CN105702935A - Preparation method of multilayer anode with porous carbon composite material - Google Patents
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H—ELECTRICITY
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- 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
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- 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
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- 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
- H01M4/134—Electrodes based on metals, Si or alloys
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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
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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- H—ELECTRICITY
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- 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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of a multilayer anode with a porous carbon composite material. According to the method provided by the invention, the activity of the material can be increased by utilizing porous carbon spheres with relatively large specific surface areas; a copper plated aluminum foil with a rough surface is selected in structure; the copper plated aluminum foil has the advantage of large specific surface area; through adoption of the relatively large specific surface area and a concave-convex structure, volume expansion of tin in a charge-discharge process can be buffered well; moreover, the structure plays a framework role; the volume expansion and shrinkage stress in the charge-discharge process can be buffered greatly; the first time charge-discharge efficiency of the anode material is 76%; when the anode material discharges in 400mA/g, after the anode material cycles for 360 cycles, the capacity retention ratio is 79%; and when the anode material discharges in 600mA/g, after the anode material cycles for 480 cycles, the capacity retention ratio is 88%. The method provided by the invention is simple in technology and easy in control and is applicable to large scale production.
Description
Technical field
The present invention relates to a kind of multilamellar negative pole preparation method possessing porous carbon composite。
Background technology
Lithium ion battery is mainly made up of shell, positive pole, negative pole, electrolyte and barrier film, and wherein negative material is mainly material with carbon element。Current business-like lithium ion battery negative material has graphite-like carbon, easy graphitized carbon (soft carbon), amorphous carbon (hard carbon) material three major types, but the theoretical specific capacity of graphite only has 372mAh/g, and manufacturing cost is high, poor safety performance;Though soft material with carbon element has substantial amounts of Turbostratic and heteroatom such as hydrogen etc. so that it is having higher specific capacity (being typically in 600-800mAh/g), but its voltage delay is big, initial coulomb efficiency is low, and it is very fast to decay, and therefore practical application is extremely restricted;Compared with soft material with carbon element, the platform of hard carbon material is relatively low, and efficiency and cycle life are all improved first, but specific capacity is lower than soft material with carbon element。
Summary of the invention
The present invention provides a kind of multilamellar negative pole preparation method possessing porous carbon composite, the negative pole using the method to prepare, and has high connductivity, high rate capability and long circulating performance。
To achieve these goals, the present invention provides a kind of multilamellar negative pole preparation method possessing porous carbon composite, and the method comprises the steps:
(1) the silicon/silicon dioxide nano composite material that porous carbon bag is wrapped up in
Octaphenyl-the POSS of 1.5mmol is dissolved in 1, the 2-dichloroethanes that 70mL temperature is about 60 DEG C, about magnetic agitation 1h at 60 DEG C, adds the AlCl of 2mmol3The CCl of catalyst and 40mL4Cross-linking agent carries out cross-linking reaction, and after reacting 10 hours, the alcoholic solution of 95wt% adding 100mL terminates reaction with the mixed solution (in mixed solution, alcoholic solution is 4:1 with the volume ratio of water) of water, filters subsequently, obtains cross-linking reaction product;
Cross-linking reaction product is carried out by the mixed solution (in mixed solution, alcoholic solution is 3:1 with the volume ratio of dilute hydrochloric acid solution) and the water that adopt the dilute hydrochloric acid solution of the alcoholic solution of 95wt% and 5wt%, then dries 12h at 80 DEG C again;Subsequently, dried cross-linking reaction product it is warming up to 900 DEG C with the heating rate of 2 DEG C/min under nitrogen atmosphere and is incubated 3h, obtaining carbonized product;
Above-mentioned carbonized product is placed in the sodium hydroxide solution of 20wt% and etches 12h, take out subsequently, through washing, filtration, dry, obtain the silicon/silicon dioxide nano composite material that porous carbon bag is wrapped up in;
(2) aluminium foil being carried out pretreatment: be sequentially carried out electrochemical deoiling, acid etching, once heavy zinc at aluminium foil surface, move back zinc, the heavy zinc of secondary and washing, the thickness of described aluminium foil is 15-20 μm;
One layer of copper coating of aluminium foil side electroplating surface after the pre-treatment also activates, and copper coating adopts pulse plating regime plating, and its surface roughness is 0.4-3.0 μm, and thickness is 2-8 μm;
Copper coating after activation is electroplated one layer of tin coating;
The silicon/silicon dioxide nano composite material that the porous carbon bag obtained on being coated with a layer on described tin coating is wrapped up in, the thickness of the silicon/silicon dioxide nanometer composite layer that porous carbon bag is wrapped up in is 80-150 μm;
(3) heat treatment: temperature is 80-100 DEG C, heat treatment time is 12-20 hour。
Preferably, the thickness of described tin coating is 0.1-1.0 μm, and electrotinning coating adopts the tin plating formula of impulse jet plating and technological parameter as follows:
Impulse jet electroplating technological parameter: electric current density: 5-15A/dm2;
PH value: 3-4;
Temperature: 45-55 DEG C;
Time: 5-20s。
The present invention can utilize the porous carbon ball with large specific surface area to promote the activity of material, structure has been selected a kind of rough surface copper facing aluminium foil, this copper facing aluminium foil has the advantage that specific surface area is big, bigger specific surface area and concaveconvex structure can well cushion stannum volumetric expansion in charge and discharge process, this structure also acts as good skeleton function simultaneously, the stress that in buffering charge and discharge process, volumetric expansion is shunk greatly。Negative material first charge-discharge efficiency is 76%, discharges with 400mA/g, circulates 360 weeks, and capability retention is 79%, discharges with 600mA/g, circulates 480 weeks, and capability retention is 88%。This inventive method technique is simple, easy to control, is suitable for large-scale production。
Detailed description of the invention
Embodiment one
Octaphenyl-the POSS of 1.5mmol is dissolved in 1, the 2-dichloroethanes that 70mL temperature is about 60 DEG C, about magnetic agitation 1h at 60 DEG C, adds the AlCl of 2mmol3The CCl of catalyst and 40mL4Cross-linking agent carries out cross-linking reaction, and after reacting 10 hours, the alcoholic solution of 95wt% adding 100mL terminates reaction with the mixed solution (in mixed solution, alcoholic solution is 4:1 with the volume ratio of water) of water, filters subsequently, obtains cross-linking reaction product。
Cross-linking reaction product is carried out by the mixed solution (in mixed solution, alcoholic solution is 3:1 with the volume ratio of dilute hydrochloric acid solution) and the water that adopt the dilute hydrochloric acid solution of the alcoholic solution of 95wt% and 5wt%, then dries 12h at 80 DEG C again;Subsequently, dried cross-linking reaction product it is warming up to 900 DEG C with the heating rate of 2 DEG C/min under nitrogen atmosphere and is incubated 3h, obtaining carbonized product。
Above-mentioned carbonized product is placed in the sodium hydroxide solution of 20wt% and etches 12h, take out subsequently, through washing, filtration, dry, obtain the silicon/silicon dioxide nano composite material that porous carbon bag is wrapped up in。
Aluminium foil being carried out pretreatment: be sequentially carried out electrochemical deoiling, acid etching, once heavy zinc at aluminium foil surface, move back zinc, the heavy zinc of secondary and washing, the thickness of described aluminium foil is 15 μm;
One layer of copper coating of aluminium foil side electroplating surface after the pre-treatment also activates, and copper coating adopts pulse plating regime plating, and its surface roughness is 0.4 μm, and thickness is 2 μm;
Copper coating after activation is electroplated one layer of tin coating;
The silicon/silicon dioxide nano composite material that the porous carbon bag obtained on being coated with a layer on described tin coating is wrapped up in, the thickness of the silicon/silicon dioxide nanometer composite layer that porous carbon bag is wrapped up in is 80 μm。
The thickness of described tin coating is 0.1 μm, and electrotinning coating adopts the tin plating formula of impulse jet plating and technological parameter as follows:
Impulse jet electroplating technological parameter: electric current density: 5A/dm2;
PH value: 3-4;
Temperature: 45 DEG C;
Time: 5s。
Carrying out heat treatment, heat treatment temperature is 80 DEG C, and heat treatment time is 12 hours。
Embodiment two
Octaphenyl-the POSS of 1.5mmol is dissolved in 1, the 2-dichloroethanes that 70mL temperature is about 60 DEG C, about magnetic agitation 1h at 60 DEG C, adds the AlCl of 2mmol3The CCl of catalyst and 40mL4Cross-linking agent carries out cross-linking reaction, and after reacting 10 hours, the alcoholic solution of 95wt% adding 100mL terminates reaction with the mixed solution (in mixed solution, alcoholic solution is 4:1 with the volume ratio of water) of water, filters subsequently, obtains cross-linking reaction product。
Cross-linking reaction product is carried out by the mixed solution (in mixed solution, alcoholic solution is 3:1 with the volume ratio of dilute hydrochloric acid solution) and the water that adopt the dilute hydrochloric acid solution of the alcoholic solution of 95wt% and 5wt%, then dries 12h at 80 DEG C again;Subsequently, dried cross-linking reaction product it is warming up to 900 DEG C with the heating rate of 2 DEG C/min under nitrogen atmosphere and is incubated 3h, obtaining carbonized product。
Above-mentioned carbonized product is placed in the sodium hydroxide solution of 20wt% and etches 12h, take out subsequently, through washing, filtration, dry, obtain the silicon/silicon dioxide nano composite material that porous carbon bag is wrapped up in。
Aluminium foil being carried out pretreatment: be sequentially carried out electrochemical deoiling, acid etching, once heavy zinc at aluminium foil surface, move back zinc, the heavy zinc of secondary and washing, the thickness of described aluminium foil is 20 μm;
One layer of copper coating of aluminium foil side electroplating surface after the pre-treatment also activates, and copper coating adopts pulse plating regime plating, and its surface roughness is 3.0 μm, and thickness is 8 μm;
Copper coating after activation is electroplated one layer of tin coating;
Being coated with the silicon/silicon dioxide nano composite material that porous carbon bag is wrapped up on described tin coating, the thickness of the silicon/silicon dioxide nanometer composite layer that porous carbon bag is wrapped up in is 150 μm。
The thickness of described tin coating is 1.0 μm, and electrotinning coating adopts the tin plating formula of impulse jet plating and technological parameter as follows:
Impulse jet electroplating technological parameter: electric current density: 15A/dm2;
PH value: 3-4;
Temperature: 55 DEG C;
Time: 20s。
Carrying out heat treatment, temperature is 100 DEG C, and heat treatment time is 20 hours。
The present invention is described by embodiment, but do not limit the invention, with reference to description of the invention, other changes of the disclosed embodiments, as the professional person for this area is readily apparent that, such change should belong within the scope that the claims in the present invention limit。
Claims (2)
1. possessing a multilamellar negative pole preparation method for porous carbon composite, the method comprises the steps:
(1) the silicon/silicon dioxide nano composite material that porous carbon bag is wrapped up in
Octaphenyl-the POSS of 1.5mmol is dissolved in 1, the 2-dichloroethanes that 70mL temperature is about 60 DEG C, about magnetic agitation 1h at 60 DEG C, adds the AlCl of 2mmol3The CCl of catalyst and 40mL4Cross-linking agent carries out cross-linking reaction, and after reacting 10 hours, the alcoholic solution of 95wt% adding 100mL terminates reaction with the mixed solution (in mixed solution, alcoholic solution is 4:1 with the volume ratio of water) of water, filters subsequently, obtains cross-linking reaction product;
Cross-linking reaction product is carried out by the mixed solution (in mixed solution, alcoholic solution is 3:1 with the volume ratio of dilute hydrochloric acid solution) and the water that adopt the dilute hydrochloric acid solution of the alcoholic solution of 95wt% and 5wt%, then dries 12h at 80 DEG C again;Subsequently, dried cross-linking reaction product it is warming up to 900 DEG C with the heating rate of 2 DEG C/min under nitrogen atmosphere and is incubated 3h, obtaining carbonized product;
Above-mentioned carbonized product is placed in the sodium hydroxide solution of 20wt% and etches 12h, take out subsequently, through washing, filtration, dry, obtain the silicon/silicon dioxide nano composite material that porous carbon bag is wrapped up in;
(2) aluminium foil being carried out pretreatment: be sequentially carried out electrochemical deoiling, acid etching, once heavy zinc at aluminium foil surface, move back zinc, the heavy zinc of secondary and washing, the thickness of described aluminium foil is 15-20 μm;
One layer of copper coating of aluminium foil side electroplating surface after the pre-treatment also activates, and copper coating adopts pulse plating regime plating, and its surface roughness is 0.4-3.0 μm, and thickness is 2-8 μm;
Copper coating after activation is electroplated one layer of tin coating;
The silicon/silicon dioxide nano composite material that the porous carbon bag obtained on being coated with a layer on described tin coating is wrapped up in, the thickness of the silicon/silicon dioxide nanometer composite layer that porous carbon bag is wrapped up in is 80-150 μm;
(3) heat treatment: temperature is 80-100 DEG C, heat treatment time is 12-20 hour。
2. the method for claim 1, it is characterised in that the thickness of described tin coating is 0.1-1.0 μm, electrotinning coating adopts the tin plating formula of impulse jet plating and technological parameter as follows:
Impulse jet electroplating technological parameter: electric current density: 5-15A/dm2;
PH value: 3-4;
Temperature: 45-55 DEG C;
Time: 5-20s。
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108365184A (en) * | 2018-01-02 | 2018-08-03 | 江苏大学 | A kind of lithium ion battery porous SiOC negative materials of rich carbon and preparation method thereof |
CN108448096A (en) * | 2018-03-29 | 2018-08-24 | 深圳市贝特瑞新能源材料股份有限公司 | A kind of hud typed amorphous carbon based composites of high power capacity, preparation method and the lithium ion battery comprising it |
WO2018187908A1 (en) * | 2017-04-10 | 2018-10-18 | 深圳市佩成科技有限责任公司 | Preparation method for ti3c2tx/sulfur-carbon composite material |
CN109065866A (en) * | 2018-08-02 | 2018-12-21 | 武汉理工大学 | A kind of silicon-carbon composite cathode material and preparation method thereof based on silsesquioxane |
CN117410480A (en) * | 2023-12-13 | 2024-01-16 | 湖南镕锂新材料科技有限公司 | Hard carbon negative electrode material of lithium battery |
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CN105280879A (en) * | 2014-05-28 | 2016-01-27 | 北京有色金属研究总院 | Silica/carbon composite porous electrode and preparation method thereof |
CN105449180A (en) * | 2015-12-30 | 2016-03-30 | 湘潭大学 | Aluminum/copper/tin/graphite multilayer structure lithium ion battery cathode material and preparation method thereof |
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2018187908A1 (en) * | 2017-04-10 | 2018-10-18 | 深圳市佩成科技有限责任公司 | Preparation method for ti3c2tx/sulfur-carbon composite material |
CN108365184A (en) * | 2018-01-02 | 2018-08-03 | 江苏大学 | A kind of lithium ion battery porous SiOC negative materials of rich carbon and preparation method thereof |
CN108448096A (en) * | 2018-03-29 | 2018-08-24 | 深圳市贝特瑞新能源材料股份有限公司 | A kind of hud typed amorphous carbon based composites of high power capacity, preparation method and the lithium ion battery comprising it |
CN108448096B (en) * | 2018-03-29 | 2021-01-01 | 贝特瑞新材料集团股份有限公司 | High-capacity core-shell type amorphous carbon-based composite material, preparation method thereof and lithium ion battery comprising same |
CN109065866A (en) * | 2018-08-02 | 2018-12-21 | 武汉理工大学 | A kind of silicon-carbon composite cathode material and preparation method thereof based on silsesquioxane |
CN109065866B (en) * | 2018-08-02 | 2021-07-06 | 武汉理工大学 | Silsesquioxane-based silicon-carbon composite negative electrode material and preparation method thereof |
CN117410480A (en) * | 2023-12-13 | 2024-01-16 | 湖南镕锂新材料科技有限公司 | Hard carbon negative electrode material of lithium battery |
CN117410480B (en) * | 2023-12-13 | 2024-03-12 | 湖南镕锂新材料科技有限公司 | Hard carbon negative electrode material of lithium battery |
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Application publication date: 20160622 |