CN103337605B - Method for preparing natural graphite cathode material of lithium ion battery by wet ball milling - Google Patents
Method for preparing natural graphite cathode material of lithium ion battery by wet ball milling Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000010406 cathode material Substances 0.000 title claims abstract description 18
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 14
- 229910021382 natural graphite Inorganic materials 0.000 title claims abstract description 14
- 238000000498 ball milling Methods 0.000 title abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 28
- 239000000047 product Substances 0.000 claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000013067 intermediate product Substances 0.000 claims abstract description 12
- 239000002270 dispersing agent Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 239000002002 slurry Substances 0.000 claims abstract description 8
- 238000005087 graphitization Methods 0.000 claims abstract 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 16
- 229910002804 graphite Inorganic materials 0.000 claims description 10
- 239000010439 graphite Substances 0.000 claims description 10
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 9
- 229910052744 lithium Inorganic materials 0.000 claims description 9
- 239000007773 negative electrode material Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 238000013467 fragmentation Methods 0.000 claims description 6
- 238000006062 fragmentation reaction Methods 0.000 claims description 6
- 239000000543 intermediate Substances 0.000 claims description 6
- 239000013081 microcrystal Substances 0.000 claims description 6
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- BNOODXBBXFZASF-UHFFFAOYSA-N [Na].[S] Chemical compound [Na].[S] BNOODXBBXFZASF-UHFFFAOYSA-N 0.000 claims description 2
- 239000003599 detergent Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 239000002245 particle Substances 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 3
- 239000000428 dust Substances 0.000 abstract description 2
- 239000013543 active substance Substances 0.000 abstract 1
- 238000005119 centrifugation Methods 0.000 abstract 1
- 239000007770 graphite material Substances 0.000 abstract 1
- 239000007791 liquid phase Substances 0.000 abstract 1
- 238000003825 pressing Methods 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- -1 neopelex Chemical compound 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- 229910001290 LiPF6 Inorganic materials 0.000 description 1
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000003913 materials processing Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- GBCAVSYHPPARHX-UHFFFAOYSA-M n'-cyclohexyl-n-[2-(4-methylmorpholin-4-ium-4-yl)ethyl]methanediimine;4-methylbenzenesulfonate Chemical compound CC1=CC=C(S([O-])(=O)=O)C=C1.C1CCCCC1N=C=NCC[N+]1(C)CCOCC1 GBCAVSYHPPARHX-UHFFFAOYSA-M 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
-
- 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 method for preparing the natural graphite cathode material of a lithium ion battery by wet ball milling. The method comprises the following steps of grinding natural graphite material to obtain an intermediate product; adding the intermediate product, water, dispersing agent and a grinding ball into a stirring ball mill for stirring and ball milling at a certain ratio; after the ball-milling slurry is subjected to centrifugation or filter pressing to obtain cathode active substance containing trace moisture; drying and carrying out cyclone separation to obtain tiny particles; according to the type of the raw material, and determining whether graphitization processing needs to be carried out to finally obtain the cathode material disclosed by the invention. Compared with the prior art, the method disclosed by the invention is characterized in that a liquid phase ball milling method is adopted, the material morphology can be greatly improved, the tap density of the material is improved, the processing performance in the electrode processing process is improved, the batch stability of the product is guaranteed, the material yield is improved, the production cost is lowered, the dust pollution on the environment is greatly reduced, and the method is simple to operate and has high production efficiency.
Description
Technical field
The present invention relates to a kind of method that wet ball grinding prepares natural graphite cathode material of lithium ion battery, be specifically related to a kind of natural graphite cathode material of lithium ion battery manufacture method.
Background technology
Lithium ion battery is ideal in the world at present is also the chargeable chemical cell that technology is the highest, compared with other batteries, lithium ion battery properties is more outstanding, have that volume is little, capacitance is large, voltage advantages of higher, lithium ion pond is mainly used in the aspects such as mobile phone, notebook computer, electric tool, electronic product at present, future will apply to the fields such as electric automobile, electric bicycle, space flight and aviation, military mobile communication facility and equipment, its demand by increasing, and is expected to present explosive growth in electric automobile field.
Lithium ion battery negative material is based on Carbon Materials, mainly contain native graphite and Delanium two kinds, native graphite and Delanium all need repeatedly to pulverize and spheroidization process it when being used as lithium cell cathode material, during but existing processing method is produced, raw material availability is lower, common product yield (stock utilization) only about 45%, and product pattern is also general, product batches is difficult to ensure to stablize, and the dust environmental pollution in production process is also more serious.Therefore improve the pattern of product and raw-material utilance, reduce and pollute and production cost, develop new preparation technology, very large facilitation can be produced to lithium battery industry.
Summary of the invention
Object of the present invention is exactly for the problem in prior art, provides a kind of preparation method of novel, natural graphite negative electrode material that quality is higher.Wet ball grinding prepares a method for natural graphite cathode material of lithium ion battery, comprises the following steps:
One, first natural graphite starting material is pulverized by one-time mechanical, and control the particle diameter of powder, obtain electrode material intermediate product;
Two, intermediate product and water, dispersant and mill ball are added agitating ball mill by a certain percentage, carry out stirring ball-milling with the rotating speed of 200 ~ 360rpm, Ball-milling Time is 15 ~ 300 minutes,
Three, by the slurry liquid part after ball milling in step 2, utilize mode that is centrifugal or press filtration, remove the most aqueous solution, obtain the negative electrode active material containing micro-moisture;
Four, the above-mentioned negative electrode active material containing micro-moisture is isolated fine particle wherein by cyclone separator after super-dry, obtain natural graphite negative electrode material.
Natural graphite starting material described in above-mentioned steps one refers to the one in natural flake graphite, natural micro crystal graphite, fixed carbon content >=95%.
The particle diameter of the intermediate product in above-mentioned steps one after pulverizing: D10 is 5 ~ 15 μm, and D99 is 30 ~ 50 μm.
The ratio of the intermediate product described in above-mentioned steps two and water, dispersant and mill ball is 1:(2 ~ 3): (1.5 ~ 3): (0.01 ~ 0.05).
Mill ball described in above-mentioned steps two is zirconium oxide balls, steel ball, agate abrading-ball, aluminium oxide abrading-ball or silicon nitride abrading-ball.
Dispersant described in above-mentioned steps two comprises any one or more than one the mixing in stearic acid, neopelex, lauryl sodium sulfate, polyvinyl alcohol, CMC, butadiene-styrene rubber Ruzhong.
Mode that is centrifugal or press filtration described in above-mentioned steps three kinds refers to one or more in the equipment such as employing horizontal type scraper centrifuger, suspended centrifuge, vertical type automatic unloading centrifugal machine or belt filter press, plate and frame type filter-press, membrane pressure filter.
Adopting centrifugal and mode that is press filtration can remove the moisture of in solution 90% ~ 97, is a kind of economic environmental protection, easily with the method for operation.But the mode removing moisture is not limited thereto.
The particle diameter of the negative material in above-mentioned steps four after sorting: D10 is 5 ~ 15 μm, and D99 is 30 ~ 50 μm
The preparation method of the present invention's carbon cathode material compared to existing technology, has following advantage:
1) preparation method of the present invention, raw material availability is higher, and product yield can reach 70 ~ 80%, and treatment process is simple, preparation method's environmental protection, and cost is lower;
2) obtained negative material granule-morphology is good, and tap density is high, and in lithium ion battery preparation process, materials processing performance is good, high comprehensive performance.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 1.
Fig. 2 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 2.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described, but the present invention is not limited thereto.
Embodiment 1
By 100Kg natural flake graphite, (granular size is about 3mm, fixed carbon content is 97%), obtaining granularity D10 by pulverizer fragmentation is 10.56 μm, D99 is 36.71 μm of shape random negative material intermediate 94.3Kg, 200 kg of water and 200 kilograms of mill balls are added at agitating ball mill (500L), open stirring at low speed, add dispersant detergent alkylate sulphur sodium and each 1 kilogram of polyvinyl alcohol again, finally negative material intermediate product is poured in mixer, open high-speed stirred, rotating speed is 240rpm, stop after 90 minutes stirring, scraper-type centrifuge is utilized by slurry to carry out centrifugal, after wherein most water removes, obtain the negative electrode active material containing micro-moisture, and then adopt and to be dried with the drying device of cyclone separator and tiny powder in being separated, obtain lithium cell cathode material finished product 75.2Kg, product yield reaches 75.2%.
Embodiment 2
By the natural scale micro crystal graphite of 100 Kg (about granular size 1.5cm, fixed carbon content is 95%), obtaining granularity D10 by pulverizer fragmentation is 7.43 μm, D99 is 26.37 μm of random negative material intermediates of shape, 200 kg of water and 180 kilograms of mill balls are added at agitating ball mill (500L), open stirring at low speed, add dispersant sodium cellulose glycolate 1.5 kilograms again, finally negative material intermediate product is added in mixer, open high-speed stirred, rotating speed is 280rpm, stop after 120 minutes stirring, plate and frame type filter-press is utilized by slurry to carry out press filtration process, after wherein most water removes, obtain the negative electrode active material containing micro-moisture, and then adopt and to be dried with the drying device of cyclone separator and tiny powder in being separated, obtain lithium cell cathode material finished product 71.4Kg, product yield reaches 71.4%.
Embodiment 3
By the natural micro crystal graphite of 100 kg (about granular size 1mm), obtaining granularity D10 by pulverizer fragmentation is 11.96 μm, D99 is 38.27 μm of random negative material intermediates of shape, 210 kg of water and 200 kilograms of mill balls are added at agitating ball mill (500L), open stirring at low speed, add dispersant sodium cellulose glycolate 1 kilogram again, finally negative material intermediate product is added in mixer, open high-speed stirred, rotating speed is 300rpm, stop after 120 minutes stirring, plate and frame type filter-press is utilized by slurry to carry out press filtration process, and then adopt and to be dried with the drying device of cyclone separator and tiny powder in being separated, obtain lithium cell cathode material finished product 72.1Kg, product yield reaches 72.1%.
Comparative example 1
By the natural scale crystallite 100kg of weight same in embodiment 1, adopting common production technology, by repeatedly pulverizing and nodularization and sorting operation, obtaining the negative material be more or less the same in particle diameter and embodiment 1, obtain finished product 58.1 Kg altogether, product yield reaches 58.1%.
Comparative example 2
By the natural scale crystallite 100kg of weight same in embodiment 2, adopting common production technology, by repeatedly pulverizing and nodularization and sorting operation, obtaining the negative material be more or less the same in particle diameter and embodiment 2, obtain finished product 50.8 Kg altogether, product yield reaches 50.8%.
Comparative example 3
By the natural micro crystal graphite 100kg of weight same in embodiment 3, adopting common production technology, by repeatedly pulverizing and nodularization and sorting operation, obtaining the negative material be more or less the same in particle diameter and embodiment 3, obtain finished product 52.3 Kg altogether, product yield reaches 52.3%.
The physical property of the negative material obtained by inspection the present invention, adopt following detecting instrument and detection method (table one), detection architecture is in table two:
Table one: physical property detecting instrument and detection method
The electrical property of the negative material obtained by inspection the present invention, test by half-cell method of testing, negative material with above embodiment and comparative example: acetylene black: PVDF(Kynoar)=93: 3: 4(weight ratio), add appropriate NMP(N-methyl pyrrolidone) furnishing pulpous state, coat on Copper Foil, within 8 hours, make negative plate through vacuum 110 DEG C of dryings; Be to electrode with metal lithium sheet, electrolyte is 1mol/L LiPF6/EC+DEC+DMC=1: 1: 1, and microporous polypropylene membrane is barrier film, is assembled into battery.Charging/discharging voltage is 0 ~ 2.0V, and charge-discharge velocity is 0.2C, carries out testing to battery performance.Detection architecture is in table two.
Table two: physical property and electrical property testing result
Known by the analysis of embodiment 1 and comparative example 1, embodiment 2 and comparative example 2, embodiment 3 and comparative example 3, through the negative material that the inventive method is obtained, the negative material that its performance and conventional production technology are produced does not have bigger difference, even part physical index is better than the negative material that conventional production technology is produced, and adopts the production technology of its rate of finished products of negative material obtained by the method all than conventional much higher.
More than show and describe general principle of the present invention, principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (1)
1. wet ball grinding prepares a method for natural graphite cathode material of lithium ion battery, comprises the following steps:
By 100Kg natural flake graphite, obtaining granularity D10 by pulverizer fragmentation is 10.56 μm, D99 is 36.71 μm of shape random negative material intermediate 94.3Kg, 200 kg of water and 200 kilograms of mill balls are added at agitating ball mill, open stirring at low speed, add dispersant detergent alkylate sulphur sodium and each 1 kilogram of polyvinyl alcohol again, finally negative material intermediate product is poured in mixer, open high-speed stirred, rotating speed is 240rpm, stop after 90 minutes stirring, scraper-type centrifuge is utilized by slurry to carry out centrifugal, after wherein most water removes, obtain the negative electrode active material containing micro-moisture, and then adopt and to be dried with the drying device of cyclone separator and tiny powder in being separated, obtain lithium cell cathode material finished product 75.2Kg.
2. wet ball grinding prepares a method for natural graphite cathode material of lithium ion battery, comprises the following steps:
By the natural scale micro crystal graphite of 100 Kg, obtaining granularity D10 by pulverizer fragmentation is 7.43 μm, D99 is 26.37 μm of random negative material intermediates of shape, 200 kg of water and 180 kilograms of mill balls are added at agitating ball mill, open stirring at low speed, add dispersant sodium cellulose glycolate 1.5 kilograms again, finally negative material intermediate product is added in mixer, open high-speed stirred, rotating speed is 280rpm, stop after 120 minutes stirring, plate and frame type filter-press is utilized by slurry to carry out press filtration process, after wherein most water removes, obtain the negative electrode active material containing micro-moisture, and then adopt and to be dried with the drying device of cyclone separator and tiny powder in being separated, and then carry out graphitization processing, obtain lithium cell cathode material finished product 71.4Kg.
3. wet ball grinding prepares a method for natural graphite cathode material of lithium ion battery, comprises the following steps:
By the natural micro crystal graphite of 100 kg, obtaining granularity D10 by pulverizer fragmentation is 11.96 μm, D99 is 38.27 μm of random negative material intermediates of shape, 210 kg of water and 200 kilograms of mill balls are added at agitating ball mill, open stirring at low speed, add dispersant sodium cellulose glycolate 1 kilogram again, finally negative material intermediate product is added in mixer, open high-speed stirred, rotating speed is 300rpm, stop after 120 minutes stirring, plate and frame type filter-press is utilized by slurry to carry out press filtration process, and then adopt and to be dried with the drying device of cyclone separator and tiny powder in being separated, and then carry out graphitization processing, obtain lithium cell cathode material finished product 72.1Kg.
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| CN103811759A (en) * | 2014-02-20 | 2014-05-21 | 深圳市贝特瑞新能源材料股份有限公司 | Modification method of natural graphite ball-milling machinery and modified natural graphite anode material |
| CN104022303B (en) * | 2014-05-08 | 2016-01-06 | 景德镇陶瓷学院 | A kind of 8YSZ electrolyte thin membrane preparation method of anode support type intermediate temperature SOFC monocell |
| CN110061237A (en) * | 2019-04-25 | 2019-07-26 | 广东工业大学 | A kind of amorphous carbon cell negative electrode material and its preparation method and application |
| CN111874901A (en) * | 2020-07-31 | 2020-11-03 | 广东凯金新能源科技股份有限公司 | Method for manufacturing long-circulating graphite |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1635650A (en) * | 2003-12-26 | 2005-07-06 | 比亚迪股份有限公司 | A negative electrode graphite material for lithium-ion secondary battery and preparation method thereof |
| CN102185135A (en) * | 2011-04-13 | 2011-09-14 | 华南理工大学 | Preparation method of tin carbon composite material for negative electrode of lithium ion batteries |
| CN103022492A (en) * | 2012-11-28 | 2013-04-03 | 上海锦众信息科技有限公司 | Method for preparing improved negative-pole graphite composite material for lithium ion battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1635650A (en) * | 2003-12-26 | 2005-07-06 | 比亚迪股份有限公司 | A negative electrode graphite material for lithium-ion secondary battery and preparation method thereof |
| CN102185135A (en) * | 2011-04-13 | 2011-09-14 | 华南理工大学 | Preparation method of tin carbon composite material for negative electrode of lithium ion batteries |
| CN103022492A (en) * | 2012-11-28 | 2013-04-03 | 上海锦众信息科技有限公司 | Method for preparing improved negative-pole graphite composite material for lithium ion battery |
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