CN109449420A - A kind of surface low-level oxidation and liquid phase coating modified graphite cathode material and preparation method thereof - Google Patents
A kind of surface low-level oxidation and liquid phase coating modified graphite cathode material and preparation method thereof Download PDFInfo
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- CN109449420A CN109449420A CN201811322205.6A CN201811322205A CN109449420A CN 109449420 A CN109449420 A CN 109449420A CN 201811322205 A CN201811322205 A CN 201811322205A CN 109449420 A CN109449420 A CN 109449420A
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention relates to materials and electrochemical field, more particularly to a kind of surface low-level oxidation and liquid phase coating modified graphite cathode material and preparation method thereof, this method passes through surface low-level oxidation, in the more micropores of graphite cathode material Surface Creation and nano pore, the memory space for increasing lithium ion, is improved its high rate performance, and by by graphite cathode material liquid phase coating, first effect is effectively improved by simple process, guarantees cycle performance.
Description
Technical field
The present invention relates to materials and electrochemical field, and in particular to a kind of surface low-level oxidation and liquid phase coating modified graphite
Negative electrode material and preparation method thereof.
Background technique
With the continuous extension of application field, lithium battery market is increased rapidly, and is studied and developed in global new energy
In occupy an important position, wherein the Rapid Expansion of new-energy automobile market has driven lithium-ion-power cell demand to soar,
Power battery gradually becomes the leading force of lithium ion battery industry growth.
Under existing lithium-ion battery system, high rate performance, energy density, service life, safety, price etc. are most important
Index, and energy density it is high, can fast charge, cheap, then be the ideal type power battery product that user most expects.As mesh
The preceding maximum lithium ion battery negative material of usage amount --- graphite type material, to lithium ion battery energy density and high rate performance
The limitation of raising is more obvious, therefore, it is negative to design and develop a kind of graphite for combining energy density with excellent rapid charging performance
Pole material is most important.Currently, the report of existing graphite negative electrode material method of modifying.Such as CN20150897454.8 is public
It opens and reports graphite fine powder and liquid phase coating agent Heat preservation mixed at high speed in high speed mixer, be added in continuous covering
It is coated to obtain presoma, carries out high-temperature process under inert gas shielding in tube furnace, kept the temperature, be cooled to room temperature
Obtain liquid phase coating modified graphite cathode material.CN201610703415.4 then disclose report it is a kind of with ultraviolet lamp by carbon substrate
Material carries out different degrees of irradiation, by the carbon on the oxygen combination carbon-based material in air, is converted to oxygen-containing functional group, realizes carbon-based
The surface low-level oxidation of material, using the material as the method for lithium ion battery negative material, the specific volume of the lithium ion battery of preparation
Amount and cycle performance are improved, but this method process is more complicated, is not suitable for industrial continuous production, and economic benefits have
Limit.
This patent is granulated the method combined with liquid phase coating using surface low-level oxidation, obtains what comprehensive performance significantly improved
Graphite cathode material.On the one hand by surface low-level oxidation, in the more micropores of graphite cathode material Surface Creation and nano pore,
The memory space for increasing lithium ion, is improved its high rate performance；On the other hand, by graphite cathode material liquid phase coating, lead to
It crosses simple process and effectively improves first effect, guarantee cycle performance.
Summary of the invention
One of the objects of the present invention is to provide the modified graphite cathode material of a kind of surface low-level oxidation and liquid phase coating,
The graphite cathode material includes that the raw material of following parts by weight is prepared: small particle graphite fine powder 60-90%, preferably 70%-
90%, more preferable 80%-90%；Pitch 1-10%, preferably 5%-10%；Liquid phase coating agent 1-10%, preferably 5%-10%.
As a further solution of the present invention, small particle graphite fine powder be selected from spherical natural graphite, spherical natural graphite,
One or more of crystalline flake graphite, artificial graphite, the partial size of graphite fine powder are 6-8 μm.
As a further solution of the present invention, liquid phase coating agent is selected from acetone, ethyl alcohol, ether, liquid phenolic resin, liquid
One or more of epoxy resin.
The invention further relates to the graphite cathode materials for providing a kind of surface low-level oxidation and liquid phase coating described above
Preparation method, which is characterized in that preparation step is as follows:
(1) little particle graphite cathode material is immersed in stir in oxidant and is aoxidized, drying for standby after deionized water processing；
(2) by the little particle graphite fine powder of step (1) surface low-level oxidation processing and pitch, liquid phase coating agent according to certain ratio
Example is added in mixing apparatus, stirs evenly；
(3) under inert gas protection by the mixture of step (2), high-temperature heat treatment, carbonization, cooling obtain the micro- oxygen in surface
The graphite cathode material of change and liquid phase coating.
As the further scheme of the present invention, wherein step (1):
Step (1) small particles graphite cathode material be selected from spherical natural graphite, spherical natural graphite, crystalline flake graphite,
One or more of artificial graphite.
Oxidant described in step (1) in nitric acid, ammonium peroxydisulfate, sulfuric acid, potassium permanganate, hydrogen peroxide one
Kind is a variety of；When oxidant is solid, it is made into saturated solution.
It is 60-100 hours that step (1) small particles graphite cathode material, which is immersed in mixing time in oxidant, preferably 60-80
Hour, reaction temperature is room temperature.
As the further scheme of the present invention, wherein step (2):
The partial size of little particle graphite fine powder described in step (2) is 6-8 μm.
Liquid phase coating agent described in step (2) is in acetone, ethyl alcohol, ether, liquid phenolic resin, liquid-state epoxy resin
One or more.
In step (2) mass percent of graphite cathode material be 60-90%, preferably 70%-90%, more preferably
80%-90%；Pitch is 1-10%, preferably 5%-10%；Liquid phase coating agent is 1-10%, preferably 5%-10%.
Mixing apparatus described in step (2) is the equipment with stirring action, preferably fusion machine, VC mixing machine etc..
Step (2) whipping temp is room temperature, and speed of agitator is set as 200-400 and turns, and preferably 300-400 turns, mixing time
For 30-60min.
As the further scheme of the present invention, wherein step (3):
Step (3) inert gas is nitrogen or argon gas, purity preferably 99% or more.
Step (3) high-temperature heat treatment temperature is 1000-1500 DEG C, preferably 1100-1300 DEG C；Carbonization time is 6-24h,
Preferably 8-18 hours, preferably 10-12 hours.
The present invention has the effect of unexpected be:
1. surface low-level oxidation of the present invention and liquid phase coating modified graphite cathode material, high rate performance obtain substantially
Degree improves, and chemical property is outstanding, and can realize industrial continuous production, and first charge-discharge efficiency is up to 94% or more, holds
Amount is greater than 350mAh/g, and granularity D50 15-17 μm, charge-discharge magnification > 10C can be used for 48V start and stop, model plane, electric tool etc.
High multiplying power lithium ion battery market；
2. the present invention, which is mixed or merged using VC, completes mixing under machine room temperature, recycle carbonization kiln line in inert gas
It is heat-treated under protection, surface low-level oxidation and liquid phase coating modification and the graphite cathode material for having granulation outcome can be obtained
Material, using the method for liquid phase coating, process route is simple, Yi Shixian industrial mass production, final finished slurrying processability
Can preferably, the liquid phase coating method that the present invention uses has granulation outcome, and compared with dynamic is granulated, this method effect is more preferable.
3. the method that the present invention is combined using surface low-level oxidation with liquid phase coating, the synthesis of modified graphite cathode material
Performance is significantly improved, and carries out surface low-level oxidation to graphite cathode material, obtained modified graphite cathode material can be generated
More micropores and nano pore, increase the memory space of lithium ion, are improved its high rate performance, liquid-coating method letter
It is single, first effect can be effectively improved, and guarantee cycle performance.
4. the present invention is led to simultaneously by the modified shortening lithium ion mobility path of graphite material liquid phase coating of preferred small particle
The lithium ion mobility channel that surface oxidation pore-creating technique further increases basal plane is crossed, improves lithium ion mobility speed, and by making
Grain technique reduces anisotropy, so as to improve its charge-discharge magnification.
Detailed description of the invention
The following further describes the present invention with reference to the drawings.
Fig. 1 is the SEM figure of embodiment 1
Specific embodiment
The present invention will be further described with reference to the examples below.Described embodiment and its result are merely to illustrate
The present invention, without the present invention described in detail in claims should will not be limited.
Comparative example 1
(1) little particle graphite cathode material is immersed in the concentrated sulfuric acid (98%) solution at room temperature and is stirred 80 hours, deionization
The graphite cathode material of surface low-level oxidation processing can be obtained in drying for standby after water process.
(2) by 6-8 μm of graphite fine powder of partial size (90%) and pitch (5%), liquid phenolic resin after the low-level oxidation of surface
(5%) it is added in fusion machine, is stirred evenly under room temperature, fusion machine speed of agitator is set as 300 turns, mixing time 30min.
(3) fused mixture is put into crucible, investment carbonization kiln line in and under inert gas protection
1100 DEG C of progress high-temperature heat treatments, carbonization time 12h are cooled to room temperature, surface low-level oxidation can be obtained and liquid phase coating changes
Property graphite cathode material.
Obtained high magnification graphite cathode material performance parameter are as follows: first charge-discharge efficiency is high by 94% or more；Capacity
348.6mAh/g；15.5 μm of granularity D50；Charge-discharge magnification < 10C.
Comparative example 2
(1) at room temperature by little particle graphite cathode material be immersed in the concentrated sulfuric acid (98%) and hydrogen peroxide (30%) (concentrated sulfuric acid:
Hydrogen peroxide=1:1) middle stirring 80 hours, the stone of surface low-level oxidation processing can be obtained in drying for standby after deionized water processing
Black negative electrode material.
(2) by 6-8 μm of graphite fine powder of partial size (90%) and pitch (5%), liquid phenolic resin after the low-level oxidation of surface
(5%) it is added in fusion machine, is stirred evenly under room temperature, fusion machine speed of agitator is set as 300 turns, mixing time 30min.
(3) fused mixture is put into crucible, investment carbonization kiln line in and under inert gas protection
1100 DEG C of progress high-temperature heat treatments, carbonization time 12h are cooled to room temperature, surface low-level oxidation can be obtained and liquid phase coating changes
Property graphite cathode material.
Obtained high magnification graphite cathode material performance parameter are as follows: first charge-discharge efficiency is up to 94% or more；Capacity
349.3mAh/g；15.3 μm of granularity D50；Charge-discharge magnification < 10C.
Comparative example 1-2 is as the result is shown: the graphite cathode material that the concentrated sulfuric acid and hydrogen peroxide are prepared as oxidant easily causes
Graphite surface layer is cracked and defect causes volume expansion and the limellar stripping of graphite in charge and discharge process.
Comparative example 3
(1) little particle graphite cathode material is immersed in ammonium peroxydisulfate (NH at room temperature4)2S2O880 are stirred in saturated solution
Hour, the graphite cathode material of surface low-level oxidation processing can be obtained in drying for standby after deionized water processing.
(2) by after the low-level oxidation of surface 6-8 μm of graphite fine powder of partial size (95%) and pitch (5%) be added fusion machine in, often
It is stirred evenly under temperature, fusion machine speed of agitator is set as 300 turns, mixing time 30min.
(3) fused mixture is put into crucible, investment carbonization kiln line in and under inert gas protection
1100 DEG C of progress high-temperature heat treatments, carbonization time 12h are cooled to room temperature, surface low-level oxidation can be obtained and liquid phase coating changes
Property graphite cathode material.
Obtained high magnification graphite cathode material performance parameter are as follows: first charge-discharge efficiency is high by 94% or more；Capacity
343.3mAh/g；13.3 μm of granularity D50；Charge-discharge magnification < 10C.
Comparative example 3 does not add liquid phase covering, and in the case, granulation outcome is unobvious, and capacity is unable to get obviously
It is promoted.
Embodiment 1
(1) little particle graphite cathode material is immersed in ammonium peroxydisulfate (NH at room temperature4)2S2O880 are stirred in saturated solution
Hour, the graphite cathode material of surface low-level oxidation processing can be obtained in drying for standby after deionized water processing.
(2) by 6-8 μm of graphite fine powder of partial size (90%) and pitch (5%), liquid phenolic resin after the low-level oxidation of surface
(5%) it is added in fusion machine, is stirred evenly under room temperature, fusion machine speed of agitator is set as 300 turns, mixing time 30min.
(3) fused mixture is put into crucible, investment carbonization kiln line in and under inert gas protection
1100 DEG C of progress high-temperature heat treatments, carbonization time 12h are cooled to room temperature, surface low-level oxidation can be obtained and liquid phase coating changes
Property graphite cathode material.
Obtained high magnification graphite cathode material performance parameter are as follows: first charge-discharge efficiency is up to 94% or more；Capacity
351.7mAh/g；16.3 μm of granularity D50；Charge-discharge magnification > 10C.
Embodiment 2
(1) little particle graphite cathode material is immersed in ammonium peroxydisulfate (NH at room temperature4)2S2O880 are stirred in saturated solution
Hour, the graphite cathode material of surface low-level oxidation processing can be obtained in drying for standby after deionized water processing.
(2) by 6-8 μm of graphite fine powder of partial size (85%) and pitch (10%), liquid phenolic resin after the low-level oxidation of surface
(5%) it is added in fusion machine, is stirred evenly under room temperature, fusion machine speed of agitator is set as 300 turns, mixing time 30min.
(3) fused mixture is put into crucible, investment carbonization kiln line in and under inert gas protection
1100 DEG C of progress high-temperature heat treatments, carbonization time 12h are cooled to room temperature, surface low-level oxidation can be obtained and liquid phase coating changes
Property graphite cathode material.
Obtained high magnification graphite cathode material performance parameter are as follows: first charge-discharge efficiency is up to 94% or more；Capacity
355.7mAh/g；17.8 μm of granularity D50；Charge-discharge magnification > 10C.
Embodiment 3
(1) little particle graphite fine powder is immersed in ammonium peroxydisulfate (NH at room temperature4)2S2O8It is stirred 80 hours in saturated solution,
Drying for standby after deionized water processing, can be obtained the graphite cathode material of surface low-level oxidation processing.
(2) by after the low-level oxidation of surface 6-8 μm of graphite cathode material of partial size (85%) and pitch (5%), liquid phenolic aldehyde tree
Rouge (10%) is added in fusion machine, stirs evenly under room temperature, and fusion machine speed of agitator is set as 300 turns, and mixing time is
30min。
(3) fused mixture is put into crucible, investment carbonization kiln line in and under inert gas protection
1100 DEG C of progress high-temperature heat treatments, carbonization time 12h are cooled to room temperature, surface low-level oxidation can be obtained and liquid phase coating changes
Property graphite cathode material.
Obtained high magnification graphite cathode material performance parameter are as follows: first charge-discharge efficiency is up to 94% or more；Capacity
350.3mAh/g；16.1 μm of granularity D50；Charge-discharge magnification > 10C.
Graphite cathode material used in present example of the present invention is artificial graphite, when it selects spherical natural graphite, class
Spherical natural graphite, crystalline flake graphite etc. can achieve the desired results.
Claims (10)
1. the graphite cathode material of a kind of surface low-level oxidation and liquid phase coating, the raw material including following parts by weight are prepared:
Small particle graphite fine powder 60-90%, preferably 70%-90%, more preferable 80%-90%；Pitch 1-10%, preferably 5%-10%；
Liquid phase coating agent 1-10%, preferably 5%-10%.
2. graphite cathode material according to claim 1, it is characterised in that: small particle graphite fine powder is selected from spherical natural stone
One or more of black, spherical natural graphite, crystalline flake graphite, artificial graphite, the partial size of graphite fine powder are 6-8 μm.
3. graphite cathode material according to claim 1, it is characterised in that: liquid phase coating agent is selected from acetone, ethyl alcohol, second
One or more of ether, liquid phenolic resin, liquid-state epoxy resin.
4. a kind of preparation method of the graphite cathode material of surface low-level oxidation described in claim 1 and liquid phase coating, special
Sign is that preparation step is as follows:
(1) little particle graphite cathode material is immersed in stir in oxidant and is aoxidized, drying for standby after deionized water processing obtains table
The graphite cathode material of face low-level oxidation processing；
(2) the little particle graphite fine powder by the processing of step (1) surface low-level oxidation adds according to a certain percentage with pitch, liquid phase coating agent
Enter in mixing apparatus, stirs evenly；
(3) under inert gas protection by the mixture of step (2), high-temperature heat treatment, carbonization, it is cooling obtain surface low-level oxidation with
And the graphite cathode material of liquid phase coating.
5. the preparation method according to claim 4, which is characterized in that little particle graphite cathode material described in step (1)
Material is selected from one or more of spherical natural graphite, spherical natural graphite, crystalline flake graphite, artificial graphite；The oxygen
Agent is selected from one or more of nitric acid, ammonium peroxydisulfate, sulfuric acid, potassium permanganate, hydrogen peroxide.
6. the preparation method according to claim 4, which is characterized in that step (1) small particles graphite cathode material is immersed in
Mixing time is 60-100 hours in oxidant, and preferably 60-80 hours, reaction temperature was room temperature.
7. the preparation method according to claim 4, which is characterized in that the grain of little particle graphite fine powder described in step (2)
Diameter is 6-8 μm；The liquid phase coating agent is selected from one of acetone, ethyl alcohol, ether, liquid phenolic resin, liquid-state epoxy resin
Or it is a variety of；The mass percent of the graphite cathode material is 60-90%, preferably 70%-90%, more preferably 80%-
90%；Pitch is 1-10%, preferably 5%-10%；Liquid phase coating agent is 1-10%, preferably 5%-10%.
8. the preparation method according to claim 4, which is characterized in that step (2) whipping temp is room temperature, and speed of agitator is set
It is set to 200-400 to turn, preferably 300-400 turns, mixing time 30-60min.
9. the preparation method according to claim 4, which is characterized in that step (3) inert gas is nitrogen or argon gas.
10. the preparation method according to claim 4, which is characterized in that step (3) high-temperature heat treatment temperature is 1000-
1500 DEG C, preferably 1100-1300 DEG C；Carbonization time is 6-24h, preferably 8-18 hours, preferably 10-12 hours.
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| CN109817957A (en) * | 2019-03-29 | 2019-05-28 | 河南九龙新能源材料有限公司 | A kind of preparation method of pitch-coating silicon doping natural flake graphite negative electrode material |
| CN109950495A (en) * | 2019-03-27 | 2019-06-28 | 溧阳紫宸新材料科技有限公司 | Preparation method, negative electrode material and the lithium ion battery of high magnification graphite cathode material |
| CN112018366A (en) * | 2020-09-10 | 2020-12-01 | 安徽科达新材料有限公司 | Graphite negative electrode material of lithium ion battery and preparation method thereof |
| CN113130876A (en) * | 2021-04-19 | 2021-07-16 | 合肥国轩高科动力能源有限公司 | Preparation method and application of acid-modified spherical natural graphite negative electrode material |
| CN113410449A (en) * | 2021-06-25 | 2021-09-17 | 广东凯金新能源科技股份有限公司 | Multiphase adjustable carbon-coated novel artificial graphite negative electrode material and preparation method thereof |
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| CN115010127A (en) * | 2022-07-20 | 2022-09-06 | 晖阳(贵州)新能源材料有限公司 | Preparation method of high-rate lithium ion battery negative electrode material |
| CN115084477A (en) * | 2022-07-08 | 2022-09-20 | 广东凯金新能源科技股份有限公司 | Preparation method of graphite cathode material, graphite cathode and application of graphite cathode material |
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| CN112018366A (en) * | 2020-09-10 | 2020-12-01 | 安徽科达新材料有限公司 | Graphite negative electrode material of lithium ion battery and preparation method thereof |
| CN113130876A (en) * | 2021-04-19 | 2021-07-16 | 合肥国轩高科动力能源有限公司 | Preparation method and application of acid-modified spherical natural graphite negative electrode material |
| CN113410449A (en) * | 2021-06-25 | 2021-09-17 | 广东凯金新能源科技股份有限公司 | Multiphase adjustable carbon-coated novel artificial graphite negative electrode material and preparation method thereof |
| CN115084477A (en) * | 2022-07-08 | 2022-09-20 | 广东凯金新能源科技股份有限公司 | Preparation method of graphite cathode material, graphite cathode and application of graphite cathode material |
| CN115010127A (en) * | 2022-07-20 | 2022-09-06 | 晖阳(贵州)新能源材料有限公司 | Preparation method of high-rate lithium ion battery negative electrode material |
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