CN102340001A - Method for preparing high-specific-capacity silicon carbon and tin carbon composite anode material - Google Patents
Method for preparing high-specific-capacity silicon carbon and tin carbon composite anode material Download PDFInfo
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- CN102340001A CN102340001A CN2011102483614A CN201110248361A CN102340001A CN 102340001 A CN102340001 A CN 102340001A CN 2011102483614 A CN2011102483614 A CN 2011102483614A CN 201110248361 A CN201110248361 A CN 201110248361A CN 102340001 A CN102340001 A CN 102340001A
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- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title abstract description 18
- 239000010405 anode material Substances 0.000 title abstract description 5
- 239000002153 silicon-carbon composite material Substances 0.000 title abstract description 3
- 239000002733 tin-carbon composite material Substances 0.000 title abstract 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 39
- 239000010439 graphite Substances 0.000 claims abstract description 33
- 239000002245 particle Substances 0.000 claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 26
- 238000002360 preparation method Methods 0.000 claims abstract description 21
- 238000000498 ball milling Methods 0.000 claims abstract description 9
- 239000002131 composite material Substances 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 34
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 25
- 229910052744 lithium Inorganic materials 0.000 claims description 25
- 239000000463 material Substances 0.000 claims description 25
- 239000010406 cathode material Substances 0.000 claims description 18
- 239000000377 silicon dioxide Substances 0.000 claims description 17
- 235000013312 flour Nutrition 0.000 claims description 16
- QWJYDTCSUDMGSU-UHFFFAOYSA-N [Sn].[C] Chemical compound [Sn].[C] QWJYDTCSUDMGSU-UHFFFAOYSA-N 0.000 claims description 14
- 239000011521 glass Substances 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 238000001694 spray drying Methods 0.000 claims description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 4
- 229910052717 sulfur Inorganic materials 0.000 claims description 4
- 239000011593 sulfur Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000003595 mist Substances 0.000 claims description 2
- 239000011159 matrix material Substances 0.000 abstract description 6
- 238000009776 industrial production Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000002349 favourable effect Effects 0.000 abstract 1
- 230000004087 circulation Effects 0.000 description 10
- 150000001875 compounds Chemical class 0.000 description 10
- 238000005303 weighing Methods 0.000 description 10
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 239000005543 nano-size silicon particle Substances 0.000 description 7
- 229910052710 silicon Inorganic materials 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- 239000011881 graphite nanoparticle Substances 0.000 description 6
- 238000001132 ultrasonic dispersion Methods 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910013870 LiPF 6 Inorganic materials 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 229910018540 Si C Inorganic materials 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000011263 electroactive material Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- -1 ethyl carbonate ester Chemical class 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000011366 tin-based material Substances 0.000 description 1
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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 method for preparing a high-specific-capacity silicon carbon and tin carbon composite anode material. The method comprises the steps of: mixing expanded graphite and lithium-embedded active powder, then adding an obtained mixture into a ball mill, and performing ball milling for 1-24h at the rotation speed of 100-600r/min to obtain the composite anode material, wherein the mass fraction of the expanded graphite is 5-90%, and the mass fraction of the lithium-embedded active powder is 10-95%. Compared with the prior art, the composite anode material synthesized in the invention has the stable specific capacity being more than 800mAh/g; the lithium-embedded active particles uniformly distribute in the expanded graphite matrix; because of the electric conductivity and the elasticity of the expanded graphite which equivalently serves as an electroconductive elastic matrix, a favorable electric contact is formed and always kept between the lithium-embedded active particles and the expanded graphite, so that the speed in capacity attenuation is effectively slowed down; in addition, the method has the advantages of cheap and easily obtainable raw materials, simple preparation process, short flow, easily controllable process, and easiness for realizing industrial production.
Description
Technical field
The invention belongs to the preparation method of negative material, belong to the preparation method that preparation is used for the composite negative pole material of lithium battery especially.
Technical background
At present, produce the lithium ion battery that uses and mainly adopt the graphite-like negative material, but the theoretical embedding lithium capacity of graphite is 372mAh/g that reality has reached 370mAh/g, therefore, the graphite-like negative material has not almost had room for promotion on capacity.
The nearly more than ten years; Various novel high power capacity and high magnification negative material are developed; Wherein silica-based and tin-based material are owing to its high specific discharge capacity (theoretical specific capacity of silicon and tin is respectively 4200mAh/g and 990mAh/g) becomes the research focus; Yet these two kinds of materials are accompanied by serious volumetric expansion and contraction in the doff lithium process, cause the electroactive material powder of detached on the electrode, finally cause capacity attenuation.Wherein, Silicon, tin base cathode material are in application process; Generally be that silicon, tin and other inactive metals (like Fe, Al, Cu etc.) are formed alloy, disclose used as negative electrode of Li-ion battery silicon-aluminum/carbon composite and preparation method thereof like Chinese patent CN03116070.0; Or material evenly spread to form composite material (like Si-C, Si-TiN etc.) in other activity or the non-active material, the Si-C composite material and the preparation method of used as negative electrode of Li-ion battery height ratio capacity disclosed like Chinese patent CN02112180.X.
Though said method has been alleviated the capacity attenuation of silicon-based anode material to a certain extent; But all to be simple physics compound or pyrocarbon coats for its mechanism; All can not fundamentally suppress the bulk effect in the charge and discharge process, capacity still can the decay quickly along with the increase of cycle-index.
Summary of the invention
Technical problem to be solved by this invention provides and a kind ofly can suppress the height ratio capacity silicon-carbon of the bulk effect in the discharge process, the preparation method of tin carbon compound cathode materials.
The technical scheme of technical solution problem of the present invention is: a kind of preparation method who prepares height ratio capacity silicon-carbon, tin carbon compound cathode materials, promptly
After the active powder of expanded graphite and embedding lithium mixed, add in the ball mill ball milling 1-24h under the rotating speed of 100r/min-600r/min again, promptly obtain composite negative pole material; The mass fraction of described expanded graphite is 5～90%, and the mass fraction of the active powder of embedding lithium is 10～95%;
The particle diameter of described expanded graphite is 1～100um, and sulfur content is less than 0.03%.
The mass fraction of the active powder of preferred embedding lithium is 20～80%;
The active powder of described embedding lithium is silica flour, glass putty or both mixtures.
The particle diameter of described silica flour is 0.05～20 μ m, preferably 0.05～1 μ m; Purity is 70%～99.9%;
The particle diameter of described glass putty is 1～100um, and purity is 90～99.9%
A kind of preparation method who prepares height ratio capacity silicon-carbon, tin carbon compound cathode materials, promptly
The active powder of expanded graphite and embedding lithium is mixed, the powder that mixes is added in the dispersion liquid, the mass ratio of powder and dispersion liquid is between 1: 10～5: 5; Adopt supersonic wave cleaning machine in 40,000 hertz; Disperseed 0.1-12 hour, in 150～250 ℃ of spray dryings, mist flow is 500mL/ hour.The mass fraction of described expanded graphite is 5～90%, and the mass fraction of the active powder of embedding lithium is 10～95%; The powder that mixes and the mass ratio of dispersion liquid are 1: 5～50;
The particle diameter that described expanded graphite is is 1～10um, and sulfur content is less than 0.03%.
The mass fraction of the active powder of preferred embedding lithium is 20～80%;
The active powder of described embedding lithium is silica flour, glass putty or both mixtures.
The particle diameter of described silica flour is 0.05～20 μ m, preferably 0.05～1 μ m; Purity is 70%～99.9%;
The particle diameter of described glass putty is 1～10um, and purity is 90～99.9%
Described dispersion liquid is water, ethanol or both mixtures.
The present invention introduces expanded graphite in silicon, the tin base cathode material; As shown in Figure 1: the conductivity of utilizing the conductivity increase negative material of expanded graphite on the one hand; The compressibility of expanded graphite can be held the volumetric expansion in silicon, the tin particles embedding lithium process simultaneously; Greatly alleviate silicon, the tin base cathode powder of detached phenomenon in charge and discharge process, thereby obtain long-life negative material.This is simple for process, is convenient to suitability for industrialized production, and the gained material has good cycle performance.
The present invention compared with prior art has following characteristics:
1, the stabilization ratio capacity of the composite negative pole material that synthesizes of the present invention is greater than 800mAh/g; Embedding lithium active particle is evenly distributed in the expanded graphite matrix; Because the conductivity and the elasticity of expanded graphite; Expanded graphite just is equivalent to an electrically conductive elastic matrix, makes to form good electrical contact and maintenance always between embedding lithium active particle and expanded graphite, thus the speed of having slowed down capacity attenuation effectively.
2, raw material is cheap and easy to get, preparation technology is simple, flow process is short, process is controlled easily, easy realization of industrial production.
Description of drawings
Fig. 1 is a principle schematic of the present invention.
Fig. 2 is the capacity cyclical stability sketch map of the prepared silicon-carbon cathode material of the present invention.
Embodiment
Below in conjunction with embodiment the present invention is done detailed explanation.
Embodiment 1:
(1) negative material is synthetic
Take by weighing 4 gram silica flours (particle diameter 0.05 μ m) and 4 gram expanded graphites, add in the ball grinder, ball milling 6 hours under the rotating speed of 400r/min again must expanded graphite and the compound of silicon nanoparticle.
(2) volume test
The material of gained is mixed according to mass ratio with conductive agent acetylene black, binding agent PVDF (Kynoar) respectively at 80: 10: 10; With NMP (1-Methyl-2-Pyrrolidone) this mixture is modulated into slurry; Evenly be coated on the Copper Foil; 100 ℃ of vacuumize 24 hours makes Experimental cell and uses pole piece.With the lithium sheet is to electrode, and electrolyte is 1mol/L LiPF
6EC (ethyl carbonate ester)+DMC (dimethyl carbonate) (volume ratio 1: 1) solution, barrier film is the celgard2400 film, in being full of the glove box of argon gas atmosphere, is assembled into CR2025 type button cell.
Discharge capacity first of the present invention detects than according to the 0.1C discharge-rate, and the charging/discharging voltage scope is 0～1.5V.
Press the battery of present embodiment made, first discharge specific capacity has reached 1273mAh/g, still remains on 800mAh/g after 100 circulations.
Like Fig. 1, shown in 2, be the capacity cyclical stability sketch map of the prepared silicon-carbon cathode material of the embodiment of the invention.Wherein, Embedding lithium active particle is evenly distributed in the expanded graphite matrix; Because the conductivity and the elasticity of expanded graphite; Expanded graphite just is equivalent to an electrically conductive elastic matrix, makes to form good electrical contact and maintenance always between embedding lithium active particle and expanded graphite, thus the speed of having slowed down capacity attenuation effectively.And raw material is cheap and easy to get, preparation technology is simple, flow process is short, process is controlled easily, easy realization of industrial production.
Embodiment 2
Take by weighing 2 gram silica flours (particle diameter 0.1 μ m), 2 gram glass puttys and 4 gram expanded graphites, add in the ball grinder, ball milling is 24 hours under the rotating speed of 100r/min, gets composite negative pole material.
The specific capacity of gained material is according to step (2) test of embodiment 1, and first discharge specific capacity has reached 1052mAh/g, still remains on 593mAh/g after 100 circulations.
Embodiment 3
Take by weighing 0.8 gram silica flour (particle diameter 1 μ m) and 7.2 gram expanded graphites, add in the ball grinder, ball milling is 1 hour under the rotating speed of 600r/min.Get the compound of expanded graphite and silicon nanoparticle.
The specific capacity of gained material is according to step (2) test of embodiment 1, and first discharge specific capacity has reached 438mAh/g, still remains on 283mAh/g after 100 circulations.
Embodiment 4
Take by weighing 7.6 gram silica flours (particle diameter 0.05 μ m) and 0.4 gram expanded graphite, add in the ball grinder, ball milling is 5 hours under the rotating speed of 300r/min, gets the compound of expanded graphite and silicon nanoparticle.
The specific capacity of gained material is according to step (2) test of embodiment 1, and first discharge specific capacity reaches 1838mAh/g, still remains on 713mAh/g after 100 circulations.
Embodiment 5
Take by weighing 2 gram silica flours (particle diameter 20 μ m) and 6 gram expanded graphites, add in the ball grinder, ball milling is 12 hours under the rotating speed of 600r/min.Get the compound of expanded graphite and silicon nanoparticle.
The specific capacity of gained material is according to step (2) test of embodiment 1, and first discharge specific capacity has reached 838mAh/g, still remains on 583mAh/g after 100 circulations.
Embodiment 6
Take by weighing 5 gram glass puttys and 3 gram expanded graphites, add in the ball grinder, ball milling is 12 hours under the rotating speed of 600r/min.Get the compound of expanded graphite and tin particles.
The specific capacity of gained material is according to step (2) test of embodiment 1, and first discharge specific capacity has reached 653mAh/g, still remains on 517mAh/g after 100 circulations.
Embodiment 7:
Take by weighing 1 gram silica flour (particle diameter 0.05 μ m) and 7 gram expanded graphites, add 40 gram ethanol, ultrasonic dispersion is after 2 hours, and with the treating capacity spray drying of 500mL/h, baking temperature is 180 ℃, promptly gets the compound of expanded graphite and silicon nanoparticle.
The specific capacity of gained material is according to step (2) test of embodiment 1, and first discharge specific capacity reaches 437mAh/g, still remains on 286mAh/g after 100 circulations.
Embodiment 8
Take by weighing 6 gram silica flours (particle diameter 0.1 μ m) and 2 gram expanded graphites, add 40 gram ethanol and 60 gram water, ultrasonic dispersion is after 0.1 hour, and with the treating capacity spray drying of 500mL/h, baking temperature is 200 ℃, promptly gets the compound of expanded graphite and silicon nanoparticle.
The specific capacity of gained material is according to step (2) test of embodiment 1, and first discharge specific capacity reaches 1137mAh/g, still remains on 786mAh/g after 100 circulations.
Embodiment 9
Take by weighing 6 gram silica flours (particle diameter 20 μ m) and 2 gram expanded graphites, add 40 gram water, ultrasonic dispersion is after 12 hours, and with the treating capacity spray drying of 500mL/h, baking temperature is 250 ℃, promptly gets the compound of expanded graphite and silicon nanoparticle.
The specific capacity of gained material is according to step (2) test of embodiment 1, and first discharge specific capacity reaches 937mAh/g, still remains on 451mAh/g after 100 circulations.
Embodiment 10
Take by weighing 3 gram glass puttys and 5 gram expanded graphites, add 40 gram ethanol, ultrasonic dispersion is after 3 hours, and with the treating capacity spray drying of 500mL/h, baking temperature is 150 ℃, promptly gets the compound of expanded graphite and tin particles.
The specific capacity of gained material is according to step (2) test of embodiment 1, and first discharge specific capacity reaches 471mAh/g, still remains on 331mAh/g after 100 circulations.
Claims (10)
1. preparation method who prepares height ratio capacity silicon-carbon, tin carbon compound cathode materials, promptly
After the active powder of expanded graphite and embedding lithium mixed, add in the ball mill ball milling 1-24h under the rotating speed of 100r/min-600r/min again, promptly obtain composite negative pole material; The mass fraction of described expanded graphite is 5～90%, and the mass fraction of the active powder of embedding lithium is 10～95%.
2. a kind of preparation method who prepares height ratio capacity silicon-carbon, tin carbon compound cathode materials according to claim 1, it is characterized in that: the particle diameter of described expanded graphite is 1～100um, and sulfur content is less than 0.03%.
3. a kind of preparation method who prepares height ratio capacity silicon-carbon, tin carbon compound cathode materials according to claim 1 is characterized in that: the mass fraction of the active powder of embedding lithium is 20～80%.
4. a kind of preparation method who prepares height ratio capacity silicon-carbon, tin carbon compound cathode materials according to claim 1 is characterized in that: the active powder of described embedding lithium is silica flour, glass putty or both mixtures.
5. a kind of preparation method who prepares height ratio capacity silicon-carbon, tin carbon compound cathode materials according to claim 4 is characterized in that: the particle diameter of described silica flour is 0.05～20 μ m, preferably 0.05～1 μ m; Purity is 70%～99.9%;
The particle diameter of described glass putty is 1～100um, and purity is 90～99.9%.
6. preparation method who prepares height ratio capacity silicon-carbon, tin carbon compound cathode materials, promptly
The active powder of expanded graphite and embedding lithium is mixed, the powder that mixes is added in the dispersion liquid, the mass ratio of powder and dispersion liquid is between 1: 10～5: 5; Adopt supersonic wave cleaning machine in 40,000 hertz; Disperseed 0.1-12 hour, in 150～250 ℃ of spray dryings, mist flow is 500mL/ hour; The mass fraction of described expanded graphite is 5～90%, and the mass fraction of the active powder of embedding lithium is 10～95%; The powder that mixes and the mass ratio of dispersion liquid are 1: 5～50.
7. a kind of preparation method who prepares height ratio capacity silicon-carbon, tin carbon compound cathode materials according to claim 6, it is characterized in that: the particle diameter that described expanded graphite is is 1～10um, and sulfur content is less than 0.03%.
8. a kind of preparation method who prepares height ratio capacity silicon-carbon, tin carbon compound cathode materials according to claim 6 is characterized in that: the mass fraction of the active powder of embedding lithium is 20～80%.
9. a kind of preparation method who prepares height ratio capacity silicon-carbon, tin carbon compound cathode materials according to claim 1 is characterized in that: the active powder of described embedding lithium is silica flour, glass putty or both mixtures.
10. a kind of preparation method who prepares height ratio capacity silicon-carbon, tin carbon compound cathode materials according to claim 1 is characterized in that: the particle diameter of described silica flour is 0.05～20 μ m, preferably 0.05～1 μ m; Purity is 70%～99.9%;
The particle diameter of described glass putty is 1～10um, and purity is 90～99.9%;
Described dispersion liquid is water, ethanol or both mixtures.
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102623682A (en) * | 2012-04-12 | 2012-08-01 | 天津理工大学 | Process for producing silicon-based carbon composite material for lithium ion battery cathode |
| CN102832374A (en) * | 2012-09-18 | 2012-12-19 | 奇瑞汽车股份有限公司 | Tin-carbon composite material, preparation method thereof and lithium-ion battery |
| CN102832376A (en) * | 2012-08-13 | 2012-12-19 | 华南理工大学 | Preparation method for silicon carbon composite material for lithium ion battery negative electrode |
| 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 |
| CN103022453A (en) * | 2013-01-10 | 2013-04-03 | 上海中聚佳华电池科技有限公司 | Lithium ion battery negative electrode material Si@SiOx/graphene composite and preparation method thereof |
| CN103531758A (en) * | 2013-09-11 | 2014-01-22 | 安泰科技股份有限公司 | Nano metal tin and graphite composite negative electrode material and preparation method thereof |
| CN103560249A (en) * | 2013-10-18 | 2014-02-05 | 中国第一汽车股份有限公司 | Multi-component composite anode material and preparation method thereof |
| CN103972483A (en) * | 2013-01-29 | 2014-08-06 | 昭和电工株式会社 | Composite electrode material |
| CN104282897A (en) * | 2013-07-10 | 2015-01-14 | 中国科学院金属研究所 | Silicon-based nanometer composite anode material for lithium ion battery and preparation method of silicon-based nanometer composite anode material |
| CN104577045A (en) * | 2014-12-20 | 2015-04-29 | 江西正拓新能源科技股份有限公司 | Silicon-carbon composite material of lithium ion battery and preparation method of silicon-carbon composite material |
| CN105047868A (en) * | 2015-06-13 | 2015-11-11 | 田东 | Preparation method of high-capacity lithium battery anode material |
| CN105355870A (en) * | 2015-10-22 | 2016-02-24 | 清华大学深圳研究生院 | Expanded graphite and nano-silicon composite material, preparation method thereof, electrode plate and battery |
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| CN108682820A (en) * | 2018-05-23 | 2018-10-19 | 厦门高容新能源科技有限公司 | A kind of silicon-carbon composite cathode material and negative plate and preparation method thereof and lithium ion battery |
| CN109904433A (en) * | 2019-03-18 | 2019-06-18 | 山东星火科学技术研究院 | Large capacity fast charging and discharging graphene lithium ion battery and its synthesis technology |
| CN109950521A (en) * | 2019-04-01 | 2019-06-28 | 大连理工大学 | The super Unsteady Casting of laser prepares lithium ion battery tin-graphite combination electrode method |
| CN113636546A (en) * | 2021-07-19 | 2021-11-12 | 西安交通大学 | Composite graphite material and preparation method and application thereof |
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