CN113488654A - Graphene composite layered conductive agent supported by carbon nano tube - Google Patents
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Abstract
The invention provides a graphene composite layered conductive agent supported by a carbon nano tube. The graphene composite material comprises layered graphene and interlayer carbon nanotubes, wherein the carbon nanotubes are generated in situ between layers of the layered graphene to support the whole layered graphene. The invention also relates to a preparation method of the graphene composite layered conductive agent supported by the carbon nano tube. Performing amide reaction on aminated cobalt-based mof and acylchlorinated graphene, and performing H reaction2S and H2Calcining in a mixed atmosphere, and finally continuously introducing ethanol to obtain the graphene composite layered conductive agent supported by the carbon nano tube. By inserting cobalt-based mof between layers of graphene and taking the cobalt-based as a growth point, carbon nanotubes grow between layers of graphene to promote the separation between the graphene, a carbon nanotube-supported graphene laminated structure is formed, and the problem of stone is solvedDue to the overlapping problem caused by pi-pi bond conjugation, the pore volume and the surface specific area of the structure are enlarged, and the conductive efficiency is improved.
Description
Technical Field
The invention relates to the technical field of graphene, in particular to a graphene composite layered conductive agent supported by a carbon nano tube.
Background
Graphene, a novel carbon material, has ultrahigh electron mobility and excellent electron conductivity, and has been widely used as a conductive additive for lithium ion batteries. Similarly, the carbon nanotube material also has excellent electronic conductivity, and the conductivity of the lithium battery can be effectively improved by taking the graphene and the carbon nanotube as the electrolyte cooperatively.
Chinese patent CN202110159492.9 discloses a carbon nanotube graphene composite conductive agent and a preparation method thereof, which uses flake graphite as a raw material, uses anhydrous ferric chloride for intercalation treatment, and then transfers the flake graphite to a high-pressure reaction kettle for heat preservation treatment to obtain ferric chloride intercalated flake graphite powder. After the ferric chloride intercalated flake graphite powder is heated by plasma arc, a reaction atmosphere is introduced under certain conditions by adopting an in-situ synthesis method to obtain a carbon nano tube graphene composite material; adding a solvent and a dispersant, grinding, and further synthesizing the carbon nanotube graphene composite conductive agent. However, the pi-pi bond conjugation between the graphene in the preparation method can cause graphene overlapping, and meanwhile, the carbon nano tube is difficult to form an effective continuous network structure, so that the conductivity is limited.
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a graphene composite layered conductive agent supported by a carbon nano tube, which solves the problem that graphene is overlapped due to pi-pi bond conjugation, thereby improving the conductivity of the material.
(II) technical scheme
In order to solve the technical problems, the invention provides the following technical scheme:
a graphene composite layered conductive agent supported by carbon nano tubes comprises layered graphene and interlayer carbon nano tubes, wherein the carbon nano tubes are generated in situ between layers of the layered graphene to support the whole layered graphene.
A preparation method of a graphene composite laminar conductive agent supported by carbon nano tubes comprises the following steps:
(1) preparation of aminated cobalt-based mof
Respectively weighing 2-aminoterephthalic acid and cobalt acetate tetrahydrate, dissolving the 2-aminoterephthalic acid and the cobalt acetate tetrahydrate in an N, N-dimethylformamide solution, dropwise adding a sodium hydroxide solution into the solution, uniformly dispersing by ultrasonic waves, transferring the solution into a high-pressure kettle, sealing, reacting, filtering to obtain purple powder, cleaning for 1-4 times by using methanol, and drying to obtain aminated cobalt-based mof;
(2) preparation of acylchlorinated graphene
Dispersing graphene oxide in tetrahydrofuran, and performing ultrasonic treatment for 1h to obtain a graphene oxide dispersion liquid; adding SOCl2Adding the obtained product into graphene oxide dispersion liquid, heating in an oil bath, refluxing, centrifuging, washing black precipitate, and removing redundant thionyl chloride to obtain acyl chlorinated graphene;
(3) preparation of graphene material with cobalt-based mof intercalated between layers
Dissolving the prepared aminated cobalt-based mof and acylchlorinated graphene in deionized water, stirring and mixing for amidation reaction, filtering, washing and drying to obtain a graphene material with cobalt-based mof inserted between layers;
(4) preparation of graphene composite layered conductive agent supported by carbon nano tube
Placing the graphene material for preparing cobalt-based mof in a corundum plate, then placing the corundum plate in a tubular furnace, firstly purging the reactor with argon flow, and then placing the reactor in a H mode2Calcining under flowing down; subsequently, H is introduced into the reactor2S and H2Continuing the reaction; introducing argon flow, cooling the reactor to 50-70 ℃, and continuously introducing ethanol into the reactor for reaction; and naturally cooling to room temperature to obtain the graphene composite layered conductive agent supported by the carbon nano tube.
Preferably, in the step (1), the mass ratio of the cobalt acetate tetrahydrate, the 2-aminoterephthalic acid, the N, N-dimethylformamide and the potassium hydroxide is 1:1-2: 30-60: 5-20 parts of;
preferably, in the step (1), the autoclave reaction condition is 80-160 ℃ for 1-3 d;
preferably, in the step (2), graphene oxide and SOCl are used2In a mass ratio of
1：1-50；
Preferably, in the step (2), graphene oxide and SOCl are used2The reaction conditions of (a) are: heating in oil bath at 60-80 deg.C, and refluxing for 12-24 hr;
preferably, in the step (3), the mass ratio of aminated cobalt-based mof, graphene chloride acylate and deionized water is as follows: 1:1-10: 10-100;
preferably, in the step (3), the amidation reaction is carried out for 8 to 12 hours at a temperature of between 60 and 70 ℃;
preferably, H in said step (4)2The reaction conditions of the down-flow tube furnace were: calcining at 600 ℃ and 900 ℃ for 15-30 minutes;
preferably, the reaction is continued in the step (4) for 10 to 40 minutes;
preferably, the reaction condition after the ethanol is introduced in the step (4) is that the reaction is carried out for 20 to 60 minutes at the temperature of between 50 and 70 ℃;
preferably, H in said step (4)2The flow rate of (A) is 50-100 sccm; h2The flow rate of S is 2-10 sccm; the flow rate of the argon gas flow is 300-500 sccm.
(III) advantageous technical effects
Compared with the prior art, the invention has the following chemical mechanism and beneficial technical effects:
(1) the invention relates to a graphene composite layered conductive agent supported by a carbon nano tube, which has the chemical mechanism that: reacting 2-amino terephthalic acid with cobalt acetate tetrahydrate, and then dropwise adding a sodium hydroxide solution to obtain aminated cobalt-based mof; mixing graphene oxide and SOCl2Reacting to obtain acyl chlorinated graphene; then, carrying out amidation reaction on the aminated cobalt-based mof and acylchlorinated graphene to obtain a graphene material with an interlayer inserted cobalt-based mof; inserting the obtained graphene material with cobalt-based mof between layers in H2S and H2Calcining in mixed atmosphere to generate Co in situ9S8The nano particles are used as an intermediate, and finally, the Co is added by a chemical vapor deposition method and ethanol is introduced9S8Further converted into metal Co nano particles with narrow size distribution, and cobalt is taken as a growth point to generate a carbon nano tube network, thereby obtaining the graphene composite laminar conductive agent supported by the carbon nano tube.
(2) According to the graphene laminated structure supported by the carbon nano tubes, the cobalt-based mof is inserted between layers of graphene, the cobalt-based is taken as a growth point, the carbon nano tubes grow between layers of graphene, and the growth of the carbon nano tubes promotes the separation of the graphene, so that the laminated structure of the graphene supported by the carbon nano tubes is formed, the problem of overlapping of the graphene due to pi-pi bond conjugation is solved, and the conductivity of the graphene is improved.
(3) According to the method, the connectivity of cobalt-based mof and graphene is enhanced by the method of grafting cobalt-based mof and the surface of graphene, the generated carbon nano tube has high dispersibility in the graphene, and meanwhile, the generated carbon nano tube three-dimensional network structure has high pore volume and large specific surface area, so that the electric connection among particles is enhanced, and the utilization rate of the carbon nano tube is improved; finally, the carbon nano tube and the graphene can generate a synergistic effect, and the conductive efficiency is improved.
Detailed Description
To achieve the above object, the present invention provides the following embodiments and examples:
example 1
A preparation method of a graphene composite laminar conductive agent supported by carbon nano tubes comprises the following steps:
(1) preparation of aminated cobalt-based mof
Respectively weighing 10g of 2-aminoterephthalic acid and 5g of cobalt acetate tetrahydrate, dissolving in 50ml of N, N-dimethylformamide solution, dropwise adding a sodium hydroxide solution into 30ml of the solution, uniformly dispersing by using ultrasonic waves, transferring the solution into an autoclave, sealing, reacting for 3 days at 160 ℃, filtering to obtain purple powder, cleaning for 1-4 times by using methanol, and drying to obtain aminated cobalt-based mof.
(2) Preparation of acylchlorinated graphene
Dispersing 5g of graphene oxide in 50ml of tetrahydrofuran, and carrying out ultrasonic treatment for 1 hour to obtain a graphene oxide dispersion liquid; adding SOCl2And adding the graphene oxide into the graphene oxide dispersion liquid, heating in an oil bath at the temperature of 80 ℃, refluxing for 24 hours, centrifuging, washing black precipitate, and removing redundant thionyl chloride to obtain the acyl chlorinated graphene.
(3) Preparation of graphene material with cobalt-based mof intercalated between layers
Dissolving 2g of prepared aminated cobalt-based mof and 10g of acylchlorinated graphene in 50ml of deionized water, stirring, carrying out amidation reaction at 70 ℃ for 12h, filtering, washing and drying to obtain the graphene material with the cobalt-based mof intercalated between layers.
(4) Preparation of graphene composite layered conductive agent supported by carbon nano tube
The graphene material for preparing the cobalt-based mof is placed in a corundum plate and then placed in a tube furnace. The reactor was first purged with a 300sccm argon flow, then with 50sccm H2Calcining at 900 deg.c for 30 min; next, 5sccmdeH was introduced into the reactor2S and H of 100sccm2Continuing the reaction for 40 minutes; then introducing argon flow of 500sccm to cool the reactor to 50 ℃, and then continuously introducing 20ml of ethanol into the reactor to react for 60 minutes; and naturally cooling to room temperature to obtain the graphene composite layered conductive agent supported by the carbon nano tube.
Example 2
A preparation method of a graphene composite laminar conductive agent supported by carbon nano tubes comprises the following steps:
(1) preparation of aminated cobalt-based mof
Respectively weighing 10g of 2-aminoterephthalic acid and 5g of cobalt acetate tetrahydrate, dissolving in 50ml of N, N-dimethylformamide solution, dropwise adding 30ml of sodium hydroxide solution into the solution, uniformly dispersing by ultrasonic waves, transferring the solution into an autoclave, sealing, reacting at 160 ℃ for 3 days, filtering to obtain purple powder, washing with methanol for 1-4 times, and drying to obtain aminated cobalt-based mof.
(2) Preparation of acylchlorinated graphene
Dispersing 5g of graphene oxide in 50ml of tetrahydrofuran, and carrying out ultrasonic treatment for 1 hour to obtain a graphene oxide dispersion liquid; adding SOCl2And adding the graphene oxide into the graphene oxide dispersion liquid, heating in an oil bath at the temperature of 80 ℃, refluxing for 24 hours, centrifuging, washing black precipitate, and removing redundant thionyl chloride to obtain the acyl chlorinated graphene.
(3) Preparation of graphene material with cobalt-based mof intercalated between layers
3g of prepared aminated cobalt-based mof and 10g of acylchlorinated graphene are dissolved in 50ml of deionized water, stirred, subjected to amidation reaction at 70 ℃ for 12 hours, filtered, washed and dried to obtain the graphene material with the cobalt-based mof intercalated between layers.
(4) Preparation of graphene composite layered conductive agent supported by carbon nano tube
Cobalt-based mof stone will be preparedThe graphene material was placed in a corundum dish and then placed in a tube furnace. The reactor was first purged with a 300sccm argon flow, then with 50sccm H2Calcining at 900 deg.c for 30 min; next, 5sccmdeH was introduced into the reactor2S and H of 100sccm2Continuing the reaction for 40 minutes; then introducing argon flow of 500sccm to cool the reactor to 50 ℃, and then continuously introducing 20ml of ethanol into the reactor to react for 60 minutes; and naturally cooling to room temperature to obtain the graphene composite layered conductive agent supported by the carbon nano tube.
Example 3
A preparation method of a graphene composite laminar conductive agent supported by carbon nano tubes comprises the following steps:
(1) preparation of aminated cobalt-based mof
Respectively weighing 10g of 2-aminoterephthalic acid and 5g of cobalt acetate tetrahydrate, dissolving in 50ml of N, N-dimethylformamide solution, dropwise adding 30ml of sodium hydroxide solution into the solution, uniformly dispersing by ultrasonic waves, transferring the solution into an autoclave, sealing, reacting at 160 ℃ for 3 days, filtering to obtain purple powder, washing with methanol for 1-4 times, and drying to obtain aminated cobalt-based mof.
(2) Preparation of acylchlorinated graphene
Dispersing 5g of graphene oxide in 50ml of tetrahydrofuran, and carrying out ultrasonic treatment for 1 hour to obtain a graphene oxide dispersion liquid; adding SOCl2And adding the graphene oxide into the graphene oxide dispersion liquid, heating in an oil bath at the temperature of 80 ℃, refluxing for 24 hours, centrifuging, washing black precipitate, and removing redundant thionyl chloride to obtain the acyl chlorinated graphene.
(3) Preparation of graphene material with cobalt-based mof intercalated between layers
4g of prepared aminated cobalt-based mof and 10g of acylchlorinated graphene are dissolved in 50ml of deionized water, stirred, subjected to amidation reaction at 70 ℃ for 12 hours, filtered, washed and dried to obtain the graphene material with the cobalt-based mof intercalated between layers.
(4) Preparation of graphene composite layered conductive agent supported by carbon nano tube
The graphene material for preparing the cobalt-based mof is placed in a corundum plate and then placed in a tube furnace. The reactor was first purged with a 300sccm argon flow, then with 50sccm H2Calcining at 900 deg.c for 30 min; next, 5sccmdeH was introduced into the reactor2S and H of 100sccm2Continuing the reaction for 40 minutes; then introducing argon flow of 500sccm to cool the reactor to 50 ℃, and then continuously introducing 20ml of ethanol into the reactor to react for 60 minutes; and naturally cooling to room temperature to obtain the graphene composite layered conductive agent supported by the carbon nano tube.
Example 4
A preparation method of a graphene composite laminar conductive agent supported by carbon nano tubes comprises the following steps:
(1) preparation of aminated cobalt-based mof
Respectively weighing 10g of 2-aminoterephthalic acid and 5g of cobalt acetate tetrahydrate, dissolving in 50ml of N, N-dimethylformamide solution, dropwise adding 30ml of sodium hydroxide solution into the solution, uniformly dispersing by ultrasonic waves, transferring the solution into an autoclave, sealing, reacting at 160 ℃ for 3 days, filtering to obtain purple powder, washing with methanol for 1-4 times, and drying to obtain aminated cobalt-based mof.
(2) Preparation of acylchlorinated graphene
Dispersing 5g of graphene oxide in 50ml of tetrahydrofuran, and carrying out ultrasonic treatment for 1 hour to obtain a graphene oxide dispersion liquid; adding SOCl2And adding the graphene oxide into the graphene oxide dispersion liquid, heating in an oil bath at the temperature of 80 ℃, refluxing for 24 hours, centrifuging, washing black precipitate, and removing redundant thionyl chloride to obtain the acyl chlorinated graphene.
(3) Preparation of graphene material with cobalt-based mof intercalated between layers
5g of prepared aminated cobalt-based mof and 10g of acylchlorinated graphene are dissolved in 50ml of deionized water, stirred, subjected to amidation reaction at 70 ℃ for 12h, filtered, washed and dried to obtain the graphene material with the cobalt-based mof intercalated between layers.
(4) Preparation of graphene composite layered conductive agent supported by carbon nano tube
The graphene material for preparing the cobalt-based mof is placed in a corundum plate and then placed in a tube furnace. The reactor was first purged with a 300sccm argon flow, then with 50sccm H2Calcining at 900 deg.c for 30 min; next, 5sccmdeH was introduced into the reactor2S and H of 100sccm2Continuing the reaction for 40 minutes; then is introduced into the chamber 500sccm argon flow, cooling the reactor to 50 ℃, and then continuously introducing 20ml ethanol into the reactor for reacting for 60 minutes; and naturally cooling to room temperature to obtain the graphene composite layered conductive agent supported by the carbon nano tube.
Comparative example 1
The preparation method of the graphene composite layered conductive agent comprises the following steps:
(1) preparation of cobalt-based mof graphene material
Dissolving 5g of cobalt-based mof and 10g of graphene oxide in 50ml of deionized water, stirring, mixing at 70 ℃ for 12h, filtering, washing and drying to obtain the cobalt-based mof graphene material.
(2) Preparation of graphene composite layered conductive agent supported by carbon nano tube
The prepared cobalt-based mof graphene material was placed in a corundum plate and then placed in a tube furnace. The reactor was first purged with a 300sccm argon flow, then with 50sccm H2Calcining at 900 deg.c for 30 min; next, 5sccmdeH was introduced into the reactor2S and H of 100sccm2Continuing the reaction for 40 minutes; then introducing argon flow of 500sccm to cool the reactor to 50 ℃, and then continuously introducing 20ml of ethanol into the reactor to react for 60 minutes; and naturally cooling to room temperature to obtain the graphene composite layered conductive agent supported by the carbon nano tube.
Comparative example 2
A preparation method of a graphene composite laminar conductive agent supported by carbon nano tubes comprises the following steps:
(1) preparation of aminated cobalt-based mof
Respectively weighing 10g of 2-aminoterephthalic acid and 5g of cobalt acetate tetrahydrate, dissolving in 50ml of N, N-dimethylformamide solution, dropwise adding 30ml of sodium hydroxide solution into the solution, uniformly dispersing by ultrasonic waves, transferring the solution into an autoclave, sealing, reacting at 160 ℃ for 3 days, filtering to obtain purple powder, washing with methanol for 1-4 times, and drying to obtain aminated cobalt-based mof.
(2) Preparation of acylchlorinated graphene
Dispersing 5g of graphene oxide in 50ml of tetrahydrofuran, and carrying out ultrasonic treatment for 1 hour to obtain a graphene oxide dispersion liquid; adding SOCl2Adding to oxygenAnd (3) melting the graphene dispersion liquid, heating in an oil bath at the temperature of 80 ℃, refluxing for 24 hours, centrifuging, washing black precipitate, and removing redundant thionyl chloride to obtain the acyl chlorinated graphene.
(3) Preparation of graphene material with cobalt-based mof intercalated between layers
5g of prepared aminated cobalt-based mof and 10g of acylchlorinated graphene are dissolved in 50ml of deionized water, stirred, subjected to amidation reaction at 70 ℃ for 12h, filtered, washed and dried to obtain the graphene material with the cobalt-based mof intercalated between layers.
(4) Preparation of graphene composite layered conductive agent
The graphene material for preparing the cobalt-based mof is placed in a corundum plate and then placed in a tube furnace. The reactor was first purged with a 300sccm argon flow, then with 50sccm H2Calcining at 900 deg.c for 70 min; and naturally cooling to room temperature to obtain the graphene composite layered conductive agent.
And (3) testing:
the graphene composite layered conductive agent obtained in examples 1-4 and comparative examples 1-2 was used to prepare a lithium ion battery with a capacity of 10Ah, and a 60 ℃ storage data test was performed, and the test results are shown in Table 1.
Table 1:
the batteries prepared from the conductive agents obtained in examples 1-4 and comparative examples 1-2 were tested for specific discharge capacity (lithium removal) at-10 deg.C and 20 deg.C according to the operating specification of the battery charge and discharge tester, and the test results are shown in Table 2
Table 2:
in summary, according to examples 1 to 4, the conductive performance and the heat resistance of the carbon nanotube-supported graphene composite layered conductive agent are gradually improved with the increase of the content of cobalt-based mof in graphene, which indicates that the graphene conductive structure prepared by the present invention has excellent conductive performance.
In comparative example 1, cobalt-based mof and graphene were not grafted by amidation reaction, and it can be seen that, in accordance with example 4, cobalt-based mof was not grafted to have poor conductivity, which may be related to the dispersibility of cobalt-based mof in graphene, so that grafting cobalt-based mof and graphene can effectively improve conductivity and heat resistance; in comparative example 2, in which the catalyst of sulfiding cobalt-based mof and removing ethanol during calcination was removed, it can be seen that the conductivity of the graphene material was reduced, possibly due to insufficient formation of a network structure of carbon nanotubes between the layers of graphene, resulting in a decrease in electrical connectivity, so sulfiding cobalt-based mof and then catalyzing with ethanol was more advantageous to the formation of carbon nanotubes, thereby forming a layered structure.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (7)
1. The graphene composite layered conductive agent supported by the carbon nano tube is characterized by comprising layered graphene and an interlayer carbon nano tube, wherein the carbon nano tube is generated in situ between layers of the layered graphene to support the whole layered graphene.
2. The carbon nanotube-supported graphene composite layered conductive agent according to claim 1, wherein a method for preparing a carbon nanotube-supported graphene composite layered conductive agent comprises the following steps:
(1) preparation of aminated cobalt-based mof
Respectively weighing 2-aminoterephthalic acid and cobalt acetate tetrahydrate, dissolving the 2-aminoterephthalic acid and the cobalt acetate tetrahydrate in an N, N-dimethylformamide solution, dropwise adding a sodium hydroxide solution into the solution, uniformly dispersing by ultrasonic waves, transferring the solution into a high-pressure kettle, sealing, reacting, filtering to obtain purple powder, cleaning for 1-4 times by using methanol, and drying to obtain aminated cobalt-based mof;
(2) preparation of acylchlorinated graphene
Dispersing graphene oxide in tetrahydrofuran, and performing ultrasonic treatment for 1h to obtain a graphene oxide dispersion liquid; adding SOCl2Adding the obtained product into graphene oxide dispersion liquid, heating in an oil bath, refluxing, centrifuging, washing black precipitate, and removing redundant thionyl chloride to obtain acyl chlorinated graphene;
(3) preparation of graphene material with cobalt-based mof intercalated between layers
Dissolving the prepared aminated cobalt-based mof and acylchlorinated graphene in deionized water, stirring and mixing for amidation reaction, filtering, washing and drying to obtain a graphene material with cobalt-based mof inserted between layers;
(4) preparation of graphene composite layered conductive agent supported by carbon nano tube
Placing the graphene material for preparing cobalt-based mof in a corundum plate, then placing the corundum plate in a tubular furnace, firstly purging the reactor with argon flow, and then placing the reactor in a H mode2Calcining under flowing down; subsequently, H is introduced into the reactor2S and H2Continuing the reaction; introducing argon flow, cooling the reactor, and continuously introducing ethanol into the reactor for reaction; and naturally cooling to room temperature to obtain the graphene composite layered conductive agent supported by the carbon nano tube.
3. The method for preparing the carbon nanotube-supported graphene composite layered conductive agent according to claim 2, wherein the mass ratio of cobalt acetate tetrahydrate, 2-aminoterephthalic acid, N-dimethylformamide and potassium hydroxide in the step (1) is 1:1-2: 30-60: 5-20 parts of; the autoclave reaction condition is that the reaction is carried out for 1-3d at the temperature of 80-160 ℃.
4. The method for preparing the carbon nanotube supported graphene composite layered conductive agent as claimed in claim 2, wherein the graphene oxide and SOCl in the step (2) are2The mass ratio of (1): 1 to 50; graphene oxide and SOCl2The reaction conditions of (a) are: heating in oil bath at 60-80 deg.C, and refluxing for 12-24 hr.
5. The method for preparing the graphene composite layered conductive agent supported by the carbon nanotubes as claimed in claim 2, wherein the mass ratio of the aminated cobalt-based mof, the acylchlorinated graphene and the deionized water in the step (3) is as follows: 1:1-10: 10-100; the amidation reaction is carried out for 8 to 12 hours at a temperature of between 60 and 70 ℃.
6. The method for preparing the carbon nanotube supported graphene composite layered conductive agent as claimed in claim 2, wherein the step (4) is performed by using H2The reaction conditions of the down-flow tube furnace were: calcining at 600 ℃ and 900 ℃ for 15-30 minutes; the continuous reaction time is 10-40 minutes; the reaction condition after the ethanol is introduced is that the reaction is carried out for 20 to 60 minutes at the temperature of between 50 and 70 ℃.
7. The method for preparing the carbon nanotube supported graphene composite layered conductive agent as claimed in claim 2, wherein the step (4) is performed by using H2The flow rate of (A) is 50-100 sccm; h2The flow rate of S is 2-10 sccm; the flow rate of the argon gas flow is 300-500 sccm.
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| CN115117349A (en) * | 2022-06-30 | 2022-09-27 | 合肥国轩高科动力能源有限公司 | Elastic conductive network conductive agent for silicon-carbon cathode of lithium ion battery, preparation method of slurry of conductive agent and lithium ion battery |
| CN115117349B (en) * | 2022-06-30 | 2023-10-10 | 合肥国轩高科动力能源有限公司 | Elastic conductive network conductive agent for silicon-carbon negative electrode of lithium ion battery, preparation method of slurry of elastic conductive network conductive agent and lithium ion battery |
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