CN102887504A - Method for preparing carbon material for lithium ion battery cathode - Google Patents
Method for preparing carbon material for lithium ion battery cathode Download PDFInfo
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- CN102887504A CN102887504A CN2012103576606A CN201210357660A CN102887504A CN 102887504 A CN102887504 A CN 102887504A CN 2012103576606 A CN2012103576606 A CN 2012103576606A CN 201210357660 A CN201210357660 A CN 201210357660A CN 102887504 A CN102887504 A CN 102887504A
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- Prior art keywords
- graphite
- powder
- ion battery
- carbon material
- lithium ion
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- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 23
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 17
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 90
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 73
- 239000010439 graphite Substances 0.000 claims abstract description 73
- 239000000843 powder Substances 0.000 claims abstract description 40
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 15
- 239000012535 impurity Substances 0.000 claims abstract description 13
- 239000002356 single layer Substances 0.000 claims abstract description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 6
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910002091 carbon monoxide Inorganic materials 0.000 claims abstract description 5
- 230000010355 oscillation Effects 0.000 claims abstract description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 4
- 239000002131 composite material Substances 0.000 claims description 16
- 229910052799 carbon Inorganic materials 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 10
- 238000012545 processing Methods 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000000151 deposition Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000005229 chemical vapour deposition Methods 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 4
- 239000013543 active substance Substances 0.000 claims description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 238000005087 graphitization Methods 0.000 claims description 4
- 239000010410 layer Substances 0.000 claims description 4
- 238000012986 modification Methods 0.000 claims description 4
- 230000004048 modification Effects 0.000 claims description 4
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 4
- 238000005554 pickling Methods 0.000 claims description 4
- 238000002203 pretreatment Methods 0.000 claims description 4
- 238000010298 pulverizing process Methods 0.000 claims description 4
- 239000001117 sulphuric acid Substances 0.000 claims description 4
- 235000011149 sulphuric acid Nutrition 0.000 claims description 4
- 230000001351 cycling effect Effects 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- 239000010409 thin film Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229910013870 LiPF 6 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- -1 ethyl carbonate ester Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 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 carbon material for a lithium ion battery cathode. The method comprises the following steps of: quickly immersing graphite in a concentrated sulfuric acid or concentrated nitric acid solution after being heated, adding a surface active agent to carry out ultrasonic oscillation, enabling the graphite to be fully oxidized and separated, restoring the product then, forming high-yield single-layer graphite, and then smashing a single-layer graphite ball into powder graphite; acid-washing the powder graphite in the concentrated sulfuric acid solution after being treated in a sodium hydroxide solution, and then water washing and drying; modifying the graphite powder after removing impurities; carrying out surface reduction treatment for modified powder graphite in an atmosphere of carbon monoxide gas; and carrying out thin-film treatment for the graphite powder after the reduction treatment. The carbon material for lithium ion battery cathode, which is prepared by the method, has the advantages that the conductivity and the cycling stability are good, the capacity is high when being used in the lithium ion battery, and the service life is long.
Description
Technical field
The present invention relates to a kind of ion cathode material lithium preparation method, relate in particular to a kind of preparation method of used as negative electrode of Li-ion battery carbon material.
Background technology
Lithium ion battery is because its energy density is high, and good cycle has been widely used since its commercialization, has replaced gradually traditional chemical power sources such as lead-acid cell.Particularly along with day by day the highlighting of energy and environment problem, New Energy Industry has obtained increasing attention.
Lithium ion battery mainly is made of positive pole, negative pole, barrier film and electrolytic solution, can the negative material that wherein prepare energy density height, power density height, have extended cycle life, cost is low be one of most active branch of this research direction, also is that can the restriction lithium ion battery continue to the determinative of the high-tech areas such as hybrid vehicle, space flight and aviation development.
The carbon materials such as graphite are as lithium ion battery negative material, and in use exist at present: poor with solvent compatibility, high-rate performance is poor, and the common embedding because of solvent molecule during first charge-discharge is peeled off carbon-coating, and reduce electrode life.The negative pole that this external cause charge and discharge cycles causes can cause the reduction of this carbon material electroconductibility with the micronization of carbon material.
Therefore, in the urgent need to a kind of good conductivity is provided, circulation ability is strong, the lithium ion battery negative pole carbon material that the life-span is long.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of used as negative electrode of Li-ion battery carbon material uses the lithium ion battery of the carbon material for negative electrode of the method preparation to have the characteristics such as good conductivity, capacity height, long service life.
To achieve these goals, the preparation method of a kind of used as negative electrode of Li-ion battery carbon material provided by the invention comprises the steps:
Step 1, pre-treatment graphite
Graphite heating is immersed rapidly after 100-300 ℃ in the vitriol oil or concentrated nitric acid solution below 10 ℃, add the tensio-active agent sonic oscillation, the abundant oxidation of graphite is separated, again product is reduced, namely forming the mono-layer graphite of high yield, then is the powder graphite of 5-10 μ m with mono-layer graphite ball mill pulverizing to particle diameter;
Step 2 is removed the impurity in the graphite
With powder graphite in 500-550 ℃ be to process 2-4 hour in the sodium hydroxide solution of 50-70% in concentration, in concentration is the sulphuric acid soln of 50-60%, carry out pickling again, then washing and dry is to remove the impurity in the powder graphite;
Step 3 is carried out modification to the graphite composite powder behind the removal impurity
Graphite composite powder and the nickel oxide that accounts for graphite quality 4-6% are mixed, put into carbide furnace, the heat-up rate of carbide furnace is set as 100 ℃/hour and begin heating, when reaching 1100 ℃, stop to heat up, under this temperature, kept 6 hours, then in 1500-1700 ℃ under nitrogen catalyzed graphitization 1-2 hour, obtain modified powder graphite;
Step 4 is reduced processing to the modified graphite powder
Under the atmosphere of CO (carbon monoxide converter) gas, in 500-700 ℃ modified powder graphite is carried out surface reduction and processed 2-4 hour;
Step 5 is carried out film to the graphite composite powder after the reduction processing and is processed
Adopt chemical Vapor deposition process, graphite composite powder after the reduction processing is carried out coating, making its surface coat last layer thickness is that the carbon of 1-2 μ m is to improve first coulombic efficiency, namely make lithium-ion electric negative pole pond carbon material, chemical vapor deposition conditions wherein: carbon source is the alkane of C1 ~ C5, depositing temperature is 700-900 ℃, and depositing time is 2-4 hour.
Wherein, carbon source described in the step 5 is preferably the alkane of C1 ~ C3, more preferably ethane.
The present invention also provides a kind of used as negative electrode of Li-ion battery carbon material of above-mentioned either method preparation.
The cathode of lithium battery carbon material of the present invention's preparation has good electroconductibility, cyclical stability, and when being used for lithium ion battery, capacity is high, long service life.
Embodiment
Embodiment one
Pre-treatment graphite
In the concentrated sulfuric acid solution that immerses rapidly after the graphite heating to 100 ℃ below 10 ℃, add the tensio-active agent sonic oscillation, the abundant oxidation of graphite is separated, again product is reduced, namely forming the mono-layer graphite of high yield, then is the powder graphite of 5 μ m with mono-layer graphite ball mill pulverizing to particle diameter.
Remove the impurity in the graphite
With powder graphite in 500 ℃ be to process 2 hours in 50% the sodium hydroxide solution in concentration, in concentration is 50% sulphuric acid soln, carry out pickling again, then washing and dry is to remove the impurity in the powder graphite.
Graphite composite powder behind the removal impurity is carried out modification
Graphite composite powder and the nickel oxide that accounts for graphite quality 4% are mixed, put into carbide furnace, the heat-up rate of carbide furnace is set as 100 ℃/hour and begin heating, when reaching 1100 ℃, stop to heat up, under this temperature, kept 6 hours, then in 1500 ℃ of catalyzed graphitizations 1 hour under nitrogen, obtain modified powder graphite.
The modified graphite powder is reduced processing
Under the atmosphere of CO (carbon monoxide converter) gas, in 500-700 ℃ modified powder graphite is carried out surface reduction and processed 2 hours.
Graphite composite powder after the reduction processing is carried out film to be processed
Adopt chemical Vapor deposition process, take ethane as carbon source, depositing temperature is 700 ℃, depositing time is 2 hours, graphite composite powder after reduction processed carries out coating, make its surface coat last layer thickness be the carbon of 1 μ m to improve first coulombic efficiency, namely make lithium-ion electric negative pole pond carbon material.
Embodiment two
Pre-treatment graphite
In the concentrated nitric acid solution that immerses rapidly after the graphite heating to 300 ℃ below 10 ℃, add the tensio-active agent sonic oscillation, the abundant oxidation of graphite is separated, again product is reduced, namely forming the mono-layer graphite of high yield, then is the powder graphite of 10 μ m with mono-layer graphite ball mill pulverizing to particle diameter.
Remove the impurity in the graphite
With powder graphite in 550 ℃ be to process 4 hours in 70% the sodium hydroxide solution in concentration, in concentration is 60% sulphuric acid soln, carry out pickling again, then washing and dry is to remove the impurity in the powder graphite.
Graphite composite powder behind the removal impurity is carried out modification
Graphite composite powder and the nickel oxide that accounts for graphite quality 6% are mixed, put into carbide furnace, the heat-up rate of carbide furnace is set as 100 ℃/hour and begin heating, when reaching 1100 ℃, stop to heat up, under this temperature, kept 6 hours, then in 1700 ℃ of catalyzed graphitizations 2 hours under nitrogen, obtain modified powder graphite.
The modified graphite powder is reduced processing
Under the atmosphere of CO (carbon monoxide converter) gas, in 700 ℃ modified powder graphite is carried out surface reduction and processed 4 hours.
Graphite composite powder after the reduction processing is carried out film to be processed
Adopt chemical Vapor deposition process, take ethane as carbon source, depositing temperature is 900 ℃, depositing time is 4 hours, graphite composite powder after reduction processed carries out coating, make its surface coat last layer thickness be the carbon of 2 μ m to improve first coulombic efficiency, namely make lithium-ion electric negative pole pond carbon material.
Comparative example
Graphite directly is ground into the powder of 10 μ m particle diameters, for subsequent use.
Adopt respectively embodiment one, two and the lithium ion battery negative pole carbon material of comparative example make the negative plate of same size, then make battery, electrolytic solution is 1.5mol/L LiPF
6EC(ethyl carbonate ester)+the DMC(dimethyl carbonate) (volume ratio 1: 1) solution, and under the condition of constant current 0.1C, carry out cycle performance test.This embodiment one with two material compare with the material of comparative example, first discharge specific capacity has promoted more than the 40-50%, cycle life has improved more than 1 times.
Claims (4)
1. the preparation method of a used as negative electrode of Li-ion battery carbon material is characterized in that, comprises the steps:
Step 1, pre-treatment graphite
Graphite heating is immersed rapidly after 100-300 ℃ in the vitriol oil or concentrated nitric acid solution below 10 ℃, add the tensio-active agent sonic oscillation, the abundant oxidation of graphite is separated, again product is reduced, namely forming the mono-layer graphite of high yield, then is the powder graphite of 5-10 μ m with mono-layer graphite ball mill pulverizing to particle diameter;
Step 2 is removed the impurity in the graphite
With powder graphite in 500-550 ℃ be to process 2-4 hour in the sodium hydroxide solution of 50-70% in concentration, in concentration is the sulphuric acid soln of 50-60%, carry out pickling again, then washing and dry is to remove the impurity in the powder graphite;
Step 3 is carried out modification to the graphite composite powder behind the removal impurity
Graphite composite powder and the nickel oxide that accounts for graphite quality 4-6% are mixed, put into carbide furnace, the heat-up rate of carbide furnace is set as 100 ℃/hour and begin heating, when reaching 1100 ℃, stop to heat up, under this temperature, kept 6 hours, then in 1500-1700 ℃ under nitrogen catalyzed graphitization 1-2 hour, obtain modified powder graphite;
Step 4 is reduced processing to the modified graphite powder
Under the atmosphere of CO (carbon monoxide converter) gas, in 500-700 ℃ modified powder graphite is carried out surface reduction and processed 2-4 hour;
Step 5 is carried out film to the graphite composite powder after the reduction processing and is processed
Adopt chemical Vapor deposition process, graphite composite powder after the reduction processing is carried out coating, making its surface coat last layer thickness is that the carbon of 1-2 μ m is to improve first coulombic efficiency, namely make lithium-ion electric negative pole pond carbon material, chemical vapor deposition conditions wherein: carbon source is the alkane of C1 ~ C5, depositing temperature is 700-900 ℃, and depositing time is 2-4 hour.
2. method according to claim 1 is characterized in that, carbon source described in the step 5 is the alkane of C1 ~ C3.
3. method according to claim 2 is characterized in that, carbon source described in the step 5 is ethane.
4. used as negative electrode of Li-ion battery carbon material of method preparation as claimed in claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201210357660.6A CN102887504B (en) | 2012-09-24 | 2012-09-24 | A kind of preparation method of carbon material for lithium ion battery cathode |
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| CN201210357660.6A CN102887504B (en) | 2012-09-24 | 2012-09-24 | A kind of preparation method of carbon material for lithium ion battery cathode |
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| CN102887504A true CN102887504A (en) | 2013-01-23 |
| CN102887504B CN102887504B (en) | 2016-08-17 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111439748A (en) * | 2020-03-12 | 2020-07-24 | 深圳市德方纳米科技股份有限公司 | Regenerated graphite material and preparation method thereof |
| CN111463438A (en) * | 2019-01-18 | 2020-07-28 | 中国科学院上海硅酸盐研究所 | Typha carbon lithium air battery positive electrode material and preparation method and application thereof |
| CN111792640A (en) * | 2020-07-31 | 2020-10-20 | 广东凯金新能源科技股份有限公司 | Spheroidal low-expansion high-capacity graphite negative electrode material, preparation method and lithium ion battery |
| CN112234171A (en) * | 2020-09-08 | 2021-01-15 | 中南大学 | Silicon-natural graphite composite material, application thereof and method for preparing silicon-natural graphite composite material by catalyzing with trace harmless impurities |
| CN112875697A (en) * | 2021-02-02 | 2021-06-01 | 广东凯金新能源科技股份有限公司 | High-energy-density low-temperature quick-charging artificial graphite material and preparation method thereof |
| US11702342B2 (en) | 2020-05-18 | 2023-07-18 | Ecograf Limited | Method of producing purified graphite |
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| CN101630737A (en) * | 2009-08-19 | 2010-01-20 | 河北理工大学 | Method for preparing tin-nickel alloy of cathode materials of lithium ion battery by electrolyzing melted salt |
| CN102544500A (en) * | 2012-03-22 | 2012-07-04 | 上海锦众信息科技有限公司 | Lithium ion battery cathode material and preparation method thereof |
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- 2012-09-24 CN CN201210357660.6A patent/CN102887504B/en not_active Expired - Fee Related
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| CN101320821A (en) * | 2007-06-04 | 2008-12-10 | 中南大学 | Energy storage device with both capacitor and lithium ion battery characteristics and manufacturing method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111463438A (en) * | 2019-01-18 | 2020-07-28 | 中国科学院上海硅酸盐研究所 | Typha carbon lithium air battery positive electrode material and preparation method and application thereof |
| CN111439748A (en) * | 2020-03-12 | 2020-07-24 | 深圳市德方纳米科技股份有限公司 | Regenerated graphite material and preparation method thereof |
| CN111439748B (en) * | 2020-03-12 | 2021-12-03 | 深圳市德方纳米科技股份有限公司 | Regenerated graphite material and preparation method thereof |
| US11702342B2 (en) | 2020-05-18 | 2023-07-18 | Ecograf Limited | Method of producing purified graphite |
| CN111792640A (en) * | 2020-07-31 | 2020-10-20 | 广东凯金新能源科技股份有限公司 | Spheroidal low-expansion high-capacity graphite negative electrode material, preparation method and lithium ion battery |
| CN111792640B (en) * | 2020-07-31 | 2022-05-06 | 广东凯金新能源科技股份有限公司 | Spheroidal low-expansion high-capacity graphite negative electrode material, preparation method and lithium ion battery |
| CN112234171A (en) * | 2020-09-08 | 2021-01-15 | 中南大学 | Silicon-natural graphite composite material, application thereof and method for preparing silicon-natural graphite composite material by catalyzing with trace harmless impurities |
| CN112875697A (en) * | 2021-02-02 | 2021-06-01 | 广东凯金新能源科技股份有限公司 | High-energy-density low-temperature quick-charging artificial graphite material and preparation method thereof |
| WO2022166058A1 (en) * | 2021-02-02 | 2022-08-11 | 广东凯金新能源科技股份有限公司 | High-energy-density low-temperature artificial graphite material for fast-charge and preparation method therefor |
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