CN116190669A - Ultralight flame-retardant negative current collector and preparation method thereof - Google Patents

Ultralight flame-retardant negative current collector and preparation method thereof Download PDF

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Publication number
CN116190669A
CN116190669A CN202211738833.9A CN202211738833A CN116190669A CN 116190669 A CN116190669 A CN 116190669A CN 202211738833 A CN202211738833 A CN 202211738833A CN 116190669 A CN116190669 A CN 116190669A
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current collector
solution
copper
retardant
conductive carbon
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杜英杰
罗英
丁赵波
解晶莹
晏莉琴
郭瑞
马尚德
杨丞
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Shanghai Institute of Space Power Sources
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Shanghai Institute of Space Power Sources
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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
    • H01M4/64—Carriers or collectors
    • H01M4/66—Selection of materials
    • H01M4/665—Composites
    • H01M4/666—Composites in the form of mixed materials
    • 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
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • 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 provides an ultralight flame-retardant negative current collector and a preparation method thereof, wherein the current collector is prepared from the following raw materials in parts by mass: 20 parts of polyimide powder; 60-70 parts of copper-plated conductive carbon nanomaterial; 1-5 parts of dispersing agent; 10-15 parts of flame retardant. The copper-plated conductive carbon nanomaterial is copper-plated conductive graphite and/or copper-plated carbon nano tubes. According to the ultra-light flame-retardant negative current collector and the preparation method thereof, polyimide powder is used as a matrix, copper-plated conductive graphite and/or copper-plated carbon nano tubes are used as conductive fillers, and flame retardants are added, so that the density of the current collector can be effectively reduced, and the conductivity and safety performance of the current collector are ensured.

Description

Ultralight flame-retardant negative current collector and preparation method thereof
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to an ultralight flame-retardant negative current collector and a preparation method thereof.
Background
In recent years, the development of lithium batteries is gradually changed, and besides meeting the basic demands of daily life of consumers, the lithium batteries are also gradually in the brand-new corner in the fields of large-scale energy storage equipment such as electric automobiles, aerospace, energy storage power stations, smart grids and the like. This places higher demands on the energy density and safety of lithium batteries.
The improvement of the current collector has important significance for improving the performance of the lithium ion battery. The weight percentage of the current collector in the lithium ion battery is 15% -18%, and reducing the density of the current collector is an effective way for improving the energy density of the battery, which is why battery manufacturers continuously strive to reduce the thickness of the current collector. However, ultra-thin current collectors sacrifice the electrical conductivity, thermal dissipation, and mechanical properties of the metal foil, which in turn reduces battery power density. Researchers develop composite current collectors with metal layers covered on two sides of a polymer, and metal coatings are manufactured on two sides of a flexible polymer and plastic by adopting methods such as vapor deposition, magnetron sputtering and the like, and the density of the composite current collectors is far lower than that of pure metal current collectors, the texture of the composite current collectors is soft, and the composite current collectors are protruding in the field of flexible batteries, but the composite current collectors have the problems of high preparation cost, limited production scale and easiness in falling of the metal coatings.
In addition, burrs of the metal current collector are an important cause of short circuit in the battery, and the characteristics of flammability and intolerance to high temperature of the polymer current collector are buried potential safety hazards in the use of the lithium battery. Therefore, the ultra-light flame-retardant current collector has wide application prospect, and the premise is that the energy density and the safety performance of the battery are improved.
Disclosure of Invention
In order to overcome the defects in the prior art, the inventor performs intensive research, and provides an ultra-light flame-retardant negative current collector and a preparation method thereof, which reduce the density of the current collector and ensure the conductivity, mechanical property and safety performance of the current collector.
The technical scheme provided by the invention is as follows:
in the first aspect, the ultra-light flame-retardant negative electrode current collector is prepared from the following raw materials in parts by mass:
Figure BDA0004032363740000021
the copper-plated conductive carbon nanomaterial is copper-plated conductive graphite and/or copper-plated carbon nano tubes.
In a second aspect, a method for preparing an ultralight flame-retardant anode current collector includes the following steps:
1. and (5) pretreatment. Boiling the conductive carbon nanomaterial in NaOH solution, and then cleaning the conductive carbon nanomaterial to be neutral by deionized water to remove oil stains on the surface of the conductive carbon nanomaterial; then placing the carbon nano-material into a roughening solution for roughening treatment, placing the carbon nano-material into a sensitization solution for sensitization treatment, finally placing the carbon nano-material into an activating solution for activation, and cleaning the carbon nano-material with distilled water to complete pretreatment of the conductive carbon nano-material.
2. And (5) reduction. And adding the pretreated conductive carbon nanomaterial into formaldehyde solution for reduction treatment.
3. And (5) electroless copper plating. And adding the pre-reduced conductive carbon nanomaterial into plating solution, and stirring until the conductive carbon nanomaterial coats the copper layer with the determined thickness, thereby completing electroless copper plating of the conductive carbon nanomaterial.
4. And (5) passivating. And (3) adding the copper-plated conductive carbon nano material into passivation solution for passivation treatment to prevent the surface copper layer from being oxidized.
5. Wet film coating. Mixing polyimide powder, copper-plated conductive carbon nano material, flame retardant and dispersing agent according to a certain proportion, adding into N, N-dimethylacetamide, fully stirring to form uniform slurry, and coating a wet film on the plate.
6. And preparing a negative electrode current collector. And (3) soaking the plate coated with the wet film in water, taking out the stripped wet film, and drying to obtain the light flame-retardant negative current collector.
According to the ultra-light flame-retardant negative electrode current collector and the preparation method thereof, the ultra-light flame-retardant negative electrode current collector has the following beneficial effects:
(1) According to the ultralight flame-retardant negative current collector and the preparation method thereof, polyimide powder is used as a matrix, copper-plated conductive graphite and/or copper-plated carbon nano tubes are used as conductive fillers, and flame retardants are added, so that the density of the current collector can be effectively reduced, and the conductivity and the safety performance of the current collector are ensured;
(2) According to the ultra-light flame-retardant negative current collector and the preparation method thereof, a wet film coating and drying mode is adopted to obtain the negative current collector, a gradient heating method is adopted in a drying mode, a solvent is dried at a lower temperature of 80-120 ℃, polyimide powder is further and completely imidized at 180-250 ℃, and impurities are eliminated;
(3) According to the ultra-light flame-retardant negative current collector and the preparation method thereof, the negative current collector is obtained by adopting a wet film coating and drying mode, the process is simple, and the mechanical properties of the current collector are ensured.
Detailed Description
The features and advantages of the present invention will become more apparent and clear from the following detailed description of the invention.
The word "exemplary" is used herein to mean "serving as an example, embodiment, or illustration. Any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments.
According to a first aspect of the invention, an ultra-light flame-retardant negative electrode current collector is provided, and the ultra-light flame-retardant negative electrode current collector is prepared from the following raw materials in parts by mass:
Figure BDA0004032363740000031
the copper-plated conductive carbon nanomaterial is copper-plated conductive graphite and/or copper-plated carbon nano tubes;
the dispersing agent is at least one of polyvinylpyrrolidone (PVP), sodium Dodecyl Sulfate (SDS), sodium Dodecyl Benzene Sulfonate (SDBS) and Cetyl Trimethyl Ammonium Bromide (CTAB).
The flame retardant is a phosphorus flame retardant or aliphatic halogenated hydrocarbon, and an organic nitrogen flame retardant and a phosphorus flame retardant can be compounded.
According to a second aspect of the invention, there is provided a method for preparing an ultra-light flame-retardant anode current collector, comprising the steps of:
and (5) pretreatment. Boiling the conductive carbon nanomaterial in NaOH solution, and then cleaning the conductive carbon nanomaterial to be neutral by deionized water to remove oil stains on the surface of the conductive carbon nanomaterial; then placing the mixture into roughening solution for roughening treatment, placing the mixture into sensitization solution for sensitization treatment, finally placing the mixture into activation solution for activation, and cleaning the mixture with distilled water.
Wherein the concentration of the NaOH solution is 20-30%. Coarsening liquid is H 2 SO 4 、HNO 3 And the concentration of the mixed solution is 20-25%. The sensitization solution is obtained by the following steps: snCl is added 2 Dissolving the powder in 35% hydrochloric acid, and diluting with water to form sensitized solution, snCl 2 The concentration is 10-20g/L, the mass fraction of hydrochloric acid is 4%, and a small amount of tin particles are added to prevent SnCl 2 And (5) oxidizing. The activation solution is obtained by: ammonia water is added dropwise into 1-2g/L silver nitrate water solution until the solution turns from brown to colorless and transparent.
And (5) reduction. And adding the pretreated conductive carbon nanomaterial into formaldehyde solution for reduction treatment, wherein the concentration of the formaldehyde solution is 10-20wt%.
And (5) electroless copper plating. Adding the pre-reduced conductive carbon nanomaterial into plating solution, and slowly magnetically stirring until the conductive carbon nanomaterial coats a copper layer with a proper thickness. When the conductive carbon nanomaterial is conductive graphite, the proportion of the conductive carbon nanomaterial added in the plating solution is less than 1.5g/L; when the conductive carbon nanomaterial is a carbon nanotube, the ratio of the conductive carbon nanomaterial to the plating solution is less than 1g/L. The plating solution comprises the following components in percentage by weight: 20-30g/L of disodium ethylenediamine tetraacetate, 20-30g/L of potassium sodium tartrate, 10-20g/L of sodium hydroxide, 15-25g/L of copper sulfate and 25-35mL/L of formaldehyde (37%). The preferred plating solution comprises the following components in percentage by weight: 25g/L of disodium ethylenediamine tetraacetate, 25g/L of potassium sodium tartrate, 15g/L of sodium hydroxide, 20g/L of copper sulfate and 30mL/L of formaldehyde (37%).
And (5) passivating. And (3) adding the copper-plated conductive carbon nano material into passivation solution for passivation treatment to prevent the surface copper layer from being oxidized. The passivation solution is benzotriazole solution with the concentration of 0.5-1wt%.
Wet film coating. Mixing polyimide powder, copper-plated conductive graphite, copper-plated carbon nano tubes, a flame retardant and a dispersing agent in proportion, adding the mixture into N, N-Dimethylacetamide (DMAC), fully stirring the mixture to form uniform slurry, and coating a wet film on a glass plate by using a coating machine, wherein the solid content of the wet film slurry is 20-30wt%.
And preparing a negative electrode current collector. And (3) placing the glass plate coated with the wet film into water for soaking for 6-18 hours, taking out the peeled wet film, placing the wet film into a vacuum oven for drying, and obtaining the light flame-retardant negative electrode current collector. Drying and adopting a gradient heating method, preserving heat for 30-60 minutes at 80-120 ℃ for evaporating solvent DMAC, and preserving heat for 60-90 minutes at 180-250 ℃ to ensure that polyimide powder is fully imidized to generate the polyimide-based ultra-light flame-retardant negative electrode current collector.
Examples
Example 1
1. And (5) pretreatment. And (3) placing the conductive graphite and the carbon nano tube in NaOH solution for boiling, and then cleaning the conductive graphite and the carbon nano tube to be neutral by deionized water to remove oil stains on the surface. Then placing the mixture into roughening solution for roughening treatment, placing the mixture into sensitization solution for sensitization treatment, and finally placing the mixture into activation solution for activation. Distilled water is cleaned. Wherein, the concentration of the NaOH solution is 25%. Coarsening liquid is H 2 SO 4 The concentration was 25%. The sensitization solution is obtained by the following steps: snCl is added 2 Dissolving the powder in 35% hydrochloric acid, and diluting with water to form sensitized solution, snCl 2 The concentration of (2) is 15g/L, the mass fraction of hydrochloric acid is 4%, and a small amount of tin particles are added to prevent SnCl 2 And (5) oxidizing. The activation solution is obtained by: ammonia was added dropwise to 2g/L of the aqueous silver nitrate solution until the solution turned from brown to colorless and transparent.
2. And (5) reduction. And adding the pretreated conductive graphite and carbon nano tubes into formaldehyde solution for reduction treatment, wherein the concentration of the formaldehyde solution is 15%.
3. And (5) electroless copper plating. Adding the pre-reduced conductive graphite and carbon nano tube into the plating solution, and slowly magnetically stirring until the conductive graphite and the carbon nano tube are coated with a copper layer with proper thickness. Wherein, the proportion of the conductive graphite added in the plating solution is 1g/L, and the proportion of the carbon nano tube added in the plating solution is 0.5g/L. The plating solution comprises the following components in concentration: 25g/L of disodium ethylenediamine tetraacetate, 25g/L of potassium sodium tartrate, 15g/L of sodium hydroxide, 20g/L of copper sulfate and 30mL/L of formaldehyde (37%).
4. And (5) passivating. And adding the copper-plated conductive graphite and the carbon nano tube into passivation solution for passivation treatment to prevent the surface copper layer from being oxidized. The passivation solution is a benzotriazol solution with the concentration of 1 weight percent.
5. Wet film coating. Polyimide powder, copper-plated conductive graphite, copper-plated carbon nanotubes, triphenyl phosphate as a flame retardant and Cetyl Trimethyl Ammonium Bromide (CTAB) as a dispersing agent are mixed according to a certain proportion, added into N, N-dimethylacetamide, fully stirred to form uniform slurry, and a wet film is coated on a glass plate by using a coating machine. Wherein, the mass ratio of polyimide powder, copper-plated conductive graphite, copper-plated carbon nano tube, dispersing agent and flame retardant is 20:50:15:3:12, the wet film slurry had a solids content of 25wt%.
6. And preparing a negative electrode current collector. And (3) placing the glass plate coated with the wet film into water for soaking for 12 hours, taking out the stripped wet film, and placing the wet film into a vacuum oven for drying to obtain the light flame-retardant negative current collector. Drying by adopting a gradient heating method, preserving heat for 60 minutes at 80 ℃, and preserving heat for 90 minutes at 200 ℃ to prepare the polyimide-based ultra-light flame-retardant negative electrode current collector. The current collector performance results are shown in table 1.
Example 2
This example 2 corresponds to example 1, except that in this example, the mass ratio of polyimide powder, copper-plated conductive graphite, copper-plated carbon nanotubes, dispersant, flame retardant is 20:65:0:3:12. the current collector performance results are shown in table 1.
Example 3
This example 3 corresponds to example 1, except that in this example, the mass ratio of polyimide powder, copper-plated conductive graphite, copper-plated carbon nanotubes, dispersant, flame retardant is 20:0:63:5:12. the current collector performance results are shown in table 1.
Comparative example
Comparative example 1
1. Wet film coating. Polyimide powder, conductive graphite (not plated with copper), carbon nanotubes (not plated with copper), a flame retardant triphenyl phosphate, and a dispersant Cetyl Trimethyl Ammonium Bromide (CTAB) are mixed and added into N, N-dimethylacetamide, and the mixture is fully stirred to form uniform slurry, and a wet film is coated on a glass plate by using a coater. Wherein, the mass ratio of polyimide powder, conductive graphite, carbon nano tube, dispersing agent and flame retardant is 20:50:15:3:12, the wet film slurry had a solids content of 25wt%.
2. And preparing a negative electrode current collector. And (3) placing the glass plate coated with the wet film into water for soaking for 12 hours, taking out the stripped wet film, placing the wet film into a vacuum oven for drying, and obtaining the light flame-retardant negative current collector. Drying by adopting a gradient heating method, preserving heat for 60 minutes at 80 ℃, and preserving heat for 90 minutes at 200 ℃ to prepare the polyimide-based ultra-light flame-retardant negative electrode current collector. The current collector performance results are shown in table 1.
TABLE 1 collector Performance results
Figure BDA0004032363740000061
Figure BDA0004032363740000071
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The invention has been described in detail in connection with the specific embodiments and exemplary examples thereof, but such description is not to be construed as limiting the invention. It will be understood by those skilled in the art that various equivalent substitutions, modifications or improvements may be made to the technical solution of the present invention and its embodiments without departing from the spirit and scope of the present invention, and these fall within the scope of the present invention. The scope of the invention is defined by the appended claims.
What is not described in detail in the present specification is a well known technology to those skilled in the art.

Claims (10)

1. The ultra-light flame-retardant negative electrode current collector is characterized by being prepared from the following raw materials in parts by mass:
Figure FDA0004032363730000011
the copper-plated conductive carbon nanomaterial is copper-plated conductive graphite and/or copper-plated carbon nano tubes.
2. The ultra-light flame-retardant negative electrode current collector according to claim 1, wherein the dispersant is at least one of polyvinylpyrrolidone (PVP), sodium Dodecyl Sulfate (SDS), sodium Dodecyl Benzene Sulfonate (SDBS), cetyl trimethylammonium bromide (CTAB).
3. The ultra-light flame-retardant negative electrode current collector according to claim 1, wherein the flame retardant is at least one of a phosphorus flame retardant, an aliphatic halogenated hydrocarbon and an organic nitrogen flame retardant compounded phosphorus flame retardant.
4. A method for preparing the ultra-light flame-retardant anode current collector according to any one of claims 1 to 3, comprising the steps of:
mixing polyimide powder, copper-plated conductive carbon nano material, flame retardant and dispersing agent according to a certain proportion, adding into N, N-dimethylacetamide, fully stirring to form uniform slurry, and coating a wet film on a plate;
and (3) soaking the plate coated with the wet film in water, taking out the stripped wet film, and drying to obtain the light flame-retardant negative current collector.
5. The method for preparing an ultra-light flame-retardant anode current collector according to claim 4, wherein the solid content of the wet film coated on the plate is 20-30wt%.
6. The method for preparing an ultralight flame retardant anode current collector of claim 4, wherein, in the step of immersing the wet film coated plate in water, taking out the peeled wet film and drying, the wet film coated plate is immersed in water for 6-18 hours.
7. The method for preparing an ultralight flame retardant anode current collector as claimed in claim 4, wherein the step of immersing the plate coated with the wet film in water and taking out the peeled wet film to perform drying treatment is performed by a gradient heating method, wherein the drying treatment is performed by a temperature-rising method at 80-120 ℃ for 30-60 minutes, and the drying treatment is performed by evaporating solvent N, N-dimethylacetamide, and then by a temperature-rising method at 180-250 ℃ for 60-90 minutes, so that polyimide powder is completely imidized, and the polyimide-based ultralight flame retardant anode current collector is generated.
8. The method for preparing an ultra-light flame-retardant anode current collector according to claim 4, further comprising a step of preparing a copper-plated conductive carbon nanomaterial, comprising:
boiling the conductive carbon nanomaterial in NaOH solution, and then cleaning the conductive carbon nanomaterial to be neutral by deionized water to remove oil stains on the surface of the conductive carbon nanomaterial; then placing the carbon nano-material into a roughening solution for roughening treatment, placing the carbon nano-material into a sensitization solution for sensitization treatment, finally placing the carbon nano-material into an activating solution for activation, and cleaning the carbon nano-material with distilled water to complete pretreatment of the conductive carbon nano-material;
adding the pretreated conductive carbon nanomaterial into formaldehyde solution for reduction treatment;
adding the pre-reduced conductive carbon nanomaterial into plating solution, and stirring until the conductive carbon nanomaterial coats a copper layer with a determined thickness, thereby completing electroless copper plating of the conductive carbon nanomaterial;
and (3) adding the copper-plated conductive carbon nano material into passivation solution for passivation treatment to prevent the surface copper layer from being oxidized.
9. The method for preparing an ultra-light flame-retardant anode current collector according to claim 8, wherein in the pretreatment step, the concentration of NaOH solution is 20-30%; and/or
In the pretreatment step, the coarsening liquid is H 2 SO 4 、HNO 3 And the concentration of the mixed solution is 20-25%; and/or
In the pretreatment step, the sensitization solution is obtained by the following steps: snCl is added 2 Dissolving the powder in 35% hydrochloric acid, and diluting with water to form sensitized solution, snCl 2 The concentration is 10-20g/L, the mass fraction of hydrochloric acid is 4%, and a small amount of tin particles are added at the same timePreventing SnCl 2 Oxidizing; and/or
In the pretreatment step, the activating solution is obtained by: dropwise adding ammonia water into 1-2g/L silver nitrate water solution until the solution turns from brown to colorless and transparent; and/or
In the reduction treatment step, the concentration of formaldehyde solution is 10-20wt%; and/or
In the passivation treatment step, the passivation solution is benzotriazole solution with the concentration of 0.5-1wt%.
10. The method for preparing an ultra-light flame-retardant negative electrode current collector according to claim 8, wherein in the electroless copper plating step, when the conductive carbon nanomaterial is conductive graphite, the ratio of the conductive carbon nanomaterial to the plating solution is <1.5g/L; when the conductive carbon nano material is a carbon nano tube, the proportion of the conductive carbon nano material added in the plating solution is less than 1g/L; and/or
In the electroless copper plating step, each component and the concentration in the plating solution are as follows: 20-30g/L of disodium ethylenediamine tetraacetate, 20-30g/L of potassium sodium tartrate, 10-20g/L of sodium hydroxide, 15-25g/L of copper sulfate and 25-35mL/L of 37% formaldehyde.
CN202211738833.9A 2022-12-30 2022-12-30 Ultralight flame-retardant negative current collector and preparation method thereof Pending CN116190669A (en)

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