CN108899521A - Utilize waste silicon powder and the compound method for preparing ion cathode material lithium of carbon - Google Patents
Utilize waste silicon powder and the compound method for preparing ion cathode material lithium of carbon Download PDFInfo
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- CN108899521A CN108899521A CN201810742441.7A CN201810742441A CN108899521A CN 108899521 A CN108899521 A CN 108899521A CN 201810742441 A CN201810742441 A CN 201810742441A CN 108899521 A CN108899521 A CN 108899521A
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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
- H01M4/366—Composites as layered products
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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
- H01M4/38—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
- 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
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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 relates to field of lithium ion battery and nanometer technique field, utilize waste silicon powder and the compound method for preparing ion cathode material lithium of carbon more particularly to a kind of.Using waste silicon powder and the compound method for preparing ion cathode material lithium of carbon, this approach includes the following steps：Step 1: the preparation of surface porosity silicon powder；Step 2: the preparation of carbon-coated porous silicon composite material.The Buddha's warrior attendant wire cutting waste silicon powder that the present invention is produced using photovoltaic factory is as silicon raw material, the silicon powder of porous structure is prepared using metal catalytic lithographic method, make its surface that there is the duct of nanostructure, in coated with carbon, it is deep into carbon-coating in the gap of silicon powder surface, keep composite construction more deep, the volume expansion of the synergistic effect limitation silicon of this carbon silicon composite structure is improved its lithium electrical property.
Description
Technical field
The present invention relates to field of lithium ion battery and nanometer technique field, utilize waste silicon powder and carbon more particularly to a kind of
The compound method for preparing ion cathode material lithium.
Background technique
Buddha's warrior attendant wire cutting silicon ingot will be the latest development trend, form silicon powder up to the 40% of gross mass in cutting process,
And the recycling of silicon powder becomes the hot spot studied now.Lithium ion battery is high with its operating voltage, energy density is big, environmental pollution
The advantages that small, becomes the research hotspot of current new energy field.The negative electrode material of Current commercial lithium ion battery is generally body
The product lower carbon material of effect, but should be its theoretical specific capacity is 372mAh/g, so it is close as high-energy to limit it
Spend the application of power supply.And the theoretical specific capacity of silicon is up to 4200mAh/g.Since there are serious bulk effect, limitations for silicon materials
Application of the silicon in lithium electrical domain.Therefore, while guaranteeing silicon materials height ratio capacity, reducing its bulk effect is to study now
Emphasis.
Summary of the invention
The object of the present invention is to provide a kind of using waste silicon powder and the compound method for preparing ion cathode material lithium of carbon, uses
This method, which prepares ion cathode material lithium, can greatly improve the regeneration value of waste silicon powder, also can solve the carbon of lithium ion battery
The problem of negative electrode material theoretical specific capacity is low and silicon is as negative electrode material bulk effect.
The purpose of the present invention is achieved through the following technical solutions：
Using waste silicon powder and the compound method for preparing ion cathode material lithium of carbon, this approach includes the following steps：
Step 1: the preparation of surface porosity silicon powder；
Step 2: the preparation of carbon-coated porous silicon composite material.
It is described using waste silicon powder and the compound method for preparing ion cathode material lithium of carbon, in the step 1, porous surface
The preparation method of structure silicon powder includes the following steps：
Step 1 takes silicon powder, by silicon powder be placed in concentration be 0.5-6mol/L HF aqueous solution in, carried out after 100-400s from
Heart separation, cleans silicon powder using distilled water after centrifuge separation, spare after cleaning；
The AgNO3 aqueous solution of step 2, the HF aqueous solution for taking 0.5-10mol/L and 0.02-0.5mol/L, after mixing,
Obtain mixed solution A；
Silicon powder after cleaning in step 1 is dissolved in mixed solution A, is taken out after placing 10-150s, obtaining adsorption has
The silicon powder of Ag nano particle；
Step 3 takes the KMnO4 aqueous solution that concentration is 0.5-10mol/LHF aqueous solution and concentration is 0.1-1.0mol/L, mixes
After closing uniformly, mixed solution B is obtained；
The silicon powder that adsorption obtained in step 2 has Ag nano particle is placed in mixed solution B, magnetic agitation is uniform
After be centrifugated, silicon powder is washed after centrifuge separation using distilled water, is dried in vacuo after washing, drying is placed on nothing
It is stored at room temperature in oxygen hothouse, obtains surface porosity silicon powder, it is spare.
It is described using waste silicon powder and the compound method for preparing ion cathode material lithium of carbon, in the step 1, HF aqueous solution
Preferred concentration is 1-5mol/L.
It is described using waste silicon powder and the compound method for preparing ion cathode material lithium of carbon, in the mixed solution B, concentration is
The H that concentration is 0.1-1.0mol/L can be used in the KMnO4 aqueous solution of 0.1-1.0mol/L2O2Solution replacement.
It is described using waste silicon powder and the compound method for preparing ion cathode material lithium of carbon, in the step 3, magnetic agitation
Time is 100-500s, and magnetic stirring speed is that 100-500 turns/s.
It is described using waste silicon powder and the compound method for preparing ion cathode material lithium of carbon, it is vacuum drying in the step 3
Temperature is 60 DEG C, and the vacuum drying time is 12h.
It is described using waste silicon powder and the compound method for preparing ion cathode material lithium of carbon, it is carbon-coated in the step 2
The preparation method of porous structure silicon powder includes the following steps：
Surface porosity silicon powder prepared by step 1 is placed in more by step 1, the dopamine solution for preparing 0.1-3mol/L
After in bar amine aqueous solution, the Tris-HCl buffer solution of pH=8.5 is added as solvent, is reacted under the conditions of 25-60 DEG C of temperature
It after 1-12h, is centrifuged after reaction, the composite material of solid is obtained after separation, then using distilled water to composite material
It is cleaned, is dried in vacuo composite material after cleaning, drying temperature is 60 DEG C, drying time 4h, composite material dry
It is spare after dry；
Step 2 takes the composite material after drying to be placed in tube furnace, is heated to 400-1000 DEG C under an argon atmosphere, carbon
Change 1-5h；After temperature is cooled to room temperature, carbon-coated porous silicon composite material is made, carbon-coated porous silicon composite material is
For ion cathode material lithium.
It further include multiple using carbon-coated porous silicon using waste silicon powder and the compound method for preparing ion cathode material lithium of carbon
The silicon cathode lithium ion battery of condensation material preparation.
Beneficial effects of the present invention：A method of ion cathode material lithium being prepared using waste silicon powder and carbon are compound, is utilized
Waste silicon powder and carbon it is compound be prepared into ion cathode material lithium can greatly improve waste silicon powder regeneration be worth, also can solve lithium from
The problem of carbon negative pole material theoretical specific capacity of sub- battery is low and silicon is as negative electrode material bulk effect.
The Buddha's warrior attendant wire cutting waste silicon powder that the present invention is produced using photovoltaic factory is as silicon raw material, using metal catalytic lithographic method
The silicon powder for preparing porous structure, the duct for making its surface have nanostructure are deep into carbon-coating in coated with carbon
In the gap of silicon powder surface, keep composite construction more deep, the volume of the synergistic effect limitation silicon of this carbon silicon composite structure is swollen
It is swollen, it is improved its lithium electrical property.
The present invention mainly uses metal catalytic preparation porous silicon powder, prepares carbon-coated silicon powder by chemical vapor deposition,
By preparing silicon cathode lithium ion battery, excellent cyclical stability and higher specific volume are illustrated in terms of chemical property
Amount, it is most important that environmental-friendly during the preparation process, low in cost, the highly-safe, advantages such as yield is big.By to diamond wire
Cutting waste silicon powder recycles again, and waste becoming treasure is made to improve product market economy value.
Specific embodiment
Invention is further described in detail With reference to embodiment.
Specific embodiment：
Using waste silicon powder and the compound method for preparing ion cathode material lithium of carbon, this approach includes the following steps：
Step 1: the preparation of surface porosity silicon powder；
Step 2: the preparation of carbon-coated porous silicon composite material.
It is described using waste silicon powder and the compound method for preparing ion cathode material lithium of carbon, in the step 1, porous surface
The preparation method of structure silicon powder includes the following steps：
Step 1 takes silicon powder, by silicon powder be placed in concentration be 0.5-6mol/L HF aqueous solution in, carried out after 100-400s from
Heart separation, cleans silicon powder using distilled water after centrifuge separation, spare after cleaning；The main purpose of this step is removal silicon
The SiO2 layer on powder surface；
The AgNO3 aqueous solution of step 2, the HF aqueous solution for taking 0.5-10mol/L and 0.02-0.5mol/L, after mixing,
Obtain mixed solution A；
Silicon powder after cleaning in step 1 is dissolved in mixed solution A, is taken out after placing 10-150s, obtaining adsorption has
The silicon powder of Ag nano particle；The Ag+ ion as have the function of control silicon powder surface reactivity；
Step 3 takes the KMnO4 aqueous solution that concentration is 0.5-10mol/LHF aqueous solution and concentration is 0.1-1.0mol/L, mixes
After closing uniformly, mixed solution B is obtained；
The silicon powder that adsorption obtained in step 2 has Ag nano particle is placed in mixed solution B, magnetic agitation is uniform
After be centrifugated, silicon powder is washed after centrifuge separation using distilled water, is dried in vacuo after washing, drying is placed on nothing
It is stored at room temperature in oxygen hothouse, obtains surface porosity silicon powder, spare, the purpose of this step is to improve the specific surface of silicon powder
Product.
It is described using waste silicon powder and the compound method for preparing ion cathode material lithium of carbon, in the step 1, HF aqueous solution
Preferred concentration is 1-5mol/L.
It is described using waste silicon powder and the compound method for preparing ion cathode material lithium of carbon, in the mixed solution B, concentration is
The H that concentration is 0.1-1.0mol/L can be used in the KMnO4 aqueous solution of 0.1-1.0mol/L2O2Solution replacement.
It is described using waste silicon powder and the compound method for preparing ion cathode material lithium of carbon, in the step 3, magnetic agitation
Time is 100-500s, and magnetic stirring speed is that 100-500 turns/s.
It is described using waste silicon powder and the compound method for preparing ion cathode material lithium of carbon, it is vacuum drying in the step 3
Temperature is 60 DEG C, and the vacuum drying time is 12h.
It is described using waste silicon powder and the compound method for preparing ion cathode material lithium of carbon, it is carbon-coated in the step 2
The preparation method of porous structure silicon powder includes the following steps：
Surface porosity silicon powder prepared by step 1 is placed in more by step 1, the dopamine solution for preparing 0.1-3mol/L
After in bar amine aqueous solution, the Tris-HCl buffer solution of pH=8.5 is added as solvent, is reacted under the conditions of 25-60 DEG C of temperature
It after 1-12h, is centrifuged after reaction, the composite material of solid is obtained after separation, then using distilled water to composite material
It is cleaned, is dried in vacuo composite material after cleaning, drying temperature is 60 DEG C, drying time 4h, composite material dry
It is spare after dry；
Step 2 takes the composite material after drying to be placed in tube furnace, is heated to 400-1000 DEG C under an argon atmosphere, carbon
Change 1-5h；After temperature is cooled to room temperature, carbon-coated porous silicon composite material is made, carbon-coated porous silicon composite material is
For ion cathode material lithium；The degree of graphitization of carbon can be improved by high temperature cabonization, provided to be applied in lithium ion battery
High conductive material.
It further include multiple using carbon-coated porous silicon using waste silicon powder and the compound method for preparing ion cathode material lithium of carbon
The silicon cathode lithium ion battery of condensation material preparation.
The preparation of the silicon cathode lithium ion battery includes the following steps：
The carbon-coated porous silicon composite material of preparation is subjected to electrochemical property test, such as under different current densities,
The reason of testing its cycle life, coulombic efficiency and AC impedance etc., and analyzing its electrochemical performance；
It is made using lithium piece as counter electrode of battery using by the present invention using polypropylene polymeric membrane as battery diaphragm
Lithium piece made of standby carbon-coated porous silicon composite material is as working electrode (cathode)；Purchase is suitable on the market again pads
Piece and battery case, then by working electrode, gasket, diaphragm, the knob for being assembled into CR 2025 in glove box to electrode and battery case
After detaining battery, button cell is sealed using sealing machine, the button cell of preparation is finally stood 12h at normal temperature makes electricity
Pond is activated, and the gasket is stainless steel；Complete the preparation of the button-shaped lithium ion battery of CR 2025.
Certainly, above description is not limitation of the present invention, and the present invention is also not limited to the example above, the art
The variations, modifications, additions or substitutions that those of ordinary skill is made within the essential scope of the present invention also belong to guarantor of the invention
Protect range.
Claims (8)
1. utilizing waste silicon powder and the compound method for preparing ion cathode material lithium of carbon, which is characterized in that this method includes following step
Suddenly：
Step 1: the preparation of surface porosity silicon powder；
Step 2: the preparation of carbon-coated porous silicon composite material.
2. utilizing waste silicon powder and the compound method for preparing ion cathode material lithium of carbon according to claim 1, which is characterized in that
In the step 1, the preparation method of surface porosity silicon powder includes the following steps：
Step 1 takes silicon powder, silicon powder is placed in the HF aqueous solution that concentration is 0.5-6mol/L, centrifugation point is carried out after 100-400s
From, silicon powder is cleaned using distilled water after centrifuge separation, it is spare after cleaning；
The AgNO3 aqueous solution of step 2, the HF aqueous solution for taking 0.5-10mol/L and 0.02-0.5mol/L obtains mixed after mixing
Close solution A；
Silicon powder after cleaning in step 1 is dissolved in mixed solution A, is taken out after placing 10-150s, obtaining adsorption has Ag to receive
The silicon powder of rice grain；
Step 3 takes the KMnO4 aqueous solution that concentration is 0.5-10mol/LHF aqueous solution and concentration is 0.1-1.0mol/L, and mixing is equal
After even, mixed solution B is obtained；
The silicon powder that adsorption obtained in step 2 has Ag nano particle is placed in mixed solution B, after magnetic agitation is uniform from
Heart separation, washs silicon powder using distilled water after centrifuge separation, is dried in vacuo after washing, and the dry anaerobic that is placed on is done
Dry normal temperature laboratory saves, and obtains surface porosity silicon powder, spare.
3. utilizing waste silicon powder and the compound method for preparing ion cathode material lithium of carbon according to claim 2, which is characterized in that
In the step 1, the preferred concentration of HF aqueous solution is 1-5mol/L.
4. utilizing waste silicon powder and the compound method for preparing ion cathode material lithium of carbon according to claim 2, which is characterized in that
In the mixed solution B, the H that concentration is 0.1-1.0mol/L is can be used in the KMnO4 aqueous solution that concentration is 0.1-1.0mol/L2O2
Solution replacement.
5. utilizing waste silicon powder and the compound method for preparing ion cathode material lithium of carbon according to claim 2, which is characterized in that
In the step 3, the time of magnetic agitation is 100-500s, and magnetic stirring speed is that 100-500 turns/s.
6. utilizing waste silicon powder and the compound method for preparing ion cathode material lithium of carbon according to claim 2, which is characterized in that
In the step 3, vacuum drying temperature is 60 DEG C, and the vacuum drying time is 12h.
7. utilizing waste silicon powder and the compound method for preparing ion cathode material lithium of carbon according to claim 1, which is characterized in that
In the step 2, the preparation method of carbon-coated porous structure silicon powder includes the following steps：
Surface porosity silicon powder prepared by step 1 is placed in dopamine by step 1, the dopamine solution for preparing 0.1-3mol/L
After in solution, the Tris-HCl buffer solution of pH=8.5 is added as solvent, reacts 1-12h under the conditions of 25-60 DEG C of temperature
Afterwards, it is centrifuged after reaction, the composite material of solid is obtained after separation, then composite material carried out using distilled water clear
It washes, is dried in vacuo composite material after cleaning, drying temperature is 60 DEG C, drying time 4h, standby after composite material is dry
With；
Step 2 takes the composite material after drying to be placed in tube furnace, is heated to 400-1000 DEG C under an argon atmosphere, and be carbonized 1-
5h；After temperature is cooled to room temperature, carbon-coated porous silicon composite material is made, carbon-coated porous silicon composite material is lithium
Ion negative electrode material.
8. according to claim 1 using waste silicon powder and the compound method for preparing ion cathode material lithium of carbon, feature exists
In, further include using carbon-coated porous silicon composite material preparation silicon cathode lithium ion battery.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109904407A (en) * | 2019-01-02 | 2019-06-18 | 昆明理工大学 | A kind of method that Buddha's warrior attendant wire cutting scrap silicon prepares lithium ion battery negative material |
| CN110157409A (en) * | 2019-05-27 | 2019-08-23 | 武汉科技大学 | A kind of porous silicon/carbon quantum dot Micron-nano composites and preparation method thereof |
| CN110931727A (en) * | 2019-10-25 | 2020-03-27 | 合肥国轩高科动力能源有限公司 | Preparation method of conductive polymer-coated silicon-based negative electrode material |
| CN111403694A (en) * | 2019-08-22 | 2020-07-10 | 杭州师范大学 | Preparation method of carbon-coated porous silicon negative electrode material |
| CN111785944A (en) * | 2020-07-20 | 2020-10-16 | 昆明理工大学 | Method for preparing porous silicon/carbon/nano metal composite anode material by plasma activation cutting of silicon waste |
| CN111799460A (en) * | 2020-07-20 | 2020-10-20 | 昆明理工大学 | Method for preparing boron-doped nano metal/porous silicon-carbon composite cathode based on cutting silicon waste |
| CN113130878A (en) * | 2021-04-02 | 2021-07-16 | 中北大学 | Preparation method and application of boron-doped silicon-based negative electrode material |
| CN116598465A (en) * | 2023-06-19 | 2023-08-15 | 深圳光风新能源科技创新中心有限公司 | High-rate lithium battery negative electrode material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109904407A (en) * | 2019-01-02 | 2019-06-18 | 昆明理工大学 | A kind of method that Buddha's warrior attendant wire cutting scrap silicon prepares lithium ion battery negative material |
| WO2020140602A1 (en) * | 2019-01-02 | 2020-07-09 | 昆明理工大学 | Porous silicon material and preparation method therefor, negative battery material, and electrochemical battery |
| CN110157409A (en) * | 2019-05-27 | 2019-08-23 | 武汉科技大学 | A kind of porous silicon/carbon quantum dot Micron-nano composites and preparation method thereof |
| CN111403694A (en) * | 2019-08-22 | 2020-07-10 | 杭州师范大学 | Preparation method of carbon-coated porous silicon negative electrode material |
| CN110931727A (en) * | 2019-10-25 | 2020-03-27 | 合肥国轩高科动力能源有限公司 | Preparation method of conductive polymer-coated silicon-based negative electrode material |
| CN111785944A (en) * | 2020-07-20 | 2020-10-16 | 昆明理工大学 | Method for preparing porous silicon/carbon/nano metal composite anode material by plasma activation cutting of silicon waste |
| CN111799460A (en) * | 2020-07-20 | 2020-10-20 | 昆明理工大学 | Method for preparing boron-doped nano metal/porous silicon-carbon composite cathode based on cutting silicon waste |
| CN111799460B (en) * | 2020-07-20 | 2022-09-09 | 昆明理工大学 | Method for preparing boron-doped nano metal/porous silicon-carbon composite cathode based on cutting silicon waste |
| CN113130878A (en) * | 2021-04-02 | 2021-07-16 | 中北大学 | Preparation method and application of boron-doped silicon-based negative electrode material |
| CN116598465A (en) * | 2023-06-19 | 2023-08-15 | 深圳光风新能源科技创新中心有限公司 | High-rate lithium battery negative electrode material and preparation method thereof |
| CN116598465B (en) * | 2023-06-19 | 2024-04-05 | 深圳光风新能源科技创新中心有限公司 | High-rate lithium battery negative electrode material and preparation method thereof |
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Application publication date: 20181127 |