CN107069015A - A kind of porous graphite doping and the preparation method of carbon coating graphite cathode material - Google Patents

A kind of porous graphite doping and the preparation method of carbon coating graphite cathode material Download PDF

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CN107069015A
CN107069015A CN201710461076.8A CN201710461076A CN107069015A CN 107069015 A CN107069015 A CN 107069015A CN 201710461076 A CN201710461076 A CN 201710461076A CN 107069015 A CN107069015 A CN 107069015A
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graphite
doping
porous
carbon
carbon coating
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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
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • 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
    • H01M4/36—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
    • 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
    • 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
    • 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 kind of doping of porous graphite and the preparation method of carbon coating graphite cathode material, the modification of porous carbon doping and carbon coating to graphite can solve graphite high rate capability it is poor the problem of, because the porous carbon of doping serves the effect of electric transmission cushion in graphite material, therefore the introducing of the cycle performance and the other carbon material of high magnification charge and discharge point performance that improve graphite material can effectively suppress common embedding effect of the electrolyte to graphite, the anti-organic solvent erosiveness of graphite is improved, the cycle performance of graphite is further improved.

Description

A kind of porous graphite doping and the preparation method of carbon coating graphite cathode material
The application is application number：2015102660462, the applying date：05 month 2015 22 days, denomination of invention：It is a kind of porous Graphite dopping and the divisional application of the preparation method of carbon coating graphite cathode material.
Technical field
The present invention relates to lithium ion battery negative material, and in particular to a kind of porous graphite doping and carbon coating graphite cathode The preparation method of material.
Background technology
With the development of automobile industry, the exhaustion of the non-renewable fossil fuel such as oil, natural gas is of increasing concern, empty Gas pollutes and room temperature effect also turns into global problem.To solve energy problem, low-carbon environment-friendly is realized, based on current energy skill The development level of art, electric vehicle engineering is increasingly becoming the emphasis direction of global economic development, the U.S., Japan, Germany, China etc. The national fuel vehicle of limitation in succession is used, and greatly develops electric car.It is used as the core component of electric automobile --- electrokinetic cell is also met Big good opportunity to develop is carried out.Electrokinetic cell refers to the battery applied to electric car, including lithium ion battery, lead-acid battery, combustion Expect battery etc., wherein, lithium ion battery is because with specific energy is high, specific power is big, self discharge is few, service life length and security are good The advantages of, it has also become the emphasis of current various countries' development.
Lithium ion battery is as the remarkable new generation of green high-energy battery of performance, and it has, and high voltage, energy density are big, follow The distinguishing feature such as ring performance is good, self discharge is small, memory-less effect, operating temperature range are wide.Present lithium ion cell electrode material Expect that positive electrode is mainly LiCoO2、LiNiO2And LiMn2O4Deng.Co systems toxicity is larger, and Ni systems synthesis condition is harsh, Mn systems Jahn-Teller effect cycle performances are bad.LiFePO4Being acknowledged as comparing in lithium ion battery of future generation has before application One of positive electrode of scape.However, the security of negative pole is then often ignored by people, current lithium ion battery negative material is main It is carbon material.
And there is relatively low lithium insertion/deintercalation current potential as the graphite type material of lithium ion battery negative material, it is suitable Reversible capacity and aboundresources, it is cheap the advantages of, be more satisfactory lithium ion battery negative material.But there is also head for it Secondary discharging efficiency is low, cycle performance is poor, it is selectively high to electrolyte the shortcomings of, be restricted graphite material application.To understand The certainly disadvantages mentioned above of graphite material, people are modified processing to graphite by various methods, and the method generally used at present is Carbon coating method.Yang Ruizhi etc. exists《Resin carbon coated graphite as lithium ion battery negative electrode research》（《Journal of Inorganic Materials》, 2000,15（4）：712—718）In with liquid-phase impregnation process in natural flake graphite Surface coating phenolic resin, filled with constant current, Electric discharge, powder microelectrode cyclic voltammetry has investigated charging-discharging performances.Test result indicates that, thermally treated phenolic resin carbon Coated graphite material puts that a capacity is higher, and cycle life is longer, can as high performance lithium ion battery negative material.He Ming Deng《The preparation of resin carbon-coated graphite and its chemical property》（《Battery》, 2003,3（5）：281—284）In in day Right micro crystal graphite particle surface coats one layer of resin carbon, and cladding processing can reduce the appearance irreversible first of natural micro crystal graphite Amount, using first mixing and then scattered method coated graphite, inside is natural micro crystal graphite, and outside is 1~2 μm of phenolic resin Pyrolytic carbon layer.The irreversible capacity that lithium ion experimental cell measures natural micro crystal graphite is 14%, the irreversible capacity of coated graphite For 7%.Cladding processing can largely reduce the irreversible capacity of natural micro crystal graphite.Chen Meng etc. exists《Pitch-coating is natural The preparation of graphite and performance study》（《Battery industry》, 2007,12（5）：298—302）Using liquid phase coating method, pitch is split Carbon coating is solved on natural spherical plumbago, to improve its cycle performance.Test result indicates that, native graphite after pitch-coating, Irreversible capacity loss has been reduced to 32.5mAh/g from 125.5mAh/g, and specific capacity is brought up to from 290.8mAh/g 365.3mAh/g, the capability retention after 50 circulations has brought up to 93.66% from 55.4%, effectively improves following for native graphite Ring performance.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of porous graphite doping and carbon coating graphite cathode material Preparation method, it is therefore intended that the problems such as solving poor graphite high-rate charge-discharge capability and anti-electrolyte organic solvent poor compatibility, Improve the cycle performance of discharge and recharge.
The present invention solve the technical scheme that is used of above-mentioned technical problem for：A kind of porous graphite doping and carbon coating graphite The preparation method of negative material, it is characterised in that comprise the following steps：
（1）Configuration concentration is 1~12 mg/mL potassium permanganate solution, adds graphite and carries out oxidation pore-creating, washing and drying is obtained To porous graphite；
（2）According to porous graphite：Graphite=（0.02~0.1）：1 ratio, while 5~20% ratio of graphite weight adds one Quantitative carbon matrix precursor, is well mixed, obtains porous graphite and graphite and carbon matrix precursor composite granule；
（3）Under inert gas shielding, the composite granule in step (2) is heated to 700~950 with 2~10 DEG C/min heatings DEG C, and continue 3~20 hours, cool down to after room temperature, pulverize and sieve, that is, obtain porous graphite doping and carbon coating graphite cathode Material.
Step（1）In graphite be native graphite, particle diameter D50≤5 μm, specific surface area >=10m2/g。
Step（2）In graphite be Delanium or native graphite, particle diameter D50 is between 5~25 μm, specific surface area≤6m2/ G, tap density >=0.7g/cm3。
Step（2）Described in carbon matrix precursor be sodium cellulose glycolate, polyvinyl alcohol, phenolic resin, epoxy resin, Portugal Mixture more than one or both of grape sugar, starch, pitch.
Step（3）Described inert gas is argon gas.
Compared with prior art, the advantage of the invention is that porous graphite doping improves the conductance of graphite with carbon coating Rate, obtained porous graphite doping is high with carbon coating graphite cathode material specific capacity, and good cycle can be widely applied to various Lithium ion battery.Meanwhile, preparation method of the invention is with low cost, and technique is simple, is suitable for large-scale industrial production.
The problem of high rate capability that porous carbon can solve graphite to the doping vario-property of graphite is poor, it is porous due to doping Carbon serves the effect of electric transmission cushion in graphite material, therefore improves the cycle performance and high magnification of graphite material The introducing of the other carbon material of charge and discharge point performance can effectively suppress common embedding effect of the electrolyte to graphite, and raising graphite resists organic molten Agent erosiveness, further improves the cycle performance of graphite.
Embodiment
The present invention is described in further detail below in conjunction with specific embodiment.
Embodiment 1
A kind of porous graphite doping and the preparation method of carbon coating graphite cathode material, comprise the following steps：
（1）5 mg/mL potassium permanganate solution is prepared, by 50g native graphite（Particle diameter D50：3.63 μm, specific surface area： 12.51m2/g）Be added in solution, then oxidation processes 60min is washed with water to neutrality, then dry for standby；
（2）According to porous graphite：Graphite（D50：10.82 μm, specific surface area：6.1m2/ g, tap density：0.96g/cm3）= 0.02：1 ratio, while the ratio of graphite weight 5% adds a certain amount of carbon matrix precursor（Pitch powder）, it is well mixed, obtains Porous graphite and graphite and carbon matrix precursor composite granule；
（3）Under inert gas shielding, the composite granule in step (2) is heated to 950 DEG C with 10 DEG C/min heatings, and hold It is continuous 3 hours, cool down to after room temperature, pulverize and sieve, that is, obtain porous graphite doping and carbon coating graphite cathode material.
Embodiment 2
A kind of porous graphite doping and the preparation method of carbon coating graphite cathode material, comprise the following steps：
（1）10 mg/mL potassium permanganate solution is prepared, by 50g native graphite（Particle diameter D50：5.42 μm, specific surface area： 18.12m2/g）Be added in solution, then oxidation processes 30min is washed with water to neutrality, then dry for standby；
（2）According to porous graphite：Graphite（D50：17.21 μm, specific surface area：5.8m2/ g, tap density：0.85g/cm3）= 0.1：1 ratio, while the ratio of graphite weight 10% adds a certain amount of carbon matrix precursor（Phenolic resin powder）, it is well mixed, Obtain porous graphite and graphite and carbon matrix precursor composite granule；
（3）Under inert gas shielding, the composite granule in step (2) is heated to 900 DEG C with 5 DEG C/min heatings, and continue 5 hours, cool down to after room temperature, pulverize and sieve, that is, obtain porous graphite doping and carbon coating graphite cathode material.
Embodiment 3
A kind of porous graphite doping and the preparation method of carbon coating graphite cathode material, comprise the following steps：
（1）8 mg/mL potassium permanganate solution is prepared, by 50g native graphite（Particle diameter D50：7.28 μm, specific surface area： 15.42m2/g）Be added in solution, then oxidation processes 50min is washed with water to neutrality, then dry for standby；
（2）According to porous graphite：Graphite（D50：8.14 μm, specific surface area：6.9m2/ g, tap density：1.04g/cm3）= 0.08：1 ratio, while the ratio of graphite weight 7% adds a certain amount of carbon matrix precursor（Epoxy resin powder）, it is well mixed, Obtain porous graphite and graphite and carbon matrix precursor composite granule；
（3）Under inert gas shielding, the composite granule in step (2) is heated to 850 DEG C with 8 DEG C/min heatings, and continue 6 hours, cool down to after room temperature, pulverize and sieve, that is, obtain porous graphite doping and carbon coating graphite cathode material.
Comparative example 1
Undressed native graphite in embodiment 1.
Comparative example 2
Undressed Delanium in embodiment 2.
Electrochemical property test
For the performance for the modification lithium-ion battery graphite cathode material for examining the inventive method preparation, entered with half-cell method of testing Row test, with above example and the negative material of comparative example：Acetylene black：PVDF（Kynoar）=95：2：3（Weight ratio）, Plus appropriate NMP（1-METHYLPYRROLIDONE）Pulpous state is tuned into, is coated on copper foil, negative pole is made within 8 hours through 110 DEG C of dryings of vacuum Piece；Using metal lithium sheet as to electrode, electrolyte is 1mol/L LiPF6/EC+DEC+DMC=1：1：1, microporous polypropylene membrane be every Film, is assembled into battery.Charging/discharging voltage is 0~2.0V, and charge-discharge velocity is 0.5C, and battery performance is carried out can test, test It the results are shown in Table 1.
Table 1 for negative material in not be the same as Example and comparative example performance comparision
The general principle and principal character and advantages of the present invention of the present invention, the technical staff of the industry has been shown and described above It should be appreciated that the present invention is not limited to the above embodiments, simply illustrate the present invention described in above-described embodiment and specification Principle, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these change and Improvement all fall within the protetion scope of the claimed invention, and the claimed scope of the invention is by appended claims and its equivalent Thing is defined.

Claims (3)

1. a kind of porous graphite doping and the preparation method of carbon coating graphite cathode material, it is characterised in that comprise the following steps：
（1）Prepare porous graphite：Configuration concentration is 1-12mg/mL potassium permanganate solution, adds graphite and carries out oxidation pore-creating, Washing and drying, obtains porous graphite；
（2）It is prepared by graphite presoma：According to porous graphite：Graphite=（0.02~0.1）：1 ratio, while the 5 of graphite weight~ 20% ratio adds a certain amount of carbon matrix precursor, is well mixed, obtains porous graphite and graphite and carbon matrix precursor composite powder Body；
（3）High-temperature process：Under inert gas shielding, the powder of drying in step (2) is heated to 2~10 DEG C/min heatings 700~950 DEG C, and continue 3-20 hours, cool down to after room temperature, pulverize and sieve, that is, obtain porous graphite doping and carbon coating Graphite cathode material.
2. a kind of doping of porous graphite and the preparation method of carbon coating graphite cathode material according to claim 1, it is special Levy and be step（1）In graphite be native graphite, particle diameter D50≤10 μm, specific surface area >=10m2/ g, step（2）In stone Ink is Delanium or native graphite, and particle diameter D50 is between 5~25 μm, specific surface area≤6m2/ g, tap density >=0.7g/cm3。
3. a kind of doping of porous graphite and the preparation method of carbon coating graphite cathode material according to claim 1, it is special Levy and be step（2）Described in carbon source presoma be sodium cellulose glycolate, polyvinyl alcohol, phenolic resin, epoxy resin, Portugal Mixture more than one or both of grape sugar, starch, pitch.
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CN109546099B (en) * 2018-10-16 2021-08-31 中航锂电（洛阳）有限公司 Graphite composite negative electrode material, preparation method thereof and lithium ion battery
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Application publication date: 20170818