CN100341173C - Method for preparing natural graphite cathode material of lithium ion battery - Google Patents
Method for preparing natural graphite cathode material of lithium ion battery Download PDFInfo
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- CN100341173C CN100341173C CNB2004100180782A CN200410018078A CN100341173C CN 100341173 C CN100341173 C CN 100341173C CN B2004100180782 A CNB2004100180782 A CN B2004100180782A CN 200410018078 A CN200410018078 A CN 200410018078A CN 100341173 C CN100341173 C CN 100341173C
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
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- Chemical Kinetics & Catalysis (AREA)
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- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
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Abstract
本发明公开了一种锂离子电池负极材料制造方法，包括如下步骤：(1)将石墨与包覆材料与溶剂混合，抽真空，脱除溶剂，将天然石墨包覆于包覆材原料中，(2)然后将物料进行热聚合，天然石墨表面获得微胶囊化的包覆层；(3)将步骤(2)所获得的产物进行炭化或将其进行石墨化，获得表面包覆人造石墨层的炭负极材料，即为本发明的锂离子电池负极材料。所获得的电池负极材料检测结果为：振实密度在1.08以上，比表面积在2.20以下，首次放电容量在350mAh/g以上(不可逆容量低于25mAh/g)，首次充放电效率在93%以上，循环450次仍保留首次容量的90%以上。本发明的方法，易于实施、包覆效果好、不可逆容量低、循环性能稳定的优点。The invention discloses a method for manufacturing a negative electrode material of a lithium ion battery, comprising the following steps: (1) mixing graphite with a coating material and a solvent, vacuuming, removing the solvent, and coating natural graphite in the raw material of the coating material, (2) Then the material is subjected to thermal polymerization, and the surface of natural graphite obtains a microencapsulated coating layer; (3) the product obtained in step (2) is carbonized or graphitized to obtain a surface-coated artificial graphite layer The carbon negative electrode material is the lithium ion battery negative electrode material of the present invention. The test results of the obtained battery negative electrode materials are: the tap density is above 1.08, the specific surface area is below 2.20, the initial discharge capacity is above 350mAh/g (irreversible capacity is below 25mAh/g), and the initial charge and discharge efficiency is above 93%. After 450 cycles, it still retains more than 90% of its initial capacity. The method of the invention has the advantages of easy implementation, good coating effect, low irreversible capacity and stable cycle performance.
Description
Technical field
The present invention relates to a kind of preparation method of cell negative electrode material, be specifically related to a kind of lithium ion battery negative material manufacture method.
Background technology
Lithium ion battery negative material mainly contains two kinds of Delanium and native graphites based on the raw material of wood-charcoal material.Delanium has MCMB such as CMS and MCMB, phase charcoal fiber MCF and graphous graphite powder in the middle of also having.Preceding two kinds of Delaniums are the negative materials that are widely adopted, has the advantage that particle shape is good, irreversible capacity loss is low, cycle life is stable, but also have production cost height, deficiency that discharge capacity is low, the discharge capacity of MCMB is generally about 320mAh/g.Irregular form graphous graphite powder is owing to exist the shortcoming that tap density is low, specific area is high to be not suitable for directly using as negative material.The native graphite cost of material is low, and its higher degree of graphitization makes it have higher embedding lithium ability, but there is the shortcoming that tap density is low, specific area is high equally in the native graphite of sheet, is not suitable for directly using as negative material.Irreversible capacity loss is very high first not pass through the natural graphite negative electrode material of modification, generally can reach 10%, owing to solvent takes place embed altogether, causes problems such as capacity attenuation is fast at circulation time.
For a long time, for the capacitance that improves Delanium, the irreversible capacity loss first that reduces native graphite improve its cycle performance, be that the emphasis, the particularly modification for native graphite of research and development proposed a lot of methods always.
Japan Patent JP10294111 carries out low temperature with pitch to graphite raw material of wood-charcoal material and coats, and must not melt after the coating to handle and slight the pulverizing, and this method is difficult to accomplish coat evenly.Japan Patent JP11246209 floods graphite and hard charcoal particle under 10～300 ℃ of temperature in pitch or tar, carry out separated from solvent and heat treatment then, this method is difficult to form at graphite and hard carbon surface and has the bitumen layer of certain thickness height polymerization, will be restricted for the raising of native graphite structural stability.Japan Patent JP2000003708 carry out roundingization with mechanical means to graphite material, floods in heavy oil, tar or pitch then, separates and washs, and sees close with JP11246209 merely from method for coating.Japan Patent JP2000182617 adopts native graphite etc. and pitch or resin or the charing altogether of its mixture, and this method can reduce the graphite material specific area, but is difficult to reach preferable control on covered effect.Japan Patent JP2000243398 is that the atmosphere of utilizing asphalt pyrolysis to produce is carried out surface treatment to graphite material, and the unlikely form of the material that is modified that makes of this method is greatly improved, thereby the raising of electrical property is restricted.Japan Patent JP2002042816 is that raw material coats with the CVD method or coats with pitch phenolic resins with aromatic hydrocarbons, and this and JP2000182617 and JP2000283398 have similarity on effect.
Summary of the invention
The technical issues that need to address of the present invention are to disclose a kind of natural graphite lithium ionic cell cathode material manufacture method, to overcome the above-mentioned defective that prior art exists.
Method of the present invention comprises the steps:
(1) graphite is mixed under 150～350 ℃ temperature with solvent with clad material, vacuumize, remove solvent, graphite is coated in the clad material;
Said graphite is native graphite, and preferred spherical native graphite, its average grain diameter D50 are 5～45 μ m, and preferred phosphorus content is at the graphite more than 99%, and the tap density of spherical native graphite preferably reaches 0.90g/cm
3More than;
Said clad material comprises by-product pitch or its mixture of coal tar, coal tar pitch, petroleum asphalt or production MCMB, and the part by weight of graphite and clad material is 1/0.03～0.10;
Said solvent comprises a kind of or its mixture in carbolineum, washing oil, dimethylbenzene, toluene or the diesel oil etc., and the weight ratio of graphite and solvent is 1: 0.1～0.5;
Term " tap density " refers to " material powder being loaded under the vibration container; after rated condition is real through battle array; measured powder density ", and this term has clear and definite definition in the bioassay standard (this standard is formulated with reference to international standard ISO3953-1977 " mensuration of metal dust-tap density ") of Q/TEZI01-2001 5.5 tap densities;
(2) then material is placed under 350～500 ℃ the temperature and carry out thermal polymerization, polymerization pressure is 0.01～10MPa, and the reaction time is 5～420 minutes, and the native graphite surface obtains the coating layer of microencapsulation;
(3) product that step (2) is obtained carries out charing under 800～2200 ℃ condition, obtain the carbon cathode material that the surface coats the charcoal layer, or with it at 2400～3000 ℃, be preferably under 2800 ℃～3000 ℃ the condition and carry out graphitization, obtain the carbon cathode material that the surface coats the Delanium layer, be lithium ion battery negative material of the present invention.
Adopt the testing standard of Q/TEZI01-2001 5.7 electrochemistry capacitances that the cell negative electrode material that is obtained is detected, its result is as follows:
Tap density is more than 1.08, and specific area is below 2.20, discharge capacity (irreversible capacity is lower than 25mAh/g) more than 350mAh/g first, and first charge-discharge efficiency is more than 93%, and circulating still keeps more than 90% of capacity first 450 times.
See by above-mentioned disclosed technical scheme, method of the present invention, easy to implement, covered effect good, specific capacity is high, irreversible capacity is low, the advantage of stable cycle performance.
Embodiment
Embodiment 1～13
Process conditions:
| Embodiment | Graphite (A) | Clad material (B) | Solvent (C) | Ratio A/B/C weight ratio | Mixing temperature ℃ | Reaction temperature ℃ | Reaction pressure MPa | Reaction time min | Charing ℃ | Graphitization ℃ |
| 1 | Spherical | Coal tar pitch | Washing oil | 1/0.08/0.4 | 200 | 450 | 0.1 | 60 | 1000 | - |
| 2 | Spherical | Coal tar pitch | Dimethylbenzene | 1/0.05/0.5 | 100 | 420 | 0.1 | 120 | - | ＞2600 |
| 3 | Spherical | Coal tar pitch | Washing oil | 1/0.10/0.2 | 200 | 500 | 0.04 | 120 | - | ＞2800 |
| 4 | Sheet | Coal tar pitch | Washing oil | 1/0.06/0.3 | 200 | 500 | 0.1 | 120 | - | ＞2800 |
| 5 | Sheet | Coal tar pitch | Washing oil | 1/0.08/0.2 | 200 | 380 | 1.0 | 420 | - | ＞2800 |
| 6 | Spherical | Coal tar | Carbolineum | 1/0.10/0.10 | 250 | 400 | 0.1 | 300 | 1300 | - |
| 7 | Spherical | Coal tar | Carbolineum | 1/0.10/0.2 | 250 | 420 | 0.1 | 180 | - | ＞2800 |
| 8 | Spherical | By-product pitch | Dimethylbenzene | 1/0.08/0.4 | 100 | 450 | 0.1 | 240 | 900 | - |
| 9 | Spherical | By-product pitch | Dimethylbenzene | 1/0.10/0.2 | 100 | 430 | 0.04 | 300 | - | ＞2600 |
| 10 | Spherical | Petroleum asphalt | Diesel oil | 1/0.07/0.3 | 90 | 450 | 0.1 | 420 | - | ＞2800 |
| 11 | Sheet | Petroleum asphalt | Diesel oil | 1/0.070.2 | 90 | 450 | 0.1 | 420 | - | ＞2800 |
| 12 | Spherical | Coal tar pitch+petroleum asphalt | Carbolineum | 1/0.05/0.10 | 250 | 500 | 1.0 | 450 | - | ＞2800 |
| 13 | Spherical | Coal tar pitch+petroleum asphalt | Washing oil | 1/0.10/0.5 | 200 | 500 | 0.03 | 500 | - | ＞2800 |
| Comparative Examples 1 native graphite | Ball-type | Do not have | Do not have | 1/0.00/0.00 | - | - | - | - | - | - |
| Comparative Examples 2 native graphites | Sheet | Do not have | Do not have | 1/0.00/0.00 | - | - | - | - | - | - |
The testing standard of employing Q/TEZI01-2001 5.7 electrochemistry capacitances detects product and two Comparative Examples of embodiment 1～13, and its result is as follows:
| Embodiment | Real density g/cm 3 | Tap density g/cm 3 | Specific area m 2/g | Discharge capacity mAh/g first | Irreversible capacity mAh/g | Discharging efficiency % first | Keep 90% capacity cycle-index |
| 1 | 2.15 | 1.15 | 1.70 | 351 | 21 | 94.4 | Do not survey |
| 2 | 2.20 | 1.10 | 1.80 | 362 | 19 | 95.0 | Do not survey |
| 3 | 2.21 | 1.09 | 2.00 | 355 | 22 | 94.2 | 450 |
| 4 | 2.19 | 1.17 | 1.60 | 360 | 22 | 94.2 | Do not survey |
| 5 | 2.22 | 1.12 | 1.70 | 361 | 23 | 94.0 | Do not survey |
| 6 | 2.09 | 1.08 | 2.20 | 357 | 20 | 94.7 | Do not survey |
| 7 | 2.18 | 1.19 | 1.78 | 365 | 17 | 95.5 | Do not survey |
| 8 | 2.20 | 1.15 | 1.60 | 359 | 23 | 94.0 | Do not survey |
| 9 | 2.21 | 1.09 | 1.90 | 350 | 24 | 93.6 | Do not survey |
| 10 | 2.20 | 1.16 | 1.80 | 365 | 21 | 94.6 | 500 |
| 11 | 2.23 | 1.13 | 1.90 | 358 | 22 | 94.2 | Do not survey |
| 12 | 2.20 | 1.16 | 1.60 | 361 | 24 | 93.8 | 450 |
| 13 | 2.19 | 1.08 | 1.90 | 360 | 20 | 94.7 | Do not survey |
| Comparative Examples 1 | 2.24 | 1.02 | 6.5 | 362 | 40 | 90.0 | 65 |
| Comparative Examples 2 | 2.25 | 0.85 | 6.3 | 367 | 44 | 89.3 | 50 |
By the result of the test of embodiment and Comparative Examples as seen, native graphite is by the technical program, and tap density is by original 1.02g/cm
3Below bring up to 1.08g/cm
3More than, specific area has kept more than the high power capacity 350mAh/g of native graphite by being reduced to more than 6.3 below 2.20, and irreversible capacity has been dropped to below the 25mAh/g.Cycle performance obviously improves, and still keeps more than 90% of capacity first 450 times by can not stable circulation bringing up to circulation.
Claims (7)
1. the lithium ion battery negative material manufacture method is characterized in that, comprises the steps:
(1) native graphite is mixed under 150～350 ℃ temperature with solvent with clad material, vacuumize, remove solvent, native graphite is coated in the coating material raw material;
Said clad material comprises by-product pitch or its mixture of coal tar, coal tar pitch, petroleum asphalt, production MCMB;
(2) material that then step (1) is obtained places under 350～500 ℃ the temperature and carries out thermal polymerization, and polymerization pressure is 0.01～10MPa, and the reaction time is 5～420 minutes;
(3) product that step (2) is obtained carries out charing under 800～2200 ℃ condition, obtain the carbon cathode material that the surface coats the charcoal layer, or it is carried out graphitization under 2400～3000 ℃ condition, obtain the carbon cathode material that the surface coats the Delanium layer, be lithium ion battery negative material.
2. method according to claim 1 is characterized in that, said native graphite, and its phosphorus content should be more than 99%.
3. method according to claim 2 is characterized in that, its average grain diameter of said native graphite D
50Be 5～45 μ m.
4. according to claim 1,2 or 3 described methods, it is characterized in that said native graphite tap density is 0.90g/cm
3Above spherical native graphite.
5. method according to claim 1 is characterized in that, the weight ratio of native graphite and clad material is 1: 0.03～0.10.
6. method according to claim 1 is characterized in that, said solvent comprises a kind of or its mixture in carbolineum, washing oil, dimethylbenzene, toluene or the diesel oil.
7. method according to claim 1 is characterized in that, the weight ratio of graphite and solvent is 1: 0.1～0.5.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100180782A CN100341173C (en) | 2004-04-29 | 2004-04-29 | Method for preparing natural graphite cathode material of lithium ion battery |
| JP2005133333A JP2005317550A (en) | 2004-04-29 | 2005-04-28 | Method for producing natural graphite lithium ion battery cathode material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100180782A CN100341173C (en) | 2004-04-29 | 2004-04-29 | Method for preparing natural graphite cathode material of lithium ion battery |
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| CN1691373A CN1691373A (en) | 2005-11-02 |
| CN100341173C true CN100341173C (en) | 2007-10-03 |
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Families Citing this family (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101186292B (en) * | 2006-11-22 | 2014-05-28 | 辽宁工程技术大学 | Method for preparing carbon cathode material and lithium iron battery using the material |
| CN101108918B (en) * | 2007-08-16 | 2010-06-30 | 湛江市新蓄能源科技有限公司 | High softening point bitumen used as lithium ion battery negative pole coating layer material and manufacture thereof |
| CN102117911B (en) * | 2009-12-30 | 2014-06-04 | 上海杉杉科技有限公司 | Graphite cathode material for lithium ion battery and preparation method thereof |
| CN101969122A (en) * | 2010-09-14 | 2011-02-09 | 东莞市迈科新能源有限公司 | A kind of core-shell structure carbon for negative electrode material of lithium ion battery and preparation method thereof |
| CN102637859B (en) * | 2012-04-06 | 2014-08-27 | 宁德新能源科技有限公司 | Lithium ion battery, graphite cathode material of lithium ion battery, and preparation method of graphite anode material |
| CN103094536A (en) * | 2013-02-05 | 2013-05-08 | 新乡远东电子科技有限公司 | High-capacity lithium ion secondary battery cathode carbon material |
| CN107316982B (en) * | 2016-04-27 | 2022-02-01 | 上海杉杉科技有限公司 | Silicon-carbon negative electrode material of lithium ion secondary battery and preparation method thereof |
| CN106848239A (en) * | 2017-02-24 | 2017-06-13 | 鞍山兴德材料科技股份有限公司 | A kind of high-grade self assembly carbon/carbon compound materials of SCC and preparation method thereof |
| CN110890529A (en) * | 2019-10-28 | 2020-03-17 | 鞍钢股份有限公司 | Method for coating graphite negative electrode material |
| CN110828798B (en) * | 2019-10-31 | 2022-06-07 | 方大炭素新材料科技股份有限公司 | Method for preparing lithium ion battery graphite negative electrode material by wet pressurizing coating |
| CN110880600B (en) * | 2019-11-21 | 2021-09-07 | 广东东岛新能源股份有限公司 | Negative electrode material with high temperature resistance, preparation method thereof and application thereof in lithium ion battery |
| CN111628146B (en) * | 2020-04-23 | 2023-09-12 | 湖南中科星城石墨有限公司 | Process for preparing lithium ion battery anode material by filling microcrystalline graphite with asphalt |
| CN114751407B (en) * | 2022-04-29 | 2024-01-26 | 广东东岛新能源股份有限公司 | Modified natural graphite negative electrode material and preparation method and application thereof |
| CN114873591B (en) * | 2022-04-29 | 2023-12-19 | 广东东岛新能源股份有限公司 | Low-temperature long-life natural graphite anode material and preparation method and application thereof |
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2004
- 2004-04-29 CN CNB2004100180782A patent/CN100341173C/en not_active Expired - Lifetime
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2005
- 2005-04-28 JP JP2005133333A patent/JP2005317550A/en active Pending
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| CN1202142A (en) * | 1995-11-14 | 1998-12-16 | 大阪瓦斯株式会社 | Negative electrode material for lithium storage battery, preparation method thereof, and lithium storage battery using the material |
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| WO2004027902A1 (en) * | 2002-09-19 | 2004-04-01 | Sharp Kabushiki Kaisha | Lithium polymer battery and method for manufacturing same |
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| JP2005317550A (en) | 2005-11-10 |
| CN1691373A (en) | 2005-11-02 |
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