CN104934579A - Preparation method for porous graphite doped and carbon coated graphite anode material - Google Patents

Preparation method for porous graphite doped and carbon coated graphite anode material Download PDF

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CN104934579A
CN104934579A CN201510266046.2A CN201510266046A CN104934579A CN 104934579 A CN104934579 A CN 104934579A CN 201510266046 A CN201510266046 A CN 201510266046A CN 104934579 A CN104934579 A CN 104934579A
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graphite
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carbon
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CN104934579B (en
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田东
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Shanghai Liming Technology Co ltd
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Priority to CN201710461064.5A priority patent/CN107275610A/en
Priority to CN201710461071.5A priority patent/CN107069014A/en
Priority to CN201710461072.XA priority patent/CN107180962A/en
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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 preparation method for a porous graphite doped and carbon coated graphite anode material. The problem of poor high-rate discharge ability of graphite can be solved due to the modification of porous carbon doping and carbon coating on graphite, since the doped porous carbon acts as an electron transmission buffer layer in a graphite material, the cycle performance and the high-rate charge/discharge ability of the graphite material are improved; moreover, the co-intercalation of an electrolyte on graphite can be effectively suppressed due to the introduction of carbon material, the corrosion resistant capability of the graphite to an organic solvent is enhanced, and the cycle performance of the graphite is further improved.

Description

The preparation method of a kind of porous graphite doping and carbon coated graphite negative material
Technical field
The present invention relates to lithium ion battery negative material, be specifically related to the preparation method of the doping of a kind of porous graphite and carbon coated graphite negative material.
Background technology
Along with the development of automobile industry, the exhaustion of the non-renewable fossil fuel such as oil, natural gas receives publicity day by day, and air pollution and room temperature effect also become global problem.For solving energy problem, realize low-carbon environment-friendly, based on the development level of current energy technology, electric vehicle engineering becomes the emphasis direction of global economic development gradually, the countries such as the U.S., Japan, Germany, China in succession limit fuel vehicle and use, and greatly develop electric motor car.As the core component of electric automobile---electrokinetic cell has also welcome large good opportunity to develop.Electrokinetic cell refers to the battery being applied to electric motor car, comprise lithium ion battery, lead-acid battery, fuel cell etc., wherein, specific energy is high, specific power is large, self discharge is few because having for lithium ion battery, long service life and the advantage such as fail safe is good, has become the emphasis of current various countries development.
Lithium ion battery as the new generation of green high-energy battery of performance brilliance, the distinguishing features such as high voltage, energy density are large, good cycle, self discharge is little, memory-less effect, operating temperature range are wide that it has.Present lithium ion battery electrode material positive electrode is mainly LiCoO 2, LiNiO 2and LiMn 2o 4deng.Co system toxicity is comparatively large, and Ni system synthesis condition is harsh, and Mn system Jahn-Teller effect cycle performance is bad.LiFePO 4be acknowledged as in lithium ion battery of future generation and compare one of positive electrode having application prospect.But the fail safe of negative pole is then often ignored by people, current lithium ion battery negative material mainly material with carbon element.
And as the graphite type material of lithium ion battery negative material, there is lower lithium embedding/deintercalation current potential, suitable reversible capacity and aboundresources, the advantage such as cheap, be more satisfactory lithium ion battery negative material.But it also exists first, and discharging efficiency is low, cycle performance is poor, to shortcomings such as electrolyte selectivity are high, make graphite material application be restricted.In order to solve the above-mentioned shortcoming of graphite material, people carry out modification by various method to graphite, and the method usually adopted at present is carbon cladding process.Yang Ruizhi etc. are at " resin carbon coated graphite is as the research of lithium ion battery negative electrode " (" Journal of Inorganic Materials ", 2000,15(4): 712-718) with liquid-phase impregnation process at natural flake graphite Surface coating phenolic resins, use constant current charge and discharge, powder microelectrode cyclic voltammetry has investigated charging-discharging performances.Experimental result shows, through heat treated phenolic resins carbon coated graphite material to put a capacity higher, cycle life is longer, can be used as the negative material of high performance lithium ion battery.He Ming etc. are at " preparation of resin carbon-coated graphite and chemical property thereof " (" battery ", 2003, at natural micro crystal graphite particle surface coated one deck resin carbon 3(5): 281-284), coated process can reduce the irreversible capacity first of natural micro crystal graphite, adopt and first mix the method coated graphite then disperseed, inside is natural micro crystal graphite, and outside is the phenolic resins pyrolysis carbon-coating of 1 ~ 2 μm.The irreversible capacity that lithium ion experimental cell records natural micro crystal graphite is 14%, and the irreversible capacity of coated graphite is 7%.Coated process can reduce the irreversible capacity of natural micro crystal graphite to a great extent.Chen Meng etc. are at " the preparation and property research of pitch-coating native graphite " (" battery industry ", 2007,12(5): 298-302) adopt liquid phase coating method, be coated on natural spherical plumbago, to improve its cycle performance by pitch cracking carbon.Experimental result shows, native graphite is after pitch-coating, irreversible capacity loss has reduced to 32.5mAh/g from 125.5mAh/g, specific capacity has brought up to 365.3mAh/g from 290.8mAh/g, capability retention after 50 circulations has brought up to 93.66% from 55.4%, effectively improves the cycle performance of native graphite.
Summary of the invention
Technical problem to be solved by this invention is to provide the preparation method of the doping of a kind of porous graphite and carbon coated graphite negative material, object is to solve the problems such as graphite high-rate charge-discharge capability difference and anti-electrolyte organic solvent poor compatibility, improves the cycle performance of discharge and recharge.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of porous graphite doping and the preparation method of carbon coated graphite negative material, is characterized in that comprising the following steps:
(1) configuration concentration is the potassium permanganate solution of 1 ~ 12 mg/mL, adds graphite and carries out oxidation pore-creating, washing and drying, obtain porous graphite;
(2) according to porous graphite: graphite=(0.02 ~ 0.1): the ratio of 1, simultaneously graphite weight 5 ~ 20% ratio add a certain amount of carbon matrix precursor, mix, obtain porous graphite and graphite and carbon matrix precursor composite granule;
(3) under inert gas shielding; composite granule in step (2) is heated up with 2 ~ 10 DEG C/min and is heated to 700 ~ 950 DEG C, and continue 3 ~ 20 hours, after room temperature is down in cooling; pulverize and sieve, namely obtain porous graphite doping and carbon coated graphite negative material.
Graphite in step (1) is native graphite, particle diameter D50≤5 μm, specific area>=10m 2/ g.
Graphite in step (2) is Delanium or native graphite, particle diameter D50 between 5 ~ 25 μm, specific area≤6m 2/ g, tap density>=0.7g/cm 3.
Carbon matrix precursor described in step (2) is one or more the mixture in sodium cellulose glycolate, polyvinyl alcohol, phenolic resins, epoxy resin, glucose, starch, pitch.
Inert gas described in step (3) is nitrogen or argon gas.
Compared with prior art, the invention has the advantages that porous graphite doping and the coated conductivity that improve graphite of carbon, obtained porous graphite doping is high with carbon coated graphite negative material specific capacity, and good cycle, can be widely used in various lithium ion battery.Meanwhile, preparation method of the present invention is with low cost, and technique is simple, is suitable for large-scale industrial production.
Porous carbon can solve the poor problem of the high rate capability of graphite to the doping vario-property of graphite, porous carbon due to doping serves the effect of electric transmission resilient coating in graphite material, the introducing of the cycle performance and the other material with carbon element of high magnification charge and discharge point performance that therefore improve graphite material can effectively suppress electrolyte to the common embedding effect of graphite, improve the anti-organic solvent erosiveness of graphite, improve the cycle performance of graphite further.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1
Porous graphite doping and a preparation method for carbon coated graphite negative material, comprise the following steps:
(1) potassium permanganate solution of 5 mg/mL is prepared, by native graphite (particle diameter D50:3.63 μm, the specific area: 12.51m of 50g 2/ g) join in solution, oxidation processes 60min, is then washed with water to neutrality, then dry for standby;
(2) according to porous graphite: graphite (D50:10.82 μm, specific area: 6.1m 2/ g, tap density: 0.96g/cm 3the ratio of)=0.02:1, simultaneously the ratio of graphite weight 5% adds a certain amount of carbon matrix precursor (pitch powder), mixes, and obtains porous graphite and graphite and carbon matrix precursor composite granule;
(3) under inert gas shielding, the composite granule in step (2) is heated up with 10 DEG C/min and is heated to 950 DEG C, and continue 3 hours, after room temperature is down in cooling, pulverize and sieve, namely obtain porous graphite doping and carbon coated graphite negative material.
Embodiment 2
Porous graphite doping and a preparation method for carbon coated graphite negative material, comprise the following steps:
(1) potassium permanganate solution of 10 mg/mL is prepared, by native graphite (particle diameter D50:5.42 μm, the specific area: 18.12m of 50g 2/ g) join in solution, oxidation processes 30min, is then washed with water to neutrality, then dry for standby;
(2) according to porous graphite: graphite (D50:17.21 μm, specific area: 5.8m 2/ g, tap density: 0.85g/cm 3the ratio of)=0.1:1, simultaneously the ratio of graphite weight 10% adds a certain amount of carbon matrix precursor (phenolic resins powder), mixes, and obtains porous graphite and graphite and carbon matrix precursor composite granule;
(3) under inert gas shielding, the composite granule in step (2) is heated up with 5 DEG C/min and is heated to 900 DEG C, and continue 5 hours, after room temperature is down in cooling, pulverize and sieve, namely obtain porous graphite doping and carbon coated graphite negative material.
Embodiment 3
Porous graphite doping and a preparation method for carbon coated graphite negative material, comprise the following steps:
(1) potassium permanganate solution of 8 mg/mL is prepared, by native graphite (particle diameter D50:7.28 μm, the specific area: 15.42m of 50g 2/ g) join in solution, oxidation processes 50min, is then washed with water to neutrality, then dry for standby;
(2) according to porous graphite: graphite (D50:8.14 μm, specific area: 6.9m 2/ g, tap density: 1.04g/cm 3the ratio of)=0.08:1, simultaneously the ratio of graphite weight 7% adds a certain amount of carbon matrix precursor (epoxy resin powder), mixes, and obtains porous graphite and graphite and carbon matrix precursor composite granule;
(3) under inert gas shielding, the composite granule in step (2) is heated up with 8 DEG C/min and is heated to 850 DEG C, and continue 6 hours, after room temperature is down in cooling, pulverize and sieve, namely obtain porous graphite doping and carbon coated graphite negative material.
Comparative example 1
Undressed native graphite in embodiment 1.
Comparative example 2
Undressed Delanium in embodiment 2.
Electrochemical property test
For the performance of modification lithium-ion battery graphite cathode material prepared by inspection the inventive method, test by half-cell method of testing, negative material with above embodiment and comparative example: acetylene black: PVDF(Kynoar)=95:2:3(weight ratio), add appropriate NMP(N-methyl pyrrolidone) furnishing pulpous state, coat on Copper Foil, within 8 hours, make negative plate through vacuum 110 DEG C of dryings; Be to electrode with metal lithium sheet, electrolyte is 1mol/L LiPF6/EC+DEC+DMC=1:1:1, and microporous polypropylene membrane is barrier film, is assembled into battery.Charging/discharging voltage is 0 ~ 2.0V, and charge-discharge velocity is 0.5C, and carry out testing to battery performance, test result is in table 1.
Table 1 is the Performance comparision of negative material in different embodiment and comparative example
More than show and describe general principle of the present invention and principal character and advantage of the present invention; the technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications; these changes and improvements all fall in the claimed scope of the invention, and application claims protection range is defined by appending claims and equivalent thereof.

Claims (7)

1. porous graphite doping and a preparation method for carbon coated graphite negative material, is characterized in that comprising the following steps:
(1) prepare porous graphite: configuration concentration is the potassium permanganate solution of 1-12 mg/mL, add graphite and carry out oxidation pore-creating, washing and drying, obtain porous graphite;
(2) graphite precursor power: by Li source compound, titanium source compound, be (0.8 ~ 0.9) according to mol ratio between the Li atom in Li source compound and the Ti atom in titanium source compound: the ratio of 1 takes, the porous graphite obtained by step (1) is added according to the ratio of Li source compound and titanium source compound total weight 5 ~ 10%, add carbon source presoma and ball-milling additive according to Li source compound and titanium source compound total weight 2 ~ 15% and 80% ~ 150% respectively simultaneously, carry out ball milling mixing, to mixing post-drying;
(3) high-temperature process: under inert gas shielding; the powder of drying in step (2) is heated up with 2 ~ 10 DEG C/min and is heated to 700 ~ 950 DEG C, and continue 3-20 hour, after room temperature is down in cooling; pulverize and sieve, namely obtain porous graphite doping and carbon coated graphite negative material.
2., according to a kind of porous graphite doping described in claim 1 and the preparation method of carbon coated graphite negative material, it is characterized in that the graphite in step (2) is Delanium or native graphite, particle diameter D50≤10 μm, specific area>=10m 2/ g.
3., according to a kind of porous graphite doping described in claim 1 and the preparation method of carbon coated graphite negative material, it is characterized in that the Li source compound in step (2) is lithium acetate, lithium sulfate, lithium oxalate, lithium carbonate, lithium hydroxide, lithium chloride, lithium phosphate, lithium nitrate or lithium sulfide.
4., according to a kind of porous graphite doping described in claim 1 and the preparation method of carbon coated graphite negative material, it is characterized in that the titanium source compound in step (2) is butyl titanate, anatase titanium dioxide, metal and stone type titanium dioxide, metatitanic acid, isopropyl titanate or titanium oxyoxalate.
5., according to a kind of porous graphite doping described in claim 1 and the preparation method of carbon coated graphite negative material, it is characterized in that the carbon source presoma described in step (2) is one or more the mixture in phenolic resins, epoxy resin, glucose, starch, pitch.
6., according to the preparation method of a kind of porous graphite doping described in claim 1 with carbon coated graphite negative material, it is characterized in that the ball-milling additive described in step (2) is a kind of in water, methyl alcohol or ethanol, isopropyl alcohol.
7., according to a kind of porous graphite doping described in claim 1 and the preparation method of carbon coated graphite negative material, it is characterized in that the inert gas described in step (3) is nitrogen or argon gas.
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CN201710461076.8A CN107069015A (en) 2015-05-22 2015-05-22 A kind of porous graphite doping and the preparation method of carbon coating graphite cathode material
CN201710461050.3A CN107221661A (en) 2015-05-22 2015-05-22 A kind of preparation method of graphite negative material of lithium ion battery
CN201710461064.5A CN107275610A (en) 2015-05-22 2015-05-22 A kind of preparation method of porous graphite doped graphite negative material
CN201710461071.5A CN107069014A (en) 2015-05-22 2015-05-22 A kind of preparation method of graphite negative material of lithium ion battery
CN201710461072.XA CN107180962A (en) 2015-05-22 2015-05-22 A kind of porous graphite doping and the preparation method of carbon coating graphite cathode material

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CN201710461050.3A Division CN107221661A (en) 2015-05-22 2015-05-22 A kind of preparation method of graphite negative material of lithium ion battery
CN201710461071.5A Division CN107069014A (en) 2015-05-22 2015-05-22 A kind of preparation method of graphite negative material of lithium ion battery
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CN109546099A (en) * 2018-10-16 2019-03-29 中航锂电（洛阳）有限公司 A kind of composite cathode material of silicon/carbon/graphite and preparation method thereof, lithium ion battery
CN110165179A (en) * 2019-05-24 2019-08-23 东莞市安德丰电池有限公司 A kind of lithium cell cathode material and preparation method thereof and the lithium battery comprising the negative electrode material
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CN109850886B (en) * 2019-01-18 2022-07-26 华南理工大学 Porous graphite material and preparation method and application thereof
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CN102769139A (en) * 2012-08-10 2012-11-07 深圳市斯诺实业发展有限公司永丰县分公司 Preparation method of high power capacity lithium ion battery cathode material

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CN107611445A (en) * 2017-09-18 2018-01-19 华南师范大学 A kind of preparation method of lithium ion battery graphite cathode material
CN109546099A (en) * 2018-10-16 2019-03-29 中航锂电（洛阳）有限公司 A kind of composite cathode material of silicon/carbon/graphite and preparation method thereof, lithium ion battery
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
CN110165179A (en) * 2019-05-24 2019-08-23 东莞市安德丰电池有限公司 A kind of lithium cell cathode material and preparation method thereof and the lithium battery comprising the negative electrode material
CN114477160A (en) * 2020-10-27 2022-05-13 武汉大学 Method for preparing high-purity porous graphite
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CN114520314B (en) * 2020-11-19 2024-02-27 湖南中科星城石墨有限公司 Negative electrode material with porous carbon coating layer, preparation method thereof and lithium ion battery
CN112952069A (en) * 2021-04-06 2021-06-11 黑龙江省宝泉岭农垦溢祥新能源材料有限公司 Production process of carbon-coated graphite negative electrode material

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