CN104934589A - Amorphous carbon deposit modified lithium titanate negative electrode material preparation method - Google Patents

Amorphous carbon deposit modified lithium titanate negative electrode material preparation method Download PDF

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Publication number
CN104934589A
CN104934589A CN201510415051.5A CN201510415051A CN104934589A CN 104934589 A CN104934589 A CN 104934589A CN 201510415051 A CN201510415051 A CN 201510415051A CN 104934589 A CN104934589 A CN 104934589A
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lithium titanate
amorphous carbon
preparation
anode material
deposition
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田东
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Priority to CN201510415051.5A priority Critical patent/CN104934589A/en
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Priority to PCT/CN2016/086277 priority patent/WO2017008614A1/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
    • H01M4/48—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
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • 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
    • H01M2220/00—Batteries for particular applications
    • H01M2220/20—Batteries in motive systems, e.g. vehicle, ship, plane
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2220/00—Batteries for particular applications
    • H01M2220/30—Batteries in portable systems, e.g. mobile phone, laptop
    • 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 an amorphous carbon deposit modified lithium titanate negative electrode material preparation method. The method comprises the steps that firstly, water solutions of lithium titanate and a transition metal compound are mixed and heated until water is evaporated, then reduction is conducted on the lithium titanate carrying the transition metal compound by using a reducing agent, then deposit is conducted on the obtained lithium titanate carrying the transition metal compound by using an amorphous carbon source, and finally, the transition metal on the lithium titanate deposited with amorphous carbon is removed by using an acid medium solution. According to the amorphous carbon deposit modified lithium titanate negative electrode material preparation method, the transition metal is used as a catalyst to enable the amorphous carbon and the lithium titanate to be composited together through chemical bonds, the amorphous carbon is deposited on the lithium titanate, a lithium titanate and amorphous carbon composite negative electrode material is obtained, the direct contact between the lithium titanate and a lithium-ion bath solution is avoided, the technical problem that the lithium titanate and the bath solution react to generate gaseousness is solved, and therefore the cycle performance of a lithium ion battery is improved. In addition, the negative electrode material obtained by the amorphous carbon deposit modified lithium titanate negative electrode material preparation method also has good rate capability.

Description

The preparation method of the deposition modified lithium titanate anode material of a kind of amorphous carbon
Technical field
The invention belongs to field of lithium ion battery, particularly relate to a kind of negative material, be specifically related to a kind of agraphitic carbon that utilizes and deposit the method for lithium titanate anode material being carried out to modification.
Background technology
Along with the development of automobile industry, oil, the exhaustion of the non-renewable fossil fuel such as natural gas receives publicity day by day, air pollution and room temperature effect also become global problem, and the fast development of national economy and the raising of living standards of the people, the dependency degree of China to crude oil grows with each passing day, Chinese energy safety is formed and directly threatened, in addition, the price fluctuation of crude oil also directly has influence on the development of Chinese national economy, along with constantly riseing of International Crude Oil, not only increase the economic pressures of middle national expenditures great number foreign exchange Imported oil, also domestic oil product market supply and demand contradiction is made more to give prominence in China's oil consumption structure, the oil of vehicles consumption accounts for over half, and present continuity significantly ascendant trend, these force people to have at searching new forms of energy, develop the quicken one's step development of electrokinetic cell and electric automobile of new vehicles aspect and be placed in more and more important position.Therefore, be more and more subject to people's attention with the secondary energy sources that green secondary cell is power, be considered to be the effective way solving lack of energy and environmental pollution.
Along with developing rapidly of the secondary energy sources being power with green secondary cell, various New-energy electric vehicle and portable electric appts, the widely using and high speed development of electric tool, also improve in succession to the requirement of chemical power source.Lithium ion battery because open circuit voltage is high, energy density is large, lightweight and self discharge is low etc., and advantage obtains increasingly extensive application in these fields.But the useful life of lithium ion battery and power-performance are also unsatisfactory, especially on electric automobile.This is because the structure of traditional graphite cathode material has height crystallization and degree of orientation characteristic, make it that solvent molecule can occur in charging process and enter graphite layers and the phenomenon causing graphite linings to peel off, cause cycle performance of battery to reduce thus, limit the application of graphite type material in power battery material.Li 4ti 5o 12as a kind of novel ion secondary battery cathode material lithium, compared with other business-like material, advantages such as having good cycle, do not react with electrolyte, security performance is high, charge and discharge platform is steady is one of the most excellent lithium ion battery negative material received much concern in recent years.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, lithium titanate material theoretical specific capacity is 175 mAh/g simultaneously, and actual specific capacity is greater than 160mAh/g, has the shortcomings such as gram volume is lower, therefore, it is very necessary for carrying out modification for lithium titanate.
Research shows amorphous carbon and lithium titanate compound to prepare the performance that obtained composite material can greatly improve lithium titanate.Amorphous carbon itself has good conductivity and anti-electrolytic corrosion performance, therefore can improve cyclical stability and the conductivity of material.
Summary of the invention
For prior art Problems existing, an object of the present invention is to provide a kind of agraphitic carbon that utilizes to deposit the method for lithium titanate anode material being carried out to modification, and concrete steps are as follows:
A) by lithium titanate and transistion metal compound aqueous solution, carry out being heated to moisture evaporation, obtain the lithium titanate that load has transistion metal compound;
B) with reducing agent by described steps A) load that obtains has the lithium titanate of transistion metal compound to reduce, and obtains the lithium titanate that load has transition metal;
C) by amorphous carbon carbon source by described step B) load that obtains has the lithium titanate of transition metal to deposit, and obtains the lithium titanate depositing amorphous carbon;
D) utilize acid medium solution by described step C) in the transition metal on the lithium titanate of amorphous carbon of depositing that obtains remove, and carry out washing to neutrality, then dry, obtain graphite-doping lithium titanate anode material.
Further, steps A) described in lithium titanate and the mass ratio of transistion metal compound be 100:(5 ~ 20).
Further, steps A) described in transistion metal compound comprise in the chloride of the chloride of nickel, the chloride of iron and cobalt one or more.
Further, steps A) described in the molar concentration of the transistion metal compound aqueous solution be preferably 0.05 ~ 0.3mol/L.
Further, steps A) described in heating-up temperature be 30 ~ 85 DEG C.
Further, step B) described in reducing agent be hydrogen.
Further, step C) described in amorphous carbon carbon source comprise gaseous hydrocarbons and/or liquid hydrocarbon.
Further, step C) described in the temperature of deposition be 600 ~ 800 DEG C, the time of deposition is 0.5 ~ 1.5 hour, and the deposition of amorphous carbon accounts for 5 ~ 20% of lithium titanate weight.
Further, step D) described in acid medium solution be hydrochloric acid solution, molar concentration is 0.01 ~ 0.5mol/L.
A kind of agraphitic carbon that utilizes provided by the invention deposits the method for lithium titanate anode material being carried out to modification, using transition metal as catalyst, make to be combined with each other by chemical bond between amorphous carbon and lithium titanate, amorphous carbon is deposited on lithium titanate, obtain the composite negative pole material of lithium titanate and amorphous carbon, avoid lithium titanate to contact with the direct of lithium-ion electrolyte, solve lithium titanate and electrolyte reaction and produce the technical problem of flatulence, thus improving the cycle performance of lithium ion battery.Further, the negative material using preparation method provided by the invention to obtain also has good high rate performance.Experimental data shows, the lithium ion battery using negative material provided by the invention to prepare is when charge and discharge cycles 2000 times, capacity retention rate is more than 95%, illustrate that the lithium ion capacity storage rate using negative material provided by the invention to prepare is higher, there is good cycle performance.
Embodiment
In order to further illustrate the present invention, below in conjunction with embodiment, certain introduction is done to technical scheme of the present invention, but can not limiting the scope of the present invention be understood as.
Embodiment 1
According to lithium titanate: NiCl 2the mass ratio of=100:10, the NiCl of configuration 0.1mol/L 2the aqueous solution, then adds lithium titanate, at the temperature of 55 DEG C dispersed with stirring evenly, dry, obtaining area load has NiCl 2lithium titanate.With hydrogen, it is reduced again, obtain the lithium titanate that area load has W metal, pass into methane gas, make agraphitic carbon at lithium titanate surface deposition, the control time is 1h, and agraphitic carbon deposition accounts for 8% of lithium titanate weight, finally with the hydrochloric acid solution of 0.1mol/L, the W metal on lithium titanate is removed, and washing is to neutral, then dries, obtains graphite-doping lithium titanate anode material.
Embodiment 2
According to lithium titanate: FeCl 3the mass ratio of=100:15, the FeCl of configuration 0.3mol/L 3the aqueous solution, then adds lithium titanate, at the temperature of 65 DEG C dispersed with stirring evenly, dry, obtaining area load has FeCl 3lithium titanate.With hydrogen, it is reduced again, obtain the lithium titanate that area load has metal Fe, pass into methane gas, make agraphitic carbon at lithium titanate surface deposition, the control time is 2h, and agraphitic carbon deposition accounts for 14% of lithium titanate weight, finally with the hydrochloric acid solution of 0.2mol/L, the metal Fe on lithium titanate is removed, and washing is to neutral, then dries, obtains graphite-doping lithium titanate anode material.
Embodiment 3
According to lithium titanate: CoCl 3the mass ratio of=100:20, the CoCl of configuration 0.5mol/L 3the aqueous solution, then adds lithium titanate, at the temperature of 85 DEG C dispersed with stirring evenly, dry, obtaining area load has CoCl 3lithium titanate.With hydrogen, it is reduced again, obtain the lithium titanate that area load has metal Co, pass into methane gas, make agraphitic carbon at lithium titanate surface deposition, the control time is 1.5h, and agraphitic carbon deposition accounts for 10% of lithium titanate weight, finally with the hydrochloric acid solution of 0.3mol/L, the metal Co on lithium titanate is removed, and washing is to neutral, then dries, obtains graphite-doping lithium titanate anode material.
Embodiment 4
According to lithium titanate: NiCl 2: FeCl 3the mass ratio of=100:10:5, the CoCl of configuration 0.2mol/L 3with the FeCl of 0.15mol/L 3the aqueous solution, then adds lithium titanate, at the temperature of 75 DEG C dispersed with stirring evenly, dry, obtaining area load has NiCl 2and FeCl 3lithium titanate.With hydrogen, it is reduced again, obtain the lithium titanate that area load has W metal and Fe, pass into methane gas, make agraphitic carbon at lithium titanate surface deposition, the control time is 1h, and agraphitic carbon deposition accounts for 8% of lithium titanate weight, finally with the hydrochloric acid solution of 0.2mol/L, the W metal on lithium titanate and Fe are removed, and washing is to neutral, then dries, obtains graphite-doping lithium titanate anode material.
Comparative example 1
Undressed lithium titanate in embodiment 1.
Half-cell detects
For the electrical property of negative 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.
Full battery testing
Negative material with embodiment and comparative example: SP:SBR(solid content 50%): CMC=94:2.5:1.5:2(weight ratio), add appropriate amount of deionized water and mix furnishing pulpous state, be applied on Copper Foil, at 90 DEG C, vacuumize drying; By LiCoO 2powder: SP:KS-6:PVDF=94:1.5:2:2.5(weight ratio), do after solvent evenly sizes mixing with NMP, be applied on aluminium foil, at 100 DEG C, vacuumize drying; By dried positive and negative electrode pole piece through roll-in, cut-parts, winding, fluid injection, sealing, formation process, make 18650 cylindrical batteries, barrier film is Celgard2400, electrolyte is 1M LiPF6 ∕ DMC:EC:DEC, use battery check device to carry out the detection of multiplying power discharging and cycle performance, test result is in table 1.
The Performance comparision of negative material in the different embodiment of table 1 and comparative example
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.

Claims (8)

1. a preparation method for the deposition modified lithium titanate anode material of amorphous carbon, its preparation process step is as follows:
A) by lithium titanate and transistion metal compound aqueous solution, carry out being heated to moisture evaporation, obtain the lithium titanate that load has transistion metal compound;
B) with reducing agent by described steps A) load that obtains has the lithium titanate of transistion metal compound to reduce, and obtains the lithium titanate that load has transition metal;
C) by amorphous carbon carbon source by described step B) load that obtains has the lithium titanate of transition metal to deposit, and obtains the lithium titanate depositing amorphous carbon;
D) utilize acid medium solution by described step C) in the transition metal on the lithium titanate of amorphous carbon of depositing that obtains remove, and carry out washing to neutrality, then dry, obtain graphite-doping lithium titanate anode material.
2. the preparation method of the deposition modified lithium titanate anode material of a kind of amorphous carbon according to claim 1, is characterized in that steps A) in the mass ratio of lithium titanate and transistion metal compound be 100:(5 ~ 20).
3. the preparation method of the deposition modified lithium titanate anode material of a kind of amorphous carbon according to claim 1, is characterized in that steps A) in transistion metal compound comprise in the chloride of the chloride of nickel, the chloride of iron and cobalt one or more.
4. the preparation method of the deposition modified lithium titanate anode material of a kind of amorphous carbon according to claim 1, is characterized in that steps A) in heating-up temperature be 30 ~ 85 DEG C.
5. the preparation method of the deposition modified lithium titanate anode material of a kind of amorphous carbon according to claim 1, is characterized in that steps A) in reducing agent be hydrogen.
6. the preparation method of the deposition modified lithium titanate anode material of a kind of amorphous carbon according to claim 1, is characterized in that step C) in amorphous carbon carbon source comprise gaseous hydrocarbons and/or liquid hydrocarbon.
7. the preparation method of the deposition modified lithium titanate anode material of a kind of amorphous carbon according to claim 1, it is characterized in that step C) in deposition temperature be 600 ~ 800 DEG C, the time of deposition is 0.5 ~ 1.5 hour, and the deposition of amorphous carbon accounts for 5 ~ 20% of lithium titanate weight.
8. the preparation method of the deposition modified lithium titanate anode material of a kind of amorphous carbon according to claim 1, is characterized in that step D) in acid medium solution be hydrochloric acid solution, molar concentration is 0.01 ~ 0.5mol/L.
CN201510415051.5A 2015-07-15 2015-07-15 Amorphous carbon deposit modified lithium titanate negative electrode material preparation method Pending CN104934589A (en)

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Application publication date: 20150923