CN107302080A - A kind of silica-base film negative material and preparation method thereof - Google Patents
A kind of silica-base film negative material and preparation method thereof Download PDFInfo
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- CN107302080A CN107302080A CN201710472669.4A CN201710472669A CN107302080A CN 107302080 A CN107302080 A CN 107302080A CN 201710472669 A CN201710472669 A CN 201710472669A CN 107302080 A CN107302080 A CN 107302080A
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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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
- H01M4/04—Processes of manufacture in general
- H01M4/043—Processes of manufacture in general involving compressing or compaction
- H01M4/0435—Rolling or calendering
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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
- H01M4/04—Processes of manufacture in general
- H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/134—Electrodes based on metals, Si or alloys
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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- H—ELECTRICITY
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- 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
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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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
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- 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 silica-base film negative material and preparation method thereof, by the way that silicon nano material and carbon source presoma common distribution are formed into slurry in a solvent, then slurry is coated in lithium battery conductive current collector, dry and roll, be finally that the silica-base film negative material for lithium ion battery is made by gained pole piece high-temperature heat treatment.By applying silica-base material nanosizing, the pore-creating of carbon source presoma and carbon coating, slurry coating film forming, the pole piece for enhanced film material adhesion are rolled and the multinomial technology such as high-temperature heat treatment, are prepared for the silica-base film negative material of excellent performance.Technique of the present invention is simple, easily operated, and the capacity of prepared silica-base film negative material is high, have extended cycle life, be adapted to commercially produce and lithium ion battery in apply.
Description
Technical field
The present invention relates to lithium ion battery negative material field, more particularly to a kind of lithium ion battery silica-base film negative pole
Material and preparation method thereof.
Background technology
With the fast development of electronic product, the demand of high energy lithium ion cell increases year by year, silicon based anode material because
Height ratio capacity receives much concern.Silicon reaches 4200 mAh/g as lithium ion battery negative material, its theoretical capacity, is current graphite
10 times of material capacity.However, huge Volume Changes can occur in charge and discharge process for silicon materials（>300 %）, easily from pole
Come off on piece, cause cycle life very short.
The main method for improving silicon materials cycle life is nanosizing, filming and Composite etc..Research is most hot at present
It is the research that nano-silicon is combined with vast scale graphite.The cycle life that this method has been exchanged for using the capacity of expendable material as cost,
Cause the energy density room for promotion of battery limited.And in CN201210396461.6 patents, disclose and use radio frequency magnetron
The method that the method for sputtering prepares silicon thin film.Silicon thin film prepared by this method, although high specific capacity can have been given play to and good
Cycle performance, but its prepare with scale is still a huge challenge, and electrode material load capacity and porosity
Control is also a challenge.
The content of the invention
It is simple, with low cost it is an object of the invention to provide a kind of technique, it can efficiently control and prepare silica-base film
Negative material and preparation method thereof, improves the preparation efficiency of silica-base film negative material, and significantly improves its load capacity and circulation
Life-span.
Therefore, technical scheme is as follows：
A kind of silica-base film negative material and preparation method thereof, comprises the following steps：
（One）Silicon nano material and carbon source presoma common distribution are formed into slurry in a solvent；
（Two）By the step（One）The slurry of preparation is coated in lithium battery conductive current collector, drying, is rolled；
（Three）By the step（Two）Middle gained pole piece is placed in vacuum or inert atmosphere, the high temperature at 400 ~ 1200 DEG C
Heat treatment, that is, be made the silica-base film negative material for lithium ion battery.
Preferably, step（One）In silicon nano material be elementary silicon, Si oxide and both compound, average grain
Footpath is 20 ~ 800 nm.Described silicon nano material can be powder morphology, or scattered in advance slurry shape
State.
Preferably, step（One）In carbon source presoma and silicon nano material weight ratio be 1:2 ~ 1:100.
Preferably, step（One）The solid content of middle slurry is no more than 60 %.
Preferably, step（Two）Thickness after middle electrode material is rolled is 0.05 ~ 50 μm.
In step（One）In, silicon nano material is the silicon materials that nanosizing is handled, and can largely improve silicon substrate thin
The cycle performance of membrane negative electrode material, while the coating thickness of material can be adjusted, to adapt to lithium ion battery pair in very large range
The design requirement of different-energy density.
In step（One）In, carbon source presoma includes the conventional organic matter or dispersant as carbon coating.Before carbon source
Drive body and mainly play a part of scattered nano silica-base material in the slurry stage；During high temperature cabonization processing, play and suppress nano-silicon material
Material grows up, prevents nano-silicon and collector alloying reaction, the porosity in regulation electrode material, improves electrode material electric conductivity
Etc. important function.
Preferably, carbon source presoma is the one or more in pitch, glucose, sucrose, resin, CMC, PVdF.
In step（One）In, by adjusting the solid content of slurry, a variety of coating processes pair such as transfer coating, spraying can be met
The requirement of slurry, while being also convenient for the thickness of electrode material.
In step（Two）In, electrode material needs to roll after the drying, to improve between nano silicon material and electrode material
Adhesion between material and conductive current collector.
The invention provides silica-base film negative material made from described silica-base film cathode material preparation method.
The invention provides silica-base film negative material made from described silica-base film cathode material preparation method in lithium
Application in terms of ion battery.
The present invention adds a small amount of carbon source presoma and realizes electrode material using the silica-base material of nanosizing as main active substances
Pore-creating, bag carbon, then rolled and subsequent high temperature Technology for Heating Processing by simply coating, the excellent silica-base film of processability is born
Pole material.The cycle performance of material can be improved using the silica-base material of nanosizing；The carbon source presoma of use is after thermal decomposition
The volumetric expansion that hole is left when can improve electrolyte wellability and the buffering silicon discharge and recharge of silica-base film negative material, and its
The formed carbon of thermal decomposition can improve the electric conductivity of electrode material again, and then ensure that the capacity of silica-base film negative material is played；
Rear Technology for Heating Processing is rolled using pole piece, the volume energy density of electrode material can be improved, while also improving nano-silicon base material
Adhesion between material and between collector, the conductive network of stabilized electrodes material, and then improve the cycle life of material.
With it is existing prepare the technical scheme of silicon thin film compared with, the invention has the advantages that：
1）The technique used is simple, with low cost, it is easy to high-volume, continuous production.
2）Appropriateness rolls the larger porosity regulation and control that liquid phase coating can also be prepared to electrode material in suitable scope, both sharp
In volumetric expansion of the buffering silicon in charge and discharge process, material capacity is conducive to play the raising with cycle life again.
3）The thickness of electrode material is easy to regulation and control, meets demand of the battery to different volumes energy density.
4）The carbonaceous conductive network that carbon source presoma is decomposed thermally to form can be with stabilized electrodes structure, while obstructing electrolyte and silicon
Sill is directly contacted, and is conducive to improving the cycle performance of material.
5）Pole piece is heat-treated after rolling, is conducive to heightening the adhesion between electrode material and collector, so that
Stabilized electrodes structure, improves the cycle performance of material.
Brief description of the drawings
Fig. 1 is the electron scanning micrograph of silica-base film negative material in embodiments of the invention 1（SEM）；
Fig. 2 is embodiments of the invention 1（Spectral line a）With comparative example 3（Spectral line b）The X-ray diffraction of silicon materials used（XRD）Spectrum
Figure；
Embodiment
Silica-base film negative material of the present invention and preparation method thereof is described in detail below in conjunction with the accompanying drawings.It should manage
Solution, specific embodiment described herein is of the invention not for limiting only to explain the present invention.
Using prepared silica-base film negative material as active material in example 1 below ~ 4 and comparative example 1 ~ 3,
2032 type button cells are made, to assess the chemical property of prepared silica-base film negative material.Wherein, metal lithium sheet is opposed
Electrode, 1 mol/L LiPF6EC/DMC（Volume ratio is 1:1）Solution make electrolyte, the micro-pore septums of Celgard 2400 are made
Barrier film.
Embodiment 1
The g of silicon slurry 50 for being 200 nm to the % of solid content 30 average grain diameter（Solvent is NMP）0.5 g PVdF are added, fully
Stirring 4 h makes slurry mixing mixing, slurry is coated uniformly in copper foil conductive current collector by coating machine, 120 DEG C of vacuum are done
Dry 12 h removes solvent, and then roller pole piece, makes electrode material thickness be down to 3 μm by 5 μm, finally under argon atmosphere
900 DEG C of 1 h of heat treatment, that is, obtain the silica-base film negative material for lithium ion battery.
Embodiment 2
By 10 g silicon monoxides and the scattered slurry for being made into solid content in ethanol for 40 % of 2 g pitches, the ball milling on ball mill
Processing, makes the average grain diameter of silicon monoxide be down to 500 nm, then slurry is coated uniformly on into the conductive afflux of copper foil by coating machine
On body, 80 DEG C of 12 h of vacuum drying remove solvent, and then roller pole piece, makes electrode material thickness be down to 20 μm by 30 μm, most
800 DEG C of 2 h of heat treatment under nitrogen protection atmosphere, that is, obtain the silica-base film negative material for lithium ion battery afterwards.
Embodiment 3
The silica flour for being 50 nm by 1 g average grain diameters and 0.05 g CMC ultrasonic disperses are made into the slurry that content is 35 % in water,
Slurry is coated uniformly in copper foil conductive current collector, 80 DEG C of 12 h of vacuum drying remove solvent, and then roller pole piece, makes electricity
Pole material thickness is down to 5 μm by 10 μm, finally under nitrogen protection atmosphere 800 DEG C heat treatment 2 h, that is, obtain for lithium from
The silica-base film negative material of sub- battery.
Embodiment 4
The average grain diameter for preparing the stable % of solid content 10 of PVP is the 100 nm g of silicon slurry 50（Solvent is alcohol）, then spray
Be coated in copper foil conductive current collector, 100 DEG C of 10 min of drying remove solvents, then roller pole piece, make electrode material thickness by
0.5 μm is down to 0.4 μm, and finally 800 DEG C of 1 h of heat treatment under argon atmosphere, that is, obtain the silicon for lithium ion battery
Base film negative material.
Comparative example 1
The g of silicon slurry 50 for being 200 nm to the % of solid content 30 average grain diameter（Solvent is NMP）0.5 g PVdF are added, fully
Stirring 4 h makes slurry mixing mixing, slurry is coated uniformly in copper foil conductive current collector by coating machine, 120 DEG C of vacuum are done
Dry 12 h removes solvent, and then roller pole piece, makes electrode material thickness be down to 3 μm by 5 μm, that is, obtains for lithium ion battery
Silica-base film negative material.
Comparative example 2
The g of silicon slurry 50 for being 200 nm the % of solid content 30 average grain diameter with coating machine（Solvent is NMP）Direct Uniform is coated
In copper foil conductive current collector, 120 DEG C of 12 h of vacuum drying remove solvent, and then roller pole piece, makes electrode material thickness by 5
μm 3 μm are down to, finally 900 DEG C of 1 h of heat treatment under argon atmosphere, that is, obtain the silica-base film for lithium ion battery
Negative material.
Comparative example 3
To the g of silicon slurry 50 that the % of solid content 30 average grain diameter is 1.5 μm（Solvent is NMP）0.5 g PVdF are added, fully
Stirring 4 h makes slurry mixing mixing, slurry is coated uniformly in copper foil conductive current collector by coating machine, 120 DEG C of vacuum are done
Dry 12 h removes solvent, and then roller pole piece, makes electrode material thickness be down to 3 μm by 5 μm, finally under argon atmosphere
900 DEG C of 1 h of heat treatment, that is, obtain the silica-base film negative material for lithium ion battery.
Reversible capacity is tested：
Effective evaluation can be carried out to the cycle performance of battery to the reversible capacity test after circulating battery some cycles, it is circulated
The difference of reversible capacity and reversible capacity first after some cycles is smaller, and its reversible capacity conservation rate is higher, i.e. capacity attenuation
Speed is slower, illustrates that the battery cycle life is longer.
In this embodiment after all reversible capacity tests of head and circulation in 50 weeks to each embodiment and comparative example
Reversible capacity test condition：Under room temperature condition, battery is subjected to constant current charge-discharge, voltage under 1000 mA/g current density
Scope is 0.01 ~ 1.5 V, and circulates reversible capacity after 50 cycles, the first all reversible capacities of record battery and circulation in 50 weeks, is calculated
Capability retention after circulation in 50 weeks.
The electrochemical property test result of 2032 type button cells prepared by the embodiment 1 ~ 4 of table 1. and comparative example 1 ~ 3：
| Project | First week reversible capacity (mAh/g) | Reversible capacity (mAh/g) after circulation in 50 weeks | Capability retention after circulation in 50 weeks |
| Embodiment 1 | 2839.5 | 1066.7 | 37.6% |
| Embodiment 2 | 1496.2 | 1124.2 | 75.1% |
| Embodiment 3 | 2614.9 | 1372.2 | 52.5% |
| Embodiment 4 | 2805.9 | 2245.4 | 80.0% |
| Comparative example 1 | 879.6 | 17.5 | 2.0% |
| Comparative example 2 | 1688.5 | 224.4 | 13.3% |
| Comparative example 3 | 2561.2 | 326.4 | 12.7% |
Comparative example 1 prepares the scheme of silica-base film material when being the non-high temperature carbonization of carbon source presoma, to compare at high temperature carbonization
The effect of reason；Comparative example 2 is the scheme that silica-base film material is prepared when carbon source presoma is not added with, to illustrate carbon source presoma
Effect；Comparative example 3 prepares the scheme of silica-base film material when being using micron silica flour, the shadow to illustrate silicon materials nanosizing
Ring.
Embodiment 1 is that silicon nano material and carbon source presoma common distribution are formed into slurry in a solvent, is then coated with
In lithium battery conductive current collector, dry and roll, finally gained pole piece high-temperature heat treatment is made for lithium ion battery
Silica-base film negative material.As Fig. 1 SEM photograph is shown, the particle diameters of nano silicon particles is about 200 nm, and pole piece can be with
It was observed that stomata and crackle.Fig. 2 spectral lines a show the XRD spectra of nano-silicon in slurry, with spectral line b（The micron silicon of comparative example 3）
Compare, diffraction peak intensity is greatly reduced, the obvious broadening of peak shape illustrates that the crystallite dimension of silicon is reduced to Nano grade.As table 1 shows
Show, gained silica-base film negative material has the high first week mAh/g of reversible capacity 2839.5 and preferable cycle life（50 weeks
Capability retention is up to 37.6 % after circulation）.Comparative example 1 does not use high-temperature process scheme and comparative example 2 without carbon source forerunner
Body scheme, all Capacity Ratios of head of material are relatively low, and capability retention, less than 15 %, illustrates adding for carbon source presoma after circulation in 50 weeks
Enter with thin-film material high-temperature process the capacity of material is played cycle life improve have important influence.Comparative example 3 then makes
With micron silicon as control, although as a result illustrating that the capacity of material is played improves（Reach 2561.2 mAh/g）, but circulation
Life-span is still very poor（Only 12.7 %）, this shows that raising of the nano silicon material to cycle performance in silica-base film material is played
Very important effect.
As shown in table 1, embodiment 2 ~ 4 successively using oxygen containing silicon monoxide material, smaller silicon nano material or
The thinner pole piece of person rolls thickness, and capability retention of the material after 50 weeks is more than 50 %.This result shows, thin by adjusting silicon substrate
The size and film thickness of oxygen content, silicon grain in membrane negative electrode material, can be achieved silica-base film negative material cycle life
Raising.
It should be readily apparent to one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to limit
The system present invention, all any modifications, equivalent substitutions and improvements for obtaining being done within spirit and principle in the present invention etc., it all should include
Within the scope of the present invention.
Claims (6)
1. a kind of silica-base film negative material and preparation method thereof, it is characterised in that comprise the following steps：
（One）Silicon nano material and carbon source presoma common distribution are formed into slurry in a solvent；
（Two）By the step（One）The slurry of preparation is coated in lithium battery conductive current collector, drying, is rolled；
（Three）By the step（Two）Middle gained pole piece is placed in vacuum or inert atmosphere, the high temperature at 400 ~ 1200 DEG C
Heat treatment, that is, be made the silica-base film negative material for lithium ion battery.
2. the preparation method of silica-base film negative material according to claim 1, it is characterised in that the step（One）In
Silicon nano material be elementary silicon, Si oxide and both compound, average grain diameter is 20 ~ 800 nm.
3. the preparation method of silica-base film negative material according to claim 1, it is characterised in that the step（One）In
Carbon source presoma and silicon nano material weight ratio be 1:2 ~ 1:100.
4. the preparation method of silica-base film negative material according to claim 1, it is characterised in that the step（One）In
Slurry solid content be no more than 60 %.
5. the preparation method of silica-base film negative material according to claim 1, it is characterised in that the step（Two）In
Thickness after electrode material is rolled is 0.05 ~ 50 μm.
6. silicon substrate made from the silica-base film cathode material preparation method according to any one of claim 1 ~ 5 claim is thin
Membrane negative electrode material as lithium ion battery negative material application.
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| CN111477835A (en) * | 2020-04-26 | 2020-07-31 | 四川聚创石墨烯科技有限公司 | Method for continuously preparing current collector-silicon-carbon negative electrode |
| CN111755682A (en) * | 2020-07-06 | 2020-10-09 | 马鞍山科达普锐能源科技有限公司 | Silicon-carbon negative electrode material and preparation method thereof |
| CN113023734A (en) * | 2021-03-03 | 2021-06-25 | 昆山宝创新能源科技有限公司 | Porous nitrogen-doped silicon-based negative electrode material and preparation method thereof, negative electrode plate and lithium ion battery |
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Application publication date: 20171027 |