chitosan 13 parts, algae clay 8 parts and silicon
Alkane coupling agent 18 parts.
A kind of preparation method of graphene composite conductive agent, described preparation method comprises the following steps:
1) Graphene is initially charged in acetic acid, is warming up to 90 DEG C, stir 3h, afterwash and dry；By Graphene, epoxy resin
Mix with the solvent of half with glass microballoon, at 60 DEG C of ultrasonic disperse 19min, obtain premixed liquid A；Supersonic frequency is 60KHz；
2) CNT, monoethanolamine are mixed with remaining solvent with acetylacetone,2,4-pentanedione iridium, at 85 DEG C, stir 40min, premixed
Liquid B；
3) by step 1) the premixed liquid A that obtains and step 2) the premixed liquid B stirring that obtains is mixed and added into auxiliary agent and conducting polymer
Agent, carries out good pressure distribution process under pressure 21000PSI, then heats to 180 DEG C, stirs 4h, grinds to form particle diameter after cooling
For 10-20nm, obtain graphene composite conductive agent.
Embodiment 3
A kind of graphene composite conductive agent, the mass fraction of the described each component of graphene composite conductive agent is: 100 parts of Graphenes, 45 parts
CNT, 45 parts of epoxy resin, 25 parts of monoethanolamine, 300 parts of solvents, 2-3 part auxiliary agent, 10 parts of conducting polymer agent, 4
Part glass microballoon and 8 parts of acetylacetone,2,4-pentanedione iridium.
Solvent is Ketocyclopentane.
Conducting polymer agent is polyaniline.
Auxiliary agent is made up of the raw material of following weight portion: hydroxyethyl cellulose 10 parts, chitosan 15 parts, algae clay 10 parts with
Silane coupler 25 parts.
A kind of preparation method of graphene composite conductive agent, described preparation method comprises the following steps:
1) Graphene is initially charged in acetic acid, is warming up to 90 DEG C, stir 3h, afterwash and dry；By Graphene, epoxy resin
Mix with the solvent of half with glass microballoon, at 65 DEG C of ultrasonic disperse 25min, obtain premixed liquid A；Supersonic frequency is 65KHz；
2) CNT, monoethanolamine are mixed with remaining solvent with acetylacetone,2,4-pentanedione iridium, at 90 DEG C, stir 60min, premixed
Liquid B；
3) by step 1) the premixed liquid A that obtains and step 2) the premixed liquid B stirring that obtains is mixed and added into auxiliary agent and conducting polymer
Agent, carries out good pressure distribution process under pressure 21000PSI, then heats to 220 DEG C, stirs 6h, grinds to form particle diameter after cooling
For 10-20nm, obtain graphene composite conductive agent.
Embodiment 4
A kind of graphene composite conductive agent, the mass fraction of the described each component of graphene composite conductive agent is: 90 parts of Graphenes, 45 parts receive
Rice carbon pipe, 30 parts of epoxy resin, 20 parts of monoethanolamine, 250 parts of solvents, 2 parts of auxiliary agents, 9 parts of conducting polymer agent, 3 parts of glass
Glass microballon and 6 parts of acetylacetone,2,4-pentanedione iridium.
Solvent is oxolane.
Conducting polymer agent is polyacetylene.
Auxiliary agent is made up of the raw material of following weight portion: hydroxyethyl cellulose 9 parts, chitosan 14 parts, algae clay 7 parts and silicon
Alkane coupling agent 23 parts.
A kind of preparation method of graphene composite conductive agent, described preparation method comprises the following steps:
1) Graphene, epoxy resin are mixed with the solvent of half with glass microballoon, at 55-65 DEG C of ultrasonic disperse 15min, obtain pre-
Mixed liquid A；Supersonic frequency is 60KHz；
2) CNT, monoethanolamine are mixed with remaining solvent with acetylacetone,2,4-pentanedione iridium, at 78-90 DEG C, stir 45min, obtain
Premixed liquid B；
3) by step 1) the premixed liquid A that obtains and step 2) the premixed liquid B stirring that obtains is mixed and added into auxiliary agent and conducting polymer
Agent, carries out good pressure distribution process under pressure 21000PSI, then heats to 190 DEG C, stirs 5h, grinds to form particle diameter after cooling
For 10-20nm, obtain graphene composite conductive agent.
Comparative example 1, with white carbon black as conductive agent.
By embodiment 1-4 the conductive agent of graphene conductive agent and comparative example 1 be fabricated to flexible packing lithium ion battery, enter
Row cycle performance is tested, and result is as follows:
Table 1, test result
| Specific capacity (mAh/g) | Efficiency (%) first | Capability retention (%) after 100 circulations | |
| Embodiment 1 | 600 | 85 | 91 |
| Embodiment 2 | 720 | 81 | 87 |
| Embodiment 3 | 866 | 78 | 89 |
| Embodiment 4 | 740 | 79 | 88 |
| Comparative example 1 | 460 | 66 | 51 |
The present invention uses graphene composite conductive agent, utilizes the electric conductivity that Graphene is excellent, improves the capacity of electrode material, reduces battery
Internal resistance, improves battery cycle life；2C multiplying power but improves 6-10%, provides cost savings so that lithium ion battery has more competing
Strive power.
It should be appreciated that to those skilled in the art, can be improved according to the above description or be converted,
And all these modifications and variations all should belong to the protection domain of claims of the present invention.
Claims (8)
1. a graphene composite conductive agent, it is characterised in that the mass fraction of the described each component of graphene composite conductive agent is: 70-100
Part Graphene, 20-45 part CNT, 30-45 part epoxy resin, 10-25 part monoethanolamine, 200-300 part solvent, 2-3
Part auxiliary agent, 7-10 part conducting polymer agent, 2-4 part glass microballoon and 3-8 part acetylacetone,2,4-pentanedione iridium.
A kind of graphene composite conductive agent the most according to claim 1, it is characterised in that described solvent be Ketohexamethylene, Ketocyclopentane,
One in ethanol, acetone, hexamethylene or oxolane.
A kind of graphene composite conductive agent the most according to claim 1, it is characterised in that described conducting polymer agent be polyacetylene,
Poly-to styrene or polyaniline.
4. according to a kind of graphene composite conductive agent described in claim 1 or 2 or 3, it is characterised in that Graphene is particle diameter distribution
In the black powder of 10 nanometer-100 microns, it is parallel by monolayer-1000 layers or constitutes close to parallel graphene sheet layer
Carbonaceous material, specific surface area is 50-1500/g.
5. according to a kind of graphene composite conductive agent described in claim 1 or 2 or 3, it is characterised in that auxiliary agent is by following weight portion
Raw material composition: hydroxyethyl cellulose 5-10 part, chitosan 10-15 part, algae clay 5-10 part and silane coupler 15-25 part.
6. the preparation method of a graphene composite conductive agent as claimed in claim 1, it is characterised in that described preparation method includes
Following steps:
1) Graphene, epoxy resin are mixed with the solvent of half with glass microballoon, at 55-65 DEG C of ultrasonic disperse 10-25min, obtain
Premixed liquid A；
2) CNT, monoethanolamine are mixed with remaining solvent with acetylacetone,2,4-pentanedione iridium, at 78-90 DEG C, stir 30-60min,
To premixed liquid B；
3) by step 1) the premixed liquid A that obtains and step 2) the premixed liquid B stirring that obtains is mixed and added into auxiliary agent and conducting polymer
Agent, carries out good pressure distribution process under pressure 21000PSI, then heats to 150-220 DEG C, stirs 3-6h, grinds after cooling
One-tenth particle diameter is 10-20nm, obtains graphene composite conductive agent.
The preparation method of a kind of graphene composite conductive agent the most according to claim 6, it is characterised in that step 1) Graphene
Be initially charged before combination in acetic acid, be warming up to 90 DEG C, stir 3h, afterwash and dry.
8. according to the preparation method of a kind of graphene composite conductive agent described in claim 6 or 7, it is characterised in that supersonic frequency is
50-65KHz。
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| CN107629625A (en) * | 2017-09-20 | 2018-01-26 | 江南载福粉末涂料（张家港）有限公司 | A kind of super anti-corrosive powder paint of graphene and preparation method thereof |
| CN107785585A (en) * | 2017-10-31 | 2018-03-09 | 南京旭羽睿材料科技有限公司 | A kind of graphene conductive agent |
| CN108091877A (en) * | 2016-11-23 | 2018-05-29 | 无锡格致新材料研发科技有限公司 | A kind of graphene denatured conductive agent and preparation method thereof |
| CN109599562A (en) * | 2018-12-17 | 2019-04-09 | 湖南艾华集团股份有限公司 | A kind of lithium battery electrocondution slurry and preparation method thereof |
| CN110165216A (en) * | 2018-04-12 | 2019-08-23 | 济南开发区星火科学技术研究院 | A kind of preparation method of graphene conductive agent |
| CN110890225A (en) * | 2019-11-13 | 2020-03-17 | 惠州学院 | Composite modified conductive agent for super capacitor and preparation method thereof |
| CN111710863A (en) * | 2020-06-28 | 2020-09-25 | 东莞市海洲新材料科技有限公司 | Graphene conductive agent, preparation method thereof, lithium ion battery cathode and lithium ion battery |
| CN116092723A (en) * | 2023-01-10 | 2023-05-09 | 厦门凯纳石墨烯技术股份有限公司 | High-dispersion high-conductivity graphene composite conductive slurry, preparation method and application |
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| CN108091877A (en) * | 2016-11-23 | 2018-05-29 | 无锡格致新材料研发科技有限公司 | A kind of graphene denatured conductive agent and preparation method thereof |
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| CN110165216A (en) * | 2018-04-12 | 2019-08-23 | 济南开发区星火科学技术研究院 | A kind of preparation method of graphene conductive agent |
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| CN111710863A (en) * | 2020-06-28 | 2020-09-25 | 东莞市海洲新材料科技有限公司 | Graphene conductive agent, preparation method thereof, lithium ion battery cathode and lithium ion battery |
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| CN116092723A (en) * | 2023-01-10 | 2023-05-09 | 厦门凯纳石墨烯技术股份有限公司 | High-dispersion high-conductivity graphene composite conductive slurry, preparation method and application |
| CN116092723B (en) * | 2023-01-10 | 2023-11-03 | 厦门凯纳石墨烯技术股份有限公司 | High-dispersion high-conductivity graphene composite conductive slurry, preparation method and application |
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