CN105226261A - The preparation method of a kind of porous silicon/graphite composite lithium ion battery negative material - Google Patents
The preparation method of a kind of porous silicon/graphite composite lithium ion battery negative material Download PDFInfo
- Publication number
- CN105226261A CN105226261A CN201510791512.9A CN201510791512A CN105226261A CN 105226261 A CN105226261 A CN 105226261A CN 201510791512 A CN201510791512 A CN 201510791512A CN 105226261 A CN105226261 A CN 105226261A
- Authority
- CN
- China
- Prior art keywords
- peach gum
- particle
- silicon
- prepared
- polycrystalline silicon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses porous silicon load zinc powder lithium cell cathode material, belong to electrode material preparation field.Interracial contact for both current silicon materials and material with carbon element is poor, to the defect that the hole inwall of silicon materials cannot be completely coated, by polysilicon chip being placed in acetone and absolute ethyl alcohol cleans and is milled to particle, subsequently under the coated gluing effect of peach gum concentrate, by high velocity air, carbon granule is loaded on polysilicon peach gum particle, finally again it calcined and mill, prepare porous silicon/graphite composite lithium ion battery negative material, effectively carbon is carried out coated to porous silicon, the present invention is by silicon and carbon compound, reduce the polarization reaction of silicon materials, reduce metal to contact to be formed with battery electrolyte as negative material and corrode, capacitance promotes 20 ~ 35%, carbon perfection is carried on polysilicon, greatly promote the life-span of battery, service time improves 20% ~ 30%.
Description
Technical field
The present invention relates to the preparation method of a kind of porous silicon/graphite composite lithium ion battery negative material, belong to electrode material preparation field.
Background technology
In lithium ion battery negative material, silicon is one of most promising high-performance lithium ion negative material.Because it has the highest theoretical specific capacity and lower removal lithium embedded voltage and fail safe is high, abundance, low price.But silicon exists serious bulk effect in charge and discharge process, cause coming off of the efflorescence of electrode material and active material, thus have a strong impact on the cyclical stability of silicon electrode material.In addition, silicon has lower electronic conductivity and poor with the compatibility of conventional electrolysis liquid, all limits the practical application of silicon materials.For improving silicon-based anode cycle performance, improve the structural stability of material in cyclic process, usually by silicon materials nanometer and Composite.Wherein, silicon nanometer can suppress the bulk effect of material to a certain extent, can also reduce the diffusion length of lithium ion simultaneously, improves electrochemical reaction speed.But its specific area is very large, increases and contacts with the direct of electrolyte, causes side reaction and irreversible capacity to increase, reduce coulombic efficiency.In addition, silicon active particle is easy to reunite in charge and discharge process, occurs " electrochemistry sintering ", accelerates capacity attenuation.
And the existing mode combined by silicon-carbon, improve the defect of silicon nanometer capacitance fall-off, this has higher electronic conductance and ionic conductance because of material with carbon element, can improve the high rate performance of silica-base material, suppresses the bulk effect of silicon in cyclic process.In addition, material with carbon element can intercept silicon and directly contact with electrolyte, reduces irreversible capacity.But shortcoming is that silicon materials and the interracial contact both material with carbon element are poor, the coated difficulty of complete uniform carbon carried out to the hole inwall of silicon materials nanoscale larger.So need one comparatively closely method for coating to prepare Si-C composite material necessary.
Summary of the invention
Technical problem to be solved by this invention: the interracial contact for both current silicon materials and material with carbon element is poor, to the defect that the hole inwall of silicon materials cannot be completely coated, provide a kind of by polysilicon chip being placed in acetone and absolute ethyl alcohol cleans and is milled to particle, subsequently under the coated gluing effect of peach gum concentrate, by high velocity air, carbon granule is loaded on polysilicon peach gum particle, finally again it calcined and mill, prepare porous silicon/graphite composite lithium ion battery negative material, effectively carbon is carried out coated to porous silicon, add the capacitance of battery.
For solving the problems of the technologies described above, the present invention adopts technical scheme as described below to be:
(1) polysilicon chip of 8 inches is placed in acetone soln, after the ultrasonic process 3 ~ 5min of 200 ~ 300W, takes out after drying, mill under being placed on 10 ~ 15MPa and it is sieved, being prepared into 100 ~ 120 object polysilicon chip particles;
(2) by mass concentration be 90% concentrated hydrochloric acid and mass concentration be the hydrogen peroxide of 25%, 3:1 is uniformly mixed by volume, form oxidizing solution, subsequently the polysilicon chip particle of preparation is placed in oxidizing solution, after its oxidizing solution that submerges completely, after its oscillation treatment to bubble-free is produced, it is filtered and collects filter residue, and to spend deionized water to its surface p H be after 7.0, being placed in the dry 2 ~ 3h of 80 ~ 90 DEG C of baking ovens, to be prepared into porous polycrystalline silicon particle for subsequent use;
(3) the fresh peach gum that will gather, with after clear water rinsing 3 ~ 5 times to its freeze drying 10 ~ 15min, to be dried complete after, be placed on pulverization process in airslide disintegrating mill and sieve, obtain the former peach gum powder of 80 ~ 100 order, subsequently, 1:100 in mass ratio, by former peach gum powder and deionized water, be uniformly mixed 2 ~ 3h, be placed on centrifugal 10 ~ 15min in the centrifuge of 4000 ~ 5000r/min subsequently, collect supernatant liquor, and Vacuum Concentration is to 1/5 of original volume, be prepared into peach gum concentrate;
(4) graphite is placed in airslide disintegrating mill, pulverize and it is sieved, be prepared into 80 ~ 120 object powdered graphites, 1:5 in mass ratio subsequently, the porous polycrystalline silicon particle of peach gum concentrate and above-mentioned preparation is uniformly mixed, and be prepared into porous polycrystalline silicon peach gum particle with the ultrasonic process 3 ~ 5min of 300 ~ 500W, continue subsequently to stir, mixing speed is 600 ~ 800r/min, in whipping process, by the powdered graphite of above-mentioned preparation by high velocity air injection apparatus, be evenly injected on porous polycrystalline silicon peach gum particle, jet-impingement speed is 500 ~ 600m/s;
(5) to be sprayed complete after, after the porous polycrystalline silicon peach gum particle of load powdered graphite being placed in 95 ~ 100 DEG C of baking ovens oven dry 2 ~ 3h, be placed in 150 ~ 270 DEG C of Muffle furnaces and tentatively carbonize, control time is 5 ~ 8h, after preliminary charing, 450 ~ 600 DEG C are warming up to again with the rate program of 10 DEG C/min, insulation charing 8 ~ 10h, it naturally cools to 20 ~ 30 DEG C to treat calcining to complete relief, collect the porous polycrystalline silicon that carbonize to be placed in 10 ~ 15MPa and to mill dispersion formation particle, a kind of porous silicon/graphite composite lithium ion battery negative material can be prepared into.
Application process of the present invention: by electrode active material, acetylene black and binding agent polyvinylidene fluoride, by quality
Than 1:15:5 mixing, be that stirring solvent evenly forms solution with 1-METHYLPYRROLIDONE, be coated on Copper Foil, tabletted after drying, then vacuumize is stand-by at 120 DEG C.Bian lithium metal is to electrode, using porous polypropylene film as the barrier film of battery assembling button cell.The deoxygenation being full of argon gas that is assembled in of battery dewaters in glove box and carries out, and the moisture control in usual glove box is at below 1ppm.Put into 1 successively by order from bottom to top, porous silicon/graphite composite lithium ion battery shell; 2, lithium sheet 3, barrier film 4, porous silicon/graphite composite lithium ion battery negative material; 5, electrolyte; 6, pad; 7, anode shell, seals the battery sealing machine sealing installed.
The present invention is compared with additive method, and Advantageous Effects is:
(1) the present invention is by silicon and carbon compound, reduces the polarization reaction of silicon materials, reduces metal and contacts to be formed with battery electrolyte as negative material and corrode, capacitance lifting 20 ~ 35%;
(2) by being carried on polysilicon by carbon perfection, greatly promote the life-span of battery, service time improves 20% ~ 30%.
Embodiment
First the polysilicon chip of 8 inches is placed in acetone soln, after the ultrasonic process 3 ~ 5min of 200 ~ 300W, takes out after drying, mill under being placed on 10 ~ 15MPa and it is sieved, being prepared into 100 ~ 120 object polysilicon chip particles; By mass concentration be 90% concentrated hydrochloric acid and mass concentration be the hydrogen peroxide of 25%, 3:1 is uniformly mixed by volume, form oxidizing solution, subsequently the polysilicon chip particle of preparation is placed in oxidizing solution, after its oxidizing solution that submerges completely, after its oscillation treatment to bubble-free is produced, it is filtered and collects filter residue, and to spend deionized water to its surface p H be after 7.0, being placed in the dry 2 ~ 3h of 80 ~ 90 DEG C of baking ovens, to be prepared into porous polycrystalline silicon particle for subsequent use; By the fresh peach gum gathered, with after clear water rinsing 3 ~ 5 times to its freeze drying 10 ~ 15min, to be dried complete after, be placed on pulverization process in airslide disintegrating mill and sieve, obtain the former peach gum powder of 80 ~ 100 order, subsequently, 1:100 in mass ratio, by former peach gum powder and deionized water, be uniformly mixed 2 ~ 3h, be placed on centrifugal 10 ~ 15min in the centrifuge of 4000 ~ 5000r/min subsequently, collect supernatant liquor, and Vacuum Concentration is to 1/5 of original volume, be prepared into peach gum concentrate; Graphite is placed in airslide disintegrating mill, pulverize and it is sieved, be prepared into 80 ~ 120 object powdered graphites, 1:5 in mass ratio subsequently, the porous polycrystalline silicon particle of peach gum concentrate and above-mentioned preparation is uniformly mixed, and be prepared into porous polycrystalline silicon peach gum particle with the ultrasonic process 3 ~ 5min of 300 ~ 500W, continue subsequently to stir, mixing speed is 600 ~ 800r/min, in whipping process, by the powdered graphite of above-mentioned preparation by high velocity air injection apparatus, be evenly injected on porous polycrystalline silicon peach gum particle, jet-impingement speed is 500 ~ 600m/s; To be sprayed complete after, after the porous polycrystalline silicon peach gum particle of load powdered graphite being placed in 95 ~ 100 DEG C of baking ovens oven dry 2 ~ 3h, be placed in 150 ~ 270 DEG C of Muffle furnaces and tentatively carbonize, control time is 5 ~ 8h, after preliminary charing, 450 ~ 600 DEG C are warming up to again with the rate program of 10 DEG C/min, insulation charing 8 ~ 10h, it naturally cools to 20 ~ 30 DEG C to treat calcining to complete relief, collect the porous polycrystalline silicon that carbonize to be placed in 10 ~ 15MPa and to mill dispersion formation particle, a kind of porous silicon/graphite composite lithium ion battery negative material can be prepared into.
Example 1
First the polysilicon chip of 8 inches is placed in acetone soln, after 200W ultrasonic process 3min, takes out after drying, mill under being placed on 10MPa and it is sieved, being prepared into 100 object polysilicon chip particles; By mass concentration be 90% concentrated hydrochloric acid and mass concentration be the hydrogen peroxide of 25%, 3:1 is uniformly mixed by volume, form oxidizing solution, subsequently the polysilicon chip particle of preparation is placed in oxidizing solution, after its oxidizing solution that submerges completely, after its oscillation treatment to bubble-free is produced, it is filtered and collects filter residue, and to spend deionized water to its surface p H be after 7.0, being placed in 80 DEG C of dry 2h of baking oven, to be prepared into porous polycrystalline silicon particle for subsequent use; By the fresh peach gum gathered, with after clear water rinsing 3 times to its freeze drying 10min, to be dried complete after, be placed on pulverization process in airslide disintegrating mill and sieve, obtain the former peach gum powder of 80 order, subsequently, 1:100 in mass ratio, by former peach gum powder and deionized water, be uniformly mixed 2h, be placed on centrifugal 10min in the centrifuge of 4000r/min subsequently, collect supernatant liquor, and Vacuum Concentration is to 1/5 of original volume, be prepared into peach gum concentrate; Graphite is placed in airslide disintegrating mill, pulverize and it is sieved, be prepared into 80 object powdered graphites, 1:5 in mass ratio subsequently, the porous polycrystalline silicon particle of peach gum concentrate and above-mentioned preparation is uniformly mixed, and be prepared into porous polycrystalline silicon peach gum particle with 300W ultrasonic process 3min, continue subsequently to stir, mixing speed is 600r/min, in whipping process, by the powdered graphite of above-mentioned preparation by high velocity air injection apparatus, be evenly injected on porous polycrystalline silicon peach gum particle, jet-impingement speed is 500m/s; To be sprayed complete after, the porous polycrystalline silicon peach gum particle of load powdered graphite is placed in after 95 DEG C of baking ovens dry 2h, be placed in 150 DEG C of Muffle furnaces and tentatively carbonize, control time is 5h, after preliminary charing, 450 DEG C are warming up to again with the rate program of 10 DEG C/min, insulation charing 8h, it naturally cools to 20 DEG C to treat calcining to complete relief, collect the porous polycrystalline silicon that carbonize to be placed in 10MPa and to mill dispersion formation particle, a kind of porous silicon/graphite composite lithium ion battery negative material can be prepared into.
By electrode active material, acetylene black and binding agent polyvinylidene fluoride, 1:15:5 mixing in mass ratio, is that stirring solvent evenly forms solution with 1-METHYLPYRROLIDONE, is coated on Copper Foil, tabletted after drying, then vacuumize is stand-by at 120 DEG C.Bian lithium metal is to electrode, using porous polypropylene film as the barrier film of battery assembling button cell.The deoxygenation being full of argon gas that is assembled in of battery dewaters in glove box and carries out, and the moisture control in usual glove box is at below 1ppm.Put into 1 successively by order from bottom to top, porous silicon/graphite composite lithium ion battery shell; 2, lithium sheet 3, barrier film 4, porous silicon/graphite composite lithium ion battery negative material; 5, electrolyte; 6, pad; 7, anode shell, seals the battery sealing machine sealing installed.
Example 2
First the polysilicon chip of 8 inches is placed in acetone soln, after 250W ultrasonic process 4min, takes out after drying, mill under being placed on 12MPa and it is sieved, being prepared into 110 object polysilicon chip particles; By mass concentration be 90% concentrated hydrochloric acid and mass concentration be the hydrogen peroxide of 25%, 3:1 is uniformly mixed by volume, form oxidizing solution, subsequently the polysilicon chip particle of preparation is placed in oxidizing solution, after its oxidizing solution that submerges completely, after its oscillation treatment to bubble-free is produced, it is filtered and collects filter residue, and to spend deionized water to its surface p H be after 7.0, being placed in 85 DEG C of dry 3h of baking oven, to be prepared into porous polycrystalline silicon particle for subsequent use; By the fresh peach gum gathered, with after clear water rinsing 4 times to its freeze drying 12min, to be dried complete after, be placed on pulverization process in airslide disintegrating mill and sieve, obtain the former peach gum powder of 90 order, subsequently, 1:100 in mass ratio, by former peach gum powder and deionized water, be uniformly mixed 3h, be placed on centrifugal 12min in the centrifuge of 4500r/min subsequently, collect supernatant liquor, and Vacuum Concentration is to 1/5 of original volume, be prepared into peach gum concentrate; Graphite is placed in airslide disintegrating mill, pulverize and it is sieved, be prepared into 100 object powdered graphites, 1:5 in mass ratio subsequently, the porous polycrystalline silicon particle of peach gum concentrate and above-mentioned preparation is uniformly mixed, and be prepared into porous polycrystalline silicon peach gum particle with 400W ultrasonic process 4min, continue subsequently to stir, mixing speed is 700r/min, in whipping process, by the powdered graphite of above-mentioned preparation by high velocity air injection apparatus, be evenly injected on porous polycrystalline silicon peach gum particle, jet-impingement speed is 550m/s; To be sprayed complete after, the porous polycrystalline silicon peach gum particle of load powdered graphite is placed in after 97 DEG C of baking ovens dry 3h, be placed in 200 DEG C of Muffle furnaces and tentatively carbonize, control time is 7h, after preliminary charing, 520 DEG C are warming up to again with the rate program of 10 DEG C/min, insulation charing 9h, it naturally cools to 25 DEG C to treat calcining to complete relief, collect the porous polycrystalline silicon that carbonize to be placed in 12MPa and to mill dispersion formation particle, a kind of porous silicon/graphite composite lithium ion battery negative material can be prepared into.
By electrode active material, acetylene black and binding agent polyvinylidene fluoride, 1:15:5 mixing in mass ratio, is that stirring solvent evenly forms solution with 1-METHYLPYRROLIDONE, is coated on Copper Foil, tabletted after drying, then vacuumize is stand-by at 120 DEG C.Bian lithium metal is to electrode, using porous polypropylene film as the barrier film of battery assembling button cell.The deoxygenation being full of argon gas that is assembled in of battery dewaters in glove box and carries out, and the moisture control in usual glove box is at below 1ppm.Put into 1 successively by order from bottom to top, porous silicon/graphite composite lithium ion battery shell; 2, lithium sheet 3, barrier film 4, porous silicon/graphite composite lithium ion battery negative material; 5, electrolyte; 6, pad; 7, anode shell, seals the battery sealing machine sealing installed.
Example 3
First the polysilicon chip of 8 inches is placed in acetone soln, after 300W ultrasonic process 5min, takes out after drying, mill under being placed on 15MPa and it is sieved, being prepared into 120 object polysilicon chip particles; By mass concentration be 90% concentrated hydrochloric acid and mass concentration be the hydrogen peroxide of 25%, 3:1 is uniformly mixed by volume, form oxidizing solution, subsequently the polysilicon chip particle of preparation is placed in oxidizing solution, after its oxidizing solution that submerges completely, after its oscillation treatment to bubble-free is produced, it is filtered and collects filter residue, and to spend deionized water to its surface p H be after 7.0, being placed in 90 DEG C of dry 3h of baking oven, to be prepared into porous polycrystalline silicon particle for subsequent use; By the fresh peach gum gathered, with after clear water rinsing 5 times to its freeze drying 15min, to be dried complete after, be placed on pulverization process in airslide disintegrating mill and sieve, obtain the former peach gum powder of 100 order, subsequently, 1:100 in mass ratio, by former peach gum powder and deionized water, be uniformly mixed 3h, be placed on centrifugal 15min in the centrifuge of 5000r/min subsequently, collect supernatant liquor, and Vacuum Concentration is to 1/5 of original volume, be prepared into peach gum concentrate; Graphite is placed in airslide disintegrating mill, pulverize and it is sieved, be prepared into 120 object powdered graphites, 1:5 in mass ratio subsequently, the porous polycrystalline silicon particle of peach gum concentrate and above-mentioned preparation is uniformly mixed, and be prepared into porous polycrystalline silicon peach gum particle with 500W ultrasonic process 5min, continue subsequently to stir, mixing speed is 800r/min, in whipping process, by the powdered graphite of above-mentioned preparation by high velocity air injection apparatus, be evenly injected on porous polycrystalline silicon peach gum particle, jet-impingement speed is 600m/s; To be sprayed complete after, the porous polycrystalline silicon peach gum particle of load powdered graphite is placed in after 100 DEG C of baking ovens dry 3h, be placed in 270 DEG C of Muffle furnaces and tentatively carbonize, control time is 8h, after preliminary charing, 600 DEG C are warming up to again with the rate program of 10 DEG C/min, insulation charing 10h, it naturally cools to 30 DEG C to treat calcining to complete relief, collect the porous polycrystalline silicon that carbonize to be placed in 15MPa and to mill dispersion formation particle, a kind of porous silicon/graphite composite lithium ion battery negative material can be prepared into.
By electrode active material, acetylene black and binding agent polyvinylidene fluoride, 1:15:5 mixing in mass ratio, is that stirring solvent evenly forms solution with 1-METHYLPYRROLIDONE, is coated on Copper Foil, tabletted after drying, then vacuumize is stand-by at 120 DEG C.Bian lithium metal is to electrode, using porous polypropylene film as the barrier film of battery assembling button cell.The deoxygenation being full of argon gas that is assembled in of battery dewaters in glove box and carries out, and the moisture control in usual glove box is at below 1ppm.Put into 1 successively by order from bottom to top, porous silicon/graphite composite lithium ion battery shell; 2, lithium sheet 3, barrier film 4, porous silicon/graphite composite lithium ion battery negative material; 5, electrolyte; 6, pad; 7, anode shell, seals the battery sealing machine sealing installed.
Claims (1)
1. a preparation method for porous silicon/graphite composite lithium ion battery negative material, is characterized in that concrete preparation process is:
(1) polysilicon chip of 8 inches is placed in acetone soln, after the ultrasonic process 3 ~ 5min of 200 ~ 300W, takes out after drying, mill under being placed on 10 ~ 15MPa and it is sieved, being prepared into 100 ~ 120 object polysilicon chip particles;
(2) by mass concentration be 90% concentrated hydrochloric acid and mass concentration be the hydrogen peroxide of 25%, 3:1 is uniformly mixed by volume, form oxidizing solution, subsequently the polysilicon chip particle of preparation is placed in oxidizing solution, after its oxidizing solution that submerges completely, after its oscillation treatment to bubble-free is produced, it is filtered and collects filter residue, and to spend deionized water to its surface p H be after 7.0, being placed in the dry 2 ~ 3h of 80 ~ 90 DEG C of baking ovens, to be prepared into porous polycrystalline silicon particle for subsequent use;
(3) the fresh peach gum that will gather, with after clear water rinsing 3 ~ 5 times to its freeze drying 10 ~ 15min, to be dried complete after, be placed on pulverization process in airslide disintegrating mill and sieve, obtain the former peach gum powder of 80 ~ 100 order, subsequently, 1:100 in mass ratio, by former peach gum powder and deionized water, after being uniformly mixed 2 ~ 3h, be placed on centrifugal 10 ~ 15min in the centrifuge of 4000 ~ 5000r/min, collect supernatant liquor, and Vacuum Concentration is to 1/5 of original volume, be prepared into peach gum concentrate;
(4) graphite is placed in airslide disintegrating mill, pulverize and it is sieved, be prepared into 80 ~ 120 object powdered graphites, 1:5 in mass ratio subsequently, the porous polycrystalline silicon particle of peach gum concentrate and above-mentioned preparation is uniformly mixed, and be prepared into porous polycrystalline silicon peach gum particle with the ultrasonic process 3 ~ 5min of 300 ~ 500W, continue subsequently to stir, mixing speed is 600 ~ 800r/min, in whipping process, by the powdered graphite of above-mentioned preparation by high velocity air injection apparatus, be evenly injected on porous polycrystalline silicon peach gum particle, jet-impingement speed is 500 ~ 600m/s;
(5) to be sprayed complete after, after the porous polycrystalline silicon peach gum particle of load powdered graphite being placed in 95 ~ 100 DEG C of baking ovens oven dry 2 ~ 3h, be placed in 150 ~ 270 DEG C of Muffle furnaces and tentatively carbonize, control time is 5 ~ 8h, after preliminary charing, 450 ~ 600 DEG C are warming up to again with the rate program of 10 DEG C/min, insulation charing 8 ~ 10h, it naturally cools to 20 ~ 30 DEG C to treat calcining to complete relief, collect the porous polycrystalline silicon that carbonize to be placed in 10 ~ 15MPa and to mill dispersion formation particle, a kind of porous silicon/graphite composite lithium ion battery negative material can be prepared into.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510791512.9A CN105226261A (en) | 2015-11-17 | 2015-11-17 | The preparation method of a kind of porous silicon/graphite composite lithium ion battery negative material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510791512.9A CN105226261A (en) | 2015-11-17 | 2015-11-17 | The preparation method of a kind of porous silicon/graphite composite lithium ion battery negative material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105226261A true CN105226261A (en) | 2016-01-06 |
Family
ID=54995085
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510791512.9A Withdrawn CN105226261A (en) | 2015-11-17 | 2015-11-17 | The preparation method of a kind of porous silicon/graphite composite lithium ion battery negative material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105226261A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106784613A (en) * | 2017-02-23 | 2017-05-31 | 华南理工大学 | A kind of porous silicon copper-plating electrode for lithium ion battery and preparation method thereof |
| CN106058242B (en) * | 2016-08-04 | 2018-09-18 | 英德市科恒新能源科技有限公司 | A kind of preparation method of nanometer of solid phase cladded type anode material of lithium battery |
| CN110311106A (en) * | 2019-06-25 | 2019-10-08 | 西北工业大学 | A method of it promoting lithium ion battery and is large current discharge safety under water |
-
2015
- 2015-11-17 CN CN201510791512.9A patent/CN105226261A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106058242B (en) * | 2016-08-04 | 2018-09-18 | 英德市科恒新能源科技有限公司 | A kind of preparation method of nanometer of solid phase cladded type anode material of lithium battery |
| CN106784613A (en) * | 2017-02-23 | 2017-05-31 | 华南理工大学 | A kind of porous silicon copper-plating electrode for lithium ion battery and preparation method thereof |
| CN110311106A (en) * | 2019-06-25 | 2019-10-08 | 西北工业大学 | A method of it promoting lithium ion battery and is large current discharge safety under water |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107507972B (en) | Preparation method of silicon-carbon negative electrode material, silicon-carbon negative electrode material and lithium ion battery | |
| CN108767195B (en) | Silicon-based electrode with adjustable pore structure and preparation method thereof | |
| CN103035890B (en) | Silicon and graphene composite electrode material and preparation method thereof | |
| CN102969489B (en) | A kind of Si-C composite material and preparation method thereof, lithium ion battery containing this material | |
| CN110289408B (en) | Nano silicon and silicon/carbon composite material based on cutting silicon waste material, preparation method and application | |
| CN102983313B (en) | Si-C composite material and preparation method thereof, lithium ion battery | |
| CN104201438B (en) | A kind of lithium-air battery based on graphene oxide-carbon paper gas catalysis electrode | |
| CN106711461A (en) | Spherical porous silicon/carbon composite material as well as preparation method and application thereof | |
| CN110085853A (en) | Aoxidize sub- silicon substrate carbon negative pole material, cathode pole piece and preparation method thereof and lithium ion battery | |
| CN109216686A (en) | A kind of lithium ion battery silicon-carbon composite material and preparation method | |
| CN106058228A (en) | Core-shell structure silicon-carbon composite material as well as preparation method and application thereof | |
| CN110416533B (en) | Ion battery composite material, preparation method thereof and ion battery | |
| CN108172775A (en) | Phosphorus-doped silicon-carbon negative electrode material for lithium ion battery and preparation method thereof | |
| CN102983317A (en) | Silicon-based composite material and preparation method thereof, silicon-carbon composite material and lithium ion battery | |
| CN110690433B (en) | Silicon-based negative electrode material for lithium ion battery and preparation method thereof | |
| CN110739455A (en) | Silicon-carbon negative electrode material, preparation method and lithium ion battery | |
| CN109767928A (en) | The synthetic method and its application of Fluorin doped carbon coating silica nano particle@carbon nano tube compound material | |
| CN102593444A (en) | Preparation method of carbon-coated lithium titanate and product of carbon-coated lithium titanate | |
| CN109659486A (en) | Preparation method, cathode and the lithium ion battery of negative electrode of lithium ion battery | |
| WO2023155333A1 (en) | Piezoelectric effect-based method for preparing high-performance lithium ion silicon-based negative electrode material and application thereof | |
| CN108807896A (en) | A kind of preparation method of nitrogen-doped carbon cladding Si-C composite material | |
| CN105226261A (en) | The preparation method of a kind of porous silicon/graphite composite lithium ion battery negative material | |
| CN113270587A (en) | Preparation method and application of high-stability silicon-based composite material constructed by in-situ fluorination | |
| CN112436148A (en) | Having TiO2Mesoporous silica negative electrode material with/C composite coating layer and preparation method thereof | |
| CN116803899A (en) | Biomass-derived hard carbon material, preparation method thereof, sodium ion battery negative electrode plate and sodium ion battery |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20160106 |
|
| WW01 | Invention patent application withdrawn after publication |