CN105489866B - A kind of lithium ion battery and its anode material and preparation method - Google Patents
A kind of lithium ion battery and its anode material and preparation method Download PDFInfo
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- CN105489866B CN105489866B CN201610034453.5A CN201610034453A CN105489866B CN 105489866 B CN105489866 B CN 105489866B CN 201610034453 A CN201610034453 A CN 201610034453A CN 105489866 B CN105489866 B CN 105489866B
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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
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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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- 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 lithium ion battery and its anode material and preparation methods, including silica supported graphene, nano-silicon, amorphous carbon, and graphite, nano-silicon, silica supported graphene, graphite and amorphous carbon mass ratio be 1:(0.1~2): (5~50): (0.5~5).The present invention by nano-silicon, silica supported graphene dispersion in a solvent, by ultrasound, stirring, it is to be mixed uniformly after remove solvent, pass through high-temperature heat treatment under an inert gas, obtain the graphene complex of nano-silicon/silica supported；Again by compound and graphite, organic carbon source dispersion in a solvent, again passes by ultrasound, stirring, and uniformly rear removing solvent to be mixed passes through high-temperature heat treatment secondary, obtains silica/graphene-based Si-C composite material.Of the invention preparation method is simple, with high specific capacity, coulombic efficiency, circulation and good rate capability when the composite material produced is used as negative electrode of lithium ion battery.
Description
[technical field]
The invention belongs to electrode of lithium cell technical fields, and in particular to a kind of lithium ion battery and its anode material and
Preparation method.
[background technique]
Lithium ion battery is big with its specific energy, operating voltage is high, self-discharge rate is small, the advantages such as small in size, light-weight already
Occupy the field 3C major part market.Current commercialized lithium ion battery negative material is mainly graphite, but theoretical capacity is only
372mAhg-1 is not able to satisfy demand of the market to high-energy density gradually.Compared with the traditional graphite negative electrode, silicon has super
High theoretical specific capacity (4200mAh/g) and lower embedding de- lithium current potential (< 0.5V), and the voltage platform of silicon is slightly above graphite,
It is difficult to that surface is caused to analyse lithium in charging, security performance is more preferable.But silicon as lithium ion battery negative material when disadvantage nor
Chang Mingxian.Firstly, silicon is semiconductor material, the conductivity of itself is lower；Secondly, in electrochemistry cyclic process, lithium ion
Insertion and abjection can make the expansion and contraction of 300% or more silica-base material volume generation, and resulting mechanicals efforts can make
Silica-base material gradually dusting, causes structure collapses, eventually leads to electrode active material and collector is detached from, lose electrical contact, into
And the cycle performance of lithium ion battery is substantially reduced.It is mainly carbon-coated by then carrying out silicon particle nanosizing at present
Method improves the cycle performance of silicon based anode material, however, the silicon-carbon composite cathode material cycle performance prepared is still not
The requirement of industrial application can be reached.
The mixture of silicon and silica stress as caused by volume change when silica can mitigate silicon charge and discharge, institute
With compared with silicon, cycle performance is more excellent.However, since the mixture of silicon and silica lacks electric conductivity, for battery
Speech, discharge capacity significantly reduces at higher current densities.Therefore, it is necessary to design a kind of novel composite material, make it simultaneously
Meet high circulation performance and high rate capability, the application of silicon substrate composite negative pole material could be made to obtain big breakthrough.
[summary of the invention]
In view of the above-mentioned deficiencies in the prior art, the technical problem to be solved by the present invention is that providing a kind of specific capacity
Height, coulombic efficiency height, good cycle, high rate performance good lithium ion battery and its anode material and preparation method.
The invention adopts the following technical scheme:
A kind of composite cathode material of lithium ion battery, including silica supported graphene, nano-silicon, amorphous carbon, with
And graphite, nano-silicon, silica supported graphene, graphite and amorphous carbon mass ratio be 1:(0.1~2): (5~50):
(0.5~5).
Further, nano-silicon is having a size of 10~200nm.
Further, silica supported graphene is obtained by being loaded on graphene oxide in situ after teos hydrolysis
?.
Further, agraphitic carbon is mainly that organic carbon source obtains after high temperature pyrolysis.
A kind of preparation method of composite cathode material of lithium ion battery, comprising the following steps:
1) in a solvent by nano-silicon, silica supported graphene dispersion, by ultrasound, stirring, it is to be mixed uniformly after
Solvent is removed, after being then raised to 600 DEG C~1000 DEG C under nitrogen and/or ar gas environment with the heating rate of 2~10 DEG C/min
Keep 0.5~for 24 hours, obtain the graphene complex of nano-silicon/silica supported；
2) compound and graphite obtained step 1), organic carbon source disperse in a solvent, to again pass by ultrasound, stirring,
Uniformly rear removing solvent to be mixed, is then raised to 600 under nitrogen and/or ar gas environment with the heating rate of 2~10 DEG C/min
DEG C~1000 DEG C after keep 0.5~for 24 hours, obtain silica/graphene-based Si-C composite material.
Further, solvent include water, ethyl alcohol, methanol, ethylene glycol, N-Methyl pyrrolidone, in NN- dimethylformamide
It is one or more.
Further, remove solvent mode be heating stirring be evaporated, be spray-dried, one of rotary evaporation.
Further, the organic carbon source in step 2 includes phenolic resin, melamine resin, epoxy resin, Vinylidene Chloride, drip
One of blueness is a variety of, compound and graphite, and the weight ratio of organic carbon source is 1:(5~150): (0.55~15).
A kind of lithium ion battery, including anode and cathode, cathode include anode material.
Further, composite material and binder, conductive agent, dispersing agent are tuned into slurry, are coated on copper foil, and through vacuum
Dry, roll-in is prepared into negative electrode tab；Anode uses metal lithium sheet, and dispersing agent is the water and ethyl alcohol that volume ratio is 1:3.
Compared with prior art, the present invention at least have the advantages that it is of the invention preparation method is simple, it is raw
With high specific capacity and coulombic efficiency when the composite material of output is used as negative electrode of lithium ion battery；The composite wood produced
There is the performance of good circulation and high rate performance when material is used as negative electrode of lithium ion battery.
[specific embodiment]
The present invention provides a kind of composite cathode material of lithium ion battery mainly by nano-silicon, silica supported graphite
Alkene, graphite and agraphitic carbon composition.Wherein, nano-silicon is having a size of 10~200nm, nano-silicon, silica supported graphene, stone
The mass ratio of ink and amorphous carbon is 1:(0.1~2): (5~50): (0.5~5).Silica supported graphene is by positive silicic acid
It loads on graphene oxide and obtains in situ after ethyl ester hydrolysis, agraphitic carbon is mainly that organic carbon source obtains after high temperature pyrolysis
It arrives.
The addition of silica supported graphene has both sides beneficial effect to electrode active material.Firstly, nano-silicon
Compound-the nano-silicon formed at high temperature with silica supported graphene/silica supported graphene complex can have
The volume expansion problem for alleviating material in nano-silicon charge and discharge process of effect, to increase the cycle performance of material.Secondly, graphite
The excellent electric conductivity of alkene increases the electric conductivity of composite cathode material of lithium ion battery, reduces the polarization phenomena of material, and
And the internal resistance of battery is reduced, so that lithium ion battery has good high rate performance.
The present invention provides a kind of preparation methods of composite cathode material of lithium ion battery, comprising the following steps:
1) to be mixed equal by ultrasound, stirring by nano-silicon, silica supported graphene dispersion in the first solvent
Solvent is removed after even, after being then raised to 600 DEG C~1000 DEG C under nitrogen or ar gas environment with the heating rate of 2~10 DEG C/min
Keep 0.5~for 24 hours, obtain the graphene complex of nano-silicon/silica supported；
2) compound and graphite, organic carbon source that step 1) obtains are dispersed in the second solvent, again pass by ultrasound, stirs
It mixes, then uniformly rear removing solvent to be mixed is raised to 600 under nitrogen or ar gas environment with the heating rate of 2~10 DEG C/min
DEG C~1000 DEG C after keep 0.5~for 24 hours, obtain silica/graphene-based Si-C composite material.
Wherein, the first solvent and the second solvent respectively include water, ethyl alcohol, methanol, ethylene glycol, N-Methyl pyrrolidone, NN-
One of dimethylformamide is a variety of.The mode for removing solvent is that heating stirring is evaporated, is spray-dried, in rotary evaporation
It is a kind of.
Organic carbon source in step 2 includes one of phenolic resin, melamine resin, epoxy resin, Vinylidene Chloride, pitch
Or a variety of, compound and graphite, the weight ratio of organic carbon source are 1:(5~150): (0.55~15).
In order to further illustrate the present invention, compound to lithium-ion capacitor cathode provided by the invention with reference to embodiments
Material and preparation method thereof is described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
1) the silica supported graphene oxide of 1 parts by weight nano-silicon, 0.1 parts by weight is dispersed in water, ultrasound
30min, stirring, it is to be mixed uniformly after at 80 DEG C heating stirring water is evaporated, then under a nitrogen, with the heating speed of 2 DEG C/min
Degree keeps the temperature the graphene complex for obtaining nano-silicon/silica supported for 24 hours after being raised to 600 DEG C；
2) compound and 11 parts by weight of graphite obtained 1 parts by weight step 1), 15 parts by weight of phenolic resin are dispersed in second
In alcohol, ultrasonic 30min, stirring, it is to be mixed uniformly after at 80 DEG C heating stirring ethyl alcohol is evaporated, then under a nitrogen, with 2 DEG C/
The heating rate of min is kept the temperature after being raised to 600 DEG C obtains required silica/graphene-based silicon-carbon cathode composite material for 24 hours.
Embodiment 2
1) the silica supported graphene oxide of 1 parts by weight nano-silicon, 2 parts by weight is dispersed in water, ultrasonic 30min,
Stirring, it is to be mixed uniformly after at 80 DEG C heating stirring water is evaporated, then under a nitrogen, be raised to the heating rate of 10 DEG C/min
The graphene complex for obtaining nano-silicon/silica supported for 24 hours is kept the temperature after 1000 DEG C；
2) compound and 150 parts by weight of graphite obtained 1 parts by weight step 1), 0.55 parts by weight melamine resin are dispersed in
In ethyl alcohol, ultrasonic 30min, stirring, it is to be mixed uniformly after at 80 DEG C heating stirring ethyl alcohol is evaporated, then under a nitrogen, with 10
DEG C/heating rate of min keeps the temperature after being raised to 1000 DEG C and obtains required silica/graphene-based silicon-carbon cathode composite wood for 24 hours
Material.
Embodiment 3
1) in ethanol by the silica supported graphene oxide dispersion of 1 parts by weight nano-silicon, 1 parts by weight, ultrasound
30min, stirring, it is to be mixed uniformly after at 80 DEG C heating stirring ethyl alcohol is evaporated, then under a nitrogen, with the heating of 10 DEG C/min
Speed keeps the temperature 0.5h after being raised to 800 DEG C, obtains the graphene complex of nano-silicon/silica supported；
2) compound and 5 parts by weight of graphite obtained 1 parts by weight step 1), 1 parts by weight pitch disperse in ethanol, to surpass
Sound 30min, stirring, it is to be mixed uniformly after at 80 DEG C heating stirring ethyl alcohol is evaporated, then under argon gas, with the liter of 10 DEG C/min
Warm speed keeps the temperature 0.5h after being raised to 800 DEG C, obtains required silica/graphene-based silicon-carbon cathode composite material.
Embodiment 4
1) in methyl alcohol by the silica supported graphene oxide dispersion of 1 parts by weight nano-silicon, 0.2 parts by weight, ultrasound
30min, stirring, it is to be mixed uniformly after at 80 DEG C heating stirring methanol is evaporated, then under argon gas, with the heating of 5 DEG C/min
Speed keeps the temperature 8h after being raised to 800 DEG C, obtains the graphene complex of nano-silicon/silica supported；
2) compound and 10 parts by weight of graphite obtained 1 parts by weight step 1), 1 parts by weight epoxy resin are dispersed in ethyl alcohol
Middle ultrasound 30min, stirring, it is to be mixed uniformly after at 80 DEG C heating stirring ethyl alcohol is done, then under argon gas, with 10 DEG C/min's
Heating rate keeps the temperature 4h after being raised to 800 DEG C, obtains required silica/graphene-based silicon-carbon cathode composite material.
Embodiment 5
1) the silica supported graphene oxide of 1 parts by weight nano-silicon, 0.1 parts by weight is dispersed in water, ultrasound
30min, stirring, it is to be mixed uniformly after at 80 DEG C heating stirring water is evaporated, then under a nitrogen, with the heating speed of 2 DEG C/min
Degree keeps the temperature the graphene complex for obtaining nano-silicon/silica supported for 24 hours after being raised to 600 DEG C；
2) compound and 11 parts by weight of graphite obtained 1 parts by weight step 1), 15 parts by weight Vinylidene Chloride are dispersed in second
In alcohol, ultrasonic 30min, stirring are to be mixed to be uniformly spray-dried, obtained powder under a nitrogen, with the heating of 2 DEG C/min
Speed is kept the temperature after being raised to 600 DEG C obtains required silica/graphene-based silicon-carbon cathode composite material for 24 hours.
Embodiment 6
1) in methyl alcohol by the silica supported graphene oxide dispersion of 1 parts by weight nano-silicon, 0.2 parts by weight, ultrasound
30min, stirring, it is to be mixed uniformly after at 80 DEG C heating stirring methanol is evaporated, then under argon gas, with the heating of 5 DEG C/min
Speed keeps the temperature 8h after being raised to 800 DEG C, obtains the graphene complex of nano-silicon/silica supported；
2) compound and 10 parts by weight of graphite obtained 1 parts by weight step 1), the dispersion of 1 parts by weight pitch surpass in ethanol
Sound 30min, stirring, it is to be mixed uniformly after at 80 DEG C rotary evaporation be evaporated, then under argon gas, with the heating rate of 10 DEG C/min
4h is kept the temperature after being raised to 800 DEG C, obtains required silica/graphene-based silicon-carbon cathode composite material.
A kind of lithium ion battery, including anode and cathode, cathode include anode material, composite material and binder,
Conductive agent, dispersing agent are tuned into slurry, are coated on copper foil, and vacuum dried, and roll-in is prepared into negative electrode tab；Anode is using gold
Belong to lithium piece, dispersing agent is the water and ethyl alcohol that volume ratio is 1:3.
Composite material prepared by Example 1~6 is as negative electrode material, with binder (LA132), conductive agent (Super-
P it) is tuned into slurry with dispersing agent (water and ethyl alcohol, volume ratio position 1:3), is coated on copper foil, and vacuum dried, roll-in, preparation
At negative electrode tab；Anode use metal lithium sheet, the organic electrolyte used be 1M LiPF6/EC+PC+DEC (molar ratio 1:1:
1), diaphragm is polypropylene, and CR2025 type button cell is made.Test condition is room temperature, charge and discharge under 0.1C, charging/discharging voltage limit
It is made as 0.005~1.5V, the experimental results showed that, after charge and discharge cycles 300 times, negative electrode of lithium ion battery provided by the invention is multiple
The specific capacity of condensation material is maintained at 80% or more；With high specific capacity and coulombic efficiency；Good circulation performance and forthright again
Energy.
The half-cell test performance for the composite material being prepared by the method for the present invention is as follows:
| Embodiment performance | 1 | 2 | 3 | 4 | 5 | 6 |
| Discharge capacity (mAh/g) for the first time | 821 | 402 | 683 | 649 | 438 | 656 |
| Coulombic efficiency (%) for the first time | 85.6 | 95.4 | 89.5 | 90.7 | 92.1 | 89.2 |
| Specific discharge capacity (mAh/g) after recycling 300 weeks | 694 | 379 | 573 | 566 | 393 | 568 |
| Recycle 300 weeks capacity retention ratios (%) | 73.0 | 94.2 | 83.9 | 87.2 | 89.9 | 86.7 |
Graphene and nano-silicon are dispersed in by graphene-based Si-C composite material prepared by the present invention during the preparation process
In solvent, be conducive to the dispersion of the two, it is suppressed that the reuniting effect of nano material also improves the dispersion effect of silicon well.
In addition, preparation method is simple for the composite cathode material of lithium ion battery of this hair offer, degree of being practical is high,
Raw material is easy to get, and reduces production cost, conducive to the extensive use of lithium ion battery, and the graphene-based Si-C composite material prepared
Capacity with higher greatly improves the cycle performance of silica-base material.
Claims (10)
1. a kind of composite cathode material of lithium ion battery, it is characterised in that: including silica supported graphene, nano-silicon, nothing
Shape carbon and graphite, the nano-silicon, silica supported graphene, graphite and amorphous carbon mass ratio be 1:(0.1
~2): (5~50): (0.5~5)；When preparation, first in a solvent by nano-silicon, silica supported graphene dispersion, pass through
Ultrasound, stirring, uniformly rear removing solvent to be mixed, then with the heating rate of 2~10 DEG C/min under nitrogen or ar gas environment
Keep 0.5 after being raised to 600 DEG C~1000 DEG C~for 24 hours, obtain the graphene complex of nano-silicon/silica supported；By what is obtained
Graphene complex disperses in a solvent, to again pass by ultrasound, stirring with graphite, organic carbon source, and uniformly rear removing to be mixed is molten
Agent, after being then raised to 600 DEG C~1000 DEG C under nitrogen or ar gas environment with the heating rate of 2~10 DEG C/min keep 0.5~
For 24 hours, silica/graphene-based Si-C composite material is obtained.
2. composite cathode material of lithium ion battery according to claim 1, which is characterized in that the nano-silicon is having a size of 10
~200nm.
3. composite cathode material of lithium ion battery according to claim 1, which is characterized in that the silica supported stone
Black alkene is obtained by being loaded on graphene oxide in situ after teos hydrolysis.
4. composite cathode material of lithium ion battery according to claim 1, which is characterized in that the agraphitic carbon is organic
Carbon source obtains after high temperature pyrolysis.
5. a kind of based on a kind of preparation method of composite cathode material of lithium ion battery described in claim 1, including following step
It is rapid:
1) in a solvent by nano-silicon, silica supported graphene dispersion, by ultrasound, stirring, uniformly rear removing to be mixed
Solvent keeps 0.5 after being then raised to 600 DEG C~1000 DEG C under nitrogen or ar gas environment with the heating rate of 2~10 DEG C/min
~for 24 hours, obtain the graphene complex of nano-silicon/silica supported；
2) compound for obtaining step 1) and graphite, organic carbon source dispersion in a solvent, again pass by ultrasound, stirring, to mixed
Solvent is removed after closing uniformly, is then raised to 600 DEG C~1000 under nitrogen or ar gas environment with the heating rate of 2~10 DEG C/min
After DEG C keep 0.5~for 24 hours, obtain silica/graphene-based Si-C composite material.
6. a kind of preparation method of composite cathode material of lithium ion battery according to claim 5, it is characterised in that: described
Solvent is one of water, ethyl alcohol, methanol, ethylene glycol, N-Methyl pyrrolidone, NN- dimethylformamide or a variety of.
7. a kind of preparation method of composite cathode material of lithium ion battery according to claim 5, it is characterised in that: described
Remove solvent mode be heating stirring be evaporated, be spray-dried, one of rotary evaporation.
8. a kind of preparation method of composite cathode material of lithium ion battery according to claim 5, it is characterised in that: described
Organic carbon source in step 2 includes one of phenolic resin, melamine resin, epoxy resin, Vinylidene Chloride, pitch or a variety of,
The compound and graphite, the weight ratio of organic carbon source are 1:(5~150): (0.55~15).
9. a kind of lithium ion battery, including anode and cathode, which is characterized in that negative electrode material is according to claim 5-8
The preparation method of composite cathode material of lithium ion battery and obtain.
10. a kind of lithium ion battery according to claim 9, it is characterised in that: the composite material and binder, conduction
Agent, dispersing agent are tuned into slurry, are coated on copper foil, and vacuum dried, and roll-in is prepared into negative electrode tab；The anode is using gold
Belong to lithium piece, the dispersing agent is the water and ethyl alcohol that volume ratio is 1:3.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106744916A (en) * | 2016-12-21 | 2017-05-31 | 上海杉杉科技有限公司 | A kind of method of modifying of high rate lithium ionic cell cathode material |
| CN107204445B (en) * | 2017-05-26 | 2019-07-19 | 郑州中科新兴产业技术研究院 | A kind of lithium ion battery three-dimensional porous silicon-carbon cathode material and preparation method thereof |
| CN108232139B (en) * | 2017-12-20 | 2020-08-28 | 中国科学院福建物质结构研究所 | Graphene composite material and preparation method thereof |
| CN108565437B (en) | 2018-05-18 | 2019-06-11 | 国家能源投资集团有限责任公司 | Si-C composite material and its preparation method and application |
| CN108565401B (en) | 2018-05-18 | 2020-12-15 | 国家能源投资集团有限责任公司 | Amorphous carbon material and preparation method and application thereof |
| CN110911731B (en) * | 2018-09-14 | 2021-01-19 | 江苏师范大学 | Preparation method of composite lithium battery |
| CN111063872A (en) * | 2019-12-10 | 2020-04-24 | 中国科学院山西煤炭化学研究所 | Silicon-carbon negative electrode material and preparation method thereof |
| CN114583148B (en) * | 2022-03-05 | 2024-04-16 | 青岛泰达华润新能源科技有限公司 | Preparation method of silicon oxide-based graphite composite anode material for lithium ion battery |
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