CN108682817A - A kind of porous silicon-carbon cathode material preparation method for lithium ion battery - Google Patents
A kind of porous silicon-carbon cathode material preparation method for lithium ion battery Download PDFInfo
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- 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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- H—ELECTRICITY
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Abstract
A kind of porous silicon-carbon cathode material preparation method for lithium ion battery belongs to new energy materials preparation and application field.Specifically include following steps：Earth silicon material is contained by the reduction of thermal reduction method first, the reaction product heat-treated using pickling obtains porous silicon, then it is combined with carbon source solution by the method for vacuum absorption, negative pressure of vacuum is utilized to act on, drive the gas in pore passage structure away, so that carbon source solution is filled into pore passage structure, solution is set to be adsorbed on the surface of porous silicon particle simultaneously, finally combine high temperature cabonization method, obtain the porous silicon-carbon composite cathode material of long circulation life, there is excellent electrochemical performance applied to lithium ion battery, higher specific discharge capacity, long circulation life, it is a kind of ideal lithium ion battery negative material.
Description
Technical field：
The present invention provides one kind to contain earth silicon material as raw material, contains titanium dioxide by the reduction of thermal reduction method
Silicon materials, the reaction product heat-treated using pickling are obtained porous silicon, then pass through the method for vacuum absorption and carbon source solution phase
In conjunction with, that is, utilize negative pressure of vacuum act on, drive the gas in pore passage structure away so that carbon source solution is filled into pore passage structure, together
When so that solution is adsorbed on the surface of porous silicon particle, finally combine high temperature cabonization method, obtain the porous silicon-carbon of long circulation life
Composite negative pole material belongs to new energy materials preparation and application field.
Background technology：
Lithium ion battery has the advantages that energy density is high, open-circuit voltage is high, self-discharge rate is low etc., in portable electronic device
It is used widely with fields such as power vehicles, still, the fast development of electronic equipment and power vehicle, to lithium ion battery
Capacity and energy density propose increasingly higher demands.Currently, in commercialized lithium-ion battery system, stone is generally used
Black class carbon is as negative material, but its theoretical capacity only has 372mAh/g, therefore there is an urgent need for develop novel high-capacity cathode material.
The theoretical specific capacity of silicon is up to 4200mAh/g, an order of magnitude higher than the specific capacity of graphite negative electrodes material, and its removal lithium embedded
Current potential is moderate, low with electrolyte reactivity, and the rich reserves in the earth's crust are cheap, is negative electrode of lithium ion battery of new generation
The ideal chose of material.
But silicon will produce during removal lithium embedded violent Volumetric expansion (>300%), it is easy to cause activity
Material powder of detached in cyclic process, electrode material weaken with collector electrical contact, battery cycle life rapid attenuation.Together
When, due to the volume expansion of silicon materials, firm surface solid dielectric film, electrode structure quilt can not be generated in the electrolytic solution
It destroys, the silicon face newly exposed can constantly form new SEI films, efficiency for charge-discharge is caused to reduce, and accelerate capacity attenuation.
For the serious bulk effect of silicon materials, an effective method is exactly to prepare porous Si-C composite material.One side
The volumetric stress during silica-base material removal lithium embedded can be effectively relieved in face, porous structure, and on the other hand, the compound of carbon can carry
The electronic conductivity of high silica-base material, the volume change of simultaneous buffering silica-base material, and the method and carbon source for passing through vacuum absorption
Solution is combined, and is acted on using negative pressure of vacuum, drives the gas in pore passage structure away so that carbon source solution is filled into pore passage structure
In, while solution being made to be adsorbed on the surface of porous silicon particle, to increase substantially the cyclical stability of silicon based anode material.
Patent CN102208634B once reported a kind of porous Si-C composite material and preparation method thereof, i.e., more by what is prepared
Hole reducing silica is porous silicon, is then coated using organic carbon source, is then heat-treated under an inert atmosphere, is made
It is standby go out porous Si-C composite material.Patent CN107910524A once reported the preparation of the porous silicon-carbon cathode material of another lithium ion
Porous silicon is added in water-soluble carbon sill aqueous solution by method, after gained suspension dry, pulverize again with carbon substrate
Material is heat-treated after evenly mixing, prepares porous silicon-carbon cathode material.It can be seen that porous Si-C composite material have become lithium from
The research hotspot of sub- negative material, but above-mentioned patent is all only to use more traditional solution agitating, and be applied to lithium
When ion battery, cycle life is poor.
Invention content：
Present invention firstly provides a kind of to contain earth silicon material as raw material, is contained first by the reduction of thermal reduction method
There is earth silicon material, the reaction product heat-treated using pickling obtains porous silicon, then passes through the method for vacuum absorption and carbon
Source solution is combined, that is, is utilized negative pressure of vacuum to act on, driven the gas in pore passage structure away so that carbon source solution is filled into duct knot
In structure, while solution being made to be adsorbed on the surface of porous silicon particle, finally combines high temperature cabonization method, obtain the more of long circulation life
Hole silicon-carbon composite cathode material, being applied to lithium ion battery has excellent chemical property, higher specific discharge capacity and length
Cycle life.
The object of the invention can be realized by technical solution below：
It is a kind of to include following step in the method for preparing porous silicon-carbon composite cathode material as raw material containing earth silicon material
Suddenly：
(1) preparation of porous silicon：
By the material containing silica and fused salt according to mass ratio 1:0-1:100 uniformly mixing, add reducing agent,
The mass ratio of material and reducing agent containing silica is 1:0.3-1:20, it is warming up to 400-1500 under inert gas protection
Between DEG C, reduction 0.1-12h postcoolings obtain reaction product A, reaction product A are then positioned over 0.1-12mol/L to room temperature
Acid solution in stir 1-48h, last centrifuge washing and drying, obtain porous silicon；
(2) preparation of porous Si-C composite material：
By step (1) treated porous silicon ultrasonic disperse in the precursor solution B of carbonaceous sources, wherein precursor solution
The mass content of carbon is the 1-70% of porous silicon quality in B；Vacuum degree (＜ is kept in 40-100 DEG C of vacuum drying oven
100Pa) 1-10h, until water evaporating completely, obtains composite precursor material C, under the protection of inert gas, be warming up to 250-
Between 1000 DEG C, heat treatment 1-24h postcoolings finally obtain porous Si-C composite material to room temperature.
The material containing silica is SiO 2 powder, mesoporous silicon oxide or diatomite, kaolin, Ai Luo
Any one in the natural products such as stone, rectorite, quartz, rice husk, the leaf of bamboo, bagasse, sand；
The reducing agent is any one or a few arbitrary proportion mixed powder in the metal powders such as magnesium, aluminium, lithium, sodium, potassium
End；
The acid solution is any one or a few arbitrary proportion mixing in hydrochloric acid, sulfuric acid, nitric acid, acetic acid, oxalic acid
Acid；
The fused salt is metal halide AxBy, and wherein A is metal cation：Li+、Na+、K+、Mg2+、Ca2+、Cs+、
Ba2+、Al3+, B F-、Cl-、Br-、I-, specifically include NaF, KF, MgF2、CaF2、CsF、BaF2、AlF3、NaCl、KCl、MgCl2、
CaCl2、CsCl、BaCl2、AlCl3、NaBr、KBr、MgBr2、CaBr2、CsBr、BaBr2、AlBr3、NaI、KI、MgI2、CaI2、
CsI、BaI2、AlI3In any one or a few arbitrary proportion blend mixture；
The inert gas be argon gas, nitrogen, it is hydrogen-argon-mixed in any one or a few arbitrary proportion gaseous mixture
Body；
The carbon source is sucrose, glucose, fructose, chitosan, phenolic resin, citric acid, starch, polyvinyl alcohol, gathers
Any one or a few arbitrary proportion carbon source in ethylene glycol, polyacrylonitrile, carboxymethyl cellulose, guar gum.
Advantages of the present invention：
(1) reaction product heat-treated by pickling obtains porous silicon, and certain space is provided for the volume expansion of silicon.
(2) it is combined with carbon source solution by the method for vacuum absorption, is acted on, driven away in pore passage structure using negative pressure of vacuum
Gas so that carbon source solution had not only been filled into hole but also had been wrapped in silicon particle surface, to alleviate the volume expansion of silicon, improved electricity
The cyclical stability of pole material.Meanwhile compound carbon material can improve the electronic conductivity of silica-base material, and improve silicon substrate
The compatibility of material and electrolyte.
(3) thermal reduction reaction required temperature is relatively low, while realizing that silicon-carbon composition operation is simple using vacuum absorption method, entirely
Special installation is not needed in reaction process, it is of low cost, it can be achieved that large-scale production.
Description of the drawings：
Fig. 1 is the TEM image of diatomite material after the packet carbon that embodiment 1 obtains；
Fig. 2 is the cycle performance curve that the porous Si-C composite material that embodiment 1 obtains assembles lithium ion battery.
Specific implementation mode
It is further illustrated the present invention below by specific embodiment, it should be understood that these embodiments are only intended to
The present invention is further understood, and should not be construed as limiting the scope of the invention also not by following embodiment for the present invention
Limitation.
Embodiment 1
(1) preparation of porous silicon
By SiO 2 powder and KF according to mass ratio 1:8 uniformly mixing, add magnesium powder, SiO 2 powder and magnesium
The mass ratio of powder is 1:1,620 DEG C are warming up under argon gas protection, reduction 5h postcoolings obtain reaction product A to room temperature,
Then reaction product A is positioned in the hydrochloric acid solution of 0.1mol/L and stirs 48h, last centrifuge washing and drying obtain porous
Silicon；
(2) preparation of porous Si-C composite material
By step (1) treated porous silicon ultrasonic disperse in sucrose solution B, carbon in wherein sucrose solution B
Mass content is the 20% of porous silicon quality；Vacuum degree (＜ 100Pa) 8h is kept in 80 DEG C of vacuum drying ovens, until water steams completely
Hair, obtains composite precursor material C, under the protection of argon gas, is warming up to 800 DEG C, heat treatment 5h postcoolings are to room temperature, most
After obtain porous Si-C composite material.
(3) preparation of electrode slice
By obtained classifying porous Si-C composite material and Super P, binder CMC according to 7:2:1 weight ratio mixing,
It is prepared into slurry and is applied in copper foil current collector, under vacuum in 80 DEG C of dry 10h, is cut into after dry a diameter of
The pole piece of 12mm, weighs and records, and it is spare to be transferred to glove box immediately.The assembly of battery is carried out in the glove box of Ar atmosphere
's.With the LiPF of 1M6/EC+DEC(VEC:VDEC=1：1)+5%FEC solution is as electrolyte, cathode pole piece lithium piece be to electrode,
It is assembled into button cell.By assembled lithium ion battery in 0.01-1.5V voltage ranges, with the current density of 50mA/g into
Row first circle charge and discharge is electro-active.After activation, in 0.01-1.5V voltage ranges, charge and discharge is carried out with the current density of 500mA/g and are followed
Ring.
Fig. 1 is the TEM image of material after the packet carbon that the present embodiment obtains, and as can be seen from the figure carbon source is not only filled into more
In pore structure, while being also wrapped in porous silicon particle surface；Fig. 2 is the porous Si-C composite material assembling that the present embodiment obtains
The cycle performance curve of lithium ion battery, as can be seen from the figure the material cycle 300 circle after capacity reach 471mAh/g, hold
Amount conservation rate is up to 98.2%, and obtaining porous Si-C composite material has excellent chemical property, longer cycle life
With good cyclical stability.
Embodiment 2
(1) preparation of porous silicon
By diatomite and NaCl according to mass ratio 1:10 uniformly mixing, add aluminium powder, the quality of diatomite and aluminium powder
Than being 1:1.2,800 DEG C are warming up under argon gas protection, reduction 3h postcoolings obtain reaction product A to room temperature, then will
Reaction product A, which is positioned in the hydrochloric acid solution of 0.5mol/L, stirs 30h, and last centrifuge washing and drying obtain porous silicon；
(2) preparation of porous Si-C composite material
By step (1) treated porous silicon ultrasonic disperse in glucose solution B, carbon member in wherein glucose solution B
The mass content of element is the 30% of porous silicon quality；Vacuum degree (＜ 100Pa) 10h is kept in 80 DEG C of vacuum drying ovens, until water
Evaporating completely obtains composite precursor material C, under the protection of argon gas, is warming up to 700 DEG C, heat treatment 8h postcoolings are extremely
Room temperature finally obtains porous Si-C composite material.
(3) preparation of electrode slice
By Si-C composite material assembled battery in the way of embodiment 1, charge and discharge blanking voltage is 0.01-1.5V.
Embodiment 3
(1) preparation of porous silicon
By kaolin and MgBr2According to mass ratio 1:6 uniformly mixing, add magnesium powder, the quality of kaolin and magnesium powder
Than being 1:0.8,700 DEG C are warming up under nitrogen gas protection, reduction 3h postcoolings obtain reaction product A to room temperature, then will
Reaction product A is positioned in the hydrochloric acid solution of 1mol/L and stirs for 24 hours, and last centrifuge washing and drying obtain porous silicon；
(2) preparation of porous Si-C composite material
By step (1) treated porous silicon ultrasonic disperse in chitosan solution B, carbon member in wherein chitosan solution B
The mass content of element is the 40% of porous silicon quality；Vacuum degree (＜ 100Pa) 5h is kept in 80 DEG C of vacuum drying ovens, until water is complete
Pervaporation obtains composite precursor material C, under the protection of argon gas, is warming up to 750 DEG C, heat treatment 4h postcoolings to room
Temperature finally obtains porous Si-C composite material.
(3) preparation of electrode slice
By Si-C composite material assembled battery in the way of embodiment 1, charge and discharge blanking voltage is 0.01-1.5V.
Embodiment 4
(1) preparation of porous silicon
By the leaf of bamboo and CaI2According to mass ratio 1:12 uniformly mixing, add magnesium powder, and the mass ratio of the leaf of bamboo and magnesium powder is
1:1.5,640 DEG C are warming up under argon gas protection, reductase 12 h postcoolings to room temperature obtain reaction product A, then will reaction
Product A, which is positioned in the hydrochloric acid solution of 3mol/L, stirs 6h, and last centrifuge washing and drying obtain porous silicon；
(2) preparation of porous Si-C composite material
By step (1) treated porous silicon ultrasonic disperse in fructose soln B, carbon in wherein shell fruit sugar juice B
Mass content be porous silicon quality 20%；Vacuum degree (＜ 100Pa) 6h is kept in 80 DEG C of vacuum drying ovens, until water is complete
Evaporation, obtains composite precursor material C, under the protection of argon gas, is warming up to 700 DEG C, heat treatment 6h postcoolings to room temperature,
Finally obtain porous Si-C composite material.
(3) preparation of electrode slice
By Si-C composite material assembled battery in the way of embodiment 1, charge and discharge blanking voltage is 0.01-1.5V.
Embodiment 5
(1) preparation of porous silicon
By sand and BaF2According to mass ratio 1:7 uniformly mixing, add magnesium powder, and the mass ratio of sand and magnesium powder is 1:
1,640 DEG C are warming up under argon gas protection, reduction 5h postcoolings obtain reaction product A, then by reaction product to room temperature
A, which is positioned in the hydrochloric acid solution of 0.2mol/L, stirs 36h, and last centrifuge washing and drying obtain porous silicon；
(2) preparation of porous Si-C composite material
By step (1) treated porous silicon ultrasonic disperse in polyacrylonitrile solution B, in wherein polyacrylonitrile solution B
The mass content of carbon is the 50% of porous silicon quality；Vacuum degree (＜ 100Pa) 7h is kept in 100 DEG C of vacuum drying ovens, directly
To water evaporating completely, composite precursor material C is obtained, under the protection of argon gas, is warming up to 700 DEG C, is heat-treated cold after 8h
But to room temperature, porous Si-C composite material is finally obtained.
(3) preparation of electrode slice
By Si-C composite material assembled battery in the way of embodiment 1, charge and discharge blanking voltage is 0.01-1.5V.
Embodiment 6
(1) preparation of porous silicon
By rice husk and CsCl according to mass ratio 1:12 uniformly mixing, add magnesium powder, and the mass ratio of rice husk and magnesium powder is
1:2,640 DEG C are warming up under nitrogen gas protection, reduction 5h postcoolings obtain reaction product A to room temperature, then produce reaction
Object A, which is positioned in the hydrochloric acid solution of 5mol/L, stirs 3h, and last centrifuge washing and drying obtain porous silicon；
(2) preparation of porous Si-C composite material
By step (1) treated porous silicon ultrasonic disperse in citric acid solution B, carbon member in wherein citric acid solution B
The mass content of element is the 10% of porous silicon quality；Vacuum degree (＜ 100Pa) 8h is kept in 80 DEG C of vacuum drying ovens, until water is complete
Pervaporation obtains composite precursor material C, under the protection of argon hydrogen, is warming up to 800 DEG C, heat treatment 5h postcoolings to room
Temperature finally obtains porous Si-C composite material.
(3) preparation of electrode slice
By Si-C composite material assembled battery in the way of embodiment 1, charge and discharge blanking voltage is 0.01-1.5V.
Embodiment 7
(1) preparation of porous silicon
By quartz and KBr according to mass ratio 1:9 uniformly mixing, add magnesium powder, the mass ratio of quartz and magnesium powder
It is 1:3,750 DEG C are warming up under argon gas protection, reductase 12 h postcoolings to room temperature obtain reaction product A, then will reaction
Product A, which is positioned in the hydrochloric acid solution of 1.2mol/L, stirs 15h, and last centrifuge washing and drying obtain porous silicon；
(2) preparation of porous Si-C composite material
By step (1) treated porous silicon ultrasonic disperse in phenol resin solution B, in wherein phenol resin solution B
The mass content of carbon is the 50% of porous silicon quality；Vacuum degree (＜ 100Pa) 10h is kept in 70 DEG C of vacuum drying ovens, directly
To water evaporating completely, composite precursor material C is obtained, under the protection of argon gas, is warming up to 850 DEG C, is heat-treated cold after 3h
But to room temperature, porous Si-C composite material is finally obtained.
(3) preparation of electrode slice is by Si-C composite material assembled battery in the way of embodiment 1, charge and discharge blanking voltage
For 0.01-1.5V.
Claims (7)
1. a kind of method to prepare porous Si-C composite material as raw material containing earth silicon material, which is characterized in that including
Following steps：
(1) preparation of porous silicon：
By the material containing silica and fused salt according to mass ratio 1:0-1:100 uniformly mixing, add metal powder also
The mass ratio of former agent, the material containing silica and metal powder reduction agent is 1:0.3-1:20, under inert gas protection
It is warming up between 400-1500 DEG C, reduction 0.1-12h postcoolings obtain reaction product A, then put reaction product A to room temperature
It is placed in the acid solution of 0.1-12mol/L and stirs 1-48h, last centrifuge washing and drying obtain porous silicon；
(2) preparation of porous Si-C composite material
By step (1) treated porous silicon ultrasonic disperse in the precursor solution B of carbonaceous sources, in wherein precursor solution B
The mass content of carbon is the 1-70% of porous silicon quality；＜ 100Pa vacuum degrees 1- is kept in 40-100 DEG C of vacuum drying oven
10h obtains composite precursor material C until water evaporating completely, under the protection of inert gas, be warming up to 250-1000 DEG C it
Between, heat treatment 1-24h postcoolings finally obtain porous Si-C composite material to room temperature.
2. a kind of side to prepare porous Si-C composite material as raw material containing earth silicon material described in accordance with the claim 1
Method, which is characterized in that in step (1), containing earth silicon material be SiO 2 powder, mesoporous silicon oxide or diatomite,
Any one in kaolin, galapectite, rectorite, quartz, rice husk, the leaf of bamboo, bagasse, sand natural products.
3. a kind of side to prepare porous Si-C composite material as raw material containing earth silicon material described in accordance with the claim 1
Method, which is characterized in that in step (1), reducing agent be magnesium, aluminium, lithium, sodium, in potassium metal powder any one or a few is arbitrary
Ratio mixed-powder.
4. a kind of side to prepare porous Si-C composite material as raw material containing earth silicon material described in accordance with the claim 1
Method, which is characterized in that in the step (1), acid solution be hydrochloric acid, sulfuric acid, nitric acid, acetic acid, in oxalic acid any one or it is several
Kind arbitrary proportion mixed acid.
5. a kind of side to prepare porous Si-C composite material as raw material containing earth silicon material described in accordance with the claim 1
Method, which is characterized in that in the step (1), the fused salt is metal halide AxBy, and wherein A is metal cation：Li+、
Na+、K+、Mg2+、Ca2+、Cs+、Ba2+、Al3+, B F-、Cl-、Br-、I-, specifically include NaF, KF, MgF2、CaF2、CsF、BaF2、
AlF3、NaCl、KCl、MgCl2、CaCl2、CsCl、BaCl2、AlCl3、NaBr、KBr、MgBr2、CaBr2、CsBr、BaBr2、
AlBr3、NaI、KI、MgI2、CaI2、CsI、BaI2、AlI3In any one or a few arbitrary proportion blend mixture.
6. a kind of side to prepare porous Si-C composite material as raw material containing earth silicon material described in accordance with the claim 1
Method, which is characterized in that in the step (1), inert gas is any one or a few arbitrary ratio in argon gas, nitrogen, hydrogen argon
Example mixed gas.
7. a kind of side to prepare porous Si-C composite material as raw material containing earth silicon material described in accordance with the claim 1
Method, which is characterized in that in the step (2), carbon source is sucrose, glucose, fructose, chitosan, phenolic resin, citric acid, shallow lake
Any one or a few arbitrary proportion in powder, polyvinyl alcohol, polyethylene glycol, polyacrylonitrile, carboxymethyl cellulose, guar gum
Carbon source.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109659529A (en) * | 2018-12-17 | 2019-04-19 | 潍坊汇成新材料科技有限公司 | A kind of preparation process of silicon-carbon cathode material |
| CN109786704A (en) * | 2019-01-15 | 2019-05-21 | 江汉大学 | A kind of preparation of silicon carbon composite materials method based on the mineral containing silica |
| CN111244421A (en) * | 2020-01-19 | 2020-06-05 | 浙江开化元通硅业有限公司 | Preparation method of silicon-graphite cathode composite material, product and application of silicon-graphite cathode composite material |
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| CN113363433A (en) * | 2021-05-10 | 2021-09-07 | 万向一二三股份公司 | Preparation method of silicon-based composite lithium battery negative electrode material |
| CN114014320A (en) * | 2021-11-18 | 2022-02-08 | 兰州城市学院 | Method for preparing carbon-silicon composite material by using algae biomass and application of carbon-silicon composite material in lithium ion battery |
| CN114044519A (en) * | 2021-11-11 | 2022-02-15 | 上海大学 | Method for preparing porous silicon material by reducing agent in controllable manner |
| WO2022126882A1 (en) * | 2020-12-15 | 2022-06-23 | 广东凯金新能源科技股份有限公司 | Silicon-carbon-based negative electrode material and preparation method thereof |
| TWI820513B (en) * | 2020-11-16 | 2023-11-01 | 南韓商大洲電子材料股份有限公司 | Porous silicon-carbon composite, preparation method thereof, and negative electrode active material comprising same |
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