CN102887504B - A kind of preparation method of carbon material for lithium ion battery cathode - Google Patents
A kind of preparation method of carbon material for lithium ion battery cathode Download PDFInfo
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- CN102887504B CN102887504B CN201210357660.6A CN201210357660A CN102887504B CN 102887504 B CN102887504 B CN 102887504B CN 201210357660 A CN201210357660 A CN 201210357660A CN 102887504 B CN102887504 B CN 102887504B
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- graphite
- powder
- lithium ion
- ion battery
- carbon
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 22
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 96
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 74
- 239000010439 graphite Substances 0.000 claims abstract description 74
- 239000000843 powder Substances 0.000 claims abstract description 42
- 239000002131 composite material Substances 0.000 claims abstract description 18
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000012535 impurity Substances 0.000 claims abstract description 13
- 239000002356 single layer Substances 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 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
- 238000005554 pickling Methods 0.000 claims abstract description 5
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 239000004094 surface-active agent Substances 0.000 claims abstract description 5
- 239000010409 thin film Substances 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
- 239000001117 sulphuric acid Substances 0.000 claims abstract description 3
- 235000011149 sulphuric acid Nutrition 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 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
- 238000000151 deposition 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
- 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
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 4
- 238000010298 pulverizing process Methods 0.000 claims description 4
- 238000003763 carbonization Methods 0.000 claims 1
- 230000008021 deposition Effects 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 10
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052744 lithium Inorganic materials 0.000 abstract description 3
- 238000000498 ball milling Methods 0.000 abstract 1
- 238000011946 reduction process Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229910001290 LiPF6 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
- 239000010408 film Substances 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
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 the preparation method of a kind of carbon material for lithium ion battery cathode, comprise the steps: in concentrated sulphuric acid rapid after graphite heating or concentrated nitric acid solution, add surfactant sonic oscillation, make the fully oxidized separation of graphite, again product is reduced, i.e. form the mono-layer graphite of high yield, then mono-layer graphite ball milling powder is broken into powder body graphite；After being processed in sodium hydroxide solution by powder body graphite, then sulfuric acid solution carries out pickling, then wash and be dried；Graphite composite powder after going the removal of impurity is modified；Under the atmosphere of CO (carbon monoxide converter) gas, modified powder graphite is carried out surface reduction process；Graphite composite powder after reduction treatment is carried out thin film process.Cathode of lithium battery material with carbon element prepared by the present invention, has good electric conductivity, cyclical stability, and when lithium ion battery, capacity is high, and service life is long.
Description
Technical field
The present invention relates to a kind of ion cathode material lithium preparation method, particularly relate to the preparation method of a kind of carbon material for lithium ion battery cathode.
Background technology
Lithium ion battery is high due to its energy density, and good cycle has had been obtained for being widely applied since its commercialization, gradually instead of the electrochmical power sources such as traditional lead-acid battery.In particular with day by day highlighting of energy and environment problem, New Energy Industry has obtained increasing attention.
Lithium ion battery is mainly made up of positive pole, negative pole, barrier film and electrolyte, can wherein prepare that energy density is high, power density high, have extended cycle life, the negative material of low cost be one of branch that this research direction is most active, is also that can restriction lithium ion battery continue the determiner to the development of the high-tech area such as hybrid vehicle, space flight and aviation.
The material with carbon elements such as graphite, as lithium ion battery negative material, the most in use exist: poor with solvent compatibility, high-rate performance is poor, and during first charge-discharge, the common embedding because of solvent molecule makes carbon-coating peeling-off, and electrode life reduces.The micronization of the negative pole carbon material that this exopathogenic factor charge and discharge cycles causes, may result in the reduction of this carbon material electric conductivity.
Therefore, in the urgent need to providing a kind of good conductivity, circulation ability is strong, the lithium ion battery negative pole carbon material of life-span length.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of carbon material for lithium ion battery cathode, the lithium ion battery of carbon material for negative electrode prepared by use the method has the features such as good conductivity, capacity height, length in service life.
To achieve these goals, the preparation method of a kind of carbon material for lithium ion battery cathode that the present invention provides comprises the steps:
Step 1, pretreating graphite
By in the concentrated sulphuric acid or the concentrated nitric acid solution that immerse rapidly less than 10 DEG C after graphite heating to 100-300 DEG C, add surfactant sonic oscillation, make the fully oxidized separation of graphite, again product is reduced, i.e. form the mono-layer graphite of high yield, then by powder body graphite that mono-layer graphite ball mill pulverizing to particle diameter is 5-10 μm；
Step 2, removes the impurity in graphite
Powder body graphite is processed 2-4 hour in 500-550 DEG C in the sodium hydroxide solution that concentration is 50-70%, then carries out pickling in the sulfuric acid solution that concentration is 50-60%, then wash and be dried, to remove the impurity in powder body graphite；
Step 3, is modified the graphite composite powder after going the removal of impurity
Graphite composite powder is mixed homogeneously with the nickel oxide accounting for graphite quality 4-6%, put in carbide furnace, the programming rate of carbide furnace is set as 100 DEG C/h begin to warm up, stop when reaching 1100 DEG C heating up, keep 6 hours at such a temperature, then in 1500-1700 DEG C of catalyzed graphitization 1-2 hour under a nitrogen, modified powder graphite is obtained；
Step 4, carries out reduction treatment to modified graphite powder body
Under the atmosphere of CO (carbon monoxide converter) gas, in 500-700 DEG C, modified powder graphite is carried out surface reduction and process 2-4 hour；
Step 5, carries out thin film process to the graphite composite powder after reduction treatment
Use chemical vapour deposition technique, graphite composite powder after reduction treatment is carried out peplos, making its Surface coating last layer thickness is that the carbon of 1-2 μm is to improve initial coulomb efficiency, i.e. prepare lithium-ion electric negative pole pond material with carbon element, wherein chemical vapor deposition conditions: carbon source is the alkane of C1 ~ C5, depositing temperature is 700-900 DEG C, and sedimentation time is 2-4 hour.
Wherein, carbon source described in step 5 is preferably the alkane of C1 ~ C3, more preferably ethane.
Present invention also offers carbon material for lithium ion battery cathode prepared by a kind of any of the above-described method.
Cathode of lithium battery material with carbon element prepared by the present invention, has good electric conductivity, cyclical stability, and when lithium ion battery, capacity is high, and service life is long.
Detailed description of the invention
Embodiment one
Pretreating graphite
By in the concentrated sulfuric acid solution immersing rapidly less than 10 DEG C after graphite heating to 100 DEG C, add surfactant sonic oscillation, make the fully oxidized separation of graphite, then product is reduced, i.e. form the mono-layer graphite of high yield, then by powder body graphite that mono-layer graphite ball mill pulverizing to particle diameter is 5 μm.
Remove the impurity in graphite
Powder body graphite is processed 2 hours in 500 DEG C in the sodium hydroxide solution that concentration is 50%, then carries out pickling in the sulfuric acid solution that concentration is 50%, then wash and be dried, to remove the impurity in powder body graphite.
Graphite composite powder after going the removal of impurity is modified
Graphite composite powder is mixed homogeneously with the nickel oxide accounting for graphite quality 4%, put in carbide furnace, the programming rate of carbide furnace is set as 100 DEG C/h begin to warm up, stop when reaching 1100 DEG C heating up, keep 6 hours at such a temperature, then in 1500 DEG C of catalyzed graphitization 1 hours under a nitrogen, modified powder graphite is obtained.
Modified graphite powder body is carried out reduction treatment
Under the atmosphere of CO (carbon monoxide converter) gas, in 500-700 DEG C, modified powder graphite is carried out surface reduction and process 2 hours.
Graphite composite powder after reduction treatment is carried out thin film process
Using chemical vapour deposition technique, with ethane as carbon source, depositing temperature is 700 DEG C, sedimentation time is 2 hours, graphite composite powder after reduction treatment is carried out peplos so that it is Surface coating last layer thickness be the carbon of 1 μm to improve initial coulomb efficiency, i.e. prepare lithium-ion electric negative pole pond material with carbon element.
Embodiment two
Pretreating graphite
By in the concentrated nitric acid solution immersing rapidly less than 10 DEG C after graphite heating to 300 DEG C, add surfactant sonic oscillation, make the fully oxidized separation of graphite, then product is reduced, i.e. form the mono-layer graphite of high yield, then by powder body graphite that mono-layer graphite ball mill pulverizing to particle diameter is 10 μm.
Remove the impurity in graphite
Powder body graphite is processed 4 hours in 550 DEG C in the sodium hydroxide solution that concentration is 70%, then carries out pickling in the sulfuric acid solution that concentration is 60%, then wash and be dried, to remove the impurity in powder body graphite.
Graphite composite powder after going the removal of impurity is modified
Graphite composite powder is mixed homogeneously with the nickel oxide accounting for graphite quality 6%, put in carbide furnace, the programming rate of carbide furnace is set as 100 DEG C/h begin to warm up, stop when reaching 1100 DEG C heating up, keep 6 hours at such a temperature, then in 1700 DEG C of catalyzed graphitization 2 hours under a nitrogen, modified powder graphite is obtained.
Modified graphite powder body is carried out reduction treatment
Under the atmosphere of CO (carbon monoxide converter) gas, in 700 DEG C, modified powder graphite is carried out surface reduction and process 4 hours.
Graphite composite powder after reduction treatment is carried out thin film process
Using chemical vapour deposition technique, with ethane as carbon source, depositing temperature is 900 DEG C, sedimentation time is 4 hours, graphite composite powder after reduction treatment is carried out peplos so that it is Surface coating last layer thickness be the carbon of 2 μm to improve initial coulomb efficiency, i.e. prepare lithium-ion electric negative pole pond material with carbon element.
Comparative example
Graphite is directly ground to the powder of 10 μm particle diameters, standby.
The lithium ion battery negative pole carbon material being respectively adopted embodiment one, two and comparative example makes the negative plate of same size, then makes battery, and electrolyte is 1.5mol/L LiPF6EC(ethyl carbonate ester)+DMC(dimethyl carbonate) (volume ratio 1: 1) solution, and be circulated performance test under conditions of constant current 0.1C.This embodiment one with two material compared with the material of comparative example, first discharge specific capacity improves more than 40-50%, and cycle life improves more than 1 times.
Claims (4)
1. the preparation method of a carbon material for lithium ion battery cathode, it is characterised in that comprise the steps:
Step 1, pretreating graphite
By in the concentrated sulphuric acid or the concentrated nitric acid solution that immerse rapidly less than 10 DEG C after graphite heating to 100-300 DEG C,
Add surfactant sonic oscillation, make the fully oxidized separation of graphite, then product is reduced, i.e. form high yield
Mono-layer graphite, then by powder body graphite that mono-layer graphite ball mill pulverizing to particle diameter is 5-10 μm；
Step 2, removes the impurity in graphite
Powder body graphite is processed 2-4 hour in the sodium hydroxide solution that concentration is 50-70% in 500-550 DEG C,
In the sulfuric acid solution that concentration is 50-60%, carry out pickling again, then wash and be dried, to remove powder body graphite
In impurity；
Step 3, is modified the graphite composite powder after going the removal of impurity
Graphite composite powder is mixed homogeneously with the nickel oxide accounting for graphite quality 4-6%, puts in carbide furnace, by carbonization
The programming rate of stove is set as 100 DEG C/h and begins to warm up, and stops when reaching 1100 DEG C heating up, at this
At a temperature of keep 6 hours, then in 1500-1700 DEG C of catalyzed graphitization 1-2 hour under a nitrogen, changed
Property powder body graphite；
Step 4, carries out reduction treatment to modified graphite powder body
Under the atmosphere of CO (carbon monoxide converter) gas, at 500-700 DEG C, modified powder body graphite is carried out surface also
Original place is managed 2-4 hour；
Step 5, carries out thin film process to the graphite composite powder after reduction treatment
Use chemical vapour deposition technique, the graphite composite powder after reduction treatment is carried out peplos so that it is on Surface coating
A layer thickness be the carbon of 1-2 μm to improve initial coulomb efficiency, i.e. prepare carbon material for lithium ion battery cathode,
Wherein chemical vapor deposition conditions: carbon source is the alkane of C1～C5, depositing temperature is 700-900 DEG C, deposition
Time is 2-4 hour.
Method the most according to claim 1, it is characterised in that carbon source described in step 5 is C1's～C3
Alkane.
Method the most according to claim 2, it is characterised in that carbon source described in step 5 is ethane.
4. the carbon material for lithium ion battery cathode that prepared by a method as claimed in claim 1.
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| 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 |
| 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 |
| WO2021232090A1 (en) | 2020-05-18 | 2021-11-25 | Ecograf Limited | Method of producing purified graphite |
| 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 |
| CN112234171B (en) * | 2020-09-08 | 2022-04-08 | 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 |
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| US5908715A (en) * | 1997-05-30 | 1999-06-01 | Hughes Electronics Corporation | Composite carbon materials for lithium ion batteries, and method of producing same |
| 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 |
| 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
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5908715A (en) * | 1997-05-30 | 1999-06-01 | Hughes Electronics Corporation | Composite carbon materials for lithium ion batteries, and method of producing same |
| 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 |
| 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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