CN110078067A - A kind of preparation method for the graphite cathode material that end face structure is controllable - Google Patents
A kind of preparation method for the graphite cathode material that end face structure is controllable Download PDFInfo
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- CN110078067A CN110078067A CN201910508566.8A CN201910508566A CN110078067A CN 110078067 A CN110078067 A CN 110078067A CN 201910508566 A CN201910508566 A CN 201910508566A CN 110078067 A CN110078067 A CN 110078067A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/23—Oxidation
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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
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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
- H01M4/58—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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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
Abstract
The invention discloses a kind of preparation methods of graphite cathode material that end face structure is controllable, comprising the following steps: (1) one group of graphite particle is placed in reaction kettle, liquid phase feed is passed through into reaction kettle, reaction kettle is sealed and placed in carbide furnace；Be passed through nitrogen into carbide furnace, and 300~950 DEG C at a temperature of handle 1~9 hour；(2) another group of graphite particle is packed into continuous rotary kiln, the mixed gas of nitrogen and oxygen is passed through into continuous rotary kiln, is handled 1~3 hour at 400~600 DEG C；(3) by step (1) graphite particle and the resulting graphite particle of step (2) mix.The armchair shape end face of graphite and the ratio of serrated end face is can be realized into controlled range with mixing in certain in graphite particle after graphite particle and oxidation processes after vaporization process, so that the performance for the graphite cathode material being prepared is improved, being used for lithium ion battery can be enhanced graphite and compatibility of electrolyte, improve cycle performance.
Description
Technical field
The present invention relates to technical field of lithium ion battery negative, in particular to a kind of graphite that end face structure is controllable is negative
The preparation method of pole material.
Background technique
Graphite cathode is the common negative electrode material of lithium ion battery.Graphite cathode particle includes end face and basal plane, lithium ion
Be embedded in end face rate be higher than six orders of magnitude of basal plane rate, so the reversible deintercalation overwhelming majority of lithium ion mainly end face into
Row.Due to the hexagonal molecular structure of graphite, also there are two types of forms for end face: " armchair shape " and " zigzag ".Due to point of end face
Minor structure difference causes the significant difference of chemical reactivity.Armchair shape end face (armchair ribbon) and serrated end face
The rational proportion of (zigzag ribbon), that is, serrated end face proportion is usually that can make between 10%~50%
Excellent dynamic performance is presented in graphite cathode.In the prior art, in graphite cathode preparation process, armchair shape end face and zigzag
End face be it is random, uncontrollable, further made of the performance of graphite cathode be also not sufficiently stable.Therefore, it is necessary to propose
A kind of new preparation aspect, can be by the burden control of armchair shape end face and serrated end face in a certain range.
As it can be seen that the prior art could be improved and improve.
Summary of the invention
Place in view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of graphite that end face structure is controllable
The preparation method of negative electrode material, it is intended to solve the ratio of armchair shape end face and serrated end face in graphite cathode material in the prior art
The uncontrollable technical problem of example.
In order to achieve the above object, this invention takes following technical schemes:
A kind of preparation method for the graphite cathode material that end face structure is controllable, which comprises the following steps:
(1) one group of graphite particle is placed in reaction kettle, filling rate is 10%~30%；Liquid phase original is passed through into reaction kettle
Material, liquid phase feed are distilled water, hydrogen peroxide, ethyl acetate or toluene；Reaction kettle is sealed and placed in carbide furnace；To carbide furnace
Inside be passed through nitrogen, and 300~950 DEG C at a temperature of handle 1~9 hour；Obtained graphite particle gives over to spare；
(2) another group of graphite particle is packed into continuous rotary kiln, filling rate is 5%~20%；To continuous rotary
It is passed through the mixed gas of nitrogen and oxygen in kiln, is handled 1~3 hour at 400~600 DEG C；Obtained graphite particle gives over to standby
With；
(3) by step (1) graphite particle and the resulting graphite particle of step (2) mix.
Further, the reaction in the preparation method of the controllable graphite cathode material of the end face structure, in step (1)
Kettle is reaction kettle made of glass material.
Further, the liquid phase in the preparation method of the controllable graphite cathode material of the end face structure, in step (1)
Raw material is distilled water.
Further, in the preparation method of the controllable graphite cathode material of the end face structure, nitrogen stream in step (1)
Amount is 1~5 cubic meters per minute.
Further, in the preparation method of the controllable graphite cathode material of the end face structure, 300 in step (1)
It is handled 5 hours at a temperature of~950 DEG C.
Further, in the preparation method of the controllable graphite cathode material of the end face structure, in step (2) nitrogen and
The range of the volume ratio of oxygen is (1: 1)~(5: 1).
Further, in the preparation method of the controllable graphite cathode material of the end face structure, in step (2) nitrogen and
The volume ratio of oxygen is 5: 1.
Further, in the preparation method of the controllable graphite cathode material of the end face structure, in step (2) nitrogen and
The flow of the mixed gas of oxygen is 5~20L/h.
The utility model has the advantages that the present invention provides a kind of preparation method of graphite cathode material that end face structure is controllable, compared to existing
There is technology, is handled by being vaporized to graphite so that the end face of one group of graphite shows armchair shape structure in the present invention；Pass through
Oxidation processes are carried out to graphite, so that zigzag structure is presented in the end face of another group of graphite；By the graphite particle after vaporization process
With the graphite particle after oxidation processes in the ratio of certain armchair shape end face and serrated end face that graphite can be realized with mixing
In controlled range, so that the performance for the graphite cathode material being prepared is improved, being used for lithium ion battery can be with
Enhance graphite and compatibility of electrolyte, improves cycle performance and be electrolysed because of the good compatibility of itself and PC base electrolyte using PC
Liquid battery core has good dynamic performance, and charge-discharge magnification is excellent in.
Specific embodiment
The present invention provides a kind of preparation method of graphite cathode material that end face structure is controllable, for make the purpose of the present invention,
Technical solution and effect are clearer, clear, and the present invention is described in more detail by the following examples.It should be appreciated that herein
Described specific examples are only used to explain the present invention, is not intended to limit the present invention.
The present invention provides a kind of preparation method of graphite cathode material that end face structure is controllable, and this method includes following step
It is rapid:
(1) one group of graphite particle is placed in reaction kettle, filling rate is 10%~30%；Liquid phase original is passed through into reaction kettle
Material, liquid phase feed are distilled water, hydrogen peroxide, ethyl acetate or toluene；Reaction kettle is sealed and placed in carbide furnace；To carbide furnace
Inside be passed through nitrogen, and 300~950 DEG C at a temperature of handle 1~9 hour；Obtained graphite particle gives over to spare；
(2) another group of graphite particle is packed into continuous rotary kiln, filling rate is 5%~20%；To continuous rotary
It is passed through the mixed gas of nitrogen and oxygen in kiln, is handled 1~3 hour at 400~600 DEG C；Obtained graphite particle gives over to standby
With；
(3) by step (1) graphite particle and the resulting graphite particle of step (2) mix.
In above-mentioned steps (1), the quality hundred of raw material shared by the liquid phase feed of addition (including graphite particle and liquid phase feed)
Divide than generally 5%~8%.
Above-mentioned steps (1), for being vaporized processing to graphite, so that the end face of graphite shows armchair shape structure, and
Armchair shape end face accounts for about the end face 99.5% of the graphite after vaporization process.
Above-mentioned steps (2) are used to carry out oxidation processes to graphite, so that zigzag structure, and sawtooth is presented in the end face of graphite
Shape end face accounts for about the 99.9% of the end face of the graphite after oxidation processes.
When carrying out step (3), the graphite particle of step (2) accounting in admixed graphite particle is improved, then admixed graphite
Serrated end face accounting also correspondingly improves in particle；When carrying out step (3), the graphite particle of step (2) is in admixed graphite
Accounting reduces in particle, then serrated end face accounting also accordingly decreases in admixed graphite particle.Pass through the stone of regulating step (2)
Serrated end face accounting in admixed graphite particle is adjusted to 10%~50% this range with can be convenient by the proportion of black particle
It is interior.
Preferably, the reaction kettle in step (1) is reaction kettle made of glass material, and it is miscellaneous not have metal in preparation process
Matter enters in graphite.
Preferably, the liquid phase feed in step (1) is distilled water, so that the advantage of lower cost of liquid phase feed.
Preferably, nitrogen flow is 1~5 cubic meters per minute in step (1), so that keeping nitrogen atmosphere in carbide furnace.
Preferably, in step (1) 300~950 DEG C at a temperature of handle 5 hours.
Preferably, the range of the volume ratio of nitrogen and oxygen is (1: 1)~(5: 1) in step (2).
Preferably, the volume ratio of nitrogen and oxygen is 5: 1 in step (2).
Preferably, the flow of the mixed gas of nitrogen and oxygen is 5~20L/h in step (2).
In order to make it easy to understand, further illustrating by the following examples.
Embodiment 1
The preparation method of the controllable graphite cathode material of the end face structure the following steps are included:
(1) one group of graphite particle is placed in reaction kettle, filling rate 10%；Liquid phase feed, liquid are passed through into reaction kettle
Phase raw material is distilled water, mass percent 5%；Reaction kettle is sealed and placed in carbide furnace；Nitrogen is passed through into carbide furnace,
Nitrogen flow be 1 cubic meters per minute, and 300 DEG C at a temperature of handle 1 hour；
(2) another group of graphite particle will be walked to be packed into continuous rotary kiln, filling rate 5%；Into continuous rotary kiln
It is passed through the mixed gas of nitrogen and oxygen, is handled 1 hour at 400 DEG C；The range of the volume ratio of the nitrogen and oxygen is 1:
1, the flow of mixed gas is 5L/h；
(3) by step (1) graphite particle and the resulting graphite particle of step (2) mix.
Embodiment 2
The preparation method of the controllable graphite cathode material of the end face structure the following steps are included:
(1) one group of graphite particle is placed in reaction kettle, filling rate 20%；Liquid phase feed, liquid are passed through into reaction kettle
Phase raw material is hydrogen peroxide, mass percent 6%；Reaction kettle is sealed and placed in carbide furnace；Nitrogen is passed through into carbide furnace,
Nitrogen flow be 3 cubic meters per minutes, and 600 DEG C at a temperature of handle 4 hours；
(2) another group of graphite particle will be walked to be packed into continuous rotary kiln, filling rate 20%；Into continuous rotary kiln
It is passed through the mixed gas of nitrogen and oxygen, is handled 2 hours at 500 DEG C；The range of the volume ratio of the nitrogen and oxygen is 3:
1, the flow of mixed gas is 10L/h；
(3) by step (1) graphite particle and the resulting graphite particle of step (2) mix.
Embodiment 3
The preparation method of the controllable graphite cathode material of the end face structure the following steps are included:
(1) one group of graphite particle is placed in reaction kettle, filling rate 30%；Liquid phase feed, liquid are passed through into reaction kettle
Phase raw material is ethyl acetate, mass percent 8%；Reaction kettle is sealed and placed in carbide furnace；Nitrogen is passed through into carbide furnace
Gas, nitrogen flow be 5 cubic meters per minutes, and 950 DEG C at a temperature of handle 9 hours；
(2) another group of graphite particle will be walked to be packed into continuous rotary kiln, filling rate 10%；Into continuous rotary kiln
It is passed through the mixed gas of nitrogen and oxygen, is handled 3 hours at 600 DEG C；The range of the volume ratio of the nitrogen and oxygen is 5:
1, the flow of mixed gas is 20L/h；
(3) by step (1) graphite particle and the resulting graphite particle of step (2) mix.
Embodiment 4
The preparation method of the controllable graphite cathode material of the end face structure the following steps are included:
(1) one group of graphite particle is placed in reaction kettle, filling rate 25%；Liquid phase feed, liquid are passed through into reaction kettle
Phase raw material is toluene, mass percent 5%；Reaction kettle is sealed and placed in carbide furnace；Nitrogen, nitrogen are passed through into carbide furnace
Throughput be 5 cubic meters per minutes, and 600 DEG C at a temperature of handle 3 hours；
(2) another group of graphite particle will be walked to be packed into continuous rotary kiln, filling rate 10%；Into continuous rotary kiln
It is passed through the mixed gas of nitrogen and oxygen, is handled 2 hours at 500 DEG C；The range of the volume ratio of the nitrogen and oxygen is 3:
1, the flow of mixed gas is 10L/h；
(3) by step (1) graphite particle and the resulting graphite particle of step (2) mix.
Embodiment 5
The preparation method of the controllable graphite cathode material of the end face structure the following steps are included:
(1) one group of graphite particle is placed in reaction kettle, filling rate 30%；Liquid phase feed, liquid are passed through into reaction kettle
Phase raw material is distilled water, mass percent 5%；Reaction kettle is sealed and placed in carbide furnace；Nitrogen is passed through into carbide furnace,
Nitrogen flow be 1 cubic meters per minute, and 300 DEG C at a temperature of handle 5 hours；
(2) another group of graphite particle will be walked to be packed into continuous rotary kiln, filling rate 15%；Into continuous rotary kiln
It is passed through the mixed gas of nitrogen and oxygen, is handled 2 hours at 600 DEG C；The range of the volume ratio of the nitrogen and oxygen is 5:
1, the flow of mixed gas is 10L/h；
(3) by step (1) graphite particle and the resulting graphite particle of step (2) mix.
Above-described embodiment 1 to the preparation-obtained graphite cathode material of embodiment 5 is tested, including step (1) institute
The accounting (following table is referred to as " step (1) armchair shape end face ") and step (2) of armchair shape end face are resulting in the graphite particle obtained
The accounting (following table is referred to as " step (2) serrated end face ") of serrated end face in graphite particle, test result is as follows:
| Test item | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Step (1) armchair shape end face | 99.4% | 99.5% | 99.45% | 99.5% | 99.6% |
| Step (2) serrated end face | 99.7% | 99.85% | 99.9% | 99.8% | 99.75% |
By table it is found that predominantly armchair shape end face in graphite particle after vaporization process, and the graphite after oxidation processes
It is mainly serrated end face in particle, further, by certain resulting graphite particle of proportion mixing step (1) and step
(2) resulting graphite particle, can mix serrated end face occupy admixed graphite particle end face ratio (usually 10%~
50%).That is, preparation method provided by the present invention can be realized armchair shape end face and the serrated end face of graphite cathode material
Ratio is controllable, and the performance of graphite cathode material is improved.Further, preparation-obtained graphite cathode material is applied to
Graphite and compatibility of electrolyte (the electrolyte first charge-discharge efficiency of base containing PC up to 90% or more) can be enhanced in lithium ion battery,
Cycle performance (capacity attenuation reduces 10% or more within 800 weeks) is improved, because of the good compatibility of itself and PC base electrolyte, uses PC
Electrolyte battery core has good dynamic performance, and charge-discharge magnification is excellent in.
It, can according to the technique and scheme of the present invention and its hair it is understood that for those of ordinary skills
Bright design is subject to equivalent substitution or change, and all these changes or replacement all should belong to protection scope of the present invention.
Claims (8)
1. a kind of preparation method for the graphite cathode material that end face structure is controllable, which comprises the following steps:
(1) one group of graphite particle is placed in reaction kettle, filling rate is 10%~30%；Liquid phase feed is passed through into reaction kettle,
Liquid phase feed is distilled water, hydrogen peroxide, ethyl acetate or toluene；Reaction kettle is sealed and placed in carbide furnace；Into carbide furnace
Be passed through nitrogen, and 300~950 DEG C at a temperature of handle 1~9 hour；Obtained graphite particle gives over to spare；
(2) another group of graphite particle is packed into continuous rotary kiln, filling rate is 5%~20%；Into continuous rotary kiln
It is passed through the mixed gas of nitrogen and oxygen, is handled 1~3 hour at 400~600 DEG C；Obtained graphite particle gives over to spare；
(3) by step (1) graphite particle and the resulting graphite particle of step (2) mix.
2. the preparation method of the controllable graphite cathode material of end face structure according to claim 1, which is characterized in that step
(1) reaction kettle in is reaction kettle made of glass material.
3. the preparation method of the controllable graphite cathode material of end face structure according to claim 1, which is characterized in that step
(1) liquid phase feed in is distilled water.
4. the preparation method of the controllable graphite cathode material of end face structure according to claim 1, which is characterized in that step
(1) nitrogen flow is 1~5 cubic meters per minute in.
5. the preparation method of the controllable graphite cathode material of end face structure according to claim 1, which is characterized in that step
(1) in 300~950 DEG C at a temperature of handle 5 hours.
6. the preparation method of the controllable graphite cathode material of end face structure according to claim 1, which is characterized in that step
(2) range of the volume ratio of nitrogen and oxygen is (1: 1)~(5: 1) in.
7. the preparation method of the controllable graphite cathode material of end face structure according to claim 1, which is characterized in that step
(2) volume ratio of nitrogen and oxygen is 5: 1 in.
8. the preparation method of the controllable graphite cathode material of end face structure according to claim 1, which is characterized in that step
(2) flow of the mixed gas of nitrogen and oxygen is 5~20L/h in.
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