CN103137952A - Lithium ion battery silicon-based composite anode material and preparation method thereof - Google Patents
Lithium ion battery silicon-based composite anode material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a lithium ion battery silicon-based composite anode material, which comprises the following steps: (1) mixing silicon powder, graphite, a dispersant and water to obtain slurry, wherein the average particle size D50 of the silicon powder and graphite is 380-500 nm; (2) performing spray granulation to obtain particles; (3) mixing a sodium carboxymethylcellulose aqueous solution with a mass volume concentration of 1.5-4.7 g/L with the particles, wherein the using amount of sodium carboxymethylcellulose is 1-3 wt% of the total amount of the silicon powder and the graphite, stirring, performing centrifugation separation, drying, sieving by using a sieve of more than 400 meshes to obtain the undersize. The invention also discloses a lithium ion battery silicon-based composite anode material prepared by the method, which has a high specific capacity, and good cycle performance.
Description
Technical field
The present invention relates to the battery electrode material field, relate in particular to a kind of silicon-based composite anode material for Li-ion battery and preparation method thereof.
Background technology
Along with the development of society's science and technology, people are increasing to the demand of high-energy-density, high power, long circulation life lithium ion battery.Negative material has important function for the raising of performance of lithium ion battery, at present the commercial Li-ion battery negative pole is generally graphite type material or with the material of carbon as matrix, its theoretical specific capacity is 372mAh/g, can't satisfy people to the demand of high-capacity electrode.Silicon and material are considered to a kind of up-and-coming negative material with its theoretical specific capacity up to 4200mAh/g, but silicium cathode larger bulk effect in process is taken off in the lithium embedding has seriously reduced its cycle performance.In order to overcome bulk effect, improve its cycle performance, the researcher has proposed the solutions such as nanometer, alloying and carbon coating, and these researchs can be alleviated volumetric expansion, improve cycle performance, the reduction irreversible capacity of silicon based anode material, improve efficient first.Yet when these improvement still fail to reach industrial the application, to the requirement of cycle performance and volumetric expansion restriction, its achievement that obtains in research is also far from industrialization.
Summary of the invention
Technical problem to be solved by this invention is in order to overcome the poor defective of existing composite material containing silicon cycle performance, provides that a kind of specific capacity is high, the silicon-based composite anode material for Li-ion battery of good cycle and preparation method thereof.
The present invention solves the problems of the technologies described above by the following technical programs.
The invention provides a kind of preparation method of silicon-based composite anode material for Li-ion battery, it comprises the steps:
(1) with silica flour, graphite, dispersant and water mixed-shaped form slurry, the average grain diameter D of wherein said silica flour and described graphite
50Be respectively 380-500nm;
(2) mist projection granulating gets particle;
(3) with the mass body volume concentrations be sodium carboxymethylcellulose (english abbreviation CMC) aqueous solution and the mixing of described particle of 1.5-4.7g/L; the consumption of wherein said sodium carboxymethylcellulose accounts for the 1-3wt% of described silica flour and described graphite total weight; stir; centrifugation; dry; cross the above sieve of 400 orders, extracting screen underflow gets final product.
In a better embodiment of the present invention, described preparation method's concrete operation step is:
Silica flour raw material, graphite raw material, described dispersant are mixed with water, and Ultrafine Grinding gets described slurry, the average grain diameter D of particle in described slurry
50Be 380-500nm;
2. mist projection granulating gets described particle;
3. described sodium carboxymethyl cellulose solution and described particle are mixed, stir, centrifugation, drying is crossed the above sieve of 400 orders, and extracting screen underflow gets final product.
Wherein, the consumption of described silica flour and described graphite is this area conventional amount used, and preferably the weight ratio of described silica flour and described graphite is 0.15-0.25: 1.
Wherein, described Ultrafine Grinding is the conventional lapping mode of this area, generally adopts ultra-fine ball milling.
Wherein, described graphite is the conventional graphite that uses in this area, is generally Delanium and/or native graphite.
Described dispersant is the conventional dispersant that uses in this area, is preferably one or more in PVP (english abbreviation PVP), sodium carboxymethylcellulose, polyvinyl alcohol (english abbreviation PVA) and polyethylene glycol (english abbreviation PEG); Be more preferably that the PVP of 5200-7200, sodium carboxymethylcellulose, the weight average molecular weight that weight average molecular weight is 5800-7200 are 5.8 * 10 for weight average molecular weight
4-8.5 * 10
4Polyvinyl alcohol and weight average molecular weight be 4700-6800 polyethylene glycol in one or more.
Described dispersant dosage is the conventional amount used of this area, and preferably, described dispersant accounts for the 2-5wt% of described silica flour and described graphite gross mass.
Preferably, the total mass ratio of the quality of described water and described silica flour, described graphite and described dispersant is 7.5-9: 1.
Described mist projection granulating is this area routine techniques, its charging rate and be the conventional parameter of this area into and out of the air port temperature; Preferably, the charging rate of described mist projection granulating is 3.6-4.6kg/h, and the intake air temperature of described mist projection granulating is 220-260 ℃, and described air outlet temperature is 100-130 ℃.
Preferably, the average grain diameter D50 of described particle is 5.7-6.7 μ m.
The stirring condition of this area routine is adopted in described stirring; Preferably, the time of described stirring is 2-3 hour, and the speed of described stirring is 80-100rpm.
The centrifugal condition of described centrifugal employing this area routine, preferably, described centrifugal speed is 4000-5000rpm.
Described drying is this area conventional drying mode, and preferably, the temperature of described drying is 80-100 ℃.
The average grain diameter D of prepared silicon-based composite anode material for Li-ion battery
50Be 6.2-7.5 μ m.
The present invention also provides a kind of silicon-based composite anode material for Li-ion battery that is made by above-mentioned preparation method.
Preferably, the average grain diameter D of described silicon-based composite anode material for Li-ion battery
50Be 6.2-7.5 μ m.
On the basis that meets this area general knowledge, above-mentioned each optimum condition, but combination in any namely get the preferred embodiments of the invention.
Agents useful for same of the present invention and raw material be commercially available getting all.
Positive progressive effect of the present invention is:
Obtained by the present invention that a kind of specific capacity is high, the silicon-based composite anode material for Li-ion battery of good cycle, its first discharge capacity surpass 800mAh/g, after charge and discharge cycles 100 times, capability retention is more than 91%.
Description of drawings
Fig. 1 is that the negative material that embodiment 1 obtains amplifies the scanning electron microscope (SEM) photograph of 3000 times.
Fig. 2 is the cyclic curve figure of the negative material that obtains of embodiment 3.
Embodiment
Mode below by embodiment further illustrates the present invention, but does not therefore limit the present invention among described scope of embodiments.The experimental technique of unreceipted actual conditions in the following example according to conventional method and condition, or is selected according to catalogue.
Ball mill in the present invention is available from the Wuxi prosperous powder equipment of celebrating Co., Ltd, and model is CXM-230 type nano level superfine ball mill;
Spray drying device is available from the super spray drying machinery of Wuxi City richness factory, and model is DIS-5 type Highspeedcentrifugingandsprayingdrier.
In following embodiment, sodium carboxymethylcellulose reaches chemical industry Co., Ltd available from Jiangyin City's perseverance, sticking sodium carboxymethylcellulose during commodity are by name; Polyvinyl alcohol is available from Guangzhou river in Henan Province Sheng chemical industry Co., Ltd, and commodity are called polyvinyl alcohol 1788; Polyethylene glycol is available from Nanjing WeiEr chemical engineering Co., Ltd, and commodity are called Macrogol 6000; PVP is available from upper nautical mile specialization industry science skill Co., Ltd, and commodity are called PVPK30; All the other are common commercial goods.
Embodiment 1
With silica flour (D
50=2.6 μ m) (available from Shanghai Shanshan Science and Technology Co., Ltd, commodity are called YT7-38, D for 125g, Delanium 500g
50=26 μ m), the 12.5g PVP mixes with 5L water, the average grain diameter D of Ultrafine Grinding 6 hours particle to the slurry
50Be 462nm, the charging rate that spray drying device is set is 3.6Kg/h, is respectively 260 ℃, 120 ℃ into and out of the air port temperature, with ball milling disposed slurry mist projection granulating, obtains average grain diameter D
50It is the spheric granules of 5.8 μ m, at room temperature it is mixed with the 4L sodium carboxymethyl cellulose solution, wherein sodium carboxymethylcellulose accounts for the 1wt% of silica flour and graphite total weight, stirred 2 hours under 80rpm, the particle that the 4000rpm centrifugation obtains divides through 90 ℃ of vacuumizes, 400 mesh sieves, obtains average grain diameter D
50It is the silica-based composite negative pole material (seeing Fig. 1) of 7.2 μ m.
The electrochemical property test method:
Utilize the performance of the silicon-based composite anode material for Li-ion battery of the present embodiment preparation for check, prepare lithium ion battery with this cell negative electrode material.
Negative material wherein: Super-P conductive agent: SBR binding agent: the weight ratio of CMC thickener is 93: 2: 2.5: 2.5, and add appropriate 1-METHYLPYRROLIDONE to mix, be coated on copper foil of affluxion body after stirring and oven dry 12 hours under vacuum.Be assembled into button cell with the lithium sheet after taking out in vacuum glove box, electrolyte is the LiPF that contains 1M
6EC-DEC (volume ratio is 1: 1) solution.Carry out under electro-chemical test constant temperature, voltage 0.005-2.0V, current density is 15mA/g.
Test result shows that the first discharge specific capacity of the silica-based composite negative pole material of preparation is 1113mAh/g, and the initial charge specific capacity is 979mAh/g, and enclosed pasture efficient is 88%, and the capability retention after 100 circulations is 91%.
Embodiment 2
With silica flour (D
50=2.6 μ m) (available from Shanghai Shanshan Science and Technology Co., Ltd, commodity are called MGS-2, D for 75g, native graphite 500g
50=18 μ m), the 17.3.g PVP mixes with 5L water, the average grain diameter D of Ultrafine Grinding 6 hours particle to the slurry
50Be 425nm, the charging rate that spray drying device is set is 3.9Kg/h, is respectively 220 ℃, 100 ℃ into and out of the air port temperature, with ball milling disposed slurry mist projection granulating, obtains average grain diameter D
50It is the spheric granules of 6.1 μ m, at room temperature it is mixed with the 4L sodium carboxymethyl cellulose solution, wherein sodium carboxymethylcellulose accounts for the 3wt% of silica flour and graphite total weight, 80rpm stirred 2 hours, the particle that the 4800rpm centrifugation obtains divides through 100 ℃ of vacuumizes, 400 mesh sieves, obtains average grain diameter D
50It is the silica-based composite negative pole material of 6.8 μ m.Electrochemical property test result with embodiment 1 shows, the first discharge specific capacity of the silica-based composite negative pole material of preparation is 850mAh/g, and the initial charge specific capacity is 757mAh/g, and enclosed pasture efficient is that 89%, 100 capability retention after circulation is 92%.
Embodiment 3
With silica flour (D
50=2.6 μ m) (available from Shanghai Shanshan Science and Technology Co., Ltd, commodity are called YT7-38, D for 100g, Delanium 500g
50=26 μ m) and the average grain diameter D of 30g polyvinyl alcohol Ultrafine Grinding 6 hours particle to the slurry in 5L water
50Be 492nm, the charging rate that spray drying device is set is 3.8Kg/h, is respectively 250 ℃, 110 ℃ into and out of the air port temperature, with ball milling disposed slurry mist projection granulating, obtains average grain diameter D
50It is the spheric granules of 5.8 μ m, at room temperature it is mixed with the 4L sodium carboxymethyl cellulose solution, wherein sodium carboxymethylcellulose accounts for the 2wt% of silica flour and graphite total weight, 100rpm stirred 2 hours, the particle that the 4600rpm centrifugation obtains divides through 100 ℃ of vacuumizes, 400 mesh sieves, obtains average grain diameter D
50It is the silica-based composite negative pole material of 6.2 μ m.Electrochemical property test with embodiment 1 the results are shown in Figure 2, and the first discharge specific capacity of the silica-based composite negative pole material of preparation is 998mAh/g, and the initial charge specific capacity is 888mAh/g, and enclosed pasture efficient is that 89%, 100 capability retention after circulation is 93%.
Embodiment 4
With silica flour (D
50=2.6 μ m) (available from Shanghai Shanshan Science and Technology Co., Ltd, commodity are called FSN-1, D for 125g, Delanium 500g
50=24 μ m), the 12.5g sodium carboxymethylcellulose mixes with 5L water, the average grain diameter D of Ultrafine Grinding 6 hours particle to the slurry
50Be 395nm, the charging rate that spray drying device is set is 4.3kg/h, is respectively 260 ℃, 130 ℃ into and out of the air port temperature, with ball milling disposed slurry mist projection granulating, obtains average grain diameter D
50It is the spheric granules of 5.7 μ m, at room temperature it is mixed with the 4L sodium carboxymethyl cellulose solution, wherein sodium carboxymethylcellulose accounts for the 3wt% of silica flour and graphite total weight, 85rpm stirred 2 hours, the particle that the 4000rpm centrifugation obtains divides through 100 ℃ of vacuumizes, 400 mesh sieves, obtains average grain diameter D
50It is the silica-based composite negative pole material of 6.3 μ m.Electrochemical property test result with embodiment 1 shows, the first discharge specific capacity of the silica-based composite negative pole material of preparation is 1080mAh/g, and the initial charge specific capacity is 940mAh/g, and enclosed pasture efficient is that 87%, 100 capability retention after circulation is 92%.
Embodiment 5
With silica flour (D
50=2.6 μ m) (available from Shanghai Shanshan Science and Technology Co., Ltd, commodity are called MSG-1, D for 100g, native graphite 500g
50=16 μ m), 12g polyvinyl alcohol, 12g sodium carboxymethylcellulose and 5L water mixes, the average grain diameter D of Ultrafine Grinding 8 hours particle to the slurry
50Be 458nm, the charging rate that spray drying device is set is 4.2kg/h, is respectively 250 ℃, 100 ℃ into and out of the air port temperature, with ball milling disposed slurry mist projection granulating, obtains average grain diameter D
50It is the spheric granules of 6.7 μ m, at room temperature it is mixed with the 4L sodium carboxymethyl cellulose solution, wherein sodium carboxymethylcellulose accounts for the 2wt% of silica flour and graphite total weight, 90rpm stirred 2.5 hours, the particle that the 5000rmp centrifugation obtains divides through 80 ℃ of vacuumizes, 400 mesh sieves, obtains average grain diameter D
50It is the silica-based composite negative pole material of 7.2 μ m.Electrochemical property test result with embodiment 1 shows, the first discharge specific capacity of the silica-based composite negative pole material of preparation is 1005mAh/g, and the initial charge specific capacity is 905mAh/g, and enclosed pasture efficient is that 90%, 100 capability retention after circulation is 94%.
Embodiment 6
With silica flour (D
50=2.6 μ m) (available from Shanghai Shanshan Science and Technology Co., Ltd, commodity are called FSN-1, D for 75g, Delanium 500g
50=24 μ m), 11.5g polyethylene glycol PEG and 5L water mixes, the average grain diameter D of Ultrafine Grinding 6 hours particle to the slurry
50Be 446 μ m, the charging rate that spray drying device is set is 3.9kg/h, is respectively 260 ℃, 110 ℃ into and out of the air port temperature, with ball milling disposed slurry mist projection granulating, obtains average grain diameter D
50It is the spheric granules of 6.5 μ m, at room temperature it is mixed with the 4L sodium carboxymethyl cellulose solution, wherein sodium carboxymethylcellulose accounts for the 2wt% of silica flour and graphite total weight, 100rpm stirred 2 hours, and the particle that the 4500rpm centrifugation obtains divides through 90 ℃ of vacuumizes, 400 mesh sieves and obtains average grain diameter D
50It is the silica-based composite negative pole material of 7.5 μ m.Electrochemical property test result with embodiment 1 shows, the first discharge specific capacity of the silica-based composite negative pole material of preparation is 832mAh/g, and the initial charge specific capacity is 740mAh/g, and enclosed pasture efficient is that 89%, 100 capability retention after circulation is 93%.
Embodiment 7
With silica flour (D
50=2.6 μ m) (available from Shanghai Shanshan Science and Technology Co., Ltd, commodity are called MSG-1, D for 110g, native graphite 500g
50=16 μ m), 18.3g PVP and 5L water mixes, the average grain diameter D of Ultrafine Grinding 6 hours particle to the slurry
50Be 428nm, the charging rate that spray drying device is set is 4.5kg/h, is respectively 250 ℃, 100 ℃ into and out of the air port temperature, with ball milling disposed slurry mist projection granulating, obtains average grain diameter D
50It is the spheric granules of 6.4 μ m, at room temperature it is mixed with the 4L sodium carboxymethyl cellulose solution, wherein sodium carboxymethylcellulose accounts for the 1wt% of silica flour and graphite total weight, 100rpm stirred 3 hours, the particle that the 4800rpm centrifugation obtains divides through 100 ℃ of vacuumizes, 400 mesh sieves, obtains average grain diameter D
50It is the silica-based composite negative pole material of 6.7 μ m.Electrochemical property test result with embodiment 1 shows, the first discharge specific capacity of the silica-based composite negative pole material of preparation is 1121mAh/g, and the initial charge specific capacity is 975mAh/g, and enclosed pasture efficient is that 87%, 100 capability retention after circulation is 91%.
Embodiment 8
With silica flour (D
50=2.6 μ m) (available from Shanghai Shanshan Science and Technology Co., Ltd, commodity are called YT7-38, D for 125g, Delanium 500g
50=26 μ m), 15.6g PVP, 15.6g polyvinyl alcohol and 5L water mixes, the average grain diameter D of Ultrafine Grinding 7 hours particle to the slurry
50Be 398nm, the charging rate that spray drying device is set is 4.6kg/h, is respectively 260 ℃, 110 ℃ into and out of the air port temperature, with ball milling disposed slurry mist projection granulating, obtains average grain diameter D
50It is the spheric granules of 5.9 μ m, at room temperature it is mixed with the 4L sodium carboxymethyl cellulose solution, wherein sodium carboxymethylcellulose accounts for the 3wt% of silica flour and graphite total weight, 80rpm stirred 2 hours, the particle that the 4000rpm centrifugation obtains divides through 100 ℃ of vacuumizes, 400 mesh sieves, obtains average grain diameter D
50It is the silica-based composite negative pole material of 6.5 μ m.Electrochemical property test result with embodiment 1 shows, the first discharge specific capacity of the silica-based composite negative pole material of preparation is 1107mAh/g, and the initial charge specific capacity is 974mAh/g, and enclosed pasture efficient is that 88%, 100 capability retention after circulation is 93%.
Embodiment 9
With silica flour (D
50=2.6 μ m) (available from Shanghai Shanshan Science and Technology Co., Ltd, commodity are called MSG-2, D for 75g, native graphite 500g
50=18 μ m), 23g PVP and 5L water mixes, the average grain diameter D of Ultrafine Grinding 8 hours particle to the slurry
50Be 488nm, the charging rate that spray drying device is set is 4.2kg/h, is respectively 220 ℃, 100 ℃ into and out of the air port temperature, with ball milling disposed slurry mist projection granulating, obtains average grain diameter D
50Be 6.5 μ m spheric granules, at room temperature it is mixed with the 4L sodium carboxymethyl cellulose solution, wherein sodium carboxymethylcellulose accounts for the 2wt% of silica flour and graphite total weight, 100rpm stirred 3 hours, the particle that the 5000rpm centrifugation obtains divides through 100 ℃ of vacuumizes, 400 mesh sieves, obtains average grain diameter D
50It is the silica-based composite negative pole material of 6.9 μ m.Electrochemical property test result with embodiment 1 shows, the first discharge specific capacity of the silica-based composite negative pole material of preparation is 842mAh/g, and the initial charge specific capacity is 749mAh/g, and enclosed pasture efficient is that 89%, 100 capability retention after circulation is 93%.
The comparative example 1
With silica flour (D
50=2.6 μ m) (available from Shanghai Shanshan Science and Technology Co., Ltd, commodity are called YT7-38, D for 125g, Delanium 500g
50=26 μ m), 12.5g PVP and 5L water mixes, the average grain diameter D of Ultrafine Grinding 6 hours particle to the slurry
50Be 462nm, the charging rate that spray drying device is set is 3.6kg/h, be respectively 260 ℃, 120 ℃ into and out of the air port temperature, with ball milling disposed slurry mist projection granulating, obtain spheric granules, 100 ℃ of vacuum drying chambers again, 400 mesh sieves divide the silica-based composite negative pole material that obtains average grain diameter D50 5.7 μ m.
Electrochemical property test result with embodiment 1 shows, the first discharge specific capacity of the silica-based composite negative pole material of preparation is 858mAh/g, and the initial charge specific capacity is 586mAh/g, and enclosed pasture efficient is that 68%, 100 capability retention after circulation is 62%.
The comparative example 2
With silica flour (D
50=2.6 μ m) (available from Shanghai Shanshan Science and Technology Co., Ltd, commodity are called YT7-38, D for 100g, Delanium 500g
50=26 μ m), 30g polyvinyl alcohol and 5L water mixes, the average grain diameter D of Ultrafine Grinding 6 hours particle to the slurry
50Be 485nm, the charging rate that spray drying device is set is 3.8kg/h, is respectively 250 ℃, 110 ℃ into and out of the air port temperature, with ball milling disposed slurry mist projection granulating, obtains spheric granules, 100 ℃ of vacuum drying chambers again, and 400 mesh sieves divide and obtain average grain diameter D
506.2 the silica-based composite negative pole material of μ m.
Electrochemical property test result with embodiment 1 shows, the first discharge specific capacity of the silica-based composite negative pole material of preparation is 1020mAh/g, and the initial charge specific capacity is 637mAh/g, and enclosed pasture efficient is that 62%, 100 capability retention after circulation is 61%.
Claims (10)
1. the preparation method of a silicon-based composite anode material for Li-ion battery, it comprises the steps:
(1) with silica flour, graphite, dispersant and water mixed-shaped form slurry, the average grain diameter D of wherein said silica flour and described graphite
50Be respectively 380-500nm;
(2) mist projection granulating gets particle;
(3) with the mass body volume concentrations be the aqueous solution and the mixing of described particle of the sodium carboxymethylcellulose of 1.5-4.7g/L; the consumption of wherein said sodium carboxymethylcellulose accounts for the 1-3wt% of described silica flour and described graphite total weight; stir; centrifugation; dry; cross the above sieve of 400 orders, extracting screen underflow gets final product.
2. preparation method as claimed in claim 1, is characterized in that, described preparation method carries out in the steps below: silica flour raw material, graphite raw material and described dispersant are mixed with water, and Ultrafine Grinding gets described slurry, the average grain diameter D of particle in described slurry
50Be 380-500nm; Carry out successively the step described in claim 1 (2) and step (3).
3. preparation method as claimed in claim 1, is characterized in that, the weight ratio of described silica flour and described graphite is 0.15-0.25: 1; Described dispersant accounts for the 2-5wt% of described silica flour and described graphite gross mass; The total mass ratio of the quality of described water and described silica flour, described graphite and described dispersant is 7.5-9: 1.
4. preparation method as claimed in claim 1 or 2, is characterized in that, described dispersant is one or more in PVP, sodium carboxymethylcellulose, polyvinyl alcohol and polyethylene glycol; Be preferably that the PVP of 5200-7200, sodium carboxymethylcellulose, the weight average molecular weight that weight average molecular weight is 5800-7200 are 5.8 * 10 for weight average molecular weight
4-8.5 * 10
4Polyvinyl alcohol and weight average molecular weight be 4700-6800 polyethylene glycol in one or more.
5. preparation method as claimed in claim 1 or 2, is characterized in that, the charging rate of described mist projection granulating is 3.6-4.6kg/h, and the intake air temperature of described mist projection granulating is 220-260 ℃, and the air outlet temperature of described mist projection granulating is 100-130 ℃.
6. preparation method as claimed in claim 1 or 2, is characterized in that, the average grain diameter D of described particle
50Be 5.7-6.7 μ m.
7. preparation method as claimed in claim 1 or 2, is characterized in that, the time of described stirring is 2-3 hour, and the speed of described stirring is 80-100rpm; Described centrifugal speed is 4000-5000rpm; The temperature of described drying is 80-100 ℃.
8. as the described preparation method of claim 1-7 any one, it is characterized in that the average grain diameter D of prepared silicon-based composite anode material for Li-ion battery
50Be 6.2-7.5 μ m.
9. silicon-based composite anode material for Li-ion battery that makes as any preparation method in claim 1-8.
10. silicon-based composite anode material for Li-ion battery as claimed in claim 9, is characterized in that, its average grain diameter D
50Be 6.2-7.5 μ m.
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| CN105655570A (en) * | 2016-04-01 | 2016-06-08 | 四川创能新能源材料有限公司 | Refining preparation method of nanoscale silicon powder material |
| WO2021128197A1 (en) * | 2019-12-26 | 2021-07-01 | 宁德新能源科技有限公司 | Negative electrode material, electrochemical device comprising same, and electronic device |
| WO2021128201A1 (en) * | 2019-12-26 | 2021-07-01 | 宁德新能源科技有限公司 | Negative electrode material, and electrochemical device and electronic device comprising same |
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| CN102244240A (en) * | 2011-06-15 | 2011-11-16 | 中南大学 | Lithium ion battery composite anode material and preparation method thereof |
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| CN102149654A (en) * | 2008-09-12 | 2011-08-10 | 法国原子能及替代能源委员会 | Process for preparing a silicon/carbon composite material, material thus prepared and electrode notably negative electrode comprising this material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105655570A (en) * | 2016-04-01 | 2016-06-08 | 四川创能新能源材料有限公司 | Refining preparation method of nanoscale silicon powder material |
| CN105655570B (en) * | 2016-04-01 | 2018-08-21 | 四川创能新能源材料有限公司 | A kind of method prepared by the fining of nano silicone powder material |
| WO2021128197A1 (en) * | 2019-12-26 | 2021-07-01 | 宁德新能源科技有限公司 | Negative electrode material, electrochemical device comprising same, and electronic device |
| WO2021128201A1 (en) * | 2019-12-26 | 2021-07-01 | 宁德新能源科技有限公司 | Negative electrode material, and electrochemical device and electronic device comprising same |
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