CN108682803A - A method of improving lithium ion battery silicon cathode material performance - Google Patents
A method of improving lithium ion battery silicon cathode material performance Download PDFInfo
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- CN108682803A CN108682803A CN201810379842.0A CN201810379842A CN108682803A CN 108682803 A CN108682803 A CN 108682803A CN 201810379842 A CN201810379842 A CN 201810379842A CN 108682803 A CN108682803 A CN 108682803A
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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
- 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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- 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 present invention discloses a kind of method improving lithium ion battery silicon cathode material performance, includes following steps：（One）It is prepared by the cathode of the sub- silicon composite of oxidation：1）A certain amount of SiO powder is weighed, is poured into the deionized water that quality is 10 times of SiO mass, then adds a certain amount of graphite and glucose；2）The solution mixed is put into high energy ball mill and carries out ball milling；3）The good persursor material of ball milling is put into tube furnace；4）The SiO/C composite materials prepared are taken out, by the way that itself and conductive agent acetylene black, binder PVDF to be mixed in a certain ratio；（Two）Prelithiation processing on electrode.The present invention carries out compound SiO materials with carbon material, then lithium metal is added in the composite and carries out prelithiation modification, modified SiO composite materials as cathode click it, and coulombic efficiency is increased to from 77% other performances of 81% or more, SiO composite materials and is also greatly improved for the first time.
Description
Technical field
The present invention relates to negative material field technology, a kind of lithium ion battery silicon cathode material performance that improves is referred in particular to
Method.
Background technology
The problems such as growth with world population and economic fast development, energy shortage, environmental pollution, is to countries in the world
Sustainable development propose severe challenge, also in watchful people's future low-carbon life the problems such as haze in urban life
Necessity.The emphasis that green energy resource is increasingly becoming development and utilizes.The Optimum utilization of green energy resource needs long-life, high specific energy
The energy storage of amount and specific power and electrical source of power are support.Lithium ion battery is high with its energy density, operating voltage is high, cycle life
Long, the advantages that load characteristic is good, charging rate is fast, safety non-pollution, certainty plays in society based on future is by electric energy
Very important effect.
Negative material is one of the key factor of lithium ion battery development, at present the negative material of commercial Li-ion battery
Graphite-like carbonaceous material is mainly used, but the graphite material capacity of practical application becomes closer to its theoretical specific capacity, it can not
Pass through the modified capacity for improving graphite again.Therefore novel anode material of the development with height ratio capacity and high security has become
The key point of lithium ion battery negative material research.SiO has the specific capacity (2443mAh/g) higher than business carbon material and excellent
Different cycle performance can largely absorb and store lithium, be the substitute that carbon negative electrode material of lithium ion cell gets a good chance of.However
The sub- silicon materials of oxidation find it by research there are first charge-discharge efficiencies it is relatively low, and the shortcomings of electric conductivity is poor.
Invention content
In view of this, in view of the deficiencies of the prior art, the present invention aims to provide a kind of raising lithium ions
The method of battery silicium cathode material property can effectively solve the sub- silicon materials of existing oxidation there are first charge-discharge efficiencies and is relatively low
And the problem that electric conductivity is poor.
To achieve the above object, the present invention is using following technical solution：
A method of lithium ion battery silicon cathode material performance is improved, includes following steps：
（One）It is prepared by the cathode of the sub- silicon composite of oxidation：
1）A certain amount of SiO powder is weighed, is poured into the deionized water that quality is 10 times of SiO mass, then adds one
Quantitative graphite and glucose；
2）The solution mixed is put into high energy ball mill and carries out ball milling, Ball-milling Time 4-8h, rotating speed 800-1200r/
m；
3）The good persursor material of ball milling is put into tube furnace, under argon atmosphere, 800-1000 DEG C is heated to, keeps the temperature 4-6h
Afterwards, room temperature is naturally cooled to；
4）The SiO/C composite materials prepared are taken out, by mixing itself and conductive agent acetylene black, binder PVDF by a certain percentage
It closes, this mixture is then modulated into slurry with 1-Methyl-2-Pyrrolidone, then uniformly dried on the remaining copper foil of coating
After be prepared into electrode film；
（Two）Prelithiation processing on electrode：
1）Under vacuum conditions, a certain amount of nano metal lithium powder is dissolved in tetrahydrofuran, is then spread in uniform in electricity
In very thin films, 1-3min is suppressed using the pressure of 2-4Mpa；
2）Electrode film is immersed in the electrolytic solution, after impregnating 1.5-2.5h, is cleaned using DMC solution, is obtained after dry
Final electrode material.
As a preferred embodiment, the grain size of the SiO powder is 10 μm.
As a preferred embodiment, the step（One）1）In weigh 45-55gSiO powder, be poured into 450-550g
Absolute ethyl alcohol in, then be added 4.5-5.5g graphite and 4.5-5.5g glucose.
As a preferred embodiment, the step（One）3）Crucible is poured into after the middle persursor material drying that ball milling is good
In, it then puts into tube furnace, under argon atmosphere, is heated to 800-1000 DEG C with 4-6 DEG C/min, after keeping the temperature 4-6h, then
Naturally cool to room temperature.
As a preferred embodiment, the step（One）4）It is middle to take out the SiO/C composite materials that prepare, by its with lead
Electric agent acetylene black, binder PVDF are uniformly mixed according to mass ratio 75: 10: 15, are then mixed this with 1-Methyl-2-Pyrrolidone
It closes object and is modulated into slurry, be evenly applied on copper foil, be put into baking oven, dried 1.5-2.5 hours at 70-90 DEG C.
As a preferred embodiment, the step（Two）1）In under vacuum conditions, by the nano metal of 160-240mg
Lithium powder is dissolved in tetrahydrofuran solution, is then spread in uniform on electrode film, after waiting tetrahydrofurans to volatilize, uses 2-
The pressure of 4Mpa suppresses 1-3min；Obtain the electrode film of prelithiation.
The present invention has clear advantage and advantageous effect compared with prior art, specifically, by above-mentioned technical proposal
Known to：
The present invention carries out compound SiO materials with carbon material, and lithium metal is then added in the composite and carries out prelithiation modification,
Modified SiO composite materials as cathode click it, and coulombic efficiency is increased to 81% or more, SiO composite materials from 77% for the first time
Other performances are also greatly improved.
Description of the drawings
Fig. 1 is to obtain SiO powder in the embodiment of the present invention 1 by the SEM of the composite material after carbon coating to be schemed；
Fig. 2 is that voltage is 0.01~2 V, 0.5C in the embodiment of the present invention 1（1C=1000 mA/g）Under the conditions of cycle performance for the first time
Figure.
Specific implementation mode
Present invention is disclosed a kind of methods improving lithium ion battery silicon cathode material performance, include following steps：
（One）It is prepared by the cathode of the sub- silicon composite of oxidation：
1）A certain amount of SiO powder is weighed, is poured into the deionized water that quality is 10 times of SiO mass, then adds one
Quantitative graphite and glucose；Specifically, 45-55gSiO powder is weighed, is poured into the absolute ethyl alcohol of 450-550g, then
In the glucose that 4.5-5.5g graphite and 4.5-5.5g is added.Also, the grain size of the SiO powder is 10 μm.
2）The solution mixed is put into high energy ball mill and carries out ball milling, Ball-milling Time 4-8h, rotating speed 800-
1200r/m。
3）The good persursor material of ball milling is put into tube furnace, under argon atmosphere, is heated to 800-1000 DEG C, heat preservation
After 4-6h, room temperature is naturally cooled to；Specifically, it will be poured into crucible after the good persursor material drying of ball milling, then put pipe into
In formula stove, under argon atmosphere, it is heated to 800-1000 DEG C with 4-6 DEG C/min, after keeping the temperature 4-6h, then naturally cools to room
Temperature.
4）The SiO/C composite materials prepared are taken out, by comparing itself and conductive agent acetylene black, binder PVDF by certain
Example mixing, then uses 1-Methyl-2-Pyrrolidone（NMP）This mixture is modulated into slurry, then uniformly on the remaining copper foil of coating,
Electrode film is prepared into after being dried；Specifically, the SiO/C composite materials prepared are taken out, by it with conductive agent acetylene black,
Binder PVDF（Kynoar）According to mass ratio 75: 10: 15 be uniformly mixed, then with 1-Methyl-2-Pyrrolidone by this
Mixture is modulated into slurry, is evenly applied on copper foil, is put into baking oven, is dried 1.5-2.5 hours at 70-90 DEG C.
（Two）Prelithiation processing on electrode：
1）Under vacuum conditions, a certain amount of nano metal lithium powder is dissolved in tetrahydrofuran, is then spread in uniform in electricity
In very thin films, 1-3min is suppressed using the pressure of 2-4Mpa；Specifically, under vacuum conditions, by the nano metal of 160-240mg
Lithium powder is dissolved in tetrahydrofuran solution, is then spread in uniform on electrode film, after waiting tetrahydrofurans to volatilize, uses 2-
The pressure of 4Mpa suppresses 1-3min；Obtain the electrode film of prelithiation.
2）Electrode film is immersed in the electrolytic solution, after impregnating 1.5-2.5h, is cleaned using DMC solution, after dry
Obtain final electrode material.
The present invention is described in further details with multiple embodiments below：
Embodiment 1：
A method of lithium ion battery silicon cathode material performance is improved, includes following steps：
（One）It is prepared by the cathode of the sub- silicon composite of oxidation：
1）A certain amount of SiO powder is weighed, is poured into the deionized water that quality is 10 times of SiO mass, then adds one
Quantitative graphite and glucose；Specifically, 45gSiO powder is weighed, is poured into the absolute ethyl alcohol of 450g, is then being added
4.5g graphite and 4.5 glucose.Also, the grain size of the SiO powder is 10 μm.
2）The solution mixed is put into high energy ball mill and carries out ball milling, Ball-milling Time 5h, rotating speed 900r/m.
3）The good persursor material of ball milling is put into tube furnace, under argon atmosphere, is heated to 800 DEG C, after keeping the temperature 5h,
Naturally cool to room temperature；Specifically, it will pour into crucible after the good persursor material drying of ball milling, then put into tube furnace,
Under argon atmosphere, 800 DEG C are heated to 5 DEG C/min, after keeping the temperature 5h, then naturally cools to room temperature.
4）The SiO/C composite materials prepared are taken out, by comparing itself and conductive agent acetylene black, binder PVDF by certain
Example mixing, then uses 1-Methyl-2-Pyrrolidone（NMP）This mixture is modulated into slurry, then uniformly on the remaining copper foil of coating,
Electrode film is prepared into after being dried；Specifically, the SiO/C composite materials prepared are taken out, by it with conductive agent acetylene black,
Binder PVDF（Kynoar）According to mass ratio 75: 10: 15 be uniformly mixed, then with 1-Methyl-2-Pyrrolidone by this
Mixture is modulated into slurry, is evenly applied on copper foil, is put into baking oven, is dried 1.5 hours at 70 DEG C.
（Two）Prelithiation processing on electrode：
1）Under vacuum conditions, a certain amount of nano metal lithium powder is dissolved in tetrahydrofuran, is then spread in uniform in electricity
In very thin films, 1min is suppressed using the pressure of 2Mpa；Specifically, under vacuum conditions, the nano metal lithium powder of 180mg is molten
Then solution is spread in uniform on electrode film in tetrahydrofuran solution, after waiting tetrahydrofurans to volatilize, use the pressure pressure of 2Mpa
1min processed；Obtain the electrode film of prelithiation.
2）Electrode film is immersed in the electrolytic solution, after impregnating 1.5h, is cleaned using DMC solution, is obtained after dry
Final electrode material.
As shown in Figure 1, schemed by the SEM of the composite material after carbon coating to obtain SiO powder in the present embodiment, it can by Fig. 1
Know, graphite coat is on SiO particles.
Method in through this embodiment will be prepared into button cell after SiO composite material prelithiation, at different conditions
Charge-discharge performance test is carried out, Fig. 2 is that voltage is 0.01-2 V, 0.5C in the present embodiment（1C=1000 mA/g）Under the conditions of it is first
Secondary cycle performance figure.It is 77% not have the processed SiO composite materials of prelithiation, theoretical first charge discharge efficiency, and after prelithiation
SiO composite materials first discharge specific capacity be 1725.6mAh/g, initial charge specific capacity be 1516.4mAh/g, fill for the first time
Discharging efficiency is 85%.
Embodiment 2：
A method of lithium ion battery silicon cathode material performance is improved, includes following steps：
（One）It is prepared by the cathode of the sub- silicon composite of oxidation：
1）A certain amount of SiO powder is weighed, is poured into the deionized water that quality is 10 times of SiO mass, then adds one
Quantitative graphite and glucose；Specifically, 50gSiO powder is weighed, is poured into the absolute ethyl alcohol of 500g, is then being added
The glucose of 5g graphite and 5g.Also, the grain size of the SiO powder is 10 μm.
2）The solution mixed is put into high energy ball mill and carries out ball milling, Ball-milling Time 6h, rotating speed 800r/m.
3）The good persursor material of ball milling is put into tube furnace, under argon atmosphere, 1000 DEG C is heated to, keeps the temperature 4h
Afterwards, room temperature is naturally cooled to；Specifically, it will be poured into crucible after the good persursor material drying of ball milling, then put tube furnace into
In, under argon atmosphere, 1000 DEG C are heated to 4 DEG C/min, after keeping the temperature 4h, then naturally cools to room temperature.
4）The SiO/C composite materials prepared are taken out, by comparing itself and conductive agent acetylene black, binder PVDF by certain
Example mixing, then uses 1-Methyl-2-Pyrrolidone（NMP）This mixture is modulated into slurry, then uniformly on the remaining copper foil of coating,
Electrode film is prepared into after being dried；Specifically, the SiO/C composite materials prepared are taken out, by it with conductive agent acetylene black,
Binder PVDF（Kynoar）According to mass ratio 75: 10: 15 be uniformly mixed, then with 1-Methyl-2-Pyrrolidone by this
Mixture is modulated into slurry, is evenly applied on copper foil, is put into baking oven, is dried 1.8 hours at 80 DEG C.
（Two）Prelithiation processing on electrode：
1）Under vacuum conditions, a certain amount of nano metal lithium powder is dissolved in tetrahydrofuran, is then spread in uniform in electricity
In very thin films, 2min is suppressed using the pressure of 2.5Mpa；Specifically, under vacuum conditions, by the nano metal lithium powder of 200mg
It is dissolved in tetrahydrofuran solution, is then spread in uniform on electrode film, after waiting tetrahydrofurans to volatilize, use the pressure of 2.5Mpa
Force 2min processed；Obtain the electrode film of prelithiation.
2）Electrode film is immersed in the electrolytic solution, after impregnating 1h, is cleaned using DMC solution, is obtained most after dry
Whole electrode material.
After tested, in the present embodiment, the first discharge specific capacity of SiO composite materials is 1698.2mAh/g, initial charge ratio
Capacity is 1487.4mAh/g, first charge-discharge efficiency 83%.
Embodiment 3：
A method of lithium ion battery silicon cathode material performance is improved, includes following steps：
（One）It is prepared by the cathode of the sub- silicon composite of oxidation：
1）A certain amount of SiO powder is weighed, is poured into the deionized water that quality is 10 times of SiO mass, then adds one
Quantitative graphite and glucose；Specifically, 55gSiO powder is weighed, is poured into the absolute ethyl alcohol of 550g, is then being added
The glucose of 5.5g graphite and 5.5g.Also, the grain size of the SiO powder is 10 μm.
2）The solution mixed is put into high energy ball mill and carries out ball milling, Ball-milling Time 7h, rotating speed 950r/m.
3）The good persursor material of ball milling is put into tube furnace, under argon atmosphere, is heated to 850 DEG C, after keeping the temperature 6h,
Naturally cool to room temperature；Specifically, it will pour into crucible after the good persursor material drying of ball milling, then put into tube furnace,
Under argon atmosphere, 850 DEG C are heated to 6 DEG C/min, after keeping the temperature 6h, then naturally cools to room temperature.
4）The SiO/C composite materials prepared are taken out, by comparing itself and conductive agent acetylene black, binder PVDF by certain
Example mixing, then uses 1-Methyl-2-Pyrrolidone（NMP）This mixture is modulated into slurry, then uniformly on the remaining copper foil of coating,
Electrode film is prepared into after being dried；Specifically, the SiO/C composite materials prepared are taken out, by it with conductive agent acetylene black,
Binder PVDF（Kynoar）According to mass ratio 75: 10: 15 be uniformly mixed, then with 1-Methyl-2-Pyrrolidone by this
Mixture is modulated into slurry, is evenly applied on copper foil, is put into baking oven, is dried 2.5 hours at 90 DEG C.
（Two）Prelithiation processing on electrode：
1）Under vacuum conditions, a certain amount of nano metal lithium powder is dissolved in tetrahydrofuran, is then spread in uniform in electricity
In very thin films, 3min is suppressed using the pressure of 3Mpa；Specifically, under vacuum conditions, the nano metal lithium powder of 170mg is molten
Then solution is spread in uniform on electrode film in tetrahydrofuran solution, after waiting tetrahydrofurans to volatilize, use the pressure pressure of 3Mpa
3min processed；Obtain the electrode film of prelithiation.
2）Electrode film is immersed in the electrolytic solution, after impregnating 2.2h, is cleaned using DMC solution, is obtained after dry
Final electrode material.
After tested, in the present embodiment, the first discharge specific capacity of SiO composite materials is 1688.6mAh/g, initial charge ratio
Capacity is 1482.8mAh/g, first charge-discharge efficiency 82%.
Embodiment 4：
A method of lithium ion battery silicon cathode material performance is improved, includes following steps：
（One）It is prepared by the cathode of the sub- silicon composite of oxidation：
1）A certain amount of SiO powder is weighed, is poured into the deionized water that quality is 10 times of SiO mass, then adds one
Quantitative graphite and glucose；Specifically, 48gSiO powder is weighed, is poured into the absolute ethyl alcohol of 480g, is then being added
The glucose of 4.8g graphite and 4.8g.Also, the grain size of the SiO powder is 10 μm.
2）The solution mixed is put into high energy ball mill and carries out ball milling, Ball-milling Time 8h, rotating speed 1000r/m.
3）The good persursor material of ball milling is put into tube furnace, under argon atmosphere, is heated to 900 DEG C, after keeping the temperature 4h,
Naturally cool to room temperature；Specifically, it will pour into crucible after the good persursor material drying of ball milling, then put into tube furnace,
Under argon atmosphere, 900 DEG C are heated to 5 DEG C/min, after keeping the temperature 4h, then naturally cools to room temperature.
4）The SiO/C composite materials prepared are taken out, by comparing itself and conductive agent acetylene black, binder PVDF by certain
Example mixing, then uses 1-Methyl-2-Pyrrolidone（NMP）This mixture is modulated into slurry, then uniformly on the remaining copper foil of coating,
Electrode film is prepared into after being dried；Specifically, the SiO/C composite materials prepared are taken out, by it with conductive agent acetylene black,
Binder PVDF（Kynoar）According to mass ratio 75: 10: 15 be uniformly mixed, then with 1-Methyl-2-Pyrrolidone by this
Mixture is modulated into slurry, is evenly applied on copper foil, is put into baking oven, is dried 2.3 hours at 75 DEG C.
（Two）Prelithiation processing on electrode：
1）Under vacuum conditions, a certain amount of nano metal lithium powder is dissolved in tetrahydrofuran, is then spread in uniform in electricity
In very thin films, 3min is suppressed using the pressure of 4Mpa；Specifically, under vacuum conditions, the nano metal lithium powder of 160mg is molten
Then solution is spread in uniform on electrode film in tetrahydrofuran solution, after waiting tetrahydrofurans to volatilize, use the pressure pressure of 4Mpa
3min processed；Obtain the electrode film of prelithiation.
2）Electrode film is immersed in the electrolytic solution, after impregnating 2.5h, is cleaned using DMC solution, is obtained after dry
Final electrode material.
After tested, in the present embodiment, the first discharge specific capacity of SiO composite materials is 1692.1mAh/g, initial charge ratio
Capacity is 1483.5mAh/g, first charge-discharge efficiency 81%.
Embodiment 5：
A method of lithium ion battery silicon cathode material performance is improved, includes following steps：
（One）It is prepared by the cathode of the sub- silicon composite of oxidation：
1）A certain amount of SiO powder is weighed, is poured into the deionized water that quality is 10 times of SiO mass, then adds one
Quantitative graphite and glucose；Specifically, 52gSiO powder is weighed, is poured into the absolute ethyl alcohol of 520g, is then being added
The glucose of 5.2g graphite and 5.2g.Also, the grain size of the SiO powder is 10 μm.
2）The solution mixed is put into high energy ball mill and carries out ball milling, Ball-milling Time 4h, rotating speed 1200r/m.
3）The good persursor material of ball milling is put into tube furnace, under argon atmosphere, is heated to 960 DEG C, after keeping the temperature 5h,
Naturally cool to room temperature；Specifically, it will pour into crucible after the good persursor material drying of ball milling, then put into tube furnace,
Under argon atmosphere, 960 DEG C are heated to 6 DEG C/min, after keeping the temperature 5h, then naturally cools to room temperature.
4）The SiO/C composite materials prepared are taken out, by comparing itself and conductive agent acetylene black, binder PVDF by certain
Example mixing, then uses 1-Methyl-2-Pyrrolidone（NMP）This mixture is modulated into slurry, then uniformly on the remaining copper foil of coating,
Electrode film is prepared into after being dried；Specifically, the SiO/C composite materials prepared are taken out, by it with conductive agent acetylene black,
Binder PVDF（Kynoar）According to mass ratio 75: 10: 15 be uniformly mixed, then with 1-Methyl-2-Pyrrolidone by this
Mixture is modulated into slurry, is evenly applied on copper foil, is put into baking oven, is dried 2.4 hours at 85 DEG C.
（Two）Prelithiation processing on electrode：
1）Under vacuum conditions, a certain amount of nano metal lithium powder is dissolved in tetrahydrofuran, is then spread in uniform in electricity
In very thin films, 2min is suppressed using the pressure of 3.5Mpa；Specifically, under vacuum conditions, by the nano metal lithium powder of 175mg
It is dissolved in tetrahydrofuran solution, is then spread in uniform on electrode film, after waiting tetrahydrofurans to volatilize, use the pressure of 3.5Mpa
Force 2min processed；Obtain the electrode film of prelithiation.
2）Electrode film is immersed in the electrolytic solution, after impregnating 2.2h, is cleaned using DMC solution, is obtained after dry
Final electrode material.
After tested, in the present embodiment, the first discharge specific capacity of SiO composite materials is 1678.9mAh/g, initial charge ratio
Capacity is 1482.1mAh/g, first charge-discharge efficiency 82%.
Embodiment 6：
A method of lithium ion battery silicon cathode material performance is improved, includes following steps：
（One）It is prepared by the cathode of the sub- silicon composite of oxidation：
1）A certain amount of SiO powder is weighed, is poured into the deionized water that quality is 10 times of SiO mass, then adds one
Quantitative graphite and glucose；Specifically, 54gSiO powder is weighed, is poured into the absolute ethyl alcohol of 540g, is then being added
The glucose of 5.4g graphite and 5.4g.Also, the grain size of the SiO powder is 10 μm.
2）The solution mixed is put into high energy ball mill and carries out ball milling, Ball-milling Time 6h, rotating speed 1100r/m.
3）The good persursor material of ball milling is put into tube furnace, under argon atmosphere, is heated to 880 DEG C, after keeping the temperature 6h,
Naturally cool to room temperature；Specifically, it will pour into crucible after the good persursor material drying of ball milling, then put into tube furnace,
Under argon atmosphere, 880 DEG C are heated to 4 DEG C/min, after keeping the temperature 6h, then naturally cools to room temperature.
4）The SiO/C composite materials prepared are taken out, by comparing itself and conductive agent acetylene black, binder PVDF by certain
Example mixing, then uses 1-Methyl-2-Pyrrolidone（NMP）This mixture is modulated into slurry, then uniformly on the remaining copper foil of coating,
Electrode film is prepared into after being dried；Specifically, the SiO/C composite materials prepared are taken out, by it with conductive agent acetylene black,
Binder PVDF（Kynoar）According to mass ratio 75: 10: 15 be uniformly mixed, then with 1-Methyl-2-Pyrrolidone by this
Mixture is modulated into slurry, is evenly applied on copper foil, is put into baking oven, is dried 2.1 hours at 78 DEG C.
（Two）Prelithiation processing on electrode：
1）Under vacuum conditions, a certain amount of nano metal lithium powder is dissolved in tetrahydrofuran, is then spread in uniform in electricity
In very thin films, 1min is suppressed using the pressure of 3.8Mpa；Specifically, under vacuum conditions, by the nano metal lithium powder of 240mg
It is dissolved in tetrahydrofuran solution, is then spread in uniform on electrode film, after waiting tetrahydrofurans to volatilize, use the pressure of 3.8Mpa
Force 1min processed；Obtain the electrode film of prelithiation.
2）Electrode film is immersed in the electrolytic solution, after impregnating 2.4h, is cleaned using DMC solution, is obtained after dry
Final electrode material.
After tested, in the present embodiment, the first discharge specific capacity of SiO composite materials is 1691.3mAh/g, initial charge ratio
Capacity is 1484.6mAh/g, first charge-discharge efficiency 82%.
The design focal point of the present invention is：The present invention carries out compound SiO materials with carbon material, then in the composite
Lithium metal is added and carries out prelithiation modification, modified SiO composite materials as cathode click it, and coulombic efficiency is carried from 77% for the first time
Other performances of height to 81% or more, SiO composite materials are also greatly improved
The above described is only a preferred embodiment of the present invention, be not intended to limit the scope of the present invention, therefore it is all
It is that any subtle modifications, equivalent variations and modifications made by above example are still fallen within according to the technical essence of the invention
In the range of technical solution of the present invention.
Claims (6)
1. a kind of method improving lithium ion battery silicon cathode material performance, it is characterised in that：Include following steps：
（One）It is prepared by the cathode of the sub- silicon composite of oxidation：
1）A certain amount of SiO powder is weighed, is poured into the deionized water that quality is 10 times of SiO mass, then adds one
Quantitative graphite and glucose；
2）The solution mixed is put into high energy ball mill and carries out ball milling, Ball-milling Time 4-8h, rotating speed 800-1200r/
m；
3）The good persursor material of ball milling is put into tube furnace, under argon atmosphere, 800-1000 DEG C is heated to, keeps the temperature 4-6h
Afterwards, room temperature is naturally cooled to；
4）The SiO/C composite materials prepared are taken out, by mixing itself and conductive agent acetylene black, binder PVDF by a certain percentage
It closes, this mixture is then modulated into slurry with 1-Methyl-2-Pyrrolidone, then uniformly dried on the remaining copper foil of coating
After be prepared into electrode film；
（Two）Prelithiation processing on electrode：
1）Under vacuum conditions, a certain amount of nano metal lithium powder is dissolved in tetrahydrofuran, is then spread in uniform in electricity
In very thin films, 1-3min is suppressed using the pressure of 2-4Mpa；
2）Electrode film is immersed in the electrolytic solution, after impregnating 1.5-2.5h, is cleaned using DMC solution, is obtained after dry
Final electrode material.
2. a kind of method improving lithium ion battery silicon cathode material performance according to claim 1, it is characterised in that：Institute
The grain size for stating SiO powder is 10 μm.
3. a kind of method improving lithium ion battery silicon cathode material performance according to claim 1, it is characterised in that：Institute
State step（One）1）In weigh 45-55gSiO powder, be poured into the absolute ethyl alcohol of 450-550g, then be added 4.5-
The glucose of 5.5g graphite and 4.5-5.5g.
4. a kind of method improving lithium ion battery silicon cathode material performance according to claim 1, it is characterised in that：Institute
State step（One）3）It pours into crucible, then puts into tube furnace, in argon gas after the middle persursor material drying that ball milling is good
Under atmosphere, it is heated to 800-1000 DEG C with 4-6 DEG C/min, after keeping the temperature 4-6h, then naturally cools to room temperature.
5. a kind of method improving lithium ion battery silicon cathode material performance according to claim 1, it is characterised in that：Institute
State step（One）4）It is middle to take out the SiO/C composite materials prepared, by it with conductive agent acetylene black, binder PVDF according to matter
Amount is uniformly mixed than 75: 10: 15, this mixture is then modulated into slurry with 1-Methyl-2-Pyrrolidone, is evenly applied to copper
It on foil, is put into baking oven, is dried 1.5-2.5 hours at 70-90 DEG C.
6. a kind of method improving lithium ion battery silicon cathode material performance according to claim 1, it is characterised in that：Institute
State step（Two）1）In under vacuum conditions, the nano metal lithium powder of 160-240mg is dissolved in tetrahydrofuran solution,
Then it is spread in uniform on electrode film, after waiting tetrahydrofurans to volatilize, 1-3min is suppressed using the pressure of 2-4Mpa；Obtain pre- lithium
The electrode film of change.
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| CN110620223A (en) * | 2019-09-25 | 2019-12-27 | 福建翔丰华新能源材料有限公司 | Lithium ion battery pre-lithiation silicon-carbon multilayer composite negative electrode material and preparation method thereof |
| WO2021056266A1 (en) * | 2019-09-25 | 2021-04-01 | 福建翔丰华新能源材料有限公司 | Lithium ion battery pre-lithiated silicon-carbon multilayer composite negative electrode material and preparation method therefor |
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