CN106601993A - Lithium ion battery negative electrode plate and preparation method therefor - Google Patents
Lithium ion battery negative electrode plate and preparation method therefor Download PDFInfo
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- CN106601993A CN106601993A CN201611246494.7A CN201611246494A CN106601993A CN 106601993 A CN106601993 A CN 106601993A CN 201611246494 A CN201611246494 A CN 201611246494A CN 106601993 A CN106601993 A CN 106601993A
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- graphite
- anode plate
- nickel
- ionic cell
- lithium ionic
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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
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
-
- 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
- H01M4/0402—Methods of deposition of the material
- H01M4/0404—Methods of deposition of the material by coating on electrode collectors
-
- 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
- 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 discloses a lithium ion battery negative electrode plate and a preparation method therefor. The lithium ion battery negative electrode plate comprises a negative electrode current collector and a negative electrode active material layer distributed on the negative electrode current collector; and the negative electrode active material layer comprises graphite, a conductive agent and a binder, wherein the surface of the graphite is coated with a nickel-based alloy layer. By performing chemical nickel-plating alloying on the graphite, the surface of the graphite is nanometer alloyed, so that the problems of low initial efficiency, high reversible capacity, poor rate capability and the like of the graphite negative electrode material are relieved, and the capacity and the rate capability of the lithium battery are further improved.
Description
Technical field
The invention belongs to technical field of lithium batteries, it is more particularly related to a kind of anode plate for lithium ionic cell and
Its preparation method.
Background technology
Lithium ion battery has big specific energy, monomer running voltage height, operating temperature range width, cycle life due to it
Long, self discharge is little, it is environmentally friendly the advantages of, have broad application prospects in the field such as portable electronics and electric automobile.
The development of lithium ion battery is maked rapid progress, and continuous with lithium ion battery material is improved with lithium ion battery production technology not
Disconnected to improve, the performance of lithium ion battery has been obviously improved, but at aspects such as energy density, high rate performances or is existed
Defect.
The development of negative material is closely related with battery performance, now widely used lithium iron phosphate battery negative electrode material collection
In in graphite-like, but it has that efficiency first is low, the defect of the aspect such as high rate performance is poor and electrolyte matching difficulty is big,
Its range of application is set to be limited significantly.Existing LiFePO4-graphite cell exist high rate performance it is not good, cannot large current charge
Shortcoming, in high rate charge-discharge, because graphite cathode can not quickly finish embedding lithium/de- lithium, causes capacity decline, temperature rise bright
It is aobvious, so as to bring certain potential safety hazard.
In view of this, it is necessory to provide a kind of anode plate for lithium ionic cell that can improve lithium battery high rate performance and capacity
And preparation method thereof.
The content of the invention
The present invention goal of the invention be：There is provided a kind of lithium ion battery that can improve lithium battery high rate performance and capacity to bear
Pole piece and preparation method thereof.
In order to realize foregoing invention purpose, the present invention provides a kind of anode plate for lithium ionic cell, and it includes negative current collector
With the negative electrode active material layer being distributed on negative current collector, the negative electrode active material layer contains graphite, conductive agent and bonding
Agent, the graphite surface is coated with nickel base alloy layer.
As anode plate for lithium ionic cell of the present invention one kind improve, the nickel base alloy layer crystallite dimension be 30～
80nm。
Improve as one kind of anode plate for lithium ionic cell of the present invention, the quality hundred of graphite in the negative electrode active material layer
It is 0.5～1% to divide than the mass percent that the mass percent for 97～99%, conductive agent is 0.2～2%, binding agent.
Improve as one kind of anode plate for lithium ionic cell of the present invention, the conductive agent contains CNT and conductive charcoal
It is black.
Improve as one kind of anode plate for lithium ionic cell of the present invention, the binding agent contains sodium carboxymethyl cellulose and fourth
Benzene rubber.
A kind of anode plate for lithium ionic cell preparation method, comprises the following steps：
1) electrochemical deoiling is carried out to graphite；
2) roughening treatment is carried out to the graphite surface after electrochemical deoiling using the acid solution with oxidisability；
3) sensitized treatment and activation processing are carried out to the graphite after roughening treatment；
4) using plating nickel-base alloy plating solution to step 3) process after graphite surface carry out Electroless Nickel-Based Alloy Plating；
5) pure water is carried out to the graphite after plating and cleans and be dried to obtain the graphite with nickel alloy plating layer；
6) graphite with nickel alloy plating layer, conductive agent and binding agent are dissolved in proportion in solvent and make slurry simultaneously
It is coated on negative current collector, after drying, cut-parts of colding pressing herein described negative plate is obtained.
Improve as one kind of anode plate for lithium ionic cell preparation method of the present invention, the step 1) it is middle using industrial wine
At least one in essence, acetone carries out electrochemical deoiling to graphite.
Improve as one kind of anode plate for lithium ionic cell preparation method of the present invention, the step 2) in there is oxidisability
Acid solution is at least one in fuming nitric aicd, concentrated sulphuric acid, boric acid.
Improve as one kind of anode plate for lithium ionic cell preparation method of the present invention, the step 3) in using SnCl2
Hydrochloric acid solution carries out sensitized treatment to graphite, and activation processing is carried out to graphite using the halogenide or silver chloride of palladium.
Improve as one kind of anode plate for lithium ionic cell preparation method of the present invention, the step 4) middle plating nickel-base alloy plating
Liquid is made up of nickel salt, complexant, non-nickel slaine, reducing agent, grain refiner and dispersant, the plating nickel-base alloy plating solution
Operating temperature is 70～90 DEG C.
Improve as one kind of anode plate for lithium ionic cell preparation method of the present invention, nickel salt in the plating nickel-base alloy plating solution
Concentration be 20～80g/L, the concentration of complexant is 30～300g/L, and the concentration of non-nickel slaine is 10～150g/L, reduction
The concentration of agent is 3～20g/L, and the concentration of grain refiner is 0.1～5g/L, and the concentration of dispersant is 1～10ml/L.
Improve as one kind of anode plate for lithium ionic cell preparation method of the present invention, the nickel salt is sulfate, the salt of nickel
Hydrochlorate or acetate.
As anode plate for lithium ionic cell preparation method of the present invention one kind improve, the non-nickel slaine be copper, stannum,
One or more in silver, zinc, the sulfate of gold or hydrochlorate, and alkali metal salt.
Improve as one kind of anode plate for lithium ionic cell preparation method of the present invention, the complexant is carboxylic acid, polyamines, sulphur
One or more in sour, nitrogenous silane.
Improve as one kind of anode plate for lithium ionic cell preparation method of the present invention, the reducing agent is hypophosphites, alkali
One or more in metallic boron hydridess, solubility borane compound.
Improve as one kind of anode plate for lithium ionic cell preparation method of the present invention, the grain refiner is lead salt, stannum
One or more in salt, zinc salt, sulfur-containing compound.
As anode plate for lithium ionic cell preparation method of the present invention one kind improve, the dispersant be isopropanol, acetone,
One or more in tetrahydrofuran, ethyl acetate, toluene, triethanolamine.
Relative to prior art, the present invention has following Advantageous Effects：
To making its nano surface alloying after graphite Electroless Nickel-Based Alloy Plating, the efficiency first of graphite cathode material is improved
The problems such as low, irreversible capacity is big, high rate performance is poor, further increases the capacity and high rate performance of lithium battery.
Description of the drawings
With reference to the accompanying drawings and detailed description, anode plate for lithium ionic cell of the present invention is described in detail, wherein：
Fig. 1 is the SEM figures of negative plate in embodiment 1.
Fig. 2 is embodiment 1 and the battery rate charge-discharge comparison diagram of comparative example 1.
Fig. 3 is that embodiment 1 circulates comparison diagram with the battery charging and discharging of comparative example 1.
Specific embodiment
In order that the goal of the invention of the present invention, technical scheme and its technique effect become apparent from, below in conjunction with accompanying drawing and tool
Body embodiment, the present invention will be described in further detail.It should be appreciated that the specific embodiment party described in this specification
Formula is not intended to limit the present invention just for the sake of explaining the present invention.
Embodiment 1
A kind of preparation method of lithium ion battery, it is comprised the following steps：
1) preparation of negative plate
Electrochemical deoiling is carried out to graphite using industrial alcohol, then roughening treatment is carried out to graphite surface using concentrated sulphuric acid,
Use SnCl respectively again2Hydrochloric acid solution and silver chloride sensitized treatment and activation processing are carried out respectively to the graphite after roughening；
Plating nickel-base alloy plating solution is consisted of：Nickel sulfate 20g/L, sodium citrate 35g/L, zinc sulfate 30g/L, sodium borohydride
5g/L, tin acetate 0.2g/L, triethanolamine 3mL/L, 80 DEG C of bath temperature, carry out Electroless Nickel-Based Alloy Plating, to plating to graphite
Graphite afterwards carries out pure water and cleans and be dried to obtain the graphite with nickel alloy plating layer, and nickel base alloy layer crystallite dimension is
72nm；
The mixture that conductive agent is CNT and conductive black is selected, binding agent is sodium carboxymethyl cellulose and butylbenzene rubber
The mixture of glue, by the graphite with nickel alloy plating layer, conductive agent and binding agent 98 are pressed:1:1 ratio is dissolved in solvent and makes
Into slurry and it is coated in copper foil current collector, after drying, cut-parts of colding pressing negative plate is obtained.
2) preparation of positive plate
Positive electrode in positive plate is 95% positive active material, 2.5% conductive agent and 2.5% binding agent composition,
Positive active material is LiFePO4, and conductive agent is that CNT (CNT) and graphite press 1:1 is combined, and binding agent is polyvinylidene fluoride
Alkene (PVDF).
Barrier film is that polyethylene (PE) wet method is double draws barrier film.
Above negative plate, positive plate and barrier film are formed into battery core by winding or lamination process, the lithium of embodiment 1 is assembled into
Ion battery.
Wherein, the SEM figures of the graphite with nickel alloy plating layer for preparing in embodiment 1 refer to shown in Fig. 1, to graphite
Its nano surface alloying is made after Electroless Nickel-Based Alloy Plating, the efficiency first for improving graphite cathode material is low, irreversible capacity
Greatly, the problems such as high rate performance difference, the capacity and high rate performance of lithium battery are further increased.
Embodiment 2
Embodiment 2 is substantially the same manner as Example 1, and difference is the preparation of negative plate：
Electrochemical deoiling is carried out to graphite using industrial alcohol, then roughening treatment is carried out to graphite surface using concentrated sulphuric acid,
Use SnCl respectively again2Hydrochloric acid solution and silver chloride sensitized treatment and activation processing are carried out respectively to the graphite after roughening；
Plating nickel-base alloy plating solution composition：Nickel dichloride. 80g/L, dodecyl sodium sulfate 100g/L, zinc chloride 150g/L, secondary phosphorus
Sour sodium 12g/L, lead acetate 5g/L, triethanolamine 10mL/L, 70 DEG C of bath temperature carries out Electroless Nickel-Based Alloy Plating to graphite, right
Graphite after plating carries out pure water and cleans and be dried to obtain the graphite with nickel alloy plating layer, and nickel base alloy layer crystallite dimension is
56nm；
The mixture that conductive agent is CNT and conductive black is selected, binding agent is sodium carboxymethyl cellulose and butylbenzene rubber
The mixture of glue, by the graphite with nickel alloy plating layer, conductive agent and binding agent 97 are pressed:2:1 ratio is dissolved in solvent and makes
Into slurry and it is coated in copper foil current collector, after drying, cut-parts of colding pressing negative plate is obtained.
Embodiment 3
Embodiment 3 is substantially the same manner as Example 1, and difference is the preparation of negative plate：
Electrochemical deoiling is carried out to graphite using industrial alcohol, then graphite surface is carried out at roughening using fuming nitric aicd
Reason, then SnCl is used respectively2Hydrochloric acid solution and Palladous chloride. sensitized treatment and activation processing are carried out respectively to the graphite after roughening；
Plating nickel-base alloy plating solution is consisted of：Nickel dichloride. 35g/L, sodium citrate 50g/L, stannous chloride 50g/L, ortho phosphorous acid
Sodium 20g/L, lead acetate 0.5g/L, isopropanol 8mL/L, 75 DEG C of bath temperature carries out Electroless Nickel-Based Alloy Plating, to plating to graphite
Graphite afterwards carries out pure water and cleans and be dried to obtain the graphite with nickel alloy plating layer, and nickel base alloy layer crystallite dimension is
68nm；
The mixture that conductive agent is CNT and conductive black is selected, binding agent is sodium carboxymethyl cellulose and butylbenzene rubber
The mixture of glue, by the graphite with nickel alloy plating layer, conductive agent and binding agent 99 are pressed:0.2:0.8 ratio is dissolved in solvent
In make slurry and be coated in copper foil current collector, obtain negative plate after drying, cut-parts of colding pressing.
Comparative example 1
Comparative example 1 is substantially the same manner as Example 1, and difference is：Graphite surface is not coated with nickel-base alloy.
Table 1 is the performance comparison of graphite in embodiment 1 and comparative example 1
| Model | Gram volume mAh/g first | Efficiency/% first |
| Graphite in embodiment 1 | ≥420 | ≥99 |
| Graphite in comparative example 1 | ≥330 | ≥90 |
Table 1 is graphite performance comparison in embodiment 1 and comparative example 1, as can be seen from the table, the plated surface of embodiment 1
There is the graphite-phase of nickel-base alloy for the gram volume first of graphite in comparative example 1 is lifted to 420mAh/g from 330mAh/g, and
First efficiency is lifted to 99% from 90%, because graphite surface is coated with nickel-base alloy, in Battery formation, reduces electrolyte
With the contact surface of graphite cathode material, so as to improve the efficiency first and gram volume first of graphite cathode material.
Fig. 2 is embodiment 1 and the lithium ion battery rate charge-discharge curve comparison figure of comparative example 1.Battery prepared by embodiment 1
6C charging constant currents ratio up to 92.54%, 3C chargings constant current ratio is 94.02%, and battery shows good high rate performance；And contrast
Battery 6C, 3C charging constant current ratio respectively 90.5%, 93.68% prepared by example 1.
Fig. 3 is embodiment 1 and the cycle performance of lithium ion battery comparison diagram of comparative example 1, it can be seen that embodiment 1
Battery with 6C circulations 510 times after, the capability retention of battery is 94.2%, and the battery of comparative example 1 is in identical bar
After circulating 350 times under part, the capability retention of battery is only 92.4%, therefore, can significantly be changed using the negative plate in the application
The capacity and circulating ratio performance of kind battery.
Can be seen that relative to prior art with reference to above detailed description of the present invention, the present invention at least has following
Advantageous Effects：
To making its nano surface alloying after graphite Electroless Nickel-Based Alloy Plating, the efficiency first of graphite cathode material is improved
The problems such as low, irreversible capacity is big, high rate performance is poor, further increases the capacity and high rate performance of lithium battery.
According to above-mentioned principle, the present invention can also carry out appropriate change and modification to above-mentioned embodiment.Therefore, this
It is bright to be not limited to specific embodiment disclosed and described above, some modifications and changes of the present invention should also be as falling into this
In the scope of the claims of invention.Although additionally, some specific terms used in this specification, these terms
Merely for convenience of description, not to any restriction of present invention composition.
Claims (17)
1. a kind of anode plate for lithium ionic cell, including negative current collector and the negative electrode active material being distributed on negative current collector
Layer, the negative electrode active material layer contains graphite, conductive agent and binding agent, it is characterised in that the graphite surface is coated with Ni-based
Alloy-layer.
2. anode plate for lithium ionic cell according to claim 1, it is characterised in that the nickel base alloy layer crystallite dimension is
30～80nm.
3. anode plate for lithium ionic cell according to claim 1, it is characterised in that graphite in the negative electrode active material layer
Mass percent be 97～99%, the mass percent of conductive agent be the mass percent of 0.2～2%, binding agent be 0.5～
1%.
4. anode plate for lithium ionic cell according to claim 1, it is characterised in that the conductive agent contain CNT and
Conductive black.
5. anode plate for lithium ionic cell according to claim 1, it is characterised in that the binding agent contains carboxymethyl cellulose
Plain sodium and butadiene-styrene rubber.
6. the preparation method of anode plate for lithium ionic cell any one of a kind of claim 1 to 5, it is characterised in that include
Following steps：
1) electrochemical deoiling is carried out to graphite；
2) roughening treatment is carried out to the graphite surface after electrochemical deoiling using the acid solution with oxidisability；
3) sensitized treatment and activation processing are carried out to the graphite after roughening treatment；
4) using plating nickel-base alloy plating solution to step 3) process after graphite surface carry out Electroless Nickel-Based Alloy Plating；
5) pure water is carried out to the graphite after plating and cleans and be dried to obtain the graphite with nickel alloy plating layer；
6) graphite with nickel alloy plating layer, conductive agent and binding agent are dissolved in proportion in solvent and make slurry and coat
On negative current collector, after drying, cut-parts of colding pressing anode plate for lithium ionic cell any one of claim 1 to 5 is obtained.
7. the preparation method of anode plate for lithium ionic cell according to claim 6, it is characterised in that the step 1) in adopt
At least one in industrial alcohol, acetone carries out electrochemical deoiling to graphite.
8. the preparation method of anode plate for lithium ionic cell according to claim 6, it is characterised in that the step 2) in have
The acid solution of oxidisability is at least one in fuming nitric aicd, concentrated sulphuric acid, boric acid.
9. the preparation method of anode plate for lithium ionic cell according to claim 6, it is characterised in that the step 3) in adopt
SnCl2Hydrochloric acid solution sensitized treatment is carried out to graphite, activation processing is carried out to graphite using the halogenide or silver chloride of palladium.
10. the preparation method of anode plate for lithium ionic cell according to claim 6, it is characterised in that the step 4) in plating
Nickel-base alloy plating solution is made up of nickel salt, non-nickel slaine, complexant, reducing agent, grain refiner and dispersant, and the plating is Ni-based
The operating temperature of alloy electroplating bath is 70～90 DEG C.
The preparation method of 11. anode plate for lithium ionic cell according to claim 10, it is characterised in that the plating nickel-base alloy
The concentration of nickel salt is 20～80g/L in plating solution, and the concentration of complexant is 30～300g/L, the concentration of non-nickel slaine is 10～
150g/L, the concentration of reducing agent is 3～20g/L, and the concentration of grain refiner is 0.1～5g/L, the concentration of dispersant is 1～
10ml/L。
The preparation method of 12. anode plate for lithium ionic cell according to claim 10, it is characterised in that the nickel salt is nickel
Sulfate, hydrochlorate or acetate.
The preparation method of 13. anode plate for lithium ionic cell according to claim 10, it is characterised in that the non-nickel slaine
For one or more in copper, stannum, silver, zinc, the sulfate of gold or hydrochlorate, and alkali metal salt.
The preparation method of 14. anode plate for lithium ionic cell according to claim 10, it is characterised in that the complexant is carboxylic
One or more in acid, polyamines, sulfonic acid, nitrogenous silane.
The preparation method of 15. anode plate for lithium ionic cell according to claim 10, it is characterised in that the reducing agent is secondary
One or more in phosphate, alkali metal borohydride, solubility borane compound.
The preparation method of 16. anode plate for lithium ionic cell according to claim 10, it is characterised in that the grain refiner
For one or more in lead salt, pink salt, zinc salt, sulfur-containing compound.
The preparation method of 17. anode plate for lithium ionic cell according to claim 10, it is characterised in that the dispersant is different
One or more in propanol, acetone, tetrahydrofuran, ethyl acetate, toluene, triethanolamine.
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| CN201611246494.7A CN106601993A (en) | 2016-12-29 | 2016-12-29 | Lithium ion battery negative electrode plate and preparation method therefor |
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| CN201611246494.7A CN106601993A (en) | 2016-12-29 | 2016-12-29 | Lithium ion battery negative electrode plate and preparation method therefor |
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| CN109817938A (en) * | 2019-02-14 | 2019-05-28 | 东北大学 | A kind of preparation method of iron-based negative electrode material |
| CN114597374A (en) * | 2022-03-21 | 2022-06-07 | 上海兰钧新能源科技有限公司 | Silica anode material and preparation method thereof |
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| CN109817938B (en) * | 2019-02-14 | 2021-11-05 | 东北大学 | Preparation method of iron-based negative electrode material |
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| CN114597374B (en) * | 2022-03-21 | 2024-02-09 | 上海兰钧新能源科技有限公司 | Silicon-oxygen negative electrode material and preparation method thereof |
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