CN106684336B - A kind of preparation method of high conjugation lithium battery carbon silicium cathode material - Google Patents
A kind of preparation method of high conjugation lithium battery carbon silicium cathode material Download PDFInfo
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- CN106684336B CN106684336B CN201611211693.4A CN201611211693A CN106684336B CN 106684336 B CN106684336 B CN 106684336B CN 201611211693 A CN201611211693 A CN 201611211693A CN 106684336 B CN106684336 B CN 106684336B
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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
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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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
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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 invention discloses a kind of preparation methods of high conjugation lithium battery carbon silicium cathode material, belong to the technical field of lithium ion battery.Clean rice husk is dried first for invention, its ball milling is obtained into rice husk powder after being cooled to room temperature, it places it in vacuum pyrolysis device, and lead to nitrogen to exclude air, it is subsequently vacuumed out, to cooling after pyrolysis oven heating, rice hull ash must be pyrolyzed, then it is mixed with hydrochloric acid solution, disperse in ultrasonic wave, filtering, collect filter cake, and it is stirred with sodium hydroxide, the dispersedly mixed dispersion liquid under ultrasonic wave, with hydrochloric acid, neopelex is placed in a beaker, it is centrifuged after being stirred, lower sediment is collected to be placed in Muffle furnace, logical argon gas excludes air, it is cooling after calcining, and calcining mixt is subjected to ball milling, obtain high conjugation lithium battery carbon silicium cathode material.The resulting conjugation lithium battery carbon silicium cathode material of the present invention has excellent cycle performance and lower Volumetric expansion, and security performance is high, can promote the use of.
Description
Technical field
The invention discloses a kind of preparation methods of high conjugation lithium battery carbon silicium cathode material, belong to lithium ion battery
Technical field.
Background technique
With the rapid development of economy, global range Energy situation is increasingly serious, the disposable energy of the tradition such as coal, petroleum
Demand still persistently increases, while also aggravating to the destruction of global ecological environment.Therefore, to cleaning, low-carbon environment-friendly and can be again
The exploitation and application of the raw energy have become the project that the mankind need joint exploration.With the development of energy storage technology, wind energy, solar energy
Etc. renewable energy application be greatly improved.Currently, the energy storage lithium ion battery that research is hotter, in portable electronic
It is widely used in equipment such as notebook and smart phone.But in order to realize lithium ion battery in environment-protecting clean, nothing
The lithium-ion electric of new generation of high-energy, high power density, high safety performance is developed in application on the new-energy automobile of disposal of pollutants
Pond is extremely urgent.
Due to lithium storage content with higher and resource abundant, silicon materials be considered as develop high-energy-density of new generation and
One of ideal candidates material of the lithium ion battery negative material of high power density.However, silicon materials capacity in use
Decaying is very fast, is subject to certain restrictions its practical application.According to the analysis, silicon materials removal lithium embedded volume expansion contraction is larger, from
And the overall structure of material is destroyed, reduce the conductivity of material, this is to cause material capacity decaying faster main
Reason.
Then silicon powder and graphite mixing and ball milling are added pitch or polymer overmold material by patent CN200810031840.9
Material ball milling again, carbonization treatment, after crushed, obtain a kind of lithium ion battery silicon-carbon composite negative pole with shell-core structure
Material, center are elemental silicon and graphite, and shell is the pyrolytic carbon of pitch or polymer overmold material, the material cell energy density
Height, good cycle.But the difference in hardness of graphite and silicon is larger, mixing and ball milling efficiency is extremely low together, graphite hardness compared with
It is small, resilient protection effect is generated for silicon in mechanical milling process, is difficult that nano-silicon is made to obtain effective ball milling.
Summary of the invention
The technical problems to be solved by the invention: larger for the difference in hardness of graphite and silicon, mixing and ball milling is imitated together
Rate is extremely low, and graphite hardness is smaller, generates resilient protection effect for silicon in mechanical milling process, is difficult that nano-silicon is made to obtain effective ball
The defect of mill.It will be reacted after rice husk thermal decomposition and pickling with sodium hydroxide the present invention provides a kind of, organic matter carbon is evenly dispersed
Into silica solution, subsequent dewatering and calcining prepares elemental silicon is uniformly coated organic matter carbon particle into simple substance silicon crystal, carbon
Grain can not form resilient protection in its mechanical milling process, to make the method for the effective ball milling of elementary silicon, the present invention will clean first
Rice husk be dried, its ball milling is obtained into rice husk powder after being cooled to room temperature, is placed it in vacuum pyrolysis device, and logical nitrogen
Air is excluded, is subsequently vacuumed out, to cooling after pyrolysis oven heating, pyrolysis rice hull ash obtained, then mixes it with hydrochloric acid solution,
In ultrasonic wave dispersion, filtering, filter cake is collected, and is stirred with sodium hydroxide, the dispersedly mixed dispersion liquid under ultrasonic wave, with
Hydrochloric acid, neopelex are placed in a beaker, and are centrifuged after being stirred, and are collected lower sediment and are placed in Muffle furnace, lead to
Argon gas excludes air, cooling after calcining, and calcining mixt is carried out ball milling, obtains high conjugation lithium battery carbon silicium cathode material.
The resulting conjugation lithium battery carbon silicium cathode material of the present invention has excellent cycle performance and lower Volumetric expansion, peace
Full performance is high, can promote the use of.
In order to solve the above technical problems, the present invention is using technical solution as described below:
(1) discarded rice husk is collected, is cleaned and is placed at 120~130 DEG C dry 2~3h, then stood and be cooled to room
Dry rice husk is placed in ball-milling device, 3~5h of ball milling at 250~300r/min by temperature, after the completion of ball milling, crosses 120 mesh
Sieve, collects to obtain rice husk powder;
(2) the rice husk powder of above-mentioned preparation is placed in vacuum pyrolysis device, lead to nitrogen exclude air, be subsequently vacuumed out to
3.5~4.0kPa is warming up to 550~600 DEG C to pyrolysis oven by 10 DEG C/min, after heat preservation is pyrolyzed 10~15min, cools to the furnace
Room temperature is prepared into pyrolysis rice hull ash;
(3) pyrolysis rice hull ash is mixed with 10% hydrochloric acid solution of mass fraction, is surpassed at 200~300W by 1:5 in mass ratio
After sound disperses 10~15min, filter cake, then 1:5 in mass ratio are filtered and collected, filter cake and 20% sodium hydroxide of mass fraction are stirred
25~30min of mixing is mixed, 10~15min of ultrasonic disperse, is prepared into mixed dispersion liquid at 200~300W;
(4) according to parts by weight, the mixed dispersion liquid of 45~50 parts of above-mentioned preparations, 10~15 parts of mass fractions are weighed respectively
10% hydrochloric acid and 5~8 parts of neopelexes are placed in a beaker, and are stirred 25~30min at 45~50 DEG C;
(5) it after the completion of to be mixed, then is centrifugated at 2500~3000r/min, collects lower sediment and be placed in Muffle
In furnace, lead to argon gas and exclude air, 3~5h of calcination processing at 1400~1500 DEG C cools to room temperature with the furnace, collects calcined mixed
Object is placed in ball grinder, 3~5h of ball milling at 250~300r/min, is crossed 200 meshes, can be prepared into a kind of high conjugation
Lithium battery carbon silicium cathode material.
Application method of the invention is: by the resulting high conjugation lithium battery carbon silicium cathode material of the present invention and conductive agent second
Acetylene black, binder PVDF are mixed with the uniform quality of 6:1:1~8:1:1, in the environment of ambient humidity is 10~15%, with N-
Methyl pyrrolidone is that solvent is applied on copper foil and dries under heat lamp, be subsequently transferred in 120 DEG C of baking oven drying 20~
For 24 hours, it is placed under tablet press machine and is compacted with 10MPa, and be cut into 0.6cm × 0.6cm~0.8cm × 0.8cm electrode slice, with lithium piece
For negative electrode, ethylene carbonate: dimethyl carbonate: methyl ethyl carbonate=1:1:8 is electrolyte, in the glove box full of argon gas
It can be made into lithium half-cell.Through detecting, the specific capacity of the resulting high conjugation lithium battery carbon silicium cathode material of the present invention is 500~
600mAh/g, obtained lithium ion battery voltage are 4~5V, and energy is 160~180Wh/kg, and has excellent cyclicity
Can, it is recycled 60~70 times, capacity retention ratio is 98~99%.
The present invention is compared with other methods, and advantageous effects are:
(1) the resulting high conjugation lithium battery carbon silicium cathode material of present invention output voltage with higher, good follow
Ring stability and higher capacity retention ratio, and low manufacture cost, storage is abundant, environmental-friendly;
(2) the resulting high conjugation lithium battery carbon silicium cathode materials chemistry stability of the present invention is strong, does not occur with electrolyte
Reaction, surface can form stable film, improve the security performance of battery.
Specific embodiment
Discarded rice husk is collected, is cleaned and is placed at 120~130 DEG C dry 2~3h, then stood and be cooled to room temperature,
Dry rice husk is placed in ball-milling device, 3~5h of ball milling at 250~300r/min, after the completion of ball milling, crosses 120 meshes, receive
Collect to obtain rice husk powder;The rice husk powder of above-mentioned preparation is placed in vacuum pyrolysis device, leads to nitrogen and excludes air, be subsequently vacuumed out
To 3.5~4.0kPa, 550~600 DEG C, after heat preservation is pyrolyzed 10~15min are warming up to pyrolysis oven by 10 DEG C/min, furnace cooling
To room temperature, it is prepared into pyrolysis rice hull ash;1:5 in mass ratio mixes pyrolysis rice hull ash with 10% hydrochloric acid solution of mass fraction,
Under 200~300W after 10~15min of ultrasonic disperse, filter cake, then 1:5 in mass ratio are filtered and collect, by filter cake and mass fraction
20% sodium hydroxide is stirred 25~30min, and 10~15min of ultrasonic disperse, is prepared into mixed dispersion liquid at 200~300W;
According to parts by weight, the mixed dispersion liquid of 45~50 parts of above-mentioned preparations, 10~15 parts of 10% hydrochloric acid of mass fraction and 5 are weighed respectively
~8 parts of neopelexes are placed in a beaker, and are stirred 25~30min at 45~50 DEG C;After the completion of to be mixed, then
It is centrifugated at 2500~3000r/min, collects lower sediment and be placed in Muffle furnace, led to argon gas and exclude air, 1400
3~5h of calcination processing at~1500 DEG C, cools to room temperature with the furnace, collects calcining mixt and is placed in ball grinder, 250~
3~5h of ball milling under 300r/min crosses 200 meshes, can be prepared into a kind of high conjugation lithium battery carbon silicium cathode material.
Example 1
Discarded rice husk is collected, is cleaned and is placed at 120 DEG C dry 2h, then stood and be cooled to room temperature, by drying of rice
Shell is placed in ball-milling device, the ball milling 4h at 250r/min, after the completion of ball milling, is crossed 120 meshes, is collected to obtain rice husk powder;It will
The rice husk powder of above-mentioned preparation is placed in vacuum pyrolysis device, is led to nitrogen and is excluded air, is subsequently vacuumed out to 3.5kPa, by 10
DEG C/min is warming up to 550 DEG C to pyrolysis oven, after heat preservation pyrolysis 10min, cools to room temperature with the furnace, be prepared into pyrolysis rice hull ash;It presses
Mass ratio 1:5 mixes pyrolysis rice hull ash with 10% hydrochloric acid solution of mass fraction, at 200W after ultrasonic disperse 10min, filtering
And filter cake is collected, then 1:5 in mass ratio, filter cake and 20% sodium hydroxide of mass fraction are stirred 20min, surpassed at 200W
Sound disperses 10min, is prepared into mixed dispersion liquid;According to parts by weight, respectively weigh 45 parts of above-mentioned preparations mixed dispersion liquid, 10
Part 10% hydrochloric acid of mass fraction and 5 parts of neopelexes are placed in a beaker, and are stirred 25min at 45 DEG C;It is to be mixed
After the completion, then at 2500r/min it is centrifugated, collects lower sediment and be placed in Muffle furnace, lead to argon gas and exclude air,
Calcination processing 3h at 1400 DEG C cools to room temperature with the furnace, collects calcining mixt and is placed in ball grinder, the ball at 250r/min
3h is ground, 200 meshes is crossed, a kind of high conjugation lithium battery carbon silicium cathode material can be prepared into.
By the resulting high conjugation lithium battery carbon silicium cathode material of the present invention and conductive agent acetylene black, binder PVDF with 6:
The uniform quality of 1:1 mixes, and in the environment of ambient humidity is 10%, is applied on copper foil simultaneously by solvent of N-Methyl pyrrolidone
It is dried under heat lamp, is subsequently transferred to dry 20h in 120 DEG C of baking oven, is placed under tablet press machine and is compacted with 10MPa, and be cut into
The electrode slice of 0.6cm × 0.6cm, using lithium piece as negative electrode: ethylene carbonate: dimethyl carbonate: methyl ethyl carbonate=1:1:8 is
Electrolyte can be made into lithium half-cell in the glove box full of argon gas.Through detecting, the resulting high conjugation lithium battery of the present invention
The specific capacity of carbon silicium cathode material is 500mAh/g, and obtained lithium ion battery voltage is 4V, energy 160Wh/kg, and is had
There is excellent cycle performance, is recycled 60 times, capacity retention ratio 98%.
Example 2
Discarded rice husk is collected, is cleaned and is placed at 130 DEG C dry 3h, then stood and be cooled to room temperature, by drying of rice
Shell is placed in ball-milling device, the ball milling 5h at 300r/min, after the completion of ball milling, is crossed 120 meshes, is collected to obtain rice husk powder;It will
The rice husk powder of above-mentioned preparation is placed in vacuum pyrolysis device, is led to nitrogen and is excluded air, is subsequently vacuumed out to 4.0kPa, by 10
DEG C/min is warming up to 600 DEG C to pyrolysis oven, after heat preservation pyrolysis 15min, cools to room temperature with the furnace, be prepared into pyrolysis rice hull ash;It presses
Mass ratio 1:5 mixes pyrolysis rice hull ash with 10% hydrochloric acid solution of mass fraction, at 300W after ultrasonic disperse 15min, filtering
And filter cake is collected, then 1:5 in mass ratio, filter cake and 20% sodium hydroxide of mass fraction are stirred 30min, surpassed at 300W
Sound disperses 15min, is prepared into mixed dispersion liquid;According to parts by weight, respectively weigh 50 parts of above-mentioned preparations mixed dispersion liquid, 15
Part 10% hydrochloric acid of mass fraction and 8 parts of neopelexes are placed in a beaker, and are stirred 30min at 50 DEG C;It is to be mixed
After the completion, then at 3000r/min it is centrifugated, collects lower sediment and be placed in Muffle furnace, lead to argon gas and exclude air,
Calcination processing 5h at 1500 DEG C cools to room temperature with the furnace, collects calcining mixt and is placed in ball grinder, the ball at 300r/min
5h is ground, 200 meshes is crossed, a kind of high conjugation lithium battery carbon silicium cathode material can be prepared into.
By the resulting high conjugation lithium battery carbon silicium cathode material of the present invention and conductive agent acetylene black, binder PVDF with 8:
The uniform quality of 1:1 mixes, and in the environment of ambient humidity is 15%, is applied on copper foil simultaneously by solvent of N-Methyl pyrrolidone
It is dried under heat lamp, is subsequently transferred to dry for 24 hours in 120 DEG C of baking oven, is placed under tablet press machine and is compacted with 10MPa, and be cut into
The electrode slice of 0.8cm × 0.8cm, using lithium piece as negative electrode, ethylene carbonate: dimethyl carbonate: methyl ethyl carbonate=1:1:8 is
Electrolyte can be made into lithium half-cell in the glove box full of argon gas.Through detecting, the resulting high conjugation lithium battery of the present invention
The specific capacity of carbon silicium cathode material is 600mAh/g, and obtained lithium ion battery voltage is 5V, energy 180Wh/kg, and is had
There is excellent cycle performance, is recycled 70 times, capacity retention ratio 99%.
Example 3
Discarded rice husk is collected, is cleaned and is placed at 125 DEG C dry 3h, then stood and be cooled to room temperature, by drying of rice
Shell is placed in ball-milling device, the ball milling 4h at 275r/min, after the completion of ball milling, is crossed 120 meshes, is collected to obtain rice husk powder;It will
The rice husk powder of above-mentioned preparation is placed in vacuum pyrolysis device, is led to nitrogen and is excluded air, is subsequently vacuumed out to 3.7kPa, by 10
DEG C/min is warming up to 575 DEG C to pyrolysis oven, after heat preservation pyrolysis 13min, cools to room temperature with the furnace, be prepared into pyrolysis rice hull ash;It presses
Mass ratio 1:5 mixes pyrolysis rice hull ash with 10% hydrochloric acid solution of mass fraction, at 250W after ultrasonic disperse 12min, filtering
And filter cake is collected, then 1:5 in mass ratio, filter cake and 20% sodium hydroxide of mass fraction are stirred 27min, surpassed at 250W
Sound disperses 13min, is prepared into mixed dispersion liquid;According to parts by weight, respectively weigh 47 parts of above-mentioned preparations mixed dispersion liquid, 13
Part 10% hydrochloric acid of mass fraction and 7 parts of neopelexes are placed in a beaker, and are stirred 28min at 43 DEG C;It is to be mixed
After the completion, then at 2750r/min it is centrifugated, collects lower sediment and be placed in Muffle furnace, lead to argon gas and exclude air,
Calcination processing 4h at 1450 DEG C cools to room temperature with the furnace, collects calcining mixt and is placed in ball grinder, the ball at 275r/min
4h is ground, 200 meshes is crossed, a kind of high conjugation lithium battery carbon silicium cathode material can be prepared into.
By the resulting high conjugation lithium battery carbon silicium cathode material of the present invention and conductive agent acetylene black, binder PVDF with 7:
The uniform quality of 1:1 mixes, and in the environment of ambient humidity is 13%, is applied on copper foil simultaneously by solvent of N-Methyl pyrrolidone
It is dried under heat lamp, is subsequently transferred to dry 22h in 120 DEG C of baking oven, is placed under tablet press machine and is compacted with 10MPa, and be cut into
The electrode slice of 0.7cm × 0.7cm, using lithium piece as negative electrode, ethylene carbonate: dimethyl carbonate: methyl ethyl carbonate=1:1:8 is
Electrolyte can be made into lithium half-cell in the glove box full of argon gas.Through detecting, the resulting high conjugation lithium battery of the present invention
The specific capacity of carbon silicium cathode material be 550mAh/g, obtained lithium ion battery voltage be 4.5V, energy 170Wh/kg, and
With excellent cycle performance, it is recycled 65 times, capacity retention ratio 98.5%.
Claims (1)
1. a kind of preparation method of high conjugation lithium battery carbon silicium cathode material, it is characterised in that specific preparation step are as follows:
(1) discarded rice husk is collected, is cleaned and is placed at 120~130 DEG C dry 2~3h, then stood and be cooled to room temperature, it will
Dry rice husk is placed in ball-milling device, 3~5h of ball milling at 250~300r/min, after the completion of ball milling, is crossed 120 meshes, is collected
Obtain rice husk powder;
(2) the rice husk powder of above-mentioned preparation is placed in vacuum pyrolysis device, leads to nitrogen and exclude air, is subsequently vacuumed out to 3.5
~4.0kPa is warming up to 550~600 DEG C to pyrolysis oven by 10 DEG C/min, after heat preservation is pyrolyzed 10~15min, cools to room with the furnace
Temperature is prepared into pyrolysis rice hull ash;
(3) 1:5 in mass ratio mixes pyrolysis rice hull ash with 10% hydrochloric acid solution of mass fraction, the ultrasound point at 200~300W
After dissipating 10~15min, filter cake, then 1:5 in mass ratio are filtered and collected, filter cake and 20% sodium hydroxide of mass fraction are stirred mixed
25~30min is closed, 10~15min of ultrasonic disperse, is prepared into mixed dispersion liquid at 200~300W;
(4) according to parts by weight, the mixed dispersion liquid of 45~50 parts of above-mentioned preparations, 10~15 parts of mass fractions 10% are weighed respectively
Hydrochloric acid and 5~8 parts of neopelexes are placed in a beaker, and are stirred 25~30min at 45~50 DEG C;
(5) it after the completion of to be mixed, then is centrifugated at 2500~3000r/min, collects lower sediment and be placed in Muffle furnace,
Logical argon gas excludes air, and 3~5h of calcination processing at 1400~1500 DEG C cools to room temperature with the furnace, collects calcining mixt simultaneously
It is placed in ball grinder, 3~5h of ball milling at 250~300r/min, crosses 200 meshes, a kind of high conjugation lithium electricity can be prepared into
Pond carbon silicium cathode material.
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CN109768249B (en) * | 2019-01-04 | 2021-05-25 | 蜂巢能源科技有限公司 | Negative electrode material of lithium ion battery, preparation method of negative electrode material and lithium ion battery |
CN110713188A (en) * | 2019-10-18 | 2020-01-21 | 中国石油大学(华东) | Method for preparing silicon-carbon negative electrode material for lithium ion battery from rice hulls |
CN112635742A (en) * | 2020-12-29 | 2021-04-09 | 惠州锂威新能源科技有限公司 | Preparation method of carbon-silicon negative electrode material of lithium ion battery, negative electrode material and lithium ion battery |
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CN104009210A (en) * | 2014-05-04 | 2014-08-27 | 昆明理工大学 | Porous silicon/carbon composite material, and preparation method and application thereof |
CN104300124A (en) * | 2014-07-22 | 2015-01-21 | 电子科技大学 | Preparation method for silicon dioxide/carbon compound and application to lithium/sodium ion batteries |
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CN105932240A (en) * | 2016-05-11 | 2016-09-07 | 武汉科技大学 | Nano-silicon-carbon compound and preparation method and application thereof |
CN105977470A (en) * | 2016-07-06 | 2016-09-28 | 威胜集团有限公司 | Silicon dioxide active carbon composite material and preparation method thereof as well as lead-carbon battery |
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CN104009210A (en) * | 2014-05-04 | 2014-08-27 | 昆明理工大学 | Porous silicon/carbon composite material, and preparation method and application thereof |
CN105098183A (en) * | 2014-05-21 | 2015-11-25 | 长春市朗欢科技有限公司 | Preparation for carbon anode material of lithium ion battery by using rice hull as raw material |
CN104300124A (en) * | 2014-07-22 | 2015-01-21 | 电子科技大学 | Preparation method for silicon dioxide/carbon compound and application to lithium/sodium ion batteries |
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