CN107601490A - A kind of fast charge graphite cathode material and preparation method thereof - Google Patents
A kind of fast charge graphite cathode material and preparation method thereof Download PDFInfo
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- CN107601490A CN107601490A CN201710683450.9A CN201710683450A CN107601490A CN 107601490 A CN107601490 A CN 107601490A CN 201710683450 A CN201710683450 A CN 201710683450A CN 107601490 A CN107601490 A CN 107601490A
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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
Abstract
The invention discloses a kind of fast charge graphite cathode material and preparation method thereof, by the way that graphite presoma is mixed with covering material, the processing of low-temperature treatment and high temperature graphitization, that is, the fast charge graphite cathode material for lithium ion battery is made.High temperature graphitization processing makes graphite presoma be changed into high power capacity graphite, covering material is transformed into constitutionally stable unformed charcoal bag coating simultaneously, be advantageous to lithium ion quickly to transmit with electrolyte interface in material, from notable graphite material charge-discharge magnification and cycle performance, its high capacity and high coulombic efficiency first also ensure that.Technique of the present invention is simple, energy consumption is low, be adapted to commercially produce and lithium ion battery in apply.
Description
Technical field
The present invention relates to lithium ion battery negative material field, more particularly to a kind of fast charge graphite cathode material and its preparation
Method.
Background technology
With the fast development of electric automobile, people, which thirst for electric car, has the performance of long continuation of the journey and fast charging and discharging, because
This, the demand of high power capacity high multiplying power lithium ion battery increases year by year.Lithium titanate has high charge and discharge because of the crystal structure of uniqueness
Electric multiplying power, however, its low gram volume and high voltage platform seriously constrain its application on electric car.Graphite has
Double more gram volumes than lithium titanate, has become the main negative material of electric automobile at present.With battery of electric vehicle pair
The demand of power continues to increase, it is accordingly required in particular to the negative material that can be used with higher charge-discharge magnification.
The defects of to overcome graphite charge-discharge magnification not high, it presently, there are the technology that processing is modified to graphite.China
Patent CN201410787061.7, fast charge graphite lithium ion battery negative pole is prepared for using graphite covered by asphalt, high temperature graphitization
Material.This method is transformed into graphite charcoal in the pitch of Graphite Coating by high temperature graphitization, and performance approaches with bulk graphite,
So high rate performance lifting is limited.Chinese patent CN201710186013.6, Delanium is prepared using high temperature graphitization, then
Charing is mixed with pitch again and prepares fast charge graphite lithium ion battery negative material.Although this method is the nothing on Graphite Coating
Sizing charcoal, but need multiple high temp to be heat-treated, complex process, high energy consumption, and surface coated charcoal is without high temperature graphitization
Processing, the fault of construction of unformed charcoal is more, and the efficiency first of material is low, poor circulation.
The content of the invention
It is an object of the invention to provide simple fast charge graphite cathode material of a kind of technique and preparation method thereof, by excellent
Select the less graphite presoma of grain diameter to shorten the path of lithium ion disengaging migration, while covered and changed by the unformed charcoal bag in surface
The anisotropy of kind graphite, improves the charge-discharge magnification performance of graphite material, while ensures high efficiency, the high appearance first of graphite
Amount and long cycle life.
To achieve the above object, technical scheme is as follows：
A kind of preparation method of fast charge graphite cathode material, it is characterised in that it comprises the steps：
（1）Graphite presoma is mixed with covering material；
（2）Under inert gas shielding, 2 ~ 10h of heat treatment is carried out in 300 ~ 800 DEG C；
（3）Graphitization.
Step（1）In, described graphite presoma mixes for the one or more of petroleum coke, needle coke or native graphite
Close；The average grain diameter D50 of graphite presoma is 3 ~ 10 μm, and described graphite presoma and the mass ratio of described covering material are
50:50~97:3。
Step（1）In, described covering material is that phenolic resin, furfuryl alcohol resin, epoxy resin, polyurethane, carbohydrate are organic
The one or any several mixing of thing.Covering material generally also contains O and/or N element, in high temperature in addition to containing C, H element
Easily it is changed into the hard charcoal of the undefined structure with rock-steady structure during graphitization, it is difficult to be transformed into graphite.Asphalt or
The essential element of coal tar pitch is C, H, and the structure of unformed charcoal can not be kept in high temperature graphitization, can be transformed into lamellar graphite,
Therefore it is different from the covering material.
Step（1）In, the average grain diameter D50 of described covering material is 1 ~ 30 μm, described graphite presoma with it is described
Covering material mass ratio be 50:50~97:3.
Step（1）In, the hybrid mode of the graphite presoma and covering material mixed for double-spiral conical mixer or
Person's liquid phase mixes, and incorporation time is 1 ~ 5h.Wherein, the solvent used in liquid phase hybrid mode is water or alcohol, solid content≤
70%。
Step（2）In, the inert gas is nitrogen, argon gas or decomposed ammonia.
Step（3）In, described graphitization temperature is 2500 ~ 3000 DEG C, and described graphitization time is 20 ~ 60h.Graphite
Change is handled, and graphite presoma is changed into graphite, ensures the high power capacity of negative material, while the coating qualitative change on surface is knot
The stable unformed charcoal of structure, ensure the high charge-discharge magnification of negative material, the high cycle performance of efficiency and length first.
Step（3）In, described graphitization step, in addition to batch mixing and screening.
Wherein, the mixing of batch mixing generally use double-spiral conical mixer or Horizontal type mixer mixing.The screening
Generally use oscillatory type screening machine sieves or gas flow sizing machine classification.The lot stability of material is ensured by batch mixing, screening is then
Ensure the regular appearance of material product, average grain diameter D50 reaches 5 ~ 20 μm, optimizes the high rate performance of material.
The invention provides fast charge graphite cathode material made from described fast charge graphite cathode material preparation method.It is flat
Equal particle diameter D50 can be between 5 ~ 20 μm, and specific surface area is in 3.0m2/ below g.
The present invention is handled by simple low-temperature treatment and high temperature graphitization, and it is kernel, unformed charcoal directly to form graphite
For the graphite material of the similar graphitized intermediate-phase carbosphere of shell, there is high capacity, high efficiency first, high discharge and recharge
Multiplying power and long cycle performance.High temperature graphitization processing forms constitutionally stable unformed charcoal bag coating, than graphite or soft carbon
Big interlamellar spacing is advantageous to lithium ion and quickly transmitted with electrolyte interface in material, so as to ensure that the high charge-discharge magnification of material
With excellent cycle performance.
Compared with the technical scheme of existing fast charge graphite cathode material, the invention has the advantages that：
1）In preparation process, constitutionally stable unformed charcoal bag is covered and graphite precursor graphitization while carried out, and technique is simple,
Cost is cheap.
2）The fast charge graphite lithium ion battery negative material of preparation has high power capacity, Gao Shouxiao, high magnification and macrocyclic concurrently
Advantage.
3）Graphite is firmly combined with the unformed charcoal bag coating in surface, and material electrolyte compatibility is good, easy to process.
Brief description of the drawings
Fig. 1 is the electron scanning micrograph of fast charge graphite cathode material in embodiments of the invention 2（SEM）
Embodiment
Fast charge graphite cathode material of the present invention and preparation method thereof is described in detail below in conjunction with the accompanying drawings.It should manage
Solution, specific embodiment described herein are of the invention not for limiting only to explain the present invention.
Using prepared graphite cathode material as active material in example 1 below ~ 4 and comparative example 1 ~ 2, it is made
2032 type button cells, with the chemical property of graphite cathode material prepared by assessment.Wherein, metal lithium sheet is made to electrode, and 1
mol/L LiPF6EC/DMC（Volume ratio is 1:1）Solution make electrolyte, the micro-pore septums of Celgard 2400 make barrier film.
Embodiment 1
By needle coke（D50 is 7.0 μm）4kg, phenolic resin（D50 is 5.0 μm）1kg is alternately added in double-spiral conical mixer
2h is mixed, is then transferred in heat-treated under medium temperature stove, and is heated to 500 DEG C of heat treatment 4h under nitrogen protection, naturally cools to room
Temperature, then at 3000 DEG C of progress 36h graphitization processings, fast charge graphite cathode material is made after batch mixing screening.
Embodiment 2
By petroleum coke（D50 is 5.0 μm）4.5kg, starch（D50 is 15.0 μm）0.5kg is alternately added double-spiral conical mixer
Middle mixing 2h, is then transferred in heat-treated under medium temperature stove, and is heated to 600 DEG C of heat treatment 3h under nitrogen protection, naturally cools to
Room temperature, then at 2800 DEG C of progress 48h graphitization processings, fast charge graphite cathode material is made after batch mixing screening.
Embodiment 3
By spherical natural graphite（D50 is 8.0 μm）4.5kg, glucose（25% aqueous solution）2kg is added in liquid phase coating machine and mixed
2h, then it is spray-dried, dry powder is transferred in heat-treated under medium temperature stove, and is heated to 550 DEG C of heat treatments under nitrogen protection
5h, room temperature is naturally cooled to, then at 2900 DEG C of progress 48h graphitization processings, fast charge graphite cathode material is made after batch mixing screening
Material.
Embodiment 4
By petroleum coke（D50 is 7.0 μm）2kg, native graphite（D50 is 8.0 μm）2kg and polyurethane（D50 is 5.0 μm）1kg is handed over
4h is mixed for adding in double-spiral conical mixer, is then transferred in heat-treated under medium temperature stove, and be heated to 650 under nitrogen protection
DEG C heat treatment 4h, naturally cools to room temperature, then at 2800 DEG C of progress 48h graphitization processings, fast charge stone is made after batch mixing screening
Black negative material.
Comparative example 1
By needle coke（D50 is 7.0 μm）4kg is placed directly within heat-treated under medium temperature stove, and is heated to 500 DEG C of heat under nitrogen protection
4h is handled, naturally cools to room temperature, then at 3000 DEG C of progress 36h graphitization processings, Delanium is made after batch mixing screening and bears
Pole material.
Comparative example 2
By needle coke（D50 is 7.0 μm）4kg, asphalt（D50 is 5.0 μm）1kg is alternately added in double-spiral conical mixer
2h is mixed, is then transferred in heat-treated under medium temperature stove, and is heated to 500 DEG C of heat treatment 4h under nitrogen protection, naturally cools to room
Temperature, then at 3000 DEG C of progress 36h graphitization processings, artificial plumbago negative pole material is made after batch mixing screening.
Electric performance test：
Can be to the capacity of battery and efficiency is effectively commented first to the volume tests of battery 0.1C low current discharge and recharges in the 1st week
Valency, and the capacity of the 2nd week 1C high current charge-discharge and the big I of ratio of surveying capacity on the 1st week effectively assess its charge-discharge magnification
Performance, separately the ratio size of the capacity under 0.5C electric currents after charge and discharge cycles some cycles and capacity first be then used to assess material
The cycle performance quality of material.
In this embodiment to each embodiment and the first Zhou Rongliang of comparative example, efficiency test, multiplying power test first
And the volume test after circulation in 100 weeks, condition are：Under room temperature condition, battery is subjected to constant current under 0.1C current density
Discharge and recharge 1 week, then carries out constant current charge-discharge the 2nd week under 1C current density, is finally carried out under 0.5C current density
Constant current charge-discharge 100 weeks, voltage range are 0.005 ~ 2.0 V, the first all charging capacitys of record battery, first efficiency, are filled within the 2nd week
The ratio of capacitance and the 1st week charging capacity（It is designated as 1C/0.1C）, the 102nd week charging capacity and the 3rd week charging capacity ratio
（It is designated as 100 weeks circulation conservation rates）.
The capacity in comparative example 1 is can be seen that from the data in table 1（357.8mAh/g）, efficiency first
（90.4%）, 1C/0.1C ratios（55.2%）And 100 weeks circulation conservation rates（90.5%）Relatively low, this explanation graphite presoma is direct
Graphited electrical property is bad.In comparative example 2, capacity（359.5mAh/g）, efficiency first（92.5%）, 1C/0.1C ratios
（65.3%）And 100 weeks circulation conservation rates（94.2%）Slightly increase, the lamellar graphite clad that this explanation pitch is formed can
Improve its electrical property to a certain degree.In embodiment 1, capacity（360.95mAh/g）Efficiency first（92.8%）It is slightly increased, but
It is 1C/0.1C ratios（80.8%）And 100 weeks circulation conservation rates（96.4%）Significantly improve, this explanation phenolic resin graphitization shape
Into constitutionally stable unformed charcoal covered effect be significantly better than pitch graphitization formed graphite charcoal covered effect.From implementation
It is equal to have given play to 1C/0.1C ratios as can be seen that the fast charge graphite cathode material prepared using the method for the invention for example 1 ~ 4
Excellent electrical more than 80% with 100 weeks circulation conservation rates more than 95%.
It should be readily apparent to one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not limiting
The system present invention, all any modification, equivalent and improvement for obtaining being done within spirit and principle in the present invention etc., all should be included
Within the scope of the present invention.
Claims (7)
1. a kind of preparation method of fast charge graphite cathode material, it is characterised in that it comprises the steps：
（1）Graphite presoma is mixed with covering material；
（2）Under inert gas shielding, 2 ~ 10h of heat treatment is carried out in 300 ~ 800 DEG C；
（3）Graphitization.
2. the preparation method of fast charge graphite cathode material as claimed in claim 1, it is characterised in that step（1）In, it is described
Graphite presoma is one or more of mixing of petroleum coke, needle coke or native graphite.
3. the preparation method of fast charge graphite cathode material as claimed in claim 1, it is characterised in that step（1）In, the stone
The average grain diameter D50 of black presoma is 3 ~ 10 μm, and the mass ratio of described graphite presoma and covering material is 50:50~97:3.
4. the preparation method of fast charge graphite cathode material as claimed in claim 1, it is characterised in that step（1）In, it is described
Covering material is phenolic resin, furfuryl alcohol resin, epoxy resin, polyurethane, the one or any several mixing of carbohydrate organic matter.
5. the preparation method of fast charge graphite cathode material as claimed in claim 1, it is characterised in that step（1）In, the bag
The average grain diameter D50 for covering material is 1 ~ 30 μm, and the mass ratio of described graphite presoma and described covering material is 50:50~
97:3。
6. the preparation method of fast charge graphite cathode material as claimed in claim 1, it is characterised in that step（3）In, it is described
Graphitization temperature is 2500 ~ 3000 DEG C, and described graphitization time is 20 ~ 60h.
It is 7. fast made from a kind of preparation method of fast charge graphite cathode material as described in any one of claim 1 ~ 6 claim
Graphite cathode material is filled, its average grain diameter D50 is between 5 ~ 20 μm, and specific surface area is in 3.0m2/ below g.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109748587A (en) * | 2018-12-29 | 2019-05-14 | 湖南中科星城石墨有限公司 | A kind of high capacity fast charge graphite cathode material and preparation method thereof |
| CN110642247A (en) * | 2019-09-30 | 2020-01-03 | 广东凯金新能源科技股份有限公司 | Artificial graphite negative electrode material, preparation method thereof and lithium ion battery |
| CN111115622A (en) * | 2019-12-25 | 2020-05-08 | 广东凯金新能源科技股份有限公司 | Quick-charging graphite and manufacturing method thereof |
| CN112421001A (en) * | 2020-11-04 | 2021-02-26 | 成都爱敏特新能源技术有限公司 | High-rate double-layer coated graphite negative electrode material, lithium ion battery and preparation method of lithium ion battery |
| CN112563453A (en) * | 2020-12-10 | 2021-03-26 | 珠海冠宇电池股份有限公司 | Negative plate and lithium ion battery comprising same |
| CN112582592A (en) * | 2020-12-11 | 2021-03-30 | 成都爱敏特新能源技术有限公司 | High-compaction and fast-filling artificial graphite material and preparation method thereof |
| CN114388727A (en) * | 2020-10-21 | 2022-04-22 | 深圳格林德能源集团有限公司 | Thick negative pole piece and preparation method thereof |
| CN115520860A (en) * | 2022-09-27 | 2022-12-27 | 大理宸宇储能新材料有限公司 | High-sulfur Jiao Gaixing and method for preparing quick-charging graphite anode material and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109748587A (en) * | 2018-12-29 | 2019-05-14 | 湖南中科星城石墨有限公司 | A kind of high capacity fast charge graphite cathode material and preparation method thereof |
| CN109748587B (en) * | 2018-12-29 | 2021-09-17 | 湖南中科星城石墨有限公司 | High-capacity quick-charging graphite negative electrode material and preparation method thereof |
| CN110642247A (en) * | 2019-09-30 | 2020-01-03 | 广东凯金新能源科技股份有限公司 | Artificial graphite negative electrode material, preparation method thereof and lithium ion battery |
| CN111115622A (en) * | 2019-12-25 | 2020-05-08 | 广东凯金新能源科技股份有限公司 | Quick-charging graphite and manufacturing method thereof |
| CN114388727A (en) * | 2020-10-21 | 2022-04-22 | 深圳格林德能源集团有限公司 | Thick negative pole piece and preparation method thereof |
| CN112421001A (en) * | 2020-11-04 | 2021-02-26 | 成都爱敏特新能源技术有限公司 | High-rate double-layer coated graphite negative electrode material, lithium ion battery and preparation method of lithium ion battery |
| CN112421001B (en) * | 2020-11-04 | 2022-02-25 | 成都爱敏特新能源技术有限公司 | High-rate double-layer coated graphite negative electrode material, lithium ion battery and preparation method of lithium ion battery |
| CN112563453A (en) * | 2020-12-10 | 2021-03-26 | 珠海冠宇电池股份有限公司 | Negative plate and lithium ion battery comprising same |
| CN112582592A (en) * | 2020-12-11 | 2021-03-30 | 成都爱敏特新能源技术有限公司 | High-compaction and fast-filling artificial graphite material and preparation method thereof |
| CN112582592B (en) * | 2020-12-11 | 2022-07-19 | 成都爱敏特新能源技术有限公司 | High-compaction and fast-filling artificial graphite material and preparation method thereof |
| CN115520860A (en) * | 2022-09-27 | 2022-12-27 | 大理宸宇储能新材料有限公司 | High-sulfur Jiao Gaixing and method for preparing quick-charging graphite anode material and application thereof |
| CN115520860B (en) * | 2022-09-27 | 2024-01-23 | 大理宸宇储能新材料有限公司 | High-sulfur Jiao Gaixing and method for preparing quick-charge graphite anode material and application thereof |
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Application publication date: 20180119 |