CN106876675B - A kind of preparation method of lithium ion battery lithium titanate composite cathode material of silicon/carbon/graphite - Google Patents
A kind of preparation method of lithium ion battery lithium titanate composite cathode material of silicon/carbon/graphite Download PDFInfo
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- CN106876675B CN106876675B CN201710178160.9A CN201710178160A CN106876675B CN 106876675 B CN106876675 B CN 106876675B CN 201710178160 A CN201710178160 A CN 201710178160A CN 106876675 B CN106876675 B CN 106876675B
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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 methods of lithium titanate composite cathode material of silicon/carbon/graphite, the present invention is by using easy-to-use mechanical mixture, equal static pressure fusion, it crushes the means such as nodularization, high temperature sintering to be distributed in lithium titanate in the three-dimensional conductive network of graphite composition, the good electrical contact between lithium titanate and graphite can be maintained.Preparation method simple and effective of the present invention, it is at low cost；Thus obtained composite negative pole material high rate performance and cycle performance significantly improve, and can be used as lithium ion battery negative material.
Description
Technical field
The present invention relates to graphite material preparation fields, and in particular to a kind of lithium ion battery lithium titanate graphite composite negative pole
The preparation method of material.
Background technique
Carbon material has that chemical potential is low, good cycle, cheap, advantages of environment protection, be it is most ideal at present,
Common lithium ion battery negative material.And in carbon material, compared with soft carbon and hard carbon, graphite material is in specific capacity, electric discharge
Platform and cost etc. have more apparent advantage.Wherein, natural graphite has many advantages, such as that specific capacity is high, cheap,
But irreversible capacity is big for the first time, and cycle performance is poor, high rate performance is poor.In order to overcome the defect of natural graphite, improve Carbon anode
The chemical property of material, reduce manufacturing cost, researcher more take to graphite carry out surface modification, coating modification,
The methods of doping vario-property, mechanically modifying, redox modification.Other negative electrode materials such as lithium titanate anode material volume production, but
Its compacted density only 2.0 g/cm3, discharge platform is higher (1.5 V), and specific capacity is lower (about 160 mAh/g), and self-conductive
Property bad (conductivity: 10-9 S/cm), current certain applications are on electric bus.
Have at present by the registration of lithium titanate and graphite-like composite negative pole material.Application No. is 2,014,103,449 91.5
Domestic patent discloses negative electrode material, preparation method and its application of a kind of lithium titanate cladding surface treated graphite.The negative electrode material
Lithium titanate clad is formed on surface treated graphite-like basis negative electrode material particle surface.The preparation of the negative electrode material
Method includes: the surface treatment procedure of (1) graphite-like basis negative electrode material；(2) lithium titanate clad in-situ preparation process.The hair
It is bright by improving the purpose of battery service performance in one layer of lithium titanate material of Graphite Coating.But this 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.
Summary of the invention
Present invention problem in view of the prior art provides a kind of lithium ion battery lithium titanate composite cathode material of silicon/carbon/graphite
Preparation method waits static pressure to merge by using easy-to-use mechanical mixture, crushes the means such as nodularization, high temperature sintering for 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.System of the present invention
Preparation Method simple and effective, it is at low cost；Thus obtained composite negative pole material high rate performance and cycle performance significantly improve, and can be used as
Lithium ion battery negative material.
To achieve the above object, the present invention is using following technical solution:
A kind of preparation method of lithium ion battery lithium titanate composite cathode material of silicon/carbon/graphite, comprising the following steps:
(1) mechanical mixture
Commercially available lithium titanate, expanded graphite powder, carbon source are added to height according to mass ratio 1:10-100:0.1-0.5
In fast blender, 1~4h of solid dispersion is carried out using 500~5000 r/min of revolving speed, obtains the mixture of three；
(2) the static pressure fusion such as
The mixture press-powder that step (1) obtains is filled into the rubber mold of iso-static pressure shaping machine, high-frequency electromagnetic is passed through
Vibration is vacuumized after sealing so that press-powder obtains closely knit, and the air between powder particle is discharged, and is put into equipped with water or oil
In high-pressure bottle, 100~200 MPa are pressurized to, are heated to 150~200 DEG C, 10~20h of pressure-maintaining and heat-preservation, after being cooled to room temperature
It is pressed into block；
(3) nodularization is crushed
After block is crushed using Universalpulverizer, crushing nodularization is carried out into pulverizer, pulverizer is set as 3-10
Platform crushes machine host electric current and is not more than 50A, and the crushing period is 15 minutes/time, and crushing the period is 2-4 times, crushes period every completion
Once be sampled detection, pulverizer revolving speed is 2000 revs/min, and air-introduced machine electric current is not more than 25A, by be classified obtain D50=
The spherical powder of 12-40um；
(4) high temperature sintering
The spherical powder for the 12-40um that step (3) obtains 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 keeps the temperature 4~18 hours, obtains lithium titanate composite cathode material of silicon/carbon/graphite.
As a preferred embodiment, commercially available lithium titanate purity as described in step (1) is greater than 99.0%, granularity 100-
1000 nm。
As a preferred embodiment, expanded graphite powder as described in step (1) is crystalline flake graphite or micro crystal graphite is
Raw material passes through the one or more of intercalation extruding air-flow crushing, and purity is greater than 99.90%, and granularity is 5-40 um.
As a preferred embodiment, carbon source as described in step (1) be glucose, sucrose, polyvinyl alcohol, polyacrylonitrile,
One or more of water soluble phenol resin, medium temperature asphalt, medium temperature coal pitch.
As a preferred embodiment, protective atmosphere used in atmosphere protection stove described in step (4) is selected from helium, nitrogen
At least one of gas, argon gas, carbon dioxide
The present invention has obvious advantages and beneficial effects compared with the existing technology, specifically, by above-mentioned technical proposal
Known to:
1, the present invention uses easy-to-use mechanical mixture, and static pressure is waited to merge, and crushes the means such as nodularization, high temperature sintering for titanium
Sour lithium is distributed in the three-dimensional conductive network of graphite composition, the good electrical contact between lithium titanate and graphite can be maintained, to mention
The high first charge-discharge efficiency and cycle performance of material.
2, the static pressure fusion such as introduce, make the compound closer of lithium titanate and graphite, can be improved volume energy density and times
Rate performance.
3, preparation method of the present invention is simple, reproducible, strong operability, is suitble to be prepared on a large scale.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Embodiment one
A kind of preparation method of lithium ion battery lithium titanate composite cathode material of silicon/carbon/graphite, comprising the following steps:
(1) mechanical mixture
It is the granularity that raw material is made by commercially available 99% purity, the lithium titanate of granularity 500nm, crystalline flake graphite is 10um swollen
Swollen powdered graphite, glucose are added in high-speed mixer according to mass ratio 1:10:0.1, using 5000 r/min of revolving speed into
Row solid dispersion 1h, obtains the mixture of three；
(2) the static pressure fusion such as
The mixture press-powder that step (1) obtains is filled into the rubber mold of iso-static pressure shaping machine, high-frequency electromagnetic is passed through
Vibration is vacuumized after sealing so that press-powder obtains closely knit, and the air between powder particle is discharged, and is put into equipped with water or oil
In high-pressure bottle, 100 MPa are pressurized to, are heated to 150 DEG C, 10 h of pressure-maintaining and heat-preservation is pressed into block after being cooled to room temperature；
(3) nodularization is crushed
After block is crushed using Universalpulverizer, crushing nodularization is carried out into pulverizer, pulverizer is set as 3,
Machine host electric current 40A is crushed, the crushing period is 15 minutes/time, and crushing the period is 2 times, crushes period every completion and is once taken out
Sample detection, pulverizer revolving speed are 2000 revs/min, air-introduced machine electric current 20A, obtain the spherical powder of the um of D50=16 by classification；
(4) high temperature sintering
The spherical powder for 16 um that step (3) obtains is placed in nitrogen atmosphere protection stove and is sintered, with 2 DEG C/min
Heating rate rise to 1000 DEG C and keep the temperature 4 hours, obtain lithium titanate composite cathode material of silicon/carbon/graphite.
Embodiment two
In the present embodiment, the lithium titanate purity 99.5% of the addition in step (1), granularity 800nm, expanded graphite raw material is micro-
Spar ink, D50 are 12 um, purity 99.96%, mass ratio 1:100:0.5, in addition to this, other processes and condition and are implemented
Example one is consistent.
Embodiment three
In the present embodiment, selection is pressurized to 200 MPa in step (2), is heated to 250 DEG C, 15 h of pressure-maintaining and heat-preservation, removes this
Except, other processes are consistent with condition and embodiment one.
Example IV
In the present embodiment, selection pulverizer is set as 5 in step (3), crushes machine host electric current 50A, and crushing the period is 3
Secondary, air-introduced machine electric current 10A obtains the spherical powder of D50=14um by classification, in addition to this, other processes and condition and implementation
Example one is consistent.
Embodiment five
In the present embodiment, atmosphere protection stove selects argon gas in step (4), rises to 800 with the heating rate of 25 DEG C/min
DEG C and keep the temperature 18 hours, in addition to this, other processes are consistent with condition and 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%.
For the performance for examining graphite cathode material, tested with half-cell test method, with porous polyimide of the invention
Coated graphite material: SBR (solid content 50%): CMC:SP=95.5:2.0:1.5:1.0 (weight ratio), add appropriate deionization
Water mixing is tuned into pulpous state, is coated on copper foil and negative electrode tab was made in dry 12 hours in vacuum oven；To electrode metal
Lithium piece forms half-cell, and electrolyte is 1M liPF6/ EC+DEC+DMC=1:1:1, and charge-discharge magnification is 0.2 C/5C, charge and discharge
Piezoelectric voltage range is 0-1.5V, and the charge and discharge electric cabinet computerizedd control carries out the acquisition and control of data.It the results are shown in Table 1
Table 1 lists the performance parameter ratio of lithium titanate graphite material made from the embodiment of the present invention Yu comparative example material
Compared with.
As can be seen from the above results: the high rate performance of lithium titanate graphite cathode material made from the embodiment of the present invention and following
Ring performance obviously increases compared with comparative example, and reason can be attributed to the present invention by easy-to-use mechanical mixture, waits static pressure
Fusion crushes the means such as nodularization, high temperature sintering and is distributed in lithium titanate in the three-dimensional conductive network of graphite composition, can maintain metatitanic acid
Good electrical contact between lithium and graphite, to improve the first charge-discharge efficiency and cycle performance of material.Introduce simultaneously etc.
Static pressure fusion, makes the compound closer of lithium titanate and graphite, volume energy density and high rate performance can be improved.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is 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, which is characterized 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 high-speed mixer, carries out 1~4h of solid dispersion using 500~5000r/min of revolving speed, obtain the mixture of three；
(2) etc. the mixture press-powder that step (1) obtains is filled into the rubber mold of iso-static pressure shaping machine by static pressure fusion, passes through high frequency
Electric and magnetic oscillation is vacuumized after sealing so that press-powder obtains closely knit, and the air between powder particle is discharged, be put into equipped with water or
In the high-pressure bottle of oil, it is pressurized to 100~200MPa, is heated to 150~200 DEG C, 10~20h of pressure-maintaining and heat-preservation is cooled to room temperature
After be pressed into block；(3) after block is crushed by crushing nodularization using Universalpulverizer, crushing ball is carried out into pulverizer
Change, pulverizer is set as 3-10 platform, crushes machine host electric current and is not more than 50A, and the crushings period is 15 minutes/time, and the crushing period is
It 2-4 times, crushes period every completion and is once sampled detection, pulverizer revolving speed is 2000 revs/min, and air-introduced machine electric current is not more than
25A obtains the spherical powder of D50=12-40um by classification；(4) spherical shape for the 12-40um that high temperature sintering obtains step (3)
Powder is placed in atmosphere protection stove and is sintered, with the heating rate of 2~25 DEG C/min rise to 400~1000 DEG C and keep the temperature 4~
18 hours, obtain lithium titanate composite cathode material of silicon/carbon/graphite.
2. a kind of preparation method of lithium ion battery lithium titanate composite cathode material of silicon/carbon/graphite according to claim 1,
Be characterized in that: commercially available lithium titanate purity as described in step (1) is greater than 99.0%, granularity 100-1000nm.
3. a kind of preparation method of lithium ion battery lithium titanate composite cathode material of silicon/carbon/graphite according to claim 1,
Be characterized in that: expanded graphite powder as described in step (1) is raw material by intercalation extruding using crystalline flake graphite and/or micro crystal graphite
What air-flow crushing obtained, purity is greater than 99.90%, granularity 5-40um.
4. a kind of preparation method of lithium ion battery lithium titanate composite cathode material of silicon/carbon/graphite according to claim 1,
Be characterized in that: the carbon source is glucose, sucrose, polyvinyl alcohol, polyacrylonitrile, water soluble phenol resin, the drip of medium temperature petroleum
One or more of green, medium temperature coal pitch.
5. a kind of preparation method of lithium ion battery lithium titanate composite cathode material of silicon/carbon/graphite according to claim 1,
Be characterized in that: protective atmosphere used in atmosphere protection stove described in step (4) is selected from helium, nitrogen, argon gas, carbon dioxide
At least one of.
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| CN109524631B (en) * | 2017-09-20 | 2021-10-12 | 上海杉杉科技有限公司 | Preparation method of high-capacity composite negative electrode 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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