CN104953098A - Preparation method of porous graphite-doped carbon-coated lithium titanate negative electrode material - Google Patents

Preparation method of porous graphite-doped carbon-coated lithium titanate negative electrode material Download PDF

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CN104953098A
CN104953098A CN201510264457.8A CN201510264457A CN104953098A CN 104953098 A CN104953098 A CN 104953098A CN 201510264457 A CN201510264457 A CN 201510264457A CN 104953098 A CN104953098 A CN 104953098A
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lithium titanate
lithium
porous graphite
preparation
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田东
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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
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • 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
    • 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
    • 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 of porous graphite-doped carbon-coated lithium titanate negative electrode material. Due to the doping and the modification of lithium titanate by porous carbon and carbon coating, the problem of poor high rate capability can be solved, and the spinel structure cannot be influenced. As the doped porous carbon and carbon coating layer plays the role of an electronic transmission buffering layer, the cycle performance of the lithium titanate material is improved, in addition, due to the introduction of a carbon precursor, the gathering of lithium titanate particles in the heat treatment process can be effectively inhibited, the diffusion coefficient of the lithium ions in the lithium titanate material can be increased. According to the preparation method, the process is simple and the industrial production is convenient.

Description

The preparation method of a kind of porous graphite doping and the coated lithium titanate anode material of carbon
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 the coated lithium titanate anode material of carbon.
Background technology
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, although carbon negative pole material is commercialization already, because the current potential of carbon to lithium metal is lower, as graphite only has 0.2 V, in charge and discharge process, easy precipitating metal lithium produces Li dendrite, puncture barrier film causes lithium battery short circuit, and especially in high rate charge-discharge process, potential safety hazard is more serious.Meanwhile, also there is solvent problem embedding altogether in graphite cathode material, causes high rate charge-discharge poor-performing.Spinel-type Li-Ti oxide lithium titanate is subject to extensive concern as a kind of zero strain material with its superior cycle performance and security performance, be considered to one of negative material that may replace current commercialization material with carbon element, have very large researching value and commercial application prospect.Compared with carbon negative electrode material, lithium titanate has a lot of advantages, wherein, the deintercalation of lithium ion in lithium titanate is reversible, and lithium ion is embedding or is deviating from the process of lithium titanate, its crystal formation does not change, change in volume is less than 1%, therefore be called as " zero strain material ", can avoid causing structural damage due to the flexible back and forth of electrode material in charge and discharge cycles, thus improve cycle performance and the useful life of electrode, decrease and increase with cycle-index and bring specific capacity significantly to decay, there is the cycle performance more excellent than Carbon anode; But because lithium titanate is a kind of insulating material, its conductivity is low, thus cause the application in lithium electricity to there is the poor problem of high rate performance, when working under high magnification environment, lithium titanate special capacity fade is rapid.And for the practical application of lithium-ion-power cell, high magnification operating characteristic determines that can it one of key factor obtaining commercial applications.
Summary of the invention
Technical problem to be solved by this invention is to provide the doping of a kind of porous graphite and the preparation method of the coated lithium titanate anode material of carbon, is intended to the problem solving lithium titanate conduction rate variance, 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 the coated lithium titanate anode material of carbon, 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) lithium titanate precursor preparation: 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 the coated lithium titanate anode material of carbon.
Graphite in step (1) is Delanium or native graphite, particle diameter D50≤5 μm, specific area>=10m 2/ g.
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.
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.
Carbon source presoma described in step (2) is one or more the mixture in phenolic resins, epoxy resin, glucose, starch, pitch.
Ball-milling additive described in step (2) is a kind of in water, methyl alcohol or ethanol, isopropyl alcohol.
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 lithium titanate of carbon, obtained porous graphite doping is high with carbon coated lithium titanate anode 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 lithium titanate to the doping vario-property of lithium titanate, and does not affect its spinel structure.Porous carbon due to doping serves the effect of electric transmission resilient coating in lithium titanate material, and therefore improve the cycle performance of lithium titanate material, the introducing of material with carbon element effectively can suppress the gathering of lithium titanate particle in heat treatment process in addition.Porous graphite prepared by the present invention has higher specific area, and therefore the high rate capability of lithium titanate will improve 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 the coated lithium titanate anode material of carbon, 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) ratio of Li:Ti=0.84:1 gets titanium dioxide 50g and lithium carbonate 19.42g respectively in molar ratio, the porous graphite 3.47g obtained by step (1) is added according to the ratio of Li source compound and titanium source compound total weight 5%, add carbon source presoma glucose 1.38g and ball-milling additive absolute ethyl alcohol 55.54g according to Li source compound and titanium source compound total weight 2% and 80% respectively simultaneously, carry out ball milling mixing 15h, then dry;
(3) high-temperature process: under inert gas shielding, is heated to 900 DEG C by the powder of drying in step (2) with 5 DEG C/min, continues 4 hours, after room temperature is down in cooling, pulverizes and sieves, and namely obtains porous graphite doping and the coated lithium titanate anode material of carbon.
Embodiment 2
Porous graphite doping and a preparation method for the coated lithium titanate anode material of carbon, comprise the following steps:
(1) potassium permanganate solution of 10 mg/mL is prepared, by Delanium (particle diameter D50:4.42 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) ratio of Li:Ti=0.84:1 gets titanium dioxide 50g and lithium carbonate 19.42g respectively in molar ratio, the porous graphite 6.25g obtained by step (1) is added according to the ratio of Li source compound and titanium source compound total weight 9%, add carbon source presoma glucose 6.94g and ball-milling additive absolute ethyl alcohol 104.1g according to Li source compound and titanium source compound total weight 10% and 150% respectively simultaneously, carry out ball milling mixing 12h, then dry;
(3) high-temperature process: under inert gas shielding; the powder of drying in step (2) is heated to 800 DEG C with 10 DEG C/min, continues 6 hours, after room temperature is down in cooling; pulverize and sieve, namely obtain porous graphite doping and the coated lithium titanate anode material of carbon.
Embodiment 3
Porous graphite doping and a preparation method for the coated lithium titanate anode material of carbon, comprise the following steps:
(1) potassium permanganate solution of 8 mg/mL is prepared, by native graphite (particle diameter D50:3.28 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) ratio of Li:Ti=0.84:1 gets titanium dioxide 50g and lithium carbonate 19.42g respectively in molar ratio, the porous graphite 6.94g obtained by step (1) is added according to the ratio of Li source compound and titanium source compound total weight 10%, add carbon source presoma glucose 10.41g and ball-milling additive absolute ethyl alcohol 83.3g according to Li source compound and titanium source compound total weight 15% and 120% respectively simultaneously, carry out ball milling mixing 10h, then dry;
(3) high-temperature process: under inert gas shielding, is heated to 850 DEG C by the powder of drying in step (2) with 7 DEG C/min, continues 5 hours, after room temperature is down in cooling, pulverizes and sieves, and namely obtains porous graphite doping and the coated lithium titanate anode material of carbon.
Comparative example 1
According to n(Li): n(Ti)=0.87, take 1000g lithium carbonate and 2161g titanium dioxide, put into after ball mill carries out ball milling mixing 8h, by the powder that mixes in atmosphere, 800 DEG C are warming up to the speed of 10 DEG C/min, be incubated 4h again, then naturally cool to room temperature, obtain lithium titanate anode material.
Electrochemical property test
For the performance of modification lithium-ion battery lithium titanate anode 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)=93:3:4(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 1.0 ~ 2.5V, 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 the coated lithium titanate anode material of carbon, 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) lithium titanate precursor preparation: 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 the coated lithium titanate anode material of carbon.
2., according to a kind of porous graphite doping described in claim 1 and the preparation method of the coated lithium titanate anode material of carbon, it is characterized in that the graphite in step (1) is Delanium or native graphite, particle diameter D50≤5 μm, specific area>=10m 2/ g.
3., according to a kind of porous graphite doping described in claim 1 and the preparation method of the coated lithium titanate anode material of carbon, 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 the coated lithium titanate anode material of carbon, 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 the coated lithium titanate anode material of carbon, 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 the coated lithium titanate anode material of carbon, 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 the coated lithium titanate anode material of carbon, it is characterized in that the inert gas described in step (3) is nitrogen or argon gas.
CN201510264457.8A 2015-05-22 2015-05-22 Preparation method of porous graphite-doped carbon-coated lithium titanate negative electrode material Pending CN104953098A (en)

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WO2016188130A1 (en) * 2015-05-22 2016-12-01 田东 Preparation method for porous graphite-doped and carbon-coated lithium titanate negative electrode material
CN108199011A (en) * 2017-11-20 2018-06-22 深圳市斯诺实业发展股份有限公司 A kind of preparation method of lithium titanate anode material
CN109075323A (en) * 2016-06-08 2018-12-21 昭和电工株式会社 Lithium ion secondary battery cathode and lithium ion secondary battery
CN109817922A (en) * 2019-01-23 2019-05-28 湖南摩根海容新材料有限责任公司 High power type lithium titanate composite material and preparation method
CN114188533A (en) * 2021-12-20 2022-03-15 湖北亿纬动力有限公司 Negative electrode material and preparation method and application thereof
CN114792606A (en) * 2022-04-20 2022-07-26 北京航空航天大学 Carbon-loaded manganese-doped sodium titanate energy storage material, preparation method and application thereof, and negative electrode plate

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WO2016188130A1 (en) * 2015-05-22 2016-12-01 田东 Preparation method for porous graphite-doped and carbon-coated lithium titanate negative electrode material
CN109075323A (en) * 2016-06-08 2018-12-21 昭和电工株式会社 Lithium ion secondary battery cathode and lithium ion secondary battery
CN108199011A (en) * 2017-11-20 2018-06-22 深圳市斯诺实业发展股份有限公司 A kind of preparation method of lithium titanate anode material
CN108199011B (en) * 2017-11-20 2021-10-26 深圳市斯诺实业发展有限公司 Preparation method of lithium titanate negative electrode material
CN109817922A (en) * 2019-01-23 2019-05-28 湖南摩根海容新材料有限责任公司 High power type lithium titanate composite material and preparation method
CN114188533A (en) * 2021-12-20 2022-03-15 湖北亿纬动力有限公司 Negative electrode material and preparation method and application thereof
CN114188533B (en) * 2021-12-20 2023-06-30 湖北亿纬动力有限公司 Negative electrode material and preparation method and application thereof
CN114792606A (en) * 2022-04-20 2022-07-26 北京航空航天大学 Carbon-loaded manganese-doped sodium titanate energy storage material, preparation method and application thereof, and negative electrode plate
CN114792606B (en) * 2022-04-20 2023-08-22 北京航空航天大学 Carbon-loaded manganese-doped sodium titanate energy storage material, preparation method and application thereof, and negative electrode plate

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