CN106876710B - Soft carbon negative electrode material for lithium ion battery and preparation method thereof - Google Patents
Soft carbon negative electrode material for lithium ion battery and preparation method thereof Download PDFInfo
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- CN106876710B CN106876710B CN201710163529.9A CN201710163529A CN106876710B CN 106876710 B CN106876710 B CN 106876710B CN 201710163529 A CN201710163529 A CN 201710163529A CN 106876710 B CN106876710 B CN 106876710B
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- soft carbon
- lithium ion
- ion battery
- negative electrode
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- 229910021384 soft carbon Inorganic materials 0.000 title claims abstract description 54
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000007773 negative electrode material Substances 0.000 title claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 13
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 11
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 11
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 11
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 11
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims abstract description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 238000003763 carbonization Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 239000000654 additive Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000010405 anode material Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 230000000996 additive effect Effects 0.000 claims description 3
- 239000011294 coal tar pitch Substances 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 238000010000 carbonizing Methods 0.000 claims description 2
- 239000011300 coal pitch Substances 0.000 claims description 2
- 239000011280 coal tar Substances 0.000 claims description 2
- 238000010907 mechanical stirring Methods 0.000 claims description 2
- 239000003921 oil Substances 0.000 claims description 2
- 239000003208 petroleum Substances 0.000 claims description 2
- 239000011301 petroleum pitch Substances 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 239000011318 synthetic pitch Substances 0.000 claims description 2
- 229920003002 synthetic resin Polymers 0.000 claims description 2
- 239000000057 synthetic resin Substances 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims 1
- 238000004321 preservation Methods 0.000 claims 1
- 230000000630 rising effect Effects 0.000 claims 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 5
- 239000010406 cathode material Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 5
- 239000007833 carbon precursor Substances 0.000 abstract description 2
- 238000007796 conventional method Methods 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- -1 molybdenum ions Chemical class 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 230000002427 irreversible effect Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 description 2
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 239000000571 coke Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229910021382 natural graphite Inorganic materials 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 1
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 229910001429 cobalt ion Inorganic materials 0.000 description 1
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 229910021385 hard carbon Inorganic materials 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002296 pyrolytic carbon Substances 0.000 description 1
- 239000011856 silicon-based particle Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
Classifications
-
- 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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
-
- 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
-
- 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
-
- 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 & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention provides a soft carbon cathode material for a lithium ion battery and a preparation method thereof, wherein ammonium molybdate and cobalt nitrate are added into a soft carbon precursor raw material, carbonization is carried out at the temperature of 900-1300 ℃, and then natural cooling is carried out to room temperature, so as to prepare the high-first-efficiency soft carbon cathode material. By the method, elemental or ionic sulfur, elemental nitrogen or ionic nitrogen in the soft carbon cathode is eliminated, the problem of low first effect of the soft carbon cathode material prepared by the conventional method is solved, and the specific capacity is greatly improved.
Description
Technical Field
The invention relates to a preparation method of a lithium ion battery material, in particular to a soft carbon negative electrode material for a lithium ion battery and a preparation method thereof.
Background
Lithium ion batteries are favored for their excellent performance, such as high capacity, high voltage, high cycling stability, high energy density, and no environmental pollution. However, the quick charge of the lithium ion battery is a great key common technology which needs to be solved urgently at present.
In the research process of the rapid charging material, the crystal face spacing of the soft carbon is larger than that of graphite, so that the rapid charging material has better high-rate charging and low-temperature charging performances and is expected to realize the rapid charging of the lithium ion battery. However, soft carbon has a significant disadvantage: the irreversible capacity of the first charge and discharge is high, namely the first effect is low.
In the prior art, soft carbon is coated on the surfaces of cathode materials such as a natural graphite cathode, a silicon-carbon cathode, a hard carbon cathode and the like, so that the performance of the original materials is partially improved. For example, patent "a negative active material and a method for preparing the same" (201610137500.9) discloses that a soft carbon matrix and silicon particles and soft carbon particles dispersed in the soft carbon matrix are further coated with a layer of soft carbon; the negative electrode material disclosed in the patent 'a negative electrode material for lithium ion battery and negative electrode sheet thereof' (201510040504.0) is formed by mixing natural graphite and artificial graphite which are coated by soft carbon according to a certain mass ratio; the patent (201510569923.3) discloses that the capacity of coke soft carbon is improved by doping heteroatom, and simultaneously, the coke soft carbon is compounded with a graphite material according to the mass ratio of 90-40: 10-60, and then an organic matter pyrolytic carbon layer is coated to prepare the carbon/carbon composite negative electrode material; a patent of a modified soft carbon negative electrode material of a lithium ion battery and a preparation method thereof (201410855276.8) discloses that graphene powder particles are doped in soft carbon powder particles; in a patent "a lithium ion battery soft carbon negative electrode material with aluminum fluoride coated on the surface and a preparation method thereof" (201410834558. X), an aluminum fluoride layer is coated on the surface of the soft carbon negative electrode material; patent "soft carbon composite negative electrode material of lithium ion battery and preparation method thereof" (201310444961.7) discloses a composite material in which the soft carbon material and graphite form disordered layers and a layered structure.
None of these methods addresses the deficiencies inherent in soft carbon materials (with respect to low first-pass efficiency).
Disclosure of Invention
The invention aims to overcome the defects of the prior art, greatly improves the specific capacity, reduces the irreversible capacity of the soft carbon cathode during the first charge and discharge on the premise of not changing other performances of the soft carbon cathode, and improves the first effect.
The invention is realized by the following technical scheme:
a preparation method of a soft carbon negative electrode material for a lithium ion battery comprises the following steps:
s1, adding additives into the raw materials, and uniformly mixing to form a mixture;
the raw material is one or more of coal tar, coal pitch, petroleum residual oil, petroleum pitch, synthetic resin and synthetic pitch;
the additives are ammonium molybdate and cobalt nitrate, and the additives are solid powder or solution dissolved in water, alcohol and the like.
S2, heating the mixture, carbonizing at the temperature of 900-1300 ℃, and naturally cooling to room temperature to prepare the high-first-efficiency soft carbon negative electrode material.
Preferably, in step S1, the additive to raw material ratio is, the additive: raw material =1: (1 to 100) (wt%)
Preferably, in step S1, the ammonium molybdate and the cobalt nitrate are uniformly distributed in the asphalt by uniformly mixing with a stirring method, where the stirring method is one or more of mechanical stirring, ultrasonic stirring, and magnetic resonance stirring.
Preferably, in step S2, the carbonization temperature is 900-.
Further, the invention claims a soft carbon negative electrode material for a lithium ion battery, which is characterized in that the soft carbon negative electrode material is prepared by the above method.
The invention has the following technical effects:
through research, the applicant finds that the existence of elemental or ionic sulfur, elemental nitrogen or ionic nitrogen in the soft carbon negative electrode is a crucial factor causing the first efficiency of the soft carbon negative electrode to be low. Therefore, the applicant adds ammonium molybdate and cobalt nitrate to the soft carbon precursor raw material, and then carbonizes the mixture to obtain the soft carbon negative electrode material. In the carbonization process, elemental sulfur or ionic sulfur existing in the raw materials reacts with molybdenum ions to generate molybdenum sulfide precipitates, and ammonium ions are volatilized in the carbonization process of the raw materials; in the carbonization process, simple substance or ionic nitrogen existing in the raw material reacts with cobalt ions to generate cobalt nitride precipitate, and nitrate ions are volatilized in the carbonization process of the raw material. By the method, elemental or ionic sulfur, elemental nitrogen or ionic nitrogen in the soft carbon cathode is eliminated, the irreversible capacity of the soft carbon cathode in the first charge and discharge is reduced, the problem of low first effect of the soft carbon cathode material prepared by the conventional method is solved, and the specific capacity is greatly improved.
Detailed Description
The invention is further illustrated below with reference to the examples.
Comparative example
The soft carbon negative electrode material without adding ammonium molybdate and cobalt nitrate is used as a comparison sample (under the same process conditions).
Example 1
Mixing ammonium molybdate: cobalt nitrate: mixing coal tar pitch =1:2:10 by weight, wherein the ammonium molybdate and the cobalt nitrate can be solid powder or solution dissolved in water, alcohol and the like, then dispersing by ultrasonic waves, heating to 900 ℃ at a heating rate of 8 ℃/min under the protection of nitrogen, then preserving the heat for 5h, and naturally cooling to room temperature to obtain the high-first-efficiency soft carbon negative electrode material.
Example 2
Mixing ammonium molybdate: cobalt nitrate: coal tar pitch =1:1:90, and the ammonium molybdate and the cobalt nitrate may be solid powders or solutions dissolved in water, alcohol, or the like. And then stirring and dispersing by adopting magnetic resonance, heating to 1300 ℃ at the heating rate of 15 ℃/min under the argon protective atmosphere, then preserving the heat for 8h, and naturally cooling to room temperature to obtain the high-efficiency soft carbon negative electrode material.
The results of testing the soft carbon negative electrode materials prepared in comparative example, example 1 and example 2 are shown in the following table:
the comparison of the table shows that the soft carbon anode material prepared by the invention solves the problem of low first efficiency and greatly improves the specific capacity.
Claims (5)
1. A preparation method of a soft carbon negative electrode material for a lithium ion battery is characterized by comprising the following steps:
s1, adding additives into the raw materials, and uniformly mixing to form a mixture;
the raw material is one or more of coal tar, coal pitch, petroleum residual oil, petroleum pitch, synthetic resin and synthetic pitch;
the additives are ammonium molybdate and cobalt nitrate, and the additives are solid powder or solution;
s2, heating the mixture, carbonizing at the temperature of 900-1300 ℃, and naturally cooling to room temperature to prepare the high-first-efficiency soft carbon negative electrode material.
2. The preparation method of the soft carbon anode material for the lithium ion battery according to claim 1, wherein the soft carbon anode material comprises the following steps: in the step S1, the weight ratio of the additive to the raw material is 1:1 to 100.
3. The preparation method of the soft carbon anode material for the lithium ion battery according to claim 1, wherein the soft carbon anode material comprises the following steps: in the step S1, the ammonium molybdate and the cobalt nitrate are uniformly distributed in the coal tar pitch by uniformly mixing with a stirring method, wherein the stirring method is one or more of mechanical stirring, ultrasonic stirring and magnetic resonance stirring.
4. The preparation method of the soft carbon anode material for the lithium ion battery according to claim 1, wherein the soft carbon anode material comprises the following steps: in step S2, the carbonization temperature is 900-1300 ℃, the temperature rising speed is 5-20 ℃/min, the heat preservation time is 2-10h, and the protective atmosphere is nitrogen or argon.
5. A soft carbon anode material for a lithium ion battery, characterized in that: the soft carbon negative electrode material is prepared by the preparation method of the soft carbon negative electrode material for the lithium ion battery according to any one of claims 1 to 4.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2016111945598 | 2016-12-22 | ||
| CN201611194559 | 2016-12-22 |
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| Publication Number | Publication Date |
|---|---|
| CN106876710A CN106876710A (en) | 2017-06-20 |
| CN106876710B true CN106876710B (en) | 2020-03-24 |
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| CN111293301B (en) * | 2020-03-17 | 2022-06-24 | 江苏科技大学 | Soft and hard carbon composite porous negative electrode material for sodium ion battery and preparation method thereof |
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| US7431822B2 (en) * | 2005-12-16 | 2008-10-07 | Chevron U.S.A. Inc. | Process for upgrading heavy oil using a reactor with a novel reactor separation system |
| FR2895416B1 (en) * | 2005-12-22 | 2011-08-26 | Inst Francais Du Petrole | SELECTIVE HYDROGENATION PROCESS USING A SULFIDE CATALYST |
| CN101468309B (en) * | 2007-12-25 | 2011-11-02 | 中国石油化工股份有限公司 | Method for preparing non-supported hydrogenation catalyst |
| CN102329637B (en) * | 2011-08-29 | 2013-04-24 | 云南昆钢煤焦化有限公司 | Intensive production method of coal tar pitch needle coke |
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Address after: Jinzhou 410600 Hunan province Ningxiang County District Changsha Quan Zhou Bei Lu (Jin Zhou Zhen Long Qiao Cun) Applicant after: Hunan Branch Star graphite Co. Address before: Jinzhou 410645 Hunan province Ningxiang County District Changsha Quanzhou Road Applicant before: HUNAN SHINZOOM TECHNOLOGY CO., LTD. |
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