CN110518242A - Hard carbon cathode material and preparation method thereof - Google Patents
Hard carbon cathode material and preparation method thereof Download PDFInfo
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- CN110518242A CN110518242A CN201910744847.3A CN201910744847A CN110518242A CN 110518242 A CN110518242 A CN 110518242A CN 201910744847 A CN201910744847 A CN 201910744847A CN 110518242 A CN110518242 A CN 110518242A
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- hard carbon
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- polyvinyl chloride
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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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
- H01M4/36—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
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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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Abstract
The present invention discloses a kind of preparation method of hard carbon cathode material, includes following steps: a certain amount of polyvinyl chloride (1) being dissolved in the in the mixed solvent of tetrahydrofuran and n,N-Dimethylformamide composition, stirring is until solution becomes transparent viscous liquid；(2) electrostatic spinning is carried out under high voltages, obtains polyvinyl chloride fibre；(3) pyrolysis gained polyvinyl chloride fibre is prepared for a kind of novel hard carbon under high temperature.The polyvinyl chloride fibre that the present invention is obtained by high temperature pyrolysis electrostatic spinning; it is prepared for that a kind of interlamellar spacing is larger, partial size is small and is evenly distributed, the novel hard carbon that surface is smooth; this lesser partial size of hard carbon expands the contact area of electrode and electrolyte; shorten the diffusion path of lithium ion; biggish interlamellar spacing is conducive to the quick deintercalation of lithium ion; significantly improve the chemical property of battery; preparation process of the present invention is simple; production cost is low; and preparation condition is controllable, is appropriate for large-scale production exploitation.
Description
Technical field
The present invention relates to new energy materials field technology, a kind of hard carbon cathode material and preparation method thereof is referred in particular to.
Background technique
Lithium ion battery from early 1990s research and develop and success since, with its superior performance (such as operating voltage is high,
Specific energy height, good cycle, long service life, operating temperature range be wide, memory-less effect, self discharge are small, pollution-free etc. excellent
Point) have become the best battery system of current comprehensive performance.But with portable electronic product miniaturization and lithium ion
Demand of the battery in aviation, military affairs and automobile industry is increasingly vigorous, and the capacity and energy density of battery urgently increase substantially.
Currently, commercial lithium-ion batteries are mainly negative as it using the modified natural graphite and artificial graphite with excellent cycling performance
Pole material, but because of its theoretical specific capacity (LiC6Vs.372mAh/g) lower, therefore people are for Novel high-specific capacity flexible, long circulating
Service life negative electrode material is placed high hopes.
The specific capacity of graphite cathode material has reached the limit, and industry starts sight to invest non-graphite material.Hard carbon
Negative electrode material has the specific capacity for being apparently higher than graphite cathode material, and there is wider intercalation potential and good lithium ion to spread
Coefficient is quickly embedded in convenient for lithium ion without precipitating metal lithium.But due to the limitation of existing hard carbon material preparation method,
Porosity is generally lower, deck structure be not it is very regular, only realize by hard carbon material embedding lithium capacity and reversible capacity relatively
Small, cryogenic property is poor, affects hard carbon material in the practicalization of field of lithium ion battery.Therefore, researcher is being
Make great efforts to improve preparation method, reduces the production cost of hard carbon material.
Summary of the invention
In view of this, in view of the deficiencies of the prior art, the present invention aims to provide a kind of hard carbon cathode materials
Material and preparation method thereof, interlamellar spacing is larger, partial size is small and be evenly distributed, surface it is smooth, while preparation process is simple, is produced into
This is low.
To achieve the above object, the present invention is using following technical solution:
A kind of preparation method of hard carbon cathode material, includes following steps:
(1) a certain amount of polyvinyl chloride is dissolved in the in the mixed solvent of tetrahydrofuran and n,N-Dimethylformamide composition, is stirred
It mixes until solution becomes transparent viscous liquid；
(2) electrostatic spinning is carried out under high voltages, obtains polyvinyl chloride fibre；
(3) pyrolysis gained polyvinyl chloride fibre is prepared for a kind of novel hard carbon under high temperature.
As a preferred embodiment, the polyvinyl chloride molecular weight is in 500-15000.
As a preferred embodiment, the polyvinyl chloride additional amount is 15-25w/V%.
As a preferred embodiment, the mass ratio of the mixed solvent is tetrahydrofuran: n,N-Dimethylformamide=2:
8, one of 3:7,3.5:6.5 and 4:6.
As a preferred embodiment, the electrostatic spinning process detailed process are as follows: under the high voltage of 17KV, PVC solution
Injected with the constant rate of speed of 0.05 mm/min, needle point between collector at a distance from be 12cm.
As a preferred embodiment, in the step (3), pyrolysis is under argon atmosphere, and temperature is 600-900 DEG C, and 0-
Heating rate is 4-8 DEG C/min between 200 DEG C, and 200 DEG C or more heating rates are 1-2 DEG C/min.
A kind of hard carbon cathode material is made using the preparation method of aforementioned hard carbon cathode material.
The present invention has obvious advantages and beneficial effects compared with the existing technology, specifically, by above-mentioned technical proposal
Known to:
The polyvinyl chloride fibre that the present invention is obtained by high temperature pyrolysis electrostatic spinning, is prepared for that a kind of interlamellar spacing is larger, partial size is small
And be evenly distributed, the novel hard carbon that surface is smooth, this lesser partial size of hard carbon expands the contact area of electrode and electrolyte,
The diffusion path of lithium ion is shortened, biggish interlamellar spacing is conducive to the quick deintercalation of lithium ion, significantly improves the electricity of battery
Chemical property, preparation process of the present invention is simple, and production cost is low, and preparation condition is controllable, is appropriate for large-scale production and opens
Hair.
Specific embodiment
Present invention discloses a kind of preparation methods of hard carbon cathode material, include following steps:
(1) a certain amount of polyvinyl chloride is dissolved in the in the mixed solvent of tetrahydrofuran and n,N-Dimethylformamide composition, is stirred
It mixes until solution becomes transparent viscous liquid.The polyvinyl chloride molecular weight is in 500-15000, the polyvinyl chloride additional amount
15-25w/V%；The mass ratio of the mixed solvent be tetrahydrofuran: n,N-Dimethylformamide=2:8,3:7,3.5:6.5 and
One of 4:6.
(2) electrostatic spinning is carried out under high voltages, obtains polyvinyl chloride fibre；The electrostatic spinning process detailed process
Are as follows: under the high voltage of 17KV, PVC solution is injected with the constant rate of speed of 0.05 mm/min, needle point between collector at a distance from be
12cm。
(3) pyrolysis gained polyvinyl chloride fibre is prepared for a kind of novel hard carbon under high temperature.Pyrolysis is temperature under argon atmosphere
It is 600-900 DEG C, and heating rate is 4-8 DEG C/min between 0-200 DEG C, 200 DEG C or more heating rates are 1-2 DEG C/min.
The invention also discloses a kind of hard carbon cathode materials, are made using the preparation method of aforementioned hard carbon cathode material.
With multiple embodiments, invention is further described in detail below:
Embodiment 1:
With the polyvinyl chloride (PVC) of Aladdin purchase for raw material, molecular weight 3000, tetrahydrofuran and n,N-Dimethylformamide
Cosolvent is made in (volume ratio 4:6) mixing, and PVC is dissolved in cosolvent by 20w/V% and is stirred, until solution becomes transparent viscous
Property liquid.Then electrostatic spinning is carried out in the case where applying 17KV voltage, PVC solution is injected with the constant speed of 0.05 mm/min, needle
The distance between point and collector are 12 cm.Pyrolysis temperature is set as 800 DEG C, heating rate is 8 in 0-200 DEG C
DEG C/min, heating rate is 2 DEG C/min between 200-800 DEG C, keeps the temperature 1.5h after reaching 800 DEG C, is finally cooled to room temperature and obtains
To hard carbon.
By the hard carbon sample comminution being prepared at uniform powder, 8:1:1 in mass ratio mixes hard carbon, carbon black, PVDF
It closing, suitable nmp solution is added, stir as homogeneous paste, be coated on copper sheet, coating layer thickness is 200 μm, negative electrode tab is formed,
Then for 24 hours, the pole piece after drying is transferred in glove box for 80 DEG C of vacuum drying, using metal lithium sheet as to electrode, is done being full of
2016 type button cells are assembled into the glove box of dry argon gas.Diaphragm is porous polypropylene film, and electrolyte is 1 mol L-1
LiPF6/ (EC+DEC) solution.By electro-chemical test, under the current density of 12 mA/g, initial reversible capacity is reachable
271mAh/g, head effect are 70%, and the reversible capacity of 215 mAh/g is still kept after 120 circle of circulation.
Embodiment 2:
With the polyvinyl chloride (PVC) of Aladdin purchase for raw material, molecular weight 500, tetrahydrofuran and n,N-Dimethylformamide
Cosolvent is made in (volume ratio 3.5:6.5) mixing, and PVC is dissolved in cosolvent by 15 w/V% and is stirred, until solution becomes
Transparent viscous liquid.Then electrostatic spinning is carried out in the case where applying 17KV voltage, PVC solution is with the constant speed of 0.05 mm/min
Injection, the distance between needle point and collector are 12 cm.Pyrolysis temperature is set as 700 DEG C, heat up speed in 0-200 DEG C
Rate is 5 DEG C/min, and heating rate is 1 DEG C/min between 200-700 DEG C, keeps the temperature 2h after reaching 700 DEG C, is finally cooled to room
Temperature obtains hard carbon.
By the hard carbon sample comminution being prepared at uniform powder, 1:10 in mass ratio is by hard carbon powder and artificial graphite
KSH-201 is uniformly mixed, and is mixed with beating mixture, acetylene black, PVDF in 8:1:1 ratio, appropriate NMP is added and makees solvent, stirs
It mixes as homogeneous paste, is coated on copper sheet, coating layer thickness is 130 μm, forms negative electrode tab, and then 80 DEG C of vacuum drying for 24 hours, are done
Pole piece after dry is transferred in glove box, using metal lithium sheet as to electrode, is assembled into the glove box full of dry argon gas
2016 type button cells.Diaphragm is porous polypropylene film, and electrolyte is 1 mol L-1 LiPF6/ (EC+DEC) solution.Pass through
Electro-chemical test, under 0.1C multiplying power, initial reversible capacity is 382 mAh/g, and head effect is 87%, is still kept after 200 circle of circulation
307 mAh/g, coulombic efficiency is close to 100%.
Comparative example 1:
With the polyvinyl chloride (PVC) of Aladdin purchase for raw material, molecular weight 3000 is put into tube furnace, under an argon atmosphere
Pyrolysis temperature is set as 800 DEG C, heating rate is 8 DEG C/min, heating rate between 200-800 DEG C in 0-200 DEG C
For 2 DEG C/min, 1.5h is kept the temperature after reaching 800 DEG C, room temperature is finally cooled to and obtains hard carbon.
By the hard carbon sample comminution being prepared at uniform powder, 8:1:1 in mass ratio mixes hard carbon, carbon black, PVDF
It closing, suitable nmp solution is added, stir as homogeneous paste, be coated on copper sheet, coating layer thickness is 200 μm, negative electrode tab is formed,
Then for 24 hours, the pole piece after drying is transferred in glove box for 80 DEG C of vacuum drying, using metal lithium sheet as to electrode, is done being full of
2016 type button cells are assembled into the glove box of dry argon gas.Diaphragm is porous polypropylene film, and electrolyte is 1 mol L-1
LiPF6/(EC+DEC) solution.By electro-chemical test, under the current density of 12 mA/g, initial reversible capacity is up to 206
MAh/g, coulombic efficiency is only 59% for the first time.
Design focal point of the invention is: the polyvinyl chloride fibre that the present invention is obtained by high temperature pyrolysis electrostatic spinning, system
For a kind of interlamellar spacing is larger, partial size is small and is evenly distributed, the novel hard carbon that surface is smooth, this lesser partial size of hard carbon expands
The contact area of electrode and electrolyte, shortens the diffusion path of lithium ion, biggish interlamellar spacing is conducive to the fast of lithium ion
Fast deintercalation significantly improves the chemical property of battery, and preparation process of the present invention is simple, and production cost is low, and preparation condition
Controllably, it is appropriate for large-scale production exploitation.
The above described is only a preferred embodiment of the present invention, be not intended to limit the scope of the present invention,
Therefore any subtle modifications, equivalent variations and modifications to the above embodiments according to the technical essence of the invention, still
Belong in the range of technical solution of the present invention.
Claims (7)
1. a kind of preparation method of hard carbon cathode material, it is characterised in that: include following steps:
(1) a certain amount of polyvinyl chloride is dissolved in the in the mixed solvent of tetrahydrofuran and n,N-Dimethylformamide composition, is stirred
It mixes until solution becomes transparent viscous liquid；
(2) electrostatic spinning is carried out under high voltages, obtains polyvinyl chloride fibre；
(3) pyrolysis gained polyvinyl chloride fibre is prepared for a kind of novel hard carbon under high temperature.
2. the preparation method of hard carbon cathode material according to claim 1, it is characterised in that: the polyvinyl chloride molecular weight
In 500-15000.
3. the preparation method of hard carbon cathode material according to claim 1, it is characterised in that: the polyvinyl chloride additional amount
For 15-25w/V%.
4. the preparation method of hard carbon cathode material according to claim 1, it is characterised in that: the quality of the mixed solvent
Ratio is tetrahydrofuran: one of n,N-Dimethylformamide=2:8,3:7,3.5:6.5 and 4:6.
5. the preparation method of hard carbon cathode material according to claim 1, it is characterised in that: the electrostatic spinning process tool
Body process are as follows: under the high voltage of 17KV, PVC solution is injected with the constant rate of speed of 0.05 mm/min, between needle point and collector
Distance is 12cm.
6. the preparation method of hard carbon cathode material according to claim 1, it is characterised in that: in the step (3), pyrolysis
It is under argon atmosphere, temperature is 600-900 DEG C, and heating rate is 4-8 DEG C/min between 0-200 DEG C, and 200 DEG C or more heat up
Rate is 1-2 DEG C/min.
7. a kind of hard carbon cathode material, it is characterised in that: using hard carbon cathode material as claimed in any one of claims 1 to 6
Preparation method is made.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114195119A (en) * | 2021-12-13 | 2022-03-18 | 杭州电子科技大学 | Hard carbon material with wide interlayer spacing and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102637898A (en) * | 2012-04-25 | 2012-08-15 | 东华大学 | Lithium ion battery and preparation method thereof |
| WO2016165633A1 (en) * | 2015-04-14 | 2016-10-20 | Byd Company Limited | Polymer composite membrane and preparation method thereof, gel electrolyte and lithium ion battery having the same |
| CN106711410A (en) * | 2016-12-02 | 2017-05-24 | 北京理工大学 | Battery negative electrode material and preparation method thereof as well as sodium-ion battery |
-
2019
- 2019-08-13 CN CN201910744847.3A patent/CN110518242A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102637898A (en) * | 2012-04-25 | 2012-08-15 | 东华大学 | Lithium ion battery and preparation method thereof |
| WO2016165633A1 (en) * | 2015-04-14 | 2016-10-20 | Byd Company Limited | Polymer composite membrane and preparation method thereof, gel electrolyte and lithium ion battery having the same |
| CN106711410A (en) * | 2016-12-02 | 2017-05-24 | 北京理工大学 | Battery negative electrode material and preparation method thereof as well as sodium-ion battery |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114195119A (en) * | 2021-12-13 | 2022-03-18 | 杭州电子科技大学 | Hard carbon material with wide interlayer spacing and preparation method thereof |
| CN114195119B (en) * | 2021-12-13 | 2023-03-10 | 杭州电子科技大学 | Hard carbon material with wide interlayer spacing and preparation method thereof |
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