CN115403033A - Conductive agent for lithium ion battery, negative electrode and preparation method thereof, and lithium ion battery - Google Patents
Conductive agent for lithium ion battery, negative electrode and preparation method thereof, and lithium ion battery Download PDFInfo
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- CN115403033A CN115403033A CN202211228553.3A CN202211228553A CN115403033A CN 115403033 A CN115403033 A CN 115403033A CN 202211228553 A CN202211228553 A CN 202211228553A CN 115403033 A CN115403033 A CN 115403033A
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 60
- 239000006258 conductive agent Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title abstract description 18
- 239000002109 single walled nanotube Substances 0.000 claims abstract description 36
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000007773 negative electrode material Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 12
- 229910052799 carbon Inorganic materials 0.000 claims description 11
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 238000005411 Van der Waals force Methods 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 238000001338 self-assembly Methods 0.000 claims description 7
- 238000005096 rolling process Methods 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000006183 anode active material Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 2
- 238000007086 side reaction Methods 0.000 abstract description 10
- 239000002041 carbon nanotube Substances 0.000 abstract description 7
- 229910021393 carbon nanotube Inorganic materials 0.000 abstract description 7
- 239000003792 electrolyte Substances 0.000 abstract description 6
- 239000000654 additive Substances 0.000 abstract description 5
- 239000002270 dispersing agent Substances 0.000 abstract description 4
- 230000009467 reduction Effects 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 3
- 238000007599 discharging Methods 0.000 abstract description 2
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 239000002002 slurry Substances 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 239000010406 cathode material Substances 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910013872 LiPF Inorganic materials 0.000 description 1
- 101150058243 Lipf gene Proteins 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
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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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- 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
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H01M4/139—Processes of manufacture
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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Abstract
The invention provides a conductive agent for a lithium ion battery, a negative electrode, a preparation method and the lithium ion battery, wherein the conductive agent is a single-walled carbon nanotube net structure formed by self-assembling pure single-walled carbon nanotubes under van der Waals acting force, namely, the conductive agent only contains one component of the single-walled carbon nanotubes, additives such as a dispersing agent and the like are not required to be added in the preparation process, the purity of the conductive agent is effectively ensured, and the preparation process of the conductive agent is simplified; moreover, when the conductive agent is used for the negative electrode of the lithium ion battery, even though the negative active material and the electrolyte can generate side reaction during the charging and discharging processes of the electrode and an SEI film is generated on the surface of the negative electrode, the conductive agent with the single-arm carbon nanotube net structure and the negative active material have good electrical contact performance, so that the problems of conductivity reduction, electric contact loss and the like caused by the side reaction (SEI film generation) of the electrode can be effectively relieved.
Description
Technical Field
The invention relates to the technical field of new energy materials and preparation thereof, and particularly relates to a conductive agent for a lithium ion battery, a negative electrode, a preparation method and the lithium ion battery.
Background
With the global energy shortage and the improvement of environmental protection consciousness, new energy becomes the current important development direction, and lithium ion batteries become a hotspot of the energy industry by virtue of the advantages of high working voltage, no memory effect, small self-discharge, long cycle life and the like, and are widely applied to mobile electronic products such as mobile phones, computers and the like.
The silicon (Si) -based negative electrode material for the lithium ion battery has the theoretical specific capacity (the theoretical specific capacity of pure silicon is 4200mAh/g, and the theoretical specific capacity of graphite is 372 mAh/g) which is far higher than that of graphite, and is a promising negative electrode material for the lithium ion battery. However, the conductivity of the silicon anode material is low, and silicon and LiPF in the electrolyte 6 The components generate side reaction to generate Li 2 SiF 6 Resulting in electrical contact failure at the electrode level, ultimately resulting in capacity loss, limiting its cycling stability and service life.
The silicon-carbon cathode material for the lithium ion battery is the preferred cathode material for the lithium ion battery with high specific capacity, wide material source and the like, but if the carbon layer is not coated strictly, the growth of a solid electrolyte is thicker, and the poor electronic conductivity and the high expansion rate of the material greatly hinder the cycle and rate performance of the silicon-carbon cathode material.
Therefore, it is necessary to alleviate the side reaction of the negative electrode for lithium ion battery, enhance the electrical contact capability of the electrode, and improve the first efficiency of the battery.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a conductive agent for a lithium ion battery, which is applied to the lithium ion battery and solves the problems of low first-effect and poor cycle performance of the silicon-carbon cathode system of the conventional lithium ion battery. In addition, due to the super strong van der waals force action between the single-walled carbon nanotube and the active silicon carbon particles of the negative electrode, the influence of side reaction on electric contact can be reduced, so that the method has wide application prospect in the electrochemical industry. On the other hand, the invention also provides a negative electrode for the lithium ion battery, a preparation method and the lithium ion battery.
The specific invention content is as follows:
in a first aspect, the invention provides a conductive agent for a lithium ion battery, wherein the conductive agent is composed of a single-walled carbon nanotube; the conductive agent is in a net-shaped single-wall carbon nanotube structure formed by self-assembly of single-wall carbon nanotubes.
Optionally, the pipe diameter of the single-walled carbon nanotube is 2-3nm, and the thickness of the reticular single-walled carbon nanotube structure is 3-10000nm.
Optionally, the sheet resistance of the mesh-shaped single-wall carbon nanotube structure is 10-50 Ω.
In a second aspect, the present invention provides a negative electrode for a lithium ion battery, the negative electrode comprising a negative electrode active material and the conductive agent of the first aspect.
Optionally, the anode active material comprises silicon @ carbon or siliconoxide @ carbon.
In a third aspect, the present invention provides a method for preparing the negative electrode for a lithium ion battery according to the second aspect, including the steps of:
s1, self-assembling the single-walled carbon nanotube into a net structure by virtue of Van der Waals force;
s2, contacting the reticular single-wall carbon nanotube structure with a negative active material, wherein the reticular single-wall carbon nanotube structure is combined with the negative active material by virtue of Van der Waals acting force;
and S3, rolling the material prepared in the step 2 and a current collector into a whole to prepare the negative electrode for the lithium ion battery.
In a fourth aspect, the present invention provides a lithium ion battery comprising the negative electrode for a lithium ion battery according to the second aspect.
Compared with the prior art, the invention has the following advantages:
the conductive agent for the lithium ion battery provided by the invention is a reticular single-wall carbon nanotube structure formed by self-assembling pure single-wall carbon nanotubes under van der Waals acting force, namely, the conductive agent only contains one component of the single-wall carbon nanotubes, and additives such as a dispersing agent and the like are not required to be added in the preparation process. The purity of the conductive agent is effectively ensured, and the preparation process of the conductive agent is simplified.
The negative electrode for the lithium ion battery comprises the negative electrode active material and the conductive agent, and the conductive agent with the net structure (the single-arm carbon nanotube net structure) and the silicon carbon negative electrode material have strong van der Waals acting force, so the conductive agent (the single-arm carbon nanotube net structure) can be self-assembled to form the battery negative electrode under the action of the van der Waals force after contacting with the silicon carbon negative electrode active material, and the preparation process of the electrode is simplified. In addition, in the electrode charging and discharging process, even though the negative active material and the electrolyte can generate side reaction to generate an SEI film on the surface of the negative electrode, the conductive agent with the single-arm carbon nanotube net structure and the negative active material have good electrical contact performance, so that the problems of conductivity reduction, electric contact loss and the like caused by the side reaction (SEI film generation) of the electrode can be effectively relieved.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present application, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 shows a scanning electron micrograph of a conductive agent provided by an embodiment of the present invention;
fig. 2 is a flowchart illustrating a method for manufacturing a negative electrode for a lithium ion battery according to an embodiment of the present invention;
fig. 3 shows a cycle performance chart of the lithium ion batteries provided in example 1 of the present invention and the comparative example.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The specific experimental procedures or conditions are not indicated in the examples and can be performed according to the procedures or conditions of the conventional experimental procedures described in the prior art in this field. The reagents and other instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
The existing conductive agent is usually stored and used in the form of conductive agent slurry, and the existing carbon nano tube conductive agent for the lithium ion battery is not well dispersed due to large molecular acting force between carbon tubes, so that a plurality of additives such as dispersing agents and the like are required to be added in the preparation process of the conductive slurry, and the difficulty and the complexity of the preparation of the conductive agent are increased to a certain extent. Meanwhile, the presence of the additive increases the internal resistance (Re) and charge transport resistance of the battery to some extent. Is not beneficial to the circulation of the battery and the first coulomb efficiency improvement.
In view of the above, the first objective of the present invention is to provide a conductive agent for lithium ion batteries, wherein the conductive agent is composed of single-walled carbon nanotubes; the conductive agent is in a net single-wall carbon nanotube structure formed by self-assembly of single-wall carbon nanotubes.
In the specific implementation, the conductive agent is a single-walled carbon nanotube net structure formed by self-assembly of pure single-walled carbon nanotubes under van der waals acting force, namely, the conductive agent only contains one component of the single-walled carbon nanotubes, the single-walled carbon nanotubes are mutually combined through physical acting force (van der waals acting force), and additives such as a dispersing agent, an adhesive and the like are not required to be added in the preparation process. The purity of the conductive agent is effectively ensured, and the preparation process of the conductive agent is simplified. Fig. 1 shows a scanning electron micrograph of a conductive agent provided in an embodiment of the present invention.
In some embodiments, the diameter of the single-walled carbon nanotube may be 2 to 3nm, and the thickness of the reticular single-walled carbon nanotube structure may be 3 to 10000nm.
In some embodiments, the sheet resistance of the reticulated single-walled carbon nanotube structure is 10-50 Ω.
A second object of the present invention is to provide a negative electrode for a lithium ion battery, the negative electrode comprising a negative electrode active material and the conductive agent according to the first aspect.
In specific implementation, the composition of the negative electrode for the lithium ion battery provided by the invention comprises a negative electrode active material and the conductive agent of the first aspect, and the conductive agent with a net structure (a net single-arm carbon nanotube structure) and the silicon carbon negative electrode material have strong van der waals acting force, so that the conductive agent can be self-assembled to form the battery negative electrode under the action of van der waals force after contacting the silicon carbon negative electrode active material, and the preparation process of the electrode is simplified. Moreover, the single-walled carbon nanotube structure cannot be corroded by electrolyte, and even though a negative active material and the electrolyte can generate side reaction to generate an SEI film on the surface of a negative electrode in the cyclic charge and discharge process, the conductive agent with the single-walled carbon nanotube net structure and the negative active material have good electrical contact performance, so that the problems of conductivity reduction, electric contact loss and the like caused by the side reaction (SEI film generation) of the electrode can be effectively relieved, the electrode still keeps good electronic and ionic conductivity, and meanwhile, the electrode material can be endowed with certain flexibility.
In some embodiments, the anode active material may be silicon @ carbon or silica @ carbon.
A third objective of the present invention is to provide a method for preparing a negative electrode for a lithium ion battery according to the second aspect, and fig. 2 shows a flowchart of a method for preparing a negative electrode for a lithium ion battery according to an embodiment of the present invention, and as shown in fig. 2, the method includes the following steps:
s1, self-assembling the single-walled carbon nanotube into a net structure by virtue of Van der Waals force;
s2, contacting a net structure formed by self-assembly of the single-walled carbon nanotubes with a negative electrode active material, wherein the net structure formed by self-assembly of the single-walled carbon nanotubes is combined with the negative electrode active material by virtue of Van der Waals acting force;
and S3, rolling the material prepared in the step 2 and a current collector into a whole to prepare the negative electrode for the lithium ion battery.
A fourth object of the present invention is a lithium ion battery comprising the negative electrode for a lithium ion battery according to the second aspect.
In specific implementation, the lithium ion battery provided by the invention has good electrical contact performance between the conductive agent with the mesh single-arm carbon nanotube structure and the negative active material, and can effectively relieve the problems of conductivity reduction, electric contact loss and the like caused by side reaction (SEI film generation) between an electrode and an electrolyte, so that the lower internal resistance (Re) and charge transfer resistance (Rct) of the battery are ensured, the cycle and the first coulombic efficiency of the battery are improved, and the lithium ion battery has wide application prospects in the electrochemical industry.
In order to make the present application more clearly understood by those skilled in the art, the conductive agent for lithium ion battery, the negative electrode and the preparation method thereof, and the lithium ion battery described in the present application will now be described in detail by the following examples.
Example 1
At normal temperature, the single-walled carbon nanotube is self-assembled into a conductive network form by Van der Waals force;
combining a silica @ carbon as an active component with a conductive network;
rolling the obtained material and a current collector into a whole, wherein the rolling thickness is 0.03mm, and preparing a pole piece;
assembling the obtained pole pieces into a lithium ion battery;
the electrochemical performance of the cells was tested using the LANDHE cell testing system and electrochemical multifunction workstation (Biologic, VSP-300).
Example 2
The difference from example 1 is that: the active substance is not silica @ carbon but silicon @ carbon.
Comparative example 1
Commercial single-walled carbon nanotube slurry was mixed with a binder, silica @ carbon, in a certain ratio (5.
Coating and drying the copper foil current collector to obtain an electrode plate;
assembling a button cell;
the electrochemical performance of the cells was tested using the LANDEH cell testing system and electrochemical multifunction workstation (Biologic, VSP-300).
Fig. 3 shows a cycle performance diagram of the lithium ion batteries provided in example 1 and comparative example of the present invention, and as shown in fig. 3, the lithium ion battery provided in example 1 of the present invention uses a mesh-shaped single-arm carbon nanotube structure as a conductive agent, and the lithium ion battery provided in comparative example uses a single-wall carbon nanotube slurry as a conductive agent, it can be seen that the cycle performance of the lithium ion battery provided in example 1 is significantly better than that of comparative example 1.
Table 1 comparison of electrochemical performance of lithium ion batteries provided in example 1 and comparative examples
Electricity-buckling battery | Example 1 | Control sample |
First discharge capacity (mAh/g) | 1785.4 | 1513.6 |
First coulombic efficiency (%) | 81.52 | 72.35 |
Internal resistance of half cell (omega) | 17.85 | 80.69 |
Resistance to charge transfer (omega) | 2.63 | 3.52 |
Table 1 shows the results of testing the electrochemical performance of the lithium ion batteries provided in example 1 and comparative example by using a LANDHE battery testing system and an electrochemical multifunctional workstation (Biologic, VSP-300), and as shown in table 1, the lithium ion battery provided in example 1 of the present invention using a one-armed carbon nanotube network as a conductive agent has better performance in terms of first discharge capacity, first coulombic efficiency, half-cell internal resistance, and charge transfer resistance than the lithium ion battery using a single-walled carbon nanotube slurry as a conductive agent in the comparative example.
The conductive agent for a lithium ion battery, the negative electrode, the preparation method and the lithium ion battery provided by the invention are described in detail, specific examples are applied in the description to explain the principle and the implementation mode of the invention, and the description of the examples is only used for helping to understand the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present invention.
Claims (7)
1. The conductive agent for the lithium ion battery is characterized in that the composition of the conductive agent is a single-walled carbon nanotube; the conductive agent is in a net single-wall carbon nanotube structure formed by self-assembly of single-wall carbon nanotubes.
2. The conductive agent as claimed in claim 1, wherein the tube diameter of the single-walled carbon nanotube is 2-3nm, and the thickness of the reticular single-walled carbon nanotube structure is 3-10000nm.
3. The conductive agent as claimed in claim 1, wherein the sheet resistance of the reticulated single-walled carbon nanotube structure is 10-50 Ω.
4. A negative electrode for a lithium ion battery, comprising a negative electrode active material and the conductive agent according to any one of claims 1 to 2.
5. The anode of claim 1, wherein the anode active material comprises silicon @ carbon or silica @ carbon;
the particle diameter of the negative electrode active material is 2 to 100 μm.
6. The method for preparing the negative electrode for the lithium ion battery according to claim 4, comprising the steps of:
s1, self-assembling the single-walled carbon nanotube into a net structure by virtue of Van der Waals force;
s2, enabling a reticular single-wall carbon nanotube structure formed by self-assembly of the single-wall carbon nanotube to be in contact with a negative electrode active material, wherein the reticular single-wall carbon nanotube structure is combined with the negative electrode active material by virtue of Van der Waals acting force;
and S3, rolling the material prepared in the step 2 and a current collector into a whole to prepare the negative electrode for the lithium ion battery.
7. A lithium ion battery comprising the negative electrode for a lithium ion battery according to claim 4.
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