CN110156005A - A kind of preparation method of the graphite cathode material of fast charge lithium ion battery - Google Patents
A kind of preparation method of the graphite cathode material of fast charge lithium ion battery Download PDFInfo
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- CN110156005A CN110156005A CN201910508567.2A CN201910508567A CN110156005A CN 110156005 A CN110156005 A CN 110156005A CN 201910508567 A CN201910508567 A CN 201910508567A CN 110156005 A CN110156005 A CN 110156005A
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- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/205—Preparation
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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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
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
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- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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Abstract
The invention discloses a kind of preparation method of the graphite cathode material of fast charge lithium ion battery, mainly comprise the steps that raw material is crushed and sieved by (1)；(2) screenings is subjected under conditions of ammonia flow graphitization processing, obtains graphite primary particle；(3) graphite primary particle and modifying agent are mixed to get powder；(4) powder is sent to carbide furnace, is handled 3~5 hours under conditions of nitrogen atmosphere, 100~250 DEG C.The graphite cathode material of fast charge lithium ion battery prepared by the present invention realizes graphite particle N doping, and modifying agent liquefies and be filled into the gap of graphite particle, improves the performances such as capacity, the fast charge of graphite cathode material.
Description
Technical field
The present invention relates to technical field of lithium ion battery negative, in particular to a kind of stone of fast charge lithium ion battery
The preparation method of black negative electrode material.
Background technique
Lithium ion battery has that energy density is high, has extended cycle life, advantages of environment protection, mobile phone, laptop,
It is used widely in the fields such as electric vehicle；But user requires also increasingly to improve to the rapid charging performance of lithium ion battery.Existing skill
In art, mainly reach modified purpose by the way that modifying agent (e.g., pitch) is arranged on the outside of graphite particle, for fast charge lithium from
Sub- battery cathode.In practical application, it is difficult to which, equably by graphite particle coating modification agent, performance increase rate is limited, it is difficult to full
The actual requirement of sufficient user.Therefore, it is necessary to propose a kind of preparation of the graphite cathode material of new fast charge lithium ion battery
Method can further improve the performance of graphite cathode material, meet user to the increasing requirement of lithium ion battery.
As it can be seen that the prior art could be improved and improve.
Summary of the invention
Place in view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of fast charge lithium ion batteries
The preparation method of graphite cathode material, it is intended to solve to pass through the general technology of modifying agent Coating Graphite Particles performance in the prior art
Problem.
In order to achieve the above object, this invention takes following technical schemes:
A kind of preparation method of the graphite cathode material of fast charge lithium ion battery, comprising the following steps:
(1) raw material is crushed and carries out screening and obtain screenings, the raw material is petroleum coke or needle coke；
(2) screenings is subjected under conditions of ammonia flow graphitization processing, obtains graphite primary particle；
(3) the resulting graphite primary particle of step (2) and modifying agent are mixed to get powder, modifying agent is pitch or tree
Rouge；
(4) step (3) resulting powder is sent to carbide furnace, under conditions of nitrogen atmosphere, 100~250 DEG C at
Reason 3~5 hours.
In the preparation method of the graphite cathode material of the fast charge lithium ion battery, the screenings in step (1) is
100~400 mesh screenings.
In the preparation method of the graphite cathode material of the fast charge lithium ion battery, graphitization temperature in step (2)
It is 2800~3200 DEG C.
In the preparation method of the graphite cathode material of the fast charge lithium ion battery, the flow of ammonia in step (2)
For 0.4~0.5m3/h。
In the preparation method of the graphite cathode material of the fast charge lithium ion battery, the pressure of ammonia in step (2)
For 0.4~0.6MPa.
In the preparation method of the graphite cathode material of the fast charge lithium ion battery, mixed in step (3) by VC
Machine mixes graphite primary particle and modifying agent, and incorporation time is 20~30 minutes.
It is warm in carbide furnace in step (4) in the preparation method of the graphite cathode material of the fast charge lithium ion battery
Degree rises to 100~250 DEG C with the rate of 5 DEG C/min.
The utility model has the advantages that the present invention provides a kind of preparation method of the graphite cathode material of fast charge lithium ion battery, phase
Than the prior art, it is graphitized under conditions of ammonia flow in the present invention, realizes the purpose for carrying out N doping to graphite particle,
Since nitrogen-atoms electronegativity is higher than carbon atom, stronger interaction is formed between the carbon-coating and lithium of N doping, this may be advantageous
It is embedded in lithium ion, improves graphite capacity and rapid charging performance.In addition, modifying agent is liquefied and is filled into graphite particle by the present invention
In gap, the modifying agent of graphite particle outer layer in traditional technology is avoided to coat uneven, thus after reinforcing graphite particle roll-in
Structural stability, in nipping process, the conduction of power faster, more evenly, enhances the high rate performance and cycle performance of pole piece, more favorably
It is spread in the inside of lithium ion, to further enhance rapid charging performance.
Specific embodiment
The present invention provides a kind of preparation method of the graphite cathode material of fast charge lithium ion battery, to make mesh of the invention
, technical solution and effect it is clearer, clear, the present invention is described in more detail by the following examples.It should be appreciated that this
Place is described, and specific examples are only used to explain the present invention, is not intended to limit the present invention.
The present invention provides a kind of preparation method of the graphite cathode material of fast charge lithium ion battery, comprising the following steps:
(1) raw material is crushed and carries out screening and obtain screenings, the raw material is petroleum coke or needle coke；
(2) screenings is subjected under conditions of ammonia flow graphitization processing, obtains graphite primary particle；
(3) the resulting graphite primary particle of step (2) and modifying agent are mixed to get powder, modifying agent is pitch or tree
Rouge；
(4) step (3) resulting powder is sent to carbide furnace, under conditions of nitrogen atmosphere, 100~250 DEG C at
Reason 3~5 hours.
In above-mentioned steps (2), ammonia thermal decomposition generates activated nitrogen atom, and constantly diffusion penetrates into graphite particle to real
The purpose of N doping is now carried out to graphite particle.The softening point of pitch or resin in above-mentioned steps (3) is 100~250 DEG C, is led to
The heat treatment of step (4) is crossed, modified grain liquefaction is adsorbed on graphite particle basal plane.
Preferably, the screenings in step (1) is 100~400 mesh screenings.
Preferably, graphitization temperature is 2800~3200 DEG C in step (2).
Preferably, the flow of ammonia is 0.4~0.5m in step (2)3/h。
Preferably, the pressure of ammonia is 0.4~0.6MPa in step (2).
Preferably, graphite primary particle and modifying agent being mixed by VC mixing machine in step (3), incorporation time is 20~
30 minutes.
Preferably, the middle carbonization in-furnace temperature of step (4) rises to 100~250 DEG C with the rate of 5 DEG C/min.
In order to make it easy to understand, further illustrating by the following examples.
Embodiment 1
(1) raw material is crushed and is sieved, obtain 100 mesh screenings, the raw material is petroleum coke；
(2) screenings is subjected under conditions of ammonia flow graphitization processing, obtains graphite primary particle；Graphitization temperature
It is 2800 DEG C；The flow of ammonia is 0.4m3/h；The pressure of ammonia is 0.4MPa；
(3) the resulting graphite primary particle of step (2) and modifying agent are mixed to get powder by VC mixing machine, when mixing
Between be 20 minutes, modifying agent is pitch；
(4) step (3) resulting powder is sent to carbide furnace, in a nitrogen atmosphere, be carbonized in-furnace temperature with 5 DEG C/
The rate of min rises to 100 DEG C, keeps the temperature 3 hours.
Embodiment 2
(1) raw material is crushed and is sieved, obtain 300 mesh screenings, the raw material is needle coke；
(2) screenings is subjected under conditions of ammonia flow graphitization processing, obtains graphite primary particle；Graphitization temperature
It is 3000 DEG C；The flow of ammonia is 0.45m3/h；The pressure of ammonia is 0.5MPa；
(3) the resulting graphite primary particle of step (2) and modifying agent are mixed to get powder by VC mixing machine, when mixing
Between be 25 minutes, modifying agent is resin；
(4) step (3) resulting powder is sent to carbide furnace, in a nitrogen atmosphere, be carbonized in-furnace temperature with 5 DEG C/
The rate of min rises to 200 DEG C, keeps the temperature 4 hours.
Embodiment 3
(1) raw material is crushed and is sieved, obtain 400 mesh screenings, the raw material is needle coke；
(2) screenings is subjected under conditions of ammonia flow graphitization processing, obtains graphite primary particle；Graphitization temperature
It is 3200 DEG C；The flow of ammonia is 0.5m3/h；The pressure of ammonia is 0.6MPa；
(3) the resulting graphite primary particle of step (2) and modifying agent are mixed to get powder by VC mixing machine, when mixing
Between be 30 minutes, modifying agent is resin；
(4) step (3) resulting powder is sent to carbide furnace, in a nitrogen atmosphere, be carbonized in-furnace temperature with 5 DEG C/
The rate of min rises to 250 DEG C, keeps the temperature 5 hours.
Embodiment 4
(1) raw material is crushed and is sieved, obtain 300 mesh screenings, the raw material be petroleum coke or；
(2) screenings is subjected under conditions of ammonia flow graphitization processing, obtains graphite primary particle；Graphitization temperature
It is 2800 DEG C；The flow of ammonia is 0.5m3/h；The pressure of ammonia is 0.6MPa；
(3) the resulting graphite primary particle of step (2) and modifying agent are mixed to get powder by VC mixing machine, when mixing
Between be 20 minutes, modifying agent is pitch；
(4) step (3) resulting powder is sent to carbide furnace, in a nitrogen atmosphere, be carbonized in-furnace temperature with 5 DEG C/
The rate of min rises to 200 DEG C, keeps the temperature 4 hours.
Embodiment 5
(1) raw material is crushed and is sieved, obtain 400 mesh screenings, the raw material is needle coke；
(2) screenings is subjected under conditions of ammonia flow graphitization processing, obtains graphite primary particle；Graphitization temperature
It is 3000 DEG C；The flow of ammonia is 0.42m3/h；The pressure of ammonia is 0.5MPa；
(3) the resulting graphite primary particle of step (2) and modifying agent are mixed to get powder by VC mixing machine, when mixing
Between be 30 minutes, modifying agent is resin；
(4) step (3) resulting powder is sent to carbide furnace, in a nitrogen atmosphere, be carbonized in-furnace temperature with 5 DEG C/
The rate of min rises to 250 DEG C, keeps the temperature 3 hours.
By property such as the resulting graphite cathode material tap density of above-described embodiment 1~5, button battery capacity, 10C reversible capacities
It can be carried out test, as a result as follows:
By above-mentioned analysis, compared with prior art, it is graphitized, is realized to stone under conditions of ammonia flow in the present invention
Black particle carries out the purpose of N doping, since nitrogen-atoms electronegativity is higher than carbon atom, is formed more between the carbon-coating and lithium of N doping
Strong interaction, this is advantageously possible for lithium ion insertion, improves graphite capacity and rapid charging performance.In addition, the present invention will be modified
Agent is liquefied and is filled into the gap of graphite particle, avoids the modifying agent of graphite particle outer layer in traditional technology from coating uneven,
To reinforce the structural stability after graphite particle roll-in, in nipping process, the conduction of power faster, more evenly, enhances pole piece
High rate performance and cycle performance are more advantageous to the inside diffusion of lithium ion, to further enhance rapid charging performance.
It, can according to the technique and scheme of the present invention and its hair it is understood that for those of ordinary skills
Bright design is subject to equivalent substitution or change, and all these changes or replacement all should belong to protection scope of the present invention.
Claims (7)
1. a kind of preparation method of the graphite cathode material of fast charge lithium ion battery, which comprises the following steps:
(1) raw material is crushed and carries out screening and obtain screenings, the raw material is petroleum coke or needle coke；
(2) screenings is subjected under conditions of ammonia flow graphitization processing, obtains graphite primary particle；
(3) the resulting graphite primary particle of step (2) and modifying agent are mixed to get powder, modifying agent is pitch or resin；
(4) step (3) resulting powder is sent to carbide furnace, under conditions of nitrogen atmosphere, 100~250 DEG C handle 3~
5 hours.
2. the preparation method of the graphite cathode material of fast charge lithium ion battery according to claim 1, which is characterized in that
Screenings in step (1) is 100~400 mesh screenings.
3. the preparation method of the graphite cathode material of fast charge lithium ion battery according to claim 1, which is characterized in that
Graphitization temperature is 2800~3200 DEG C in step (2).
4. the preparation method of the graphite cathode material of fast charge lithium ion battery according to claim 1, which is characterized in that
The flow of ammonia is 0.4~0.5m in step (2)3/h。
5. the preparation method of the graphite cathode material of fast charge lithium ion battery according to claim 1, which is characterized in that
The pressure of ammonia is 0.4~0.6MPa in step (2).
6. the preparation method of the graphite cathode material of fast charge lithium ion battery according to claim 1, which is characterized in that
Graphite primary particle and modifying agent are mixed by VC mixing machine in step (3), incorporation time is 20~30 minutes.
7. the preparation method of the graphite cathode material of fast charge lithium ion battery according to claim 1, which is characterized in that
Carbonization in-furnace temperature rises to 100~250 DEG C with the rate of 5 DEG C/min in step (4).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111584866A (en) * | 2020-05-27 | 2020-08-25 | 安徽科达新材料有限公司 | Preparation method of high-rate artificial graphite negative electrode material |
| CN113363466A (en) * | 2021-06-16 | 2021-09-07 | 广东凯金新能源科技股份有限公司 | Low-cost graphite negative electrode material based on crucible crushed aggregates and preparation method thereof |
| CN114068885A (en) * | 2020-07-30 | 2022-02-18 | 湖南中科星城石墨有限公司 | Graphite material with porous carbon layer and preparation method and application thereof |
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| CN107369823A (en) * | 2017-07-25 | 2017-11-21 | 广东海洋大学 | A kind of lithium ion battery artificial composite cathode material of silicon/carbon/graphite and preparation method thereof |
| CN107507979A (en) * | 2016-06-14 | 2017-12-22 | 上海杉杉科技有限公司 | A kind of preparation method of high jolt ramming artificial plumbago negative pole material |
| CN110203921A (en) * | 2019-06-13 | 2019-09-06 | 广东凯金新能源科技股份有限公司 | A kind of preparation method of lithium ion battery modified natural graphite |
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2019
- 2019-06-13 CN CN201910508567.2A patent/CN110156005A/en active Pending
Patent Citations (4)
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| CN102034975A (en) * | 2010-11-15 | 2011-04-27 | 中国科学院青岛生物能源与过程研究所 | Nitrogen-doped graphite carbon serving as anode material of lithium ion battery, and preparation method and application thereof |
| CN107507979A (en) * | 2016-06-14 | 2017-12-22 | 上海杉杉科技有限公司 | A kind of preparation method of high jolt ramming artificial plumbago negative pole material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111584866A (en) * | 2020-05-27 | 2020-08-25 | 安徽科达新材料有限公司 | Preparation method of high-rate artificial graphite negative electrode material |
| CN114068885A (en) * | 2020-07-30 | 2022-02-18 | 湖南中科星城石墨有限公司 | Graphite material with porous carbon layer and preparation method and application thereof |
| CN113363466A (en) * | 2021-06-16 | 2021-09-07 | 广东凯金新能源科技股份有限公司 | Low-cost graphite negative electrode material based on crucible crushed aggregates and preparation method thereof |
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