CN106654156A - Preparation method of lithium ion cell negative electrode piece - Google Patents
Preparation method of lithium ion cell negative electrode piece Download PDFInfo
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- CN106654156A CN106654156A CN201611255715.7A CN201611255715A CN106654156A CN 106654156 A CN106654156 A CN 106654156A CN 201611255715 A CN201611255715 A CN 201611255715A CN 106654156 A CN106654156 A CN 106654156A
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- Prior art keywords
- preparation
- lithium ion
- negative electrode
- composite
- ion battery
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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
- H01M4/04—Processes of manufacture in general
- H01M4/0438—Processes of manufacture in general by electrochemical processing
- H01M4/045—Electrochemical coating; Electrochemical impregnation
- H01M4/0452—Electrochemical coating; Electrochemical impregnation from solutions
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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
-
- 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
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
-
- 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 a preparation method of a lithium ion cell negative electrode piece. The preparation method comprises the following steps: 1) uniformly mixing carbon material and silicon-based material to obtain a compound material, wherein the mass percent of the carbon material in the compound material is 90%-95%; 2) orderly performing chemical degreasing, chemical roughening, sensitization treatment and activation treatment on the compound material; 3) immersing the compound material into a plating solution, performing chemical plating for 1-2min at the temperature of 70-90 DEG C, wherein the plating solution comprises copper salt in concentration of 20-80g/L, other metal salt in concentration of 10-150g/L, coordination agent in concentration of 100-300g/L, reducing agent in concentration of 3-20g/L, grain refiner in concentration of 0.1-5g/L, and dispersing agent in concentration of 1-10g/L; and 4) performing mechanical stirring and ultrasonic treatment, and immersing the negative current collector into the plating solution to perform the compound chemical plating.
Description
【Technical field】
The invention belongs to cell art, more particularly to a kind of preparation method of lithium ion battery negative electrode.
【Background technology】
Lithium ion battery due to specific energy is big, monomer running voltage height, operating temperature range width, have extended cycle life,
Self discharge is little, it is environmentally friendly the advantages of, have broad application prospects in the field such as portable electronics and electric motor car.It is wide at present
General use graphite-like lithium ion battery negative material, but exist first efficiency it is low, high rate performance is poor, electrolyte difficulty of matching
The defect of the aspect such as big.In high rate charge-discharge, because graphite negative electrodes material can not quickly finish embedding lithium/de- lithium, lead
Capacity is caused to decline, temperature rise is obvious, so as to bring certain potential safety hazard.Additionally, in order to lift high rate performance, can typically improve and lead
The content of electric agent, but also result in the reduction of battery capacity.
In consideration of it, real be necessary to provide a kind of preparation method of lithium ion battery negative electrode to overcome disadvantages described above.
【The content of the invention】
Present invention proposition is a kind of can to improve the electric conductivity of lithium ion battery, while taking into account the lithium of gram volume and high rate performance
The preparation method of ion battery cathode pole piece.
A kind of preparation method of lithium ion battery negative electrode that the present invention is provided, comprises the following steps：
1) carbon materials and silica-base material are uniformly mixed to get into carbon materials in composite, and the composite
Mass fraction is 90%-95%；
2) electrochemical deoiling, chemistry roughening, sensitized treatment and activation processing are carried out successively to the composite；
3) composite is immersed in plating solution, chemical plating 1-2min is carried out at a temperature of 70-90 DEG C；The plating solution
Including going back for the mantoquita, other slaines of 10-150g/L, the complexant of 100-300g/L, 3-20g/L that concentration is 20-80g/L
The dispersant of former agent, the grain refiner of 0.1-5g/L and 1-10g/L；
4) mechanical agitation and supersound process are carried out, and negative current collector is immersed in the plating solution carries out composite electroless-plating.
In a preferred embodiment, step 1) in, the carbon materials is CNT, carbon nano-fiber, carbon are received
At least one in rice ball, Graphene, graphite.
In a preferred embodiment, step 1) in, the silica-base material is nano-silicon, nano silicon oxide, silicon nanometer
At least one in line, nano-tube, porous silica material.
In a preferred embodiment, step 2) in, by the composite be put into industrial alcohol, acetone wherein one
Electrochemical deoiling is carried out in kind or mixed solution.
In a preferred embodiment, step 2) in, by electrochemical deoiling after the composite washed, then
Being put in fuming nitric aicd, concentrated sulphuric acid, one kind of boric acid or wherein several mixed solutions carries out chemical roughening.
In a preferred embodiment, step 2) in, the composite after chemistry roughening is washed, then
It is put into SnCl2Hydrochloric acid solution in carry out sensitized treatment.
In a preferred embodiment, step 2) in, by sensitized treatment after the composite washed, then
Being put in the halogenide of palladium or silver nitrate solution carries out activation processing.
In a preferred embodiment, step 3) in, the mantoquita be copper sulfate, copper chloride, wherein the one of Schweinfurt green
Kind；Described other slaines are nickel, stannum, silver, zinc, the sulfate of gold, chloride or ammonium salt, or the one of which of alkali metal salt
Or it is several；The complexant is carboxylic acid, polyamines, sulfonic acid, the one of which of nitrogenous silane or several；The reducing agent is hypophosphorous acid
Salt, alkali metal borohydride, the one of which of solubility borane compound or several；The grain refiner be lead salt, pink salt,
Zinc salt, the one of which of sulfur-containing compound or several；The dispersant is alcohol, acetone, tetrahydrofuran, ethyl acetate, toluene
One of which is several.
In a preferred embodiment, step 4) in, mechanical agitation intensity is 400-2000r/min, ultrasonic frequency
For 20-130KHz.
In a preferred embodiment, step 4) in, the negative current collector is Copper Foil, and silicon-carbon microgranule is in Copper Foil table
Volume fraction in the deposited plating layer in face is 30%-40%.
The preparation method of the lithium ion battery negative electrode that the present invention is provided, carries out being made after chemical plating to Si-C composite material
Make it be deposited on copper foil of affluxion body surface by Ni-P again, it is not necessary to use binding agent, further improve negative electrode
The problems such as efficiency first of material is low, irreversible capacity is big, high rate performance is poor, further improves the capacity of lithium battery and forthright again
Energy.The method also has process is simple, the controllable advantage of cathode pole piece thickness.
【Description of the drawings】
The schematic flow sheet of the preparation method of the lithium ion battery negative electrode that Fig. 1 is provided for the present invention.
Fig. 2 be Fig. 1 shown in lithium ion battery negative electrode preparation method in a specific embodiment obtained lithium
The SEM figures of negative pole piece of battery.
Fig. 3 be Fig. 2 shown in lithium ion battery negative electrode with compare charging/discharging voltage-appearance of the pole piece under different multiplying
Amount curve comparison.
Fig. 4 is the lithium ion battery negative electrode and the charge and discharge cycles curve comparison for compareing pole piece shown in Fig. 2.
【Specific embodiment】
Fig. 1 is refer to, the present invention provides a kind of preparation method of lithium ion battery negative electrode, comprises the following steps：
1) carbon materials and silica-base material are uniformly mixed to get into carbon materials in composite, and the composite
Mass fraction is 90%-95%, and correspondingly, the mass fraction of the silica-base material is 10%-5%.Specifically, the carbon material
Expect at least one in CNT, carbon nano-fiber, Nano carbon balls, Graphene, graphite；The silica-base material is nanometer
At least one in silicon, nano silicon oxide, silicon nanowires, nano-tube, porous silica material.
2) electrochemical deoiling, chemistry roughening, sensitized treatment and activation processing are carried out successively to the composite.Specifically,
The composite is put in industrial alcohol, the one of which of acetone or mixed solution first carry out electrochemical deoiling；To change again
Learn the composite after oil removing to be washed, be put into fuming nitric aicd, concentrated sulphuric acid, one kind of boric acid or wherein several mixing molten
Chemical roughening is carried out in liquid；Next the composite after chemistry roughening is washed, is put into SnCl2Hydrochloric acid solution
In carry out sensitized treatment；Finally by sensitized treatment after the composite washed, be put into the halogenide or silver nitrate of palladium
Activation processing is carried out in solution.
3) composite is immersed in plating solution, chemical plating 1-2min is carried out at a temperature of 70-90 DEG C；The plating solution
Including going back for the mantoquita, other slaines of 10-150g/L, the complexant of 100-300g/L, 3-20g/L that concentration is 20-80g/L
The dispersant of former agent, the grain refiner of 0.1-5g/L and 1-10g/L.Specifically, the mantoquita is copper sulfate, copper chloride, vinegar
The one of which of sour copper；Described other slaines are nickel, stannum, silver, zinc, the sulfate of gold, chloride or ammonium salt, or alkali metal
The one of which of salt is several；The complexant is carboxylic acid, polyamines, sulfonic acid, the one of which of nitrogenous silane or several；It is described to go back
Former agent is hypophosphites, alkali metal borohydride, the one of which of solubility borane compound or several；The grain refiner
For lead salt, pink salt, zinc salt, the one of which of sulfur-containing compound or several；The dispersant is alcohol, acetone, tetrahydrofuran, acetic acid
Ethyl ester, the one of which of toluene or several.
4) mechanical agitation and supersound process are carried out, and negative current collector is immersed in the plating solution carries out composite electroless-plating.
Negative current collector Jing after composite electroless-plating is the lithium ion prepared by the preparation method of lithium ion battery negative electrode of the present invention
Negative pole piece of battery；Originally specifically, mechanical agitation intensity is 400-2000r/min, and ultrasonic frequency is 20-130KHz.It is described
Negative current collector is Copper Foil, and volume fraction of the silicon-carbon microgranule in the deposited plating layer of copper foil surface is 30%-40%.
Using the composite by carbon materials and silica-base material in the preparation method of the lithium ion battery negative electrode,
Principle is as follows：The actual capacity of graphite negative electrodes material is lower than theoretical capacity, and cycle performance is poor, and essential problem is graphite wafer
The surface texture defect caused by reaction inhomogeneities between side, the face of body.Pure silicon negative material is in a completely charged state
Specific capacity can reach 4200mAh/g, and far above traditional graphite cathode material, but silicium cathode material is in Li+When embedded
Time can cause silicium cathode material lattice that serious expansion occurs, and up to 300%, this can cause silicium cathode efflorescence, come off so as to lead
Send a telegraph the Capacity decline in pond.Therefore the present invention carries out compound use using carbon materials and silica-base material, by composite
Carry out surface metal cladding process, can suppress volumetric expansion, improve its reversible specific capacity, initial coulomb efficiency, cycle performance,
The performances such as heavy-current discharge.
In present embodiment, the nano carbon microsphere that mass fraction is 95% is mixed with the nano-silicon that mass fraction is 5%
It is even to be configured to composite.
Further, the composite is put into into industrial alcohol and acetone according to 1:The mixing of 1 volume ratio configuration is molten
Electrochemical deoiling is carried out in liquid；The composite after by electrochemical deoiling is washed, and is placed into and carry out in fuming nitric aicd chemistry
Roughening；The composite after chemistry roughening is washed, SnCl is placed into2Concentration for 5g/L hydrochloric acid solution in carry out
Sensitized treatment 3min；The composite after by sensitized treatment is washed, and places into the Palladous chloride. that concentration is 0.5g/L molten
Activation processing 10min is carried out in liquid.
Further, by activation processing after the composite washed, and immerse in plating solution, in 90 DEG C of temperature
Under carry out chemical plating 2min.The plating solution includes copper sulfate, the nickel sulfate of 30g/L, the citric acid of 100g/L of the concentration for 20g/L
The formaldehyde of sodium, the sodium hypophosphite of 20g/L, the lead acetate of 0.1g/L and 1g/L.
Further, mechanical agitation carried out with the stirring intensity of 2000r/min, ultrasound carried out with the frequency of 130KHz, most
Afterwards composite electroless-plating will be carried out in Copper Foil plating solution of the immersion containing the composite, you can obtain lithium ion battery negative electrode,
The pole piece has acid bronze alloy-silicon-carbon composite deposite, its SEM (Scanning electron microscope) collection of illustrative plates such as Fig. 2
It is shown.
As control, using traditional method by nano carbon microsphere/nano-silicon, binding agent, conductive agent according to 98:1:1 ratio
Make slurry and be coated on Copper Foil and make control cathode pole piece, winding makes ferric phosphate lithium cell.Obtained by present embodiment
Lithium ion battery negative electrode and the performance comparison such as Fig. 3 and Fig. 4 institutes for compareing ferric phosphate lithium cell made by cathode pole piece winding
Show.As a result show：Ferric phosphate lithium cell prepared by the lithium ion battery negative electrode obtained by present embodiment is in different charge and discharges
High rate performance under electric multiplying power is better than the ferric phosphate lithium cell prepared by control cathode pole piece.The lithium obtained by present embodiment
After ferric phosphate lithium cell prepared by ion battery cathode pole piece circulates 510 weeks under 6C multiplying powers, capability retention is 94.2%, by
After circulating 350 weeks under ferric phosphate lithium cell 6C multiplying powers prepared by control cathode pole piece, capability retention is 92.4%.
The preparation method of the lithium ion battery negative electrode that the present invention is provided, carries out being made after chemical plating to Si-C composite material
Make it be deposited on copper foil of affluxion body surface by Ni-P again, it is not necessary to use binding agent, further improve negative electrode
The problems such as efficiency first of material is low, irreversible capacity is big, high rate performance is poor, further improves the capacity of lithium battery and forthright again
Energy.The method also has process is simple, the controllable advantage of cathode pole piece thickness.
Presently preferred embodiments of the present invention is the foregoing is only, is to combine specific preferred implementation to institute of the present invention
The further description of work, it is impossible to assert the present invention be embodied as be confined to these explanations.It is all the present invention spirit and
Any modification, equivalent and improvement for being made within principle etc., should be included in protection scope of the present invention.
Claims (10)
1. a kind of preparation method of lithium ion battery negative electrode, it is characterised in that：Comprise the following steps：
1) carbon materials and silica-base material are uniformly mixed to get the quality of carbon materials in composite, and the composite
Fraction is 90%-95%；
2) electrochemical deoiling, chemistry roughening, sensitized treatment and activation processing are carried out successively to the composite；
3) composite is immersed in plating solution, chemical plating 1-2min is carried out at a temperature of 70-90 DEG C；The plating solution includes
Concentration is mantoquita, other slaines of 10-150g/L, the complexant of 100-300g/L, the reduction of 3-20g/L of 20-80g/L
The dispersant of agent, the grain refiner of 0.1-5g/L and 1-10g/L；
4) mechanical agitation and supersound process are carried out, and negative current collector is immersed in the plating solution carries out composite electroless-plating.
2. the preparation method of lithium ion battery negative electrode as claimed in claim 1, it is characterised in that：Step 1) in, it is described
Carbon materials is at least one in CNT, carbon nano-fiber, Nano carbon balls, Graphene, graphite.
3. the preparation method of lithium ion battery negative electrode as claimed in claim 1, it is characterised in that：Step 1) in, it is described
Silica-base material is at least one in nano-silicon, nano silicon oxide, silicon nanowires, nano-tube, porous silica material.
4. the preparation method of lithium ion battery negative electrode as claimed in claim 1, it is characterised in that：Step 2) in, by institute
Stating composite and being put in industrial alcohol, the one of which of acetone or mixed solution carries out electrochemical deoiling.
5. the preparation method of lithium ion battery negative electrode as claimed in claim 1, it is characterised in that：Step 2) in, will change
Learn the composite after oil removing to be washed, be then placed in fuming nitric aicd, concentrated sulphuric acid, one kind of boric acid or wherein several mixed
Closing in solution carries out chemical roughening.
6. the preparation method of lithium ion battery negative electrode as claimed in claim 1, it is characterised in that：Step 2) in, will change
Learn the composite after roughening to be washed, be then placed in SnCl2Hydrochloric acid solution in carry out sensitized treatment.
7. the preparation method of lithium ion battery negative electrode as claimed in claim 1, it is characterised in that：Step 2) in, will be quick
The composite after change is processed is washed, and is then placed in carrying out activation processing in the halogenide of palladium or silver nitrate solution.
8. the preparation method of lithium ion battery negative electrode as claimed in claim 1, it is characterised in that：Step 3) in, it is described
Mantoquita is copper sulfate, copper chloride, the one of which of Schweinfurt green；Described other slaines be nickel, stannum, silver, zinc, gold sulfate,
Chloride or ammonium salt, or the one of which or several of alkali metal salt；The complexant is carboxylic acid, polyamines, sulfonic acid, nitrogenous silane
One of which or several；The reducing agent be hypophosphites, alkali metal borohydride, wherein the one of solubility borane compound
Plant or several；The grain refiner is lead salt, pink salt, zinc salt, the one of which of sulfur-containing compound or several；The dispersant
For alcohol, acetone, tetrahydrofuran, ethyl acetate, the one of which of toluene or several.
9. the preparation method of lithium ion battery negative electrode as claimed in claim 1, it is characterised in that：Step 4) in, machinery
Stirring intensity is 400-2000r/min, and ultrasonic frequency is 20-130KHz.
10. the preparation method of lithium ion battery negative electrode as claimed in claim 1, it is characterised in that：Step 4) in, it is described
Negative current collector is Copper Foil, and volume fraction of the silicon-carbon microgranule in the deposited plating layer of copper foil surface is 30%-40%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611255715.7A CN106654156A (en) | 2016-12-30 | 2016-12-30 | Preparation method of lithium ion cell negative electrode piece |
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| CN201611255715.7A CN106654156A (en) | 2016-12-30 | 2016-12-30 | Preparation method of lithium ion cell negative electrode piece |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108624907A (en) * | 2018-04-26 | 2018-10-09 | 复旦大学 | Nonmetal basal body efficient catalytic electrode and preparation method thereof |
| CN110923769A (en) * | 2019-10-21 | 2020-03-27 | 肇庆理士电源技术有限公司 | Electroplating method of thin lead coating of carbon grid of lead-carbon battery |
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|---|---|---|---|---|
| CN108624907A (en) * | 2018-04-26 | 2018-10-09 | 复旦大学 | Nonmetal basal body efficient catalytic electrode and preparation method thereof |
| CN110923769A (en) * | 2019-10-21 | 2020-03-27 | 肇庆理士电源技术有限公司 | Electroplating method of thin lead coating of carbon grid of lead-carbon battery |
| CN110923769B (en) * | 2019-10-21 | 2021-04-20 | 肇庆理士电源技术有限公司 | Electroplating method of thin lead coating of carbon grid of lead-carbon battery |
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Effective date of registration: 20191101 Address after: 518000 Shenyu Science and Technology Park, No. 68 Lanjingbei Road, Laokeng Community, Longtian Street, Pingshan District, Shenzhen City, Guangdong Province, 101 Applicant after: Shenzhen Anding New Energy Technology Development Co., Ltd. Address before: 518000 Guangdong Province, Shenzhen City Pingshan Pingshan community Zhu Keng Industrial Zone 9 1-3 Applicant before: Shenzhen Optimum Battery Co., Ltd. |
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Application publication date: 20170510 |