CN110534744A - A kind of lithium ion battery negative material and preparation method thereof, lithium ion battery negative electrode and button cell - Google Patents
A kind of lithium ion battery negative material and preparation method thereof, lithium ion battery negative electrode and button cell Download PDFInfo
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- CN110534744A CN110534744A CN201910723436.6A CN201910723436A CN110534744A CN 110534744 A CN110534744 A CN 110534744A CN 201910723436 A CN201910723436 A CN 201910723436A CN 110534744 A CN110534744 A CN 110534744A
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- lithium ion
- ion battery
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- graphene
- negative material
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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
- H01M10/04—Construction or manufacture in general
- H01M10/0422—Cells or battery with cylindrical casing
- H01M10/0427—Button cells
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
-
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a kind of lithium ion battery negative material and preparation method thereof, lithium ion battery negative electrode and button cell, the preparation method of lithium ion battery negative material includes the following steps: graphene powder and water ultrasonic mixing；Source of iron presoma and ultrasonic mixing is added, so that Fe3+Graphene sheet layer two sides self assembly and adhere to；Graphene powder mixing is added again, so that the graphene being added again is in self assembly；Acquisition material, which is heat-treated, after centrifugal dehydration treatment obtains the lithium ion battery negative material.The application provides a kind of preparation method of the lithium ion battery negative material of " sandwich " formula graphene/ferriferous oxide, and this method carries out modified to ferriferous oxide using big size graphene and is modified.It is this that there is " sandwich " formula structure protection supporting role can be played to iron oxide particle, while the introducing of graphene enhances the electric conductivity of composite material, so that the specific capacity and cycle life of battery have been significantly improved.
Description
Technical field
The present invention relates to a kind of lithium electric material fields, more particularly to a kind of lithium ion battery negative material.
Background technique
Lithium ion battery has that voltage platform is high as a kind of commercialized secondary cell, energy density it is big and
It is the advantages that good cycling stability, most potential in electrochmical power source and enjoy great popularity, play the part of in people's daily life at present
Drill key player, with all kinds of portable electronic devices and electric vehicle update iteration and energy storage field it is flourishing
Development, energy density and cycle life to lithium ion battery propose requirements at the higher level.The positive and negative pole material of battery is lithium-ion electric
Key component in pond plays decisive role to chemical property.Current positive electrode is mainly LiFePO4, cobalt acid lithium
And ternary material, and negative electrode material is mainly based on the carbon materials such as graphite.These materials have certain limitation, so that battery
It cannot be considered in terms of height ratio capacity and high safety performance.
Summary of the invention
In view of the foregoing deficiencies of prior art, the purpose of the present invention is to provide a kind of lithium ion battery negative materials
And its preparation method and application, for solving the problems of the prior art.
In order to achieve the above objects and other related objects, the present invention obtains by the following technical programs.
The present invention provides a kind of preparation method of lithium ion battery negative material, includes the following steps:
1) by graphene powder and water ultrasonic mixing；
2) source of iron presoma and ultrasonic mixing is added, so that Fe3+Graphene sheet layer two sides self assembly and adhere to；
3) graphene powder mixing is added again, so that the graphene being added again is in self assembly；
4) material is obtained after centrifugal dehydration treatment to be heat-treated and obtain the lithium ion battery negative material.
Preferably, the graphene with a thickness of 0.2~0.7nm, 1 μm of graphene sheet layer diagonal length >.It is highly preferred that
The big size graphene is to be prepared using electrochemical stripping method.Graphene therein surface element during electrolytic preparation
Divide and be oxidized, containing a certain amount of oxygen-containing group, while its surface defect is less, good conductivity.
Preferably, the source of iron presoma is selected from Fe (NO3)3·9H2O, Fe2(CO3)3, FeCl3And Fe (OH)3In one
Kind is a variety of.
Preferably, the quality of source of iron presoma is 30~60 times of graphene powder quality.
Preferably, the temperature of heat treatment is 450 DEG C~750 DEG C；The time of heat treatment is 1h~7h.It is obtained by heat treatment
A variety of ferriferous oxides.
Technical solution according to the present invention is first freeze-dried before heat treatment, and the temperature of freeze-drying is not higher than -5
℃。
Technical solution according to the present invention can promote source of iron presoma to dissolve in water by addition aqueous solution of nitric acid
The invention also discloses a kind of lithium ion battery negative materials prepared using preparation method as described above.
The invention also discloses a kind of lithium ion battery negative electrode, the lithium ion battery negative electrode includes using such as
The composite layer that lithium ion battery negative material described above is formed.
Preferably, the composite layer comprises the following components in parts by weight:
5~10 parts by weight of lithium ion battery negative material
1~5 parts by weight of conductive black
0.5~3 parts by weight of binder.
Grinding whether be in order to refine and uniformly mixing each component granularity.Preferably, it is used to form composite layer
The granularity of lithium ion battery negative material is that mesh number is greater than 50 mesh.Preferably, it is used to form the conductive black of composite layer
Granularity is that mesh number is greater than 50 mesh.Preferably, the granularity for being used to form the binder of composite material is that mesh number is greater than 50 mesh.
Preferably, the binder is polyvinylidene fluoride.
Preferably, the lithium ion battery negative electrode further includes copper foil, and the composite layer is attached to the copper foil
Surface.
Preferably, the method that the composite layer is formed are as follows: by lithium ion battery negative material, conductive black and bonding
Slurry is made in agent in organic solvent, then coated and dried.It is highly preferred that the organic solvent is N-Methyl pyrrolidone.
The invention also discloses a kind of button cells, including lithium ion battery negative electrode as described above.
Preferably, electrolyte is LiPF that mass concentration is 0.1~5mol/L in the button cell6Solution, solution
Solvent is the mixture of ethylene carbonate and diethyl carbonate；Diaphragm is polypropylene diaphragm.
It is highly preferred that the volume ratio of ethylene carbonate and diethyl carbonate is 1:(0.5~3 in the solvent).
The application provides a kind of preparation side of the lithium ion battery negative material of " sandwich " formula graphene/ferriferous oxide
Method, this method carry out modified to ferriferous oxide using big size graphene and are modified.It is this to have " sandwich " formula structure be with
Protection supporting role is played to iron oxide particle, while the introducing of graphene enhances the electric conductivity of composite material, so that electric
The specific capacity and cycle life in pond have been significantly improved.
Detailed description of the invention
Fig. 1 is sandwich style anode material forming process and structural schematic diagram in the application
Fig. 2 (a) is 550-G/Fe2O3(a) and (b) AC impedance figure after circulation before button cell circulation
Fig. 2 (b) is 650-G/Fe3O4(a) and (b) AC impedance figure after circulation before button cell circulation
Fig. 3 (a) is 550-G/Fe2O3Button cell is in 1A g-1The voltage of constant current charge-discharge test is carried out under current density
Curve
Fig. 3 (b) is 650-G/Fe3O4Button cell is in 1A g-1The voltage of constant current charge-discharge test is carried out under current density
Curve
Fig. 3 (c) is 550-G/Fe2O3Button cell long circulating performance map
Fig. 3 (d) is 650-G/Fe3O4Button cell long circulating performance map
Fig. 3 (e) is 550-G/Fe2O3Button cell high rate performance
Fig. 3 (f) is 650-G/Fe3O4Button cell high rate performance
Specific embodiment
Embodiments of the present invention are illustrated by particular specific embodiment below, those skilled in the art can be by this explanation
Content disclosed by book is understood other advantages and efficacy of the present invention easily.
Before further describing the specific embodiments of the present invention, it should be appreciated that protection scope of the present invention is not limited to down
State specific specific embodiment；It is also understood that term used in the embodiment of the present invention is specific specific in order to describe
Embodiment, rather than limiting the scope of protection of the present invention.The test method of actual conditions is not specified in the following example,
Usually according to normal condition, or according to condition proposed by each manufacturer.
When embodiment provides numberical range, it should be appreciated that except non-present invention is otherwise noted, two ends of each numberical range
Any one numerical value can be selected between point and two endpoints.Unless otherwise defined, the present invention used in all technologies and
Scientific term is identical as the normally understood meaning of those skilled in the art of the present technique.Except specific method, equipment used in embodiment,
Outside material, grasp and record of the invention according to those skilled in the art to the prior art can also be used and this
Any method, equipment and the material of the similar or equivalent prior art of method described in inventive embodiments, equipment, material come real
The existing present invention.
The present invention provides a kind of preparation method of lithium ion battery negative material, includes the following steps:
1) by graphene powder and water ultrasonic mixing；
2) source of iron presoma and ultrasonic mixing is added so that Fe3+ graphene sheet layer two sides self assembly and adhere to；
3) graphene powder mixing is added again, so that the graphene being added again is in self assembly；
4) material is obtained after centrifugal dehydration treatment to be heat-treated and obtain the lithium ion battery negative material.
Embodiment 1
By the graphene dispersion of 30mg in the water of 60ml, the Fe (NO of 5g is added3)3·9H2O, and 90mg is added again
Graphene prepares lithium ion battery negative material according to the method described above, then lithium ion battery negative material, conductive black
And PVDF is mixed according to 6:1:1 ratio, NMP is added, slurry is prepared, be prepared into button cell.
Reference electrode is made using metal lithium sheet, is characterized.
The heat treatment for having carried out 550 DEG C and 650 DEG C in the present embodiment respectively obtains two kinds of lithium ion battery negative materials,
550-G/Fe2O3And 650-G/Fe3O4。
As shown in Figure 2, it can be seen that two kinds of composite materials after introducing graphene are smaller in high frequency region semicircle, exchange resistance
It is anti-to be significantly less than pure ferriferous oxide cathode, illustrate that graphene improves the electronic conductivity of composite material, promotes charge and discharge
Effective progress of redox reaction in the process.
(a) and (b) is respectively 550-G/Fe in Fig. 32O3And 650-G/Fe3O4Button cell is in 1A g-1Under current density into
The voltage curve of row constant current charge-discharge test；(c) (d) show button cell long circulating performance map, 550-G/Fe2O3Sample exists
1A g-1After carrying out 300 charge and discharge cycles under current density, it is still able to maintain about 500mAh g-1Specific discharge capacity, and 650-
G/Fe3O4Sample can then keep 565mAh g-1Specific discharge capacity, hence it is evident that higher than pure Fe2O3And Fe3O4Cathode.This be by
The electric conductivity of composite material is improved in the presence of graphene, the structure of " sandwich " can be provided to iron oxide particle simultaneously
Certain protection support, prevents it to be detached from collector due to granule atomization in discharge and recharge reaction.
From Fig. 3 (e) and (f) it can be seen that 550-G/Fe2O3And 650-G/Fe3O4Ratio of the cathode under different current densities
Capacity is superior to pure Fe2O3And Fe3O4Comparative sample possesses good high rate performance.
Embodiment 2
By the graphene dispersion of 30mg in the water of 60ml, the Fe (NO of 4g is added3)3·9H2O, and 90mg is added again
Graphene prepares lithium ion battery negative material according to the method described above, then lithium ion battery negative material, conductive black
And PVDF is mixed according to 5:2:1 ratio, NMP is added, slurry is prepared, be prepared into button cell.
The heat treatment for having carried out 450 DEG C and 750 DEG C in the present embodiment respectively obtains two kinds of lithium ion battery negative materials.
Embodiment 3
By the graphene dispersion of 30mg in the water of 60ml, the Fe (NO of 6g is added3)3·9H2O, and 90mg is added again
Graphene prepares lithium ion battery negative material according to the method described above, then lithium ion battery negative material, conductive black
And PVDF is mixed according to 10:4:3 ratio, NMP is added, slurry is prepared, be prepared into button cell.
The heat treatment for having carried out 550 DEG C and 650 DEG C in the present embodiment respectively obtains two kinds of lithium ion battery negative materials.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology all without departing from the spirit and scope of the present invention, carries out modifications and changes to above-described embodiment.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should be covered by the claims of the present invention.
Claims (10)
1. a kind of preparation method of lithium ion battery negative material, includes the following steps:
1) by graphene powder and water ultrasonic mixing；
2) source of iron presoma and ultrasonic mixing is added, so that Fe3+Graphene sheet layer two sides self assembly and adhere to；
3) graphene powder mixing is added again, so that the graphene being added again is in self assembly；
4) material is obtained after centrifugal dehydration treatment to be heat-treated and obtain the lithium ion battery negative material.
2. preparation method according to claim 1, which is characterized in that the graphene with a thickness of 0.2~0.7nm, stone
Black 1 μm of alkene lamella diagonal length >.
3. preparation method according to claim 1, which is characterized in that including one of following feature or a variety of:
The source of iron presoma is selected from Fe (NO3)3·9H2O, Fe2(CO3)3, FeCl3And Fe (OH)3One of or it is a variety of；
The quality of source of iron presoma is 30~60 times of graphene powder quality；
The temperature of heat treatment is 450 DEG C~750 DEG C；The time of heat treatment is 1h~7h；
It is first freeze-dried before heat treatment, the temperature of freeze-drying is not higher than -5 DEG C.
4. a kind of lithium ion battery negative material prepared using preparation method as claimed in any one of claims 1 to 3.
5. a kind of lithium ion battery negative electrode, which is characterized in that the lithium ion battery negative electrode includes using such as right
It is required that the composite layer that lithium ion battery negative material described in 4 is formed.
6. lithium ion battery negative electrode according to claim 5, which is characterized in that the composite layer includes following
The component of parts by weight:
5~10 parts by weight of lithium ion battery negative material
1~5 parts by weight of conductive black
0.5~3 parts by weight of binder.
7. lithium ion battery negative electrode according to claim 6, which is characterized in that the binder is to gather inclined difluoro second
Alkene.
8. lithium ion battery negative electrode according to claim 5, which is characterized in that including one of following feature or
It is a variety of:
The lithium ion battery negative electrode further includes copper foil, and the composite layer is attached to the copper foil surface；
The method that the composite layer is formed are as follows: by lithium ion battery negative material, conductive black and binder organic molten
Slurry is made in agent, it is then coated and dried.
9. a kind of button cell, which is characterized in that using such as the described in any item negative electrode of lithium ion battery poles of claim 5~8
Piece.
10. button cell according to claim 9, which is characterized in that electrolyte is mass concentration in the button cell
For the LiPF of 0.1~5mol/L6Solution, the solvent of solution are the mixture of ethylene carbonate and diethyl carbonate；Diaphragm is poly-
Propylene diaphragm.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102646817A (en) * | 2011-02-16 | 2012-08-22 | 中国科学院金属研究所 | Graphene/metal oxide composite cathode material for lithium ion battery and preparation |
| CN104810509A (en) * | 2015-03-31 | 2015-07-29 | 浙江大学 | Ferroferric oxide/graphene three-dimensional composite structure as well as preparation method and application thereof |
| CN105206817A (en) * | 2015-10-20 | 2015-12-30 | 上海应用技术学院 | Carbon-coated iron-based/grapheme lithium ion battery cathode material and preparation method |
| CN106848220A (en) * | 2017-01-17 | 2017-06-13 | 陕西科技大学 | A kind of preparation method of Graphene iron oxide graphene composite structure cell negative electrode material |
| CN107195891A (en) * | 2017-06-30 | 2017-09-22 | 绍兴文理学院 | A kind of preparation method of lithium battery graphene composite negative pole |
| CN107452943A (en) * | 2017-07-13 | 2017-12-08 | 陕西科技大学 | A kind of preparation method of graphene-supported ferriferous oxide self assembly class mulberries structure lithium ion battery negative material |
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2019
- 2019-08-06 CN CN201910723436.6A patent/CN110534744A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102646817A (en) * | 2011-02-16 | 2012-08-22 | 中国科学院金属研究所 | Graphene/metal oxide composite cathode material for lithium ion battery and preparation |
| CN104810509A (en) * | 2015-03-31 | 2015-07-29 | 浙江大学 | Ferroferric oxide/graphene three-dimensional composite structure as well as preparation method and application thereof |
| CN105206817A (en) * | 2015-10-20 | 2015-12-30 | 上海应用技术学院 | Carbon-coated iron-based/grapheme lithium ion battery cathode material and preparation method |
| CN106848220A (en) * | 2017-01-17 | 2017-06-13 | 陕西科技大学 | A kind of preparation method of Graphene iron oxide graphene composite structure cell negative electrode material |
| CN107195891A (en) * | 2017-06-30 | 2017-09-22 | 绍兴文理学院 | A kind of preparation method of lithium battery graphene composite negative pole |
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Application publication date: 20191203 |