CN106876675A - A kind of lithium ion battery preparation method of lithium titanate composite cathode material of silicon/carbon/graphite - Google Patents
A kind of lithium ion battery preparation method of lithium titanate composite cathode material of silicon/carbon/graphite Download PDFInfo
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- CN106876675A CN106876675A CN201710178160.9A CN201710178160A CN106876675A CN 106876675 A CN106876675 A CN 106876675A CN 201710178160 A CN201710178160 A CN 201710178160A CN 106876675 A CN106876675 A CN 106876675A
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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
- H01M4/364—Composites as mixtures
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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
- 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
- H01M4/48—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
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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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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- 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 lithium ion battery preparation method of lithium titanate composite cathode material of silicon/carbon/graphite, the present invention is by using simple and easy to do mechanical mixture, isostatic pressed is merged, crush the means such as nodularization, high temperature sintering lithium titanate is distributed in the three-dimensional conductive network of graphite composition, the good electrical contact between lithium titanate and graphite can be maintained.Preparation method is simple of the present invention is efficient, low cost；Thus obtained composite negative pole material high rate performance and cycle performance are significantly improved, and can be used as lithium ion battery negative material.
Description
Technical field
The present invention relates to graphite material preparation field, and in particular to a kind of lithium ion battery lithium titanate graphite composite negative pole
The preparation method of material.
Background technology
Carbon material has low chemical potential, good cycle, cheap, advantages of environment protection, be at present it is most preferable,
Conventional lithium ion battery negative material.And in carbon material, compared with soft carbon and hard carbon, graphite material is in specific capacity, electric discharge
The aspect such as platform and cost has more obvious advantage.Wherein, native graphite has the advantages that specific capacity is high, cheap,
But irreversible capacity is big first, and cycle performance is poor, high rate performance is poor.In order to overcome the defect of native graphite, improve Carbon anode
The chemical property of material, reduces manufacturing cost, being taken researcher more graphite is carried out modified surface, coating modification,
The method such as doping vario-property, mechanically modifying, redox be modified.Other negative materials such as lithium titanate anode material volume production, but
Its compacted density only 2.0 g/cm3, discharge platform is (1.5 V) higher, and specific capacity is relatively low (about 160 mAh/g), and self-conductive
Bad (the electrical conductivity of property:10-9 S/cm), current certain applications are on electric bus.
Existing reporting for work lithium titanate and graphite-like composite negative pole material at present.Application No. 2,014,103,449 91.5
Domestic patent discloses a kind of negative material of lithium titanate cladding surface treated graphite, preparation method and its application.The negative material
Lithium titanate clad is formed with the negative material particle surface of surface treated graphite-like basis.The preparation of the negative material
Method includes：(1) surface treatment procedure of graphite-like basis negative material；(2) lithium titanate clad in-situ preparation operation.The hair
It is bright by one layer of lithium titanate material of Graphite Coating, improving the purpose of battery performance.But the method not than
On capacity, initial coulomb efficiency, high rate performance do not have greatly improved, lithium titanate clad is a micron clad, too thick, by force
Degree is extremely difficult to ideal.
The content of the invention
The present invention is directed to existing technical problem, there is provided a kind of lithium ion battery lithium titanate composite cathode material of silicon/carbon/graphite
Preparation method, by using simple and easy to do mechanical mixture, isostatic pressed fusion crushes the means such as nodularization, high temperature sintering by metatitanic acid
Lithium is distributed in the three-dimensional conductive network of graphite composition, can maintain the good electrical contact between lithium titanate and graphite.Present invention system
Preparation Method simple and effective, low cost；Thus obtained composite negative pole material high rate performance and cycle performance are significantly improved, and be can be used as
Lithium ion battery negative material.
To achieve the above object, the present invention is using following technical scheme：
A kind of lithium ion battery preparation method of lithium titanate composite cathode material of silicon/carbon/graphite, comprises the following steps：
（1）Mechanical mixture
By commercially available lithium titanate, expanded graphite powder, carbon source according to mass ratio 1:10-100:0.1-0.5 is added to high-speed stirring
Mix in machine, 1~4h of solid dispersion is carried out using the r/min of rotating speed 500~5000, obtain the mixture of three；
（2）Isostatic pressed is merged
By step（1）The mixture press-powder for obtaining is filled into the rubber mold of iso-static pressure shaping machine, is vibrated by high-frequency electromagnetic,
So that press-powder obtains closely knit, vacuumized after sealing, the air between discharge powder particle is put into the pressure-volume high equipped with water or oil
In device, 100~200 MPa are pressurized to, are heated to 150~200 DEG C, 10~20h of pressure-maintaining and heat-preservation is pressed into after being cooled to room temperature
Block；
（3）Crush nodularization
After block is crushed using Universalpulverizer, crushing nodularization is carried out into pulverizer, pulverizer is set to 3-10 platforms, powder
Broken machine host electric current is not more than 50A, and the crushing cycle is 15 minutes/time, and the cycle of crushing is 2-4 times, and the crushing cycle often completes once
Detection is sampled, pulverizer rotating speed is 2000 revs/min, and air-introduced machine electric current is not more than 25A, and D50=12- is obtained by classification
The spherical powder of 40um；
（4）High temperature sintering
By step（3）The spherical powder of the 12-40um for obtaining is placed in atmosphere protection stove and is sintered, with 2~25 DEG C/
The heating rate of min rises to 400~1000 DEG C and is incubated 4~18 hours, obtains lithium titanate composite cathode material of silicon/carbon/graphite.
As a kind of preferred scheme, step（1）Described in commercially available lithium titanate purity be more than 99.0%, granularity is 100-
1000 nm。
As a kind of preferred scheme, step（1）Described in expanded graphite powder be for crystalline flake graphite or micro crystal graphite
Raw material by the expanded air-flow crushing of intercalation one or more, purity be more than 99.90%, granularity be 5-40 um.
As a kind of preferred scheme, step（1）Described in carbon source for glucose, sucrose, polyvinyl alcohol, polyacrylonitrile,
One or more in water soluble phenol resin, middle fire stons oil asphalt, medium temperature coal pitch.
As a kind of preferred scheme, step（4）Described in atmosphere protection stove in the protective atmosphere that uses be selected from helium, nitrogen
At least one in gas, argon gas, carbon dioxide
The present invention has clear advantage and beneficial effect compared with prior art, specifically, as shown from the above technical solution：
1st, the present invention uses simple and easy to do mechanical mixture, and isostatic pressed fusion crushes the means such as nodularization, high temperature sintering by lithium titanate
It is distributed in the three-dimensional conductive network of graphite composition, the good electrical contact between lithium titanate and graphite can be maintained, so as to improve
The first charge-discharge efficiency and cycle performance of material.
2nd, introduce isostatic pressed fusion, make lithium titanate and graphite it is compound more closely, can improve volume energy density and times
Rate performance.
3rd, preparation method of the present invention is simple, reproducible, workable, is adapted to be prepared on a large scale.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all
Belong to the scope of protection of the invention.
Embodiment one
A kind of lithium ion battery preparation method of lithium titanate composite cathode material of silicon/carbon/graphite, comprises the following steps：
（1）Mechanical mixture
It is that the granularity that raw material is made is 10um expansion stones by commercially available 99% purity, the lithium titanate of granularity 500nm, crystalline flake graphite
Ink powder end, glucose are according to mass ratio 1:10:0.1 is added in homogenizer, is consolidated using the r/min of rotating speed 5000
State disperses 1h, obtains the mixture of three；
（2）Isostatic pressed is merged
By step（1）The mixture press-powder for obtaining is filled into the rubber mold of iso-static pressure shaping machine, is vibrated by high-frequency electromagnetic,
So that press-powder obtains closely knit, vacuumized after sealing, the air between discharge powder particle is put into the pressure-volume high equipped with water or oil
In device, 100 MPa are pressurized to, are heated to 150 DEG C, the h of pressure-maintaining and heat-preservation 10 is pressed into block after being cooled to room temperature；
（3）Crush nodularization
After block is crushed using Universalpulverizer, crushing nodularization is carried out into pulverizer, pulverizer is set to 3, crushes
Machine host electric current 40A, the crushing cycle is 15 minutes/time, and the cycle of crushing is 2 times, and the crushing cycle often completes once to be sampled inspection
Survey, pulverizer rotating speed is 2000 revs/min, air-introduced machine electric current 20A obtains the spherical powder of D50=16 um by classification；
（4）High temperature sintering
By step（3）The spherical powder of 16 um for obtaining is placed in nitrogen atmosphere protection stove and is sintered, with 2 DEG C/min's
Heating rate rises to 1000 DEG C and is incubated 4 hours, obtains lithium titanate composite cathode material of silicon/carbon/graphite.
Embodiment two
In the present embodiment, step（1）In addition lithium titanate purity 99.5%, granularity 800nm, expanded graphite raw material microlite
Ink, D50 are 12 um, purity 99.96%, mass ratio 1:100:0.5, in addition, other processes and condition and embodiment one
It is consistent.
Embodiment three
In the present embodiment, step（2）Middle selection is pressurized to 200 MPa, is heated to 250 DEG C, the h of pressure-maintaining and heat-preservation 15, in addition,
Other processes are consistent with condition with embodiment one.
Example IV
In the present embodiment, step（3）Middle selection pulverizer is set to 5, crushes machine host electric current 50A, and the cycle of crushing is 3 times,
Air-introduced machine electric current 10A, the spherical powder of D50=14um is obtained by classification, in addition, other processes and condition and embodiment
One is consistent.
Embodiment five
In the present embodiment, step（4）Middle atmosphere protection stove selects argon gas, and 800 DEG C are risen to simultaneously with the heating rate of 25 DEG C/min
Insulation 18 hours, in addition, other processes are consistent with condition with embodiment one.
Comparative example one
Using the natural spherical plumbago powder as a comparison case 1 of phosphorus content 99.95%.
Comparative example two
Using the lithium titanate anode material as a comparison case 2 of the commercially available 500nm of purity 99.9%.
To check the performance of graphite cathode material, tested with half-cell method of testing, use porous polyimide of the invention
Coated graphite material:SBR (solid content 50%):CMC:SP=95.5:2.0:1.5:1.0 (weight ratios), plus appropriate deionization
Water mixing is tuned into pulpous state, coats on Copper Foil and is made negative plate within 12 hours in drying in vacuum drying chamber；To electrode metal
Lithium piece constitutes half-cell, and electrolyte is 1M liPF6/ EC+DEC+DMC=1:1:1, charge-discharge magnification is 0.2 C/5C, charge and discharge
Piezoelectric voltage scope is 0-1.5V, and the discharge and recharge cabinet for computerizeing control carries out the collection and control of data.The results are shown in Table 1
Table 1 lists lithium titanate graphite material obtained in the embodiment of the present invention and compares with the performance parameter of comparative example material.
As can be seen from the above results：The high rate performance and cyclicity of lithium titanate graphite cathode material obtained in the embodiment of the present invention
Can substantially increase compared with comparative example, reason can be attributed to the present invention by simple and easy to do mechanical mixture, and isostatic pressed is merged,
Crush nodularization, the means such as high temperature sintering lithium titanate is distributed in the three-dimensional conductive network of graphite composition, can maintain lithium titanate with
Good electrical contact between graphite, so as to improve the first charge-discharge efficiency and cycle performance of material.Isostatic pressed is introduced simultaneously
Fusion, makes lithium titanate compound tightr with graphite, can improve volume energy density and high rate performance.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding can carry out various changes, modification, replacement to these embodiments without departing from the principles and spirit of the present invention
And modification, the scope of the present invention be defined by the appended.
Claims (5)
1. a kind of lithium ion battery preparation method of lithium titanate composite cathode material of silicon/carbon/graphite, it is characterised in that it includes following
Step：（1）Mechanical mixture is by commercially available lithium titanate, expanded graphite powder, carbon source according to mass ratio 1:10-100:0.1-0.5
It is added in homogenizer, 1~4h of solid dispersion is carried out using the r/min of rotating speed 500~5000, obtains the mixture of three；
（2）Isostatic pressed is merged step（1）The mixture press-powder for obtaining is filled into the rubber mold of iso-static pressure shaping machine, by high frequency
Air between electric and magnetic oscillation so that press-powder obtains closely knit, is vacuumized after sealing, discharge powder particle, be put into equipped with water or
In the high-pressure bottle of oil, 100~200 MPa are pressurized to, are heated to 150~200 DEG C, 10~20h of pressure-maintaining and heat-preservation is cooled to room
Block is pressed into after temperature；（3）After crushing nodularization crushes block using Universalpulverizer, crushing ball is carried out into pulverizer
Change, pulverizer is set to 3-10 platforms, crush machine host electric current and be not more than 50A, the crushings cycle is 15 minutes/time, the crushing cycle is
2-4 times, the crushing cycle often completes once to be sampled detection, and pulverizer rotating speed is 2000 revs/min, and air-introduced machine electric current is not more than
25A, the spherical powder of D50=12-40um is obtained by classification；（4）High temperature sintering is by step（3）The 12-40um's for obtaining is spherical
Powder is placed in atmosphere protection stove and is sintered, and rises to 400~1000 DEG C with the heating rate of 2~25 DEG C/min and protects
Temperature 4~18 hours, obtains lithium titanate composite cathode material of silicon/carbon/graphite.
2. a kind of lithium ion battery according to claim 1 preparation method of lithium titanate composite cathode material of silicon/carbon/graphite, its
It is characterised by：Step（1）Described in commercially available lithium titanate purity be more than 99.0%, granularity be 100-1000 nm.
3. a kind of lithium ion battery according to claim 1 preparation method of lithium titanate composite cathode material of silicon/carbon/graphite, its
It is characterised by：Step（1）Described in expanded graphite powder for crystalline flake graphite or micro crystal graphite be that raw material is expanded by intercalation
Air-flow crushing one or more, purity be more than 99.90%, granularity be 5-40 um.
4. a kind of lithium ion battery according to claim 1 preparation method of lithium titanate composite cathode material of silicon/carbon/graphite, its
It is characterised by：Described carbon source is glucose, sucrose, polyvinyl alcohol, polyacrylonitrile, water soluble phenol resin, the oil drip of middle fire stons
One or more in blue or green, medium temperature coal pitch.
5. a kind of lithium ion battery according to claim 1 preparation method of lithium titanate composite cathode material of silicon/carbon/graphite, its
It is characterised by：Step（4）Described in atmosphere protection stove in the protective atmosphere that uses be selected from helium, nitrogen, argon gas, carbon dioxide
In at least one.
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Cited By (3)
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| CN109524631A (en) * | 2017-09-20 | 2019-03-26 | 上海杉杉科技有限公司 | A kind of preparation method of high capacity composite negative pole material |
| CN112271276A (en) * | 2020-11-17 | 2021-01-26 | 银川市核芯科技有限公司 | Processing technology for positive electrode of lithium electronic battery |
| CN115000373A (en) * | 2022-06-08 | 2022-09-02 | 万向一二三股份公司 | Preparation method of lithium titanate/graphite composite negative electrode material |
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Inventor after: Li Mei Inventor after: Zhou Pengwei Inventor after: Zhao Donghui Inventor before: Lin Xuan Inventor before: Li Mei Inventor before: Zhou Pengwei Inventor before: Zhao Donghui |
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| GR01 | Patent grant |