CN109768235A - A kind of lithium ion battery negative material and preparation method thereof - Google Patents
A kind of lithium ion battery negative material and preparation method thereof Download PDFInfo
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- CN109768235A CN109768235A CN201811582042.5A CN201811582042A CN109768235A CN 109768235 A CN109768235 A CN 109768235A CN 201811582042 A CN201811582042 A CN 201811582042A CN 109768235 A CN109768235 A CN 109768235A
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention belongs to the technical field of lithium ion battery, it is specifically related to a kind of lithium ion battery negative material and preparation method thereof.The negative electrode material is the composite material that unformed meso-porous carbon material adulterates that nitrogen-atoms is formed, wherein unformed meso-porous carbon material is to be formed by high molecular foam material by carbonization in advance.Since the porous structure of the doping nitrogen-atoms of controlledly synthesis out effectively improves the specific capacity and cycle performance of lithium ion battery, the volume expansion and the problem of low specific capacity in charge and discharge process of the lithium ion battery negative material of prior art preparation is overcome, the specific capacity and cyclical stability of lithium ion battery are effectively improved.
Description
Technical field
The invention belongs to the technical field of lithium ion battery, it is specifically related to a kind of lithium ion battery negative material and its system
Preparation Method.
Background technique
Can charging-discharging lithium ion battery (LIBs) be always leading practical energy storage technology, as a kind of key energy storage fill
It sets, lithium ion battery (LIBs) is widely used to portable consumer electronics, electric car and hybrid vehicle.Graphite due to
Its high coulomb efficiency, stability and safety and the negative electrode material for being commonly used as business.However it there is also some disadvantages, examples
Such as low (the 372mAh g of theoretical specific capacity-1).Researcher has been carried out a large amount of effort and looks for and develop for next generation LIB
Negative electrode material replace graphite.Usually, it is desirable that lithium ion battery negative material meets claimed below to realize that high power is forthright
Can: (1) Li+Fast transfer and abjection;(2) high conductivity (swift electron migration);(3) shorten Li+Length between electronics
Degree;(4) quick Li+With the structural stability in electronic transmission process.Therefore for maximizing Li+/ electronics transfer and shortening pass
The strategy of defeated approach is highly desirable to.Due to the good combination of stratified pore architectures, excellent stability and big surface area, layering are situated between
Hole porous carbon materials have performance outstanding, such as catalysis, absorption, energy storage and conversion in various applications.
In the past few decades, it is quickly grown by the petroleum base polymeric material that non-renewable resources manufacture, they have been answered
For extensive field, such as civilian, industrial and military installations.Polystyrene (PS) is a kind of tree synthesized by styrene (SM)
Rouge belongs to one of five kinds of general thermoplastic synthetic resins.Polystyrene has excellent processability, low cost and excellent machinery
Performance is widely used in biomedicine, household products, electronic and electrical industry, food containers and packaging etc..However polystyrene exists
A large amount of heat and toxic hazard are readily ignited and released in combustion process, and which has limited it in electronics and electrical industry
Development and potential application, it is therefore necessary to for polystyrene add efficient flame-retarding agent to improve its fire protecting performance.
Summary of the invention
It is an object of the invention to a kind of lithium ion battery negative material and its system are provided for above-mentioned defect
Preparation Method, which is the composite material that unformed meso-porous carbon material adulterates that nitrogen-atoms is formed, wherein unformed mesoporous carbon
Material is to be formed by high molecular foam material by carbonization in advance.Due to the porous structure for the doping nitrogen-atoms that controlledly synthesis comes out
The effective specific capacity and cycle performance for improving lithium ion battery, overcomes the lithium ion battery negative material of prior art preparation
The volume expansion and the problem of low specific capacity in charge and discharge process, specific capacity and the circulation for effectively improving lithium ion battery are steady
It is qualitative.The preparation method is led to after high molecular foam material is dry using high molecular material foaming synthesis high molecular foam material
Pre- carbonization is crossed, unformed meso-porous carbon material is obtained, then unformed meso-porous carbon material and thiocarbamide are prepared through high-temperature calcination without fixed
The lithium ion battery negative material of type meso-porous carbon material doping nitrogen-atoms.
The technical solution of the present invention is as follows: a kind of lithium ion battery negative material is that unformed meso-porous carbon material adulterates nitrogen-atoms
It is formed
Composite material, wherein unformed meso-porous carbon material is to be formed by high molecular foam material by carbonization in advance.
A kind of preparation method of the lithium ion battery negative material, first foams high molecular material；Then to
Foaming knot
The resulting high molecular foam material of reaction is collected after beam to be carbonized in advance, and unformed meso-porous carbon material is obtained；Finally by nothing
Sizing meso-porous carbon material and thiocarbamide, which are placed in tube furnace, carries out high-temperature calcination to get unformed meso-porous carbon material doping nitrogen-atoms
Composite material.
The mass ratio of the unformed meso-porous carbon material and thiocarbamide is 1:1.
The mass ratio of the unformed meso-porous carbon material and thiocarbamide is 1:3.
The mass ratio of the unformed meso-porous carbon material and thiocarbamide is 1:5.
The high molecular material is polystyrene.
The preparation method of the lithium ion battery negative material, comprising the following steps:
(1) high molecular foam material: Polystyrene powder is dried first；Then by the Polystyrene powder of drying, fire retardant
Melt blending in bispin screw rod is placed in foaming agent and is squeezed out；The stick of all extrusions is finally subjected to water-bath cooling, is granulated,
It is dry, obtain high molecular foam material；
(2) pre- carbonization: high molecular foam material obtained by step (1) is placed in the calcining of tube furnace high temperature, is obtained after calcining
Unformed meso-porous carbon material；
(3) high-temperature calcination: being placed in the calcining of tube furnace high temperature for unformed meso-porous carbon material and thiocarbamide obtained by step (2), cooling
To room temperature to get the composite material of unformed meso-porous carbon material doping nitrogen-atoms.
The preparation method of the lithium ion battery negative material, comprising the following specific steps
(1) high molecular foam material: Polystyrene powder is dried 4 hours at 80~90 DEG C first；Then by the poly- of drying
Styrene powder, fire retardant and foaming agent are placed in melt blending in bispin screw rod and are squeezed out, wherein comparing polyphenyl according to quality
Ethylene: fire retardant: foaming agent 1:2:1；Screw speed is 200rpm, and at least eight screw rod heater is cased on the screw rod, is led to
It crosses screw rod heater control extruding temperature and is followed successively by 5 DEG C, 190 DEG C, 190 DEG C, 190 DEG C, 190 DEG C, 195 DEG C according to the direction of extrusion
With 205 DEG C, the sticks of all extrusions is finally subjected to water-bath cooling to room temperature, is granulated, it is 4 hours dry at 80 DEG C, obtain high score
Sub- foamed material；
(2) pre- carbonization: being placed in the calcining of tube furnace high temperature for high molecular foam material obtained by step (1), and calcination temperature is 800~
900 DEG C, calcination time 4h obtains unformed meso-porous carbon material after calcining；
(3) unformed meso-porous carbon material and thiocarbamide obtained by step (2) high-temperature calcination: are placed in the calcining of tube furnace high temperature, calcining
Temperature is 500 DEG C, calcination time 2h；It is cooled to room temperature to get the composite material of unformed meso-porous carbon material doping nitrogen-atoms.
The invention has the benefit that lithium ion battery negative material of the present invention is the doping of unformed meso-porous carbon material
The composite material that nitrogen-atoms is formed, wherein unformed meso-porous carbon material is to be formed by high molecular foam material by carbonization in advance.
High molecular foam material is prepared by macromolecule foaming technology first, is then carbonized in advance under conditions of high temperature
Obtain unformed meso-porous carbon material, unformed meso-porous carbon material has a biggish specific surface area, and the nanostructure in cavity can be with
Additional cushion space is provided.Situ Nitrogen Doping can not only increase charging capacity simultaneously, can also improve the electrification of carbon material
It learns performance and expands the interlamellar spacing of carbon material because electronic conductivity can be improved in the doping of nitrogen-atoms, be conducive to lithium ion progress
Insertion and abjection, improve the high rate performance of battery.
The unformed meso-porous carbon material doping nitrogen-atoms that the present invention prepares, which is used as lithium ion battery negative material, to be shown
The high rate performance and stability for improving lithium ion battery are write, promotes the capacity and service life of battery, this is to lithium ion battery
Industrialized realize has positive meaning.
Detailed description of the invention
Fig. 1 is the picture of the scanning electron microscope of unformed meso-porous carbon material.
Fig. 2 is the transmission electron microscope picture that unformed meso-porous carbon material adulterates nitrogen-atoms composite material.
Fig. 3 is that prepared unformed meso-porous carbon material adulterates nitrogen-atoms composite material as lithium ion battery negative material
When applied to lithium ion battery current density be 1A g-1Electrochemistry under lower discharging condition recycles figure, and wherein NPC-1 represents real
Example 1 is applied, NPC-3 represents embodiment 2, and NPC-5 represents embodiment 3.
Specific embodiment
Below by embodiment, the invention will be further described.Wherein involved raw material pass through Shanghai Mike
Woods reagent Co., Ltd is purchased.
Embodiment 1
The lithium ion battery negative material is the composite material that unformed meso-porous carbon material adulterates that nitrogen-atoms is formed, wherein without fixed
Type
Meso-porous carbon material is to be formed by high molecular foam material by carbonization in advance.
The preparation method of the lithium ion battery negative material, comprising the following specific steps
(1) high molecular foam material: Polystyrene powder is dried 4 hours at 80 DEG C first, it is therefore an objective to by extra moisture
It gets rid of；Then the Polystyrene powder of drying, fire retardant and foaming agent are placed in melt blending in bispin screw rod and squeezed
Out, wherein according to quality than polystyrene: fire retardant: foaming agent 1:2:1；Screw speed is 200rpm, is covered on the screw rod
There are 8 screw rod heaters, 105 DEG C, 185 DEG C, 190 are followed successively by according to the direction of extrusion by the temperature that the control of screw rod heater squeezes out
DEG C, 190 DEG C, 190 DEG C, 190 DEG C, 195 DEG C and 205 DEG C, the sticks of all extrusions is finally subjected to water-bath cooling to room temperature, is granulated
Cylindrical particle is cut directly by cutting machine, it is 4 hours dry at 80 DEG C, obtain high molecular foam material；
(2) high molecular foam material obtained by step (1) pre- carbonization: is placed in the calcining of tube furnace high temperature, calcination temperature 800
DEG C, calcination time 4h obtains unformed meso-porous carbon material after calcining；
(3) high-temperature calcination: unformed meso-porous carbon material obtained by step (2) and thiocarbamide are placed in tube furnace according to mass ratio 1:1
High-temperature calcination, calcination temperature are 500 DEG C, calcination time 2h；It is cooled to room temperature former to get unformed meso-porous carbon material doping nitrogen
The composite material of son.
As seen from Figure 1, the unformed meso-porous carbon material pattern being prepared is lamellar structure, and is had on lamella many big
Hole and mesoporous.
From Figure 2 it can be seen that the unformed meso-porous carbon material doping nitrogen-atoms composite material of preparation is porous structure.
Embodiment 2
The preparation method of the lithium ion battery negative material, comprising the following specific steps
(1) high molecular foam material: Polystyrene powder is dried 4 hours at 80 DEG C first, it is therefore an objective to by extra moisture
It gets rid of；Then the Polystyrene powder of drying, fire retardant and foaming agent are placed in melt blending in bispin screw rod and squeezed
Out, wherein according to quality than polystyrene: fire retardant: foaming agent 1:2:1；Screw speed is 200rpm, is covered on the screw rod
There are 8 screw rod heaters, 105 DEG C, 185 DEG C, 190 are followed successively by according to the direction of extrusion by the temperature that the control of screw rod heater squeezes out
DEG C, 190 DEG C, 190 DEG C, 190 DEG C, 195 DEG C and 205 DEG C, the sticks of all extrusions is finally subjected to water-bath cooling to room temperature, is granulated,
It is 4 hours dry at 80 DEG C, obtain high molecular foam material；
(2) high molecular foam material obtained by step (1) pre- carbonization: is placed in the calcining of tube furnace high temperature, calcination temperature 900
DEG C, calcination time 4h obtains unformed meso-porous carbon material after calcining；
(3) high-temperature calcination: unformed meso-porous carbon material obtained by step (2) and thiocarbamide are placed in tube furnace according to mass ratio 1:3
High-temperature calcination, calcination temperature are 500 DEG C, calcination time 2h；It is cooled to room temperature former to get unformed meso-porous carbon material doping nitrogen
The composite material of son.
Embodiment 3
The preparation method of the lithium ion battery negative material, comprising the following specific steps
(1) high molecular foam material: Polystyrene powder is dried 4 hours at 80 DEG C first, it is therefore an objective to by extra moisture
It gets rid of；Then the Polystyrene powder of drying, fire retardant and foaming agent are placed in melt blending in bispin screw rod and squeezed
Out, wherein according to quality than polystyrene: fire retardant: foaming agent 1:2:1；Screw speed is 200rpm, is covered on the screw rod
There are 8 screw rod heaters, 105 DEG C, 185 DEG C, 190 are followed successively by according to the direction of extrusion by the temperature that the control of screw rod heater squeezes out
DEG C, 190 DEG C, 190 DEG C, 190 DEG C, 195 DEG C and 205 DEG C, the sticks of all extrusions is finally subjected to water-bath cooling to room temperature, is granulated,
It is 4 hours dry at 80 DEG C, obtain high molecular foam material；
(2) high molecular foam material obtained by step (1) pre- carbonization: is placed in the calcining of tube furnace high temperature, calcination temperature 800
DEG C, calcination time 4h obtains unformed meso-porous carbon material after calcining；
(3) high-temperature calcination: unformed meso-porous carbon material obtained by step (2) and thiocarbamide are placed in tube furnace according to mass ratio 1:5
High-temperature calcination, calcination temperature are 500 DEG C, calcination time 2h；It is cooled to room temperature former to get unformed meso-porous carbon material doping nitrogen
The composite material of son.
As seen from Figure 3, unformed meso-porous carbon material doping nitrogen-atoms composite material prepared by embodiment 3 is as lithium ion
When cell negative electrode material is applied to lithium ion battery, battery has recycled 50 circles under conditions of current density is 1A/g and can also protect
The specific capacity in 600mAh/g is held, and stability is relatively good.
Claims (8)
1. a kind of lithium ion battery negative material, which is characterized in that the negative electrode material is that unformed meso-porous carbon material adulterates nitrogen original
The composite material that son is formed, wherein unformed meso-porous carbon material is to be formed by high molecular foam material by carbonization in advance.
2. a kind of preparation method of lithium ion battery negative material described in claim 1, which is characterized in that first by macromolecule material
Material foams；Then it is collected after to be foamed and reacts resulting high molecular foam material and be carbonized in advance, obtained unformed
Meso-porous carbon material；Finally unformed meso-porous carbon material and thiocarbamide are placed in tube furnace and carry out high-temperature calcination to get unformed Jie
The composite material of hole carbon material doping nitrogen-atoms.
3. the preparation method of lithium ion battery negative material according to claim 2, which is characterized in that described unformed mesoporous
The mass ratio of carbon material and thiocarbamide is 1:1.
4. the preparation method of lithium ion battery negative material according to claim 2, which is characterized in that described unformed mesoporous
The mass ratio of carbon material and thiocarbamide is 1:3.
5. the preparation method of lithium ion battery negative material according to claim 2, which is characterized in that described unformed mesoporous
The mass ratio of carbon material and thiocarbamide is 1:5.
6. the preparation method of lithium ion battery negative material according to claim 2, which is characterized in that the high molecular material
For polystyrene.
7. the preparation method of lithium ion battery negative material according to claim 6, comprising the following steps:
(1) high molecular foam material: Polystyrene powder is dried first；Then by the Polystyrene powder of drying, fire retardant
Melt blending in bispin screw rod is placed in foaming agent and is squeezed out；The stick of all extrusions is finally subjected to water-bath cooling, is granulated,
It is dry, obtain high molecular foam material；
(2) pre- carbonization: high molecular foam material obtained by step (1) is placed in the calcining of tube furnace high temperature, is obtained after calcining
Unformed meso-porous carbon material；
(3) high-temperature calcination: being placed in the calcining of tube furnace high temperature for unformed meso-porous carbon material and thiocarbamide obtained by step (2), cooling
To room temperature to get the composite material of unformed meso-porous carbon material doping nitrogen-atoms.
8. the preparation method of lithium ion battery negative material according to claim 7, comprising the following specific steps
(1) high molecular foam material: Polystyrene powder is dried 4 hours at 80~90 DEG C first；Then by the poly- of drying
Styrene powder, fire retardant and foaming agent are placed in melt blending in bispin screw rod and are squeezed out, wherein comparing polyphenyl according to quality
Ethylene: fire retardant: foaming agent 1:2:1；Screw speed is 200rpm, and at least eight screw rod heater is cased on the screw rod, is led to
It crosses screw rod heater control extrusion temperature and is followed successively by 5 DEG C, 190 DEG C, 190 DEG C, 190 DEG C, 190 DEG C, 195 DEG C according to the direction of extrusion
With 205 DEG C, the sticks of all extrusions is finally subjected to water-bath cooling to room temperature, is granulated, it is 4 hours dry at 80 DEG C, obtain high score
Sub- foamed material；
(2) pre- carbonization: being placed in the calcining of tube furnace high temperature for high molecular foam material obtained by step (1), and calcination temperature is 800~
900 DEG C, calcination time 4h obtains unformed meso-porous carbon material after calcining；
(3) unformed meso-porous carbon material and thiocarbamide obtained by step (2) high-temperature calcination: are placed in the calcining of tube furnace high temperature, calcining
Temperature is 500 DEG C, calcination time 2h；It is cooled to room temperature to get the composite material of unformed meso-porous carbon material doping nitrogen-atoms.
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Citations (5)
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| CN107311140A (en) * | 2017-05-27 | 2017-11-03 | 深圳大学 | A kind of preparation method of lithium ion battery negative material |
| CN107331833A (en) * | 2017-05-27 | 2017-11-07 | 深圳大学 | A kind of preparation method of anode material of lithium-ion battery |
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| CN108622893A (en) * | 2018-03-29 | 2018-10-09 | 深圳大学 | A kind of preparation method and porous carbon materials of porous carbon materials |
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2018
- 2018-12-24 CN CN201811582042.5A patent/CN109768235A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107311140A (en) * | 2017-05-27 | 2017-11-03 | 深圳大学 | A kind of preparation method of lithium ion battery negative material |
| CN107331833A (en) * | 2017-05-27 | 2017-11-07 | 深圳大学 | A kind of preparation method of anode material of lithium-ion battery |
| CN107275578A (en) * | 2017-07-05 | 2017-10-20 | 中国矿业大学 | A kind of method that use nitrogen-doped porous carbon material makes kalium ion battery negative pole |
| CN108166103A (en) * | 2017-12-28 | 2018-06-15 | 北京航空航天大学 | A kind of technique for preparing N doping amorphous carbon nano-fiber for carbon source using chitin and its application in energy storage |
| CN108622893A (en) * | 2018-03-29 | 2018-10-09 | 深圳大学 | A kind of preparation method and porous carbon materials of porous carbon materials |
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Application publication date: 20190517 |