CN108777303A - A kind of biomass derived hard carbon/graphene anode material of lithium-ion battery and preparation method thereof - Google Patents
A kind of biomass derived hard carbon/graphene anode material of lithium-ion battery and preparation method thereof Download PDFInfo
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- CN108777303A CN108777303A CN201810531471.3A CN201810531471A CN108777303A CN 108777303 A CN108777303 A CN 108777303A CN 201810531471 A CN201810531471 A CN 201810531471A CN 108777303 A CN108777303 A CN 108777303A
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- biomass
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- ion battery
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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
- H01M4/362—Composites
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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 biomass derived hard carbon/graphene anode material of lithium-ion battery and preparation method thereof, this method first dissolves biomass to obtain biomass solution, and graphene oxide and biomass solution are then pressed 1:The mass ratio of 0.01-0.1 uniformly mixes, and obtains mixed solution, then obtain the negative material by centrifugation, washing, freeze-drying, high-temperature calcination respectively.The preparation method uses sol-gel method, first biomass is dissolved, then it is mixed with graphene uniform, breaks through the upright method for connecing high-temperature calcination and obtaining hard carbon of standard biologic, composite effect can be effectively improved, and then promotes performance of the material as sodium-ion battery cathode.Graphene does not occur significantly to reunite in negative material of the present invention, and is well combined with biomass derived hard carbon；Under the current density of 1A/g, after recycling 1000 times, specific capacity may remain in 210.2mAh/g, so it is with higher specific capacitance and good cycle performance.
Description
Technical field
The present invention relates to electrochemical material technical field more particularly to a kind of biomass derived hard carbon/graphene sodium ions
Cell negative electrode material and preparation method thereof.
Background technology
Increasingly failure with fossil fuel energy and its caused environmental problem, demand day of the mankind for new energy
It is beneficial urgent, and wherein lithium ion battery has been widely used in Mobile portable formula electronic equipment, and be also to rise recently
The first choice of new-energy automobile power battery.But lithium is not a kind of abundant resource, the content in the earth's crust only has
0.0065%.Sodium-ion battery has similar operation principle with lithium ion battery, and sodium resource reserve is abundant, and exploitation is simple,
It is cheap, to the advantage that cannot be compared with lithium ion battery.On the other hand, relative to lithium ion battery, sodium ion
Radius be 1.5 times of lithium ion, cause graphitic carbon interlamellar spacing (0.335nm) to be unfavorable for the embedding de- process of sodium ion, therefore negative
Pole material needs more researchs.
In recent years, hard carbon material applies the research in sodium-ion battery gradually to increase as negative material.Yuliang
[Nano Letters, 2012,12 (7) such as Cao:3783-3787] pyrolysis hollow Nano line presoma prepare hollow Nano carbon line,
It applies in sodium-ion battery, shows 251mAh g-1High reversible specific capacity and 82.2% capacity retention ratio (cycle
After 400 weeks).Although hard carbon presents good performance and becomes a kind of negative material for most having application prospect, but prepare
The presoma of hard carbon is generally artificial synthesized resin, these presomas cause since cost is higher and it is very low to produce carbon rate
The higher price of hard carbon, to considerably increase the cost of sodium-ion battery, it is difficult to its advantage is highlighted in huge competition,
So the price for how reducing hard carbon is the key that realize that it is applied in inexpensive sodium-ion battery.
In the presoma of numerous hard carbons, biomass as carbon source with its environment friendly, it is at low cost the features such as, become system
The focus of standby hard carbon material.Yunming Li et al. [Journal of Materials Chemistry A, 2015,3 (1):
71-77] using sucrose as carbon source, using two-step method (low-temperature hydrothermal-high temperature carbonization) different pyrolysis temperatures (1000 DEG C, 1300 DEG C,
1600 DEG C) carbon ball is prepared, when pyrolysis temperature is 1600 DEG C, electrode material shows best chemical property, is recycling 100 weeks
Reversible specific capacity 290mAh/g later, capacity retention ratio 93%.Tingzhou Yang etc. [Advanced Materials,
2016,28(3):539-545] using the bean dregs of rich nitrogen as raw material, nitrogen-doped carbon thin slice is prepared, specific capacity of the cycle after 50 weeks is protected
It holds in 247.5mAh/g.Although above method specific capacity is higher, still remain that irreversible capacity is big, high rate performance is poor and decaying
Soon, stablize the problem of cyclicity difference.Some researches show that the interfacial property that package is expected to improvement material is carried out to hard carbon material, can press down
With electrolyte side reaction occurs for carbon base body processed.
Graphene is to pass through sp by carbon atom2Hybrid form interconnects and the two-dimensional material of the monatomic thickness of formation,
Since it is with higher sodium ion diffusion coefficient, therefore desirable for having excellent high rate performance.However in actual use, it passes through
Often since the reunion of graphene sheet layer leads to the reduction of energy density and power density.Therefore, the dilute reunion of graphite how is reduced
Seem extremely important.
It is graphene and biomass derived hard carbon is compound, on the one hand, to effectively reduce the dilute reunion of graphite, make it more
It plays a role well；On the other hand, the interfacial property that hard carbon material can be improved, it is secondary to inhibit carbon base body and electrolyte to occur
Reaction.This is a kind of effective thinking of high-performance anode material of lithium-ion battery design.
In addition, the hard carbon that method described in document is prepared is the direct high-temperature calcination of biomass, be unfavorable for
Graphene it is compound.
In view of this, a kind of biomass derived hard carbon/graphene anode material of lithium-ion battery of present invention offer and its system
Preparation Method.
Invention content
Based on the above the deficiencies in the prior art, technical problem solved by the invention is to provide a kind of biomass derived hard
Carbon graphite alkene anode material of lithium-ion battery and preparation method thereof, graphene does not occur significantly to reunite in the negative material, and
It is well combined with biomass derived hard carbon, and there is higher specific capacitance and good cycle performance；Preparation method uses
Sol-gel method first dissolves biomass, then it is mixed with graphene uniform, can effectively improve composite effect, Jin Erti
Rise performance of the material as sodium-ion battery cathode.
It is negative that in order to solve the above technical problem, the present invention provides a kind of biomass derived hard carbon/graphene sodium-ion batteries
Some or all of pole material preparation method, including following technical characteristic：
A kind of preparation method of biomass derived hard carbon/graphene anode material of lithium-ion battery, includes the following steps：First
Biomass is dissolved to obtain biomass solution, then graphene oxide and biomass solution are uniformly mixed in proportion, mixed
Solution is closed, then obtains the negative material by centrifugation, washing, freeze-drying, high-temperature calcination respectively.
As an improvement of the above technical solution, the mass ratio of biomass derived and graphene is 1 in the mixed solution:
0.01-0.1。
As an improvement of the above technical solution, in the mixed solution graphene oxide a concentration of 2-8mg/mL.
As an improvement of the above technical solution, the biomass includes native cellulose, starch, chitin etc..
As an improvement of the above technical solution, the washing methods is specially：Using deionized water, methanol, ethyl alcohol, N-N
Any one or two kinds of washed products in methylene formamide 2-6 times.
As an improvement of the above technical solution, the high-temperature burning process carries out in argon gas atmosphere, heating rate 4-8
DEG C/min, calcination temperature is 600-800 DEG C, insulation reaction 2-4h.
The technical solution of the application can also be accomplished by the following way, and biomass derived is prepared using the above method
Hard carbon/graphene anode material of lithium-ion battery.
Compared with prior art, technical scheme of the present invention has the advantages that：
1) graphene does not occur significantly to reunite in the negative material, and is well combined with biomass derived hard carbon；In 1A/
Under the current density of g, after recycling 1000 times, specific capacity may remain in 210.2mAh/g, so it is with higher specific capacitance
And good cycle performance；
2) preparation method uses sol-gel method, first dissolves biomass, then it is mixed with graphene uniform, dashes forward
The upright method for connecing high-temperature calcination and obtaining hard carbon of broken standard biologic, preparation method of the present invention can effectively improve compound effect
Fruit, and then promote performance of the material as sodium-ion battery cathode.
Above description is only the general introduction of technical solution of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, and in order to allow the above and other objects, features and advantages of the present invention can
It is clearer and more comprehensible, below in conjunction with preferred embodiment, detailed description are as follows.
Description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, will simply be situated between to the attached drawing of embodiment below
It continues.
Fig. 1 is the SEM figures of biomass derived hard carbon/grapheme material prepared by the embodiment of the present invention 1；
Fig. 2 is the TEM figures of biomass derived hard carbon/grapheme material prepared by the embodiment of the present invention 1；
Fig. 3 is biomass derived hard carbon/grapheme material of the preparation of the embodiment of the present invention 3 as sodium-ion battery cathode material
The performance test results figure of material.
Specific implementation mode
The following detailed description of the present invention specific implementation mode, as part of this specification, by embodiment come
Illustrate that the principle of the present invention, other aspects of the present invention, feature and its advantage will become apparent by the detailed description.
Embodiment 1
According to cellulose：Graphene oxide=1：0.1 mass ratio takes the graphene oxide of a concentration of 4mg/ml of 20ml molten
Liquid, the cellulose solution that 20g mass fractions are 4wt% are in flask, and magnetic agitation for 24 hours, it is equal to obtain graphene dispersion under room temperature
Even collosol-gelatum system.The sol-gel is tied up to again under the rotating speed of 7000rpm and is centrifuged at 15 DEG C, centrifugation gained is heavy
Shallow lake deionized water and ethyl alcohol respectively washing 3 times, are then freeze-dried, obtain cellulose/graphene complex.Again by the compound
Be transferred in tube furnace, 700 DEG C be warming up to 6 DEG C/min in argon gas atmosphere, heat preservation 2h to get to biomass derived hard carbon/
Graphene complex.
The preparation process of cellulose solution used in the present embodiment is：By NaOH, urea, deionized water in mass ratio 7：
12：81 are mixed to get mixed solution, which is cooled to -12.3 DEG C in advance, and 8g cottons are added to the mixed of the precooling immediately
It closes in solution (200ml), quickly stirs 3min, obtain transparent cellulose solution.This solution centrifuges under the rotating speed of 7000rpm
Deaeration obtains the transparency cellulose solution of mass fraction about 4wt%.
The SEM figures and TEM figures of biomass derived hard carbon/graphene complex prepared by embodiment 1 are respectively such as Fig. 1 and Fig. 2
It is shown.As can be seen from Figure 1, product is laminated composites, and porosity is high, and apparent agglomeration does not occur for graphene；From Fig. 2
It can be seen that, graphene is well combined with biomass derived hard carbon, and graphene uniform is wrapped on hard carbon outer layer.
Embodiment 2
According to chitin：Graphene oxide=1：0.01 mass ratio takes the graphene oxide of a concentration of 4mg/ml of 2ml molten
Liquid, the chitin solution that 20g mass fractions are 4wt% are in flask, and magnetic agitation for 24 hours, it is equal to obtain graphene dispersion under room temperature
Even collosol-gelatum system.The sol-gel is tied up to again under the rotating speed of 7000rpm and is centrifuged at 15 DEG C, centrifugation gained is heavy
Shallow lake deionized water and ethyl alcohol respectively washing 3 times, are then freeze-dried, obtain chitin/graphene complex.Again by the compound
Be transferred in tube furnace, 700 DEG C be warming up to 6 DEG C/min in argon gas atmosphere, heat preservation 2h to get to biomass derived hard carbon/
Graphene complex.
The preparation process of chitin solution used in the present embodiment is：By KOH, urea, deionized water in mass ratio 7：
12：81 are mixed to get mixed solution, which is cooled to -12.5 DEG C in advance, and the lobster shell of 8g washes cleans is added immediately
Into the mixed solution (200ml) of the precooling, 3min is quickly stirred, obtains transparent chitin solution.This solution is in 7000rpm
Rotating speed under evacuation and centrifugal degassing, obtain the transparent chitin solution of mass fraction about 4wt%.
Embodiment 3
According to cellulose：Graphene oxide=1：0.05 mass ratio, take 10ml graphene oxide solutions (2mg/ml) with
For 10g cellulose solutions (4wt%) in flask, magnetic agitation for 24 hours, obtains the uniform collosol-gelatum system of graphene dispersion.Again
The sol-gel is tied up under the rotating speed of 7000rpm and is centrifuged at 15 DEG C, centrifugation gained precipitation deionized water and ethyl alcohol is each
Washing 3 times, is then freeze-dried, obtains cellulose/graphene complex.It transfers them in tube furnace again, in argon atmosphere
In with 6 DEG C/min be warming up to 700 DEG C, keep the temperature 2h, both biomass derived hard carbon/graphene complex.Fiber in the present embodiment
The preparation process of plain solution is same as above.
Performance test
Biomass derived hard carbon/graphene complex prepared by embodiment 3 is as anode material of lithium-ion battery in 1A/g
For specific capacity under current density as shown in figure 3, after cycle 1000 times, specific capacity is still maintained at 210.2mAh/g, illustrates it
With higher specific capacitance and good cycle performance.
The above is the preferred embodiment of the present invention, cannot limit the right model of the present invention with this certainly
It encloses, it is noted that for those skilled in the art, without departing from the principle of the present invention, may be used also
To make several improvement and variation, these are improved and variation is also considered as protection scope of the present invention.
Claims (7)
1. a kind of preparation method of biomass derived hard carbon/graphene anode material of lithium-ion battery, which is characterized in that including with
Lower step：First biomass is dissolved to obtain biomass solution, then uniformly mixes graphene oxide and biomass solution in proportion
It closes, obtains mixed solution, then obtain the negative material by centrifugation, washing, freeze-drying, high-temperature calcination respectively.
2. a kind of preparation side of biomass derived hard carbon/graphene anode material of lithium-ion battery according to claim 1
Method, which is characterized in that the mass ratio of biomass and graphene is 1 in the mixed solution:0.01-0.1.
3. a kind of preparation side of biomass derived hard carbon/graphene anode material of lithium-ion battery according to claim 1
Method, which is characterized in that a concentration of 2-8mg/mL of graphene oxide in the mixed solution.
4. a kind of preparation side of biomass derived hard carbon/graphene anode material of lithium-ion battery according to claim 1
Method, which is characterized in that the biomass includes native cellulose, starch, chitin.
5. a kind of preparation side of biomass derived hard carbon/graphene anode material of lithium-ion battery according to claim 1
Method, which is characterized in that the washing methods is specially：Using appointing in deionized water, methanol, ethyl alcohol, N-N methylene formamides
Meaning one or two kinds of washed products 2-6 times.
6. a kind of preparation side of biomass derived hard carbon/graphene anode material of lithium-ion battery according to claim 1
Method, which is characterized in that high-temperature burning process carries out in argon gas atmosphere, and heating rate is 4-8 DEG C/min, calcination temperature 600-
800 DEG C, insulation reaction 2-4h.
7. a kind of biomass derived hard carbon prepared according to any one of claim 1-6 the methods/graphene sodium ion electricity
Pond negative material, which is characterized in that biomass derived hard carbon/graphene anode material of lithium-ion battery uses above-mentioned preparation side
Method.
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Cited By (8)
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| CN109950520A (en) * | 2019-03-15 | 2019-06-28 | 深圳市本征方程石墨烯技术股份有限公司 | A kind of nitrogenous graphene coated biomass carbon negative electrode material and preparation method thereof |
| CN113839034A (en) * | 2021-09-23 | 2021-12-24 | 深圳华算科技有限公司 | Sodium ion battery negative electrode material, preparation method thereof and sodium ion battery |
| CN114156456A (en) * | 2021-12-08 | 2022-03-08 | 西北工业大学 | High-capacity rapid charge-discharge graphene @ hard carbon composite material, preparation method thereof and application of composite material in sodium ion battery |
| CN114506841A (en) * | 2022-04-19 | 2022-05-17 | 中科南京绿色制造产业创新研究院 | Biomass-graphene composite electrode material and preparation method and application thereof |
| CN114873579A (en) * | 2022-05-10 | 2022-08-09 | 山东能源集团有限公司 | Composite carbon microsphere, preparation method and application thereof |
| CN115020668A (en) * | 2022-06-27 | 2022-09-06 | 广州鹏辉能源科技股份有限公司 | Carbon-based negative electrode for sodium/potassium ion battery and preparation method thereof |
| CN115974045A (en) * | 2022-12-06 | 2023-04-18 | 江西师范大学 | Method for preparing hard carbon by chemical gel synergistic basic metal oxide template method and application thereof |
| CN116845222A (en) * | 2023-08-16 | 2023-10-03 | 湖南金阳烯碳新材料股份有限公司 | Hard carbon/graphene composite anode material for sodium ion battery and preparation method thereof |
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| CN109950520A (en) * | 2019-03-15 | 2019-06-28 | 深圳市本征方程石墨烯技术股份有限公司 | A kind of nitrogenous graphene coated biomass carbon negative electrode material and preparation method thereof |
| CN109950520B (en) * | 2019-03-15 | 2022-05-31 | 深圳市本征方程石墨烯技术股份有限公司 | Nitrogen-containing graphene-coated biomass carbon negative electrode material and preparation method thereof |
| CN113839034A (en) * | 2021-09-23 | 2021-12-24 | 深圳华算科技有限公司 | Sodium ion battery negative electrode material, preparation method thereof and sodium ion battery |
| CN114156456A (en) * | 2021-12-08 | 2022-03-08 | 西北工业大学 | High-capacity rapid charge-discharge graphene @ hard carbon composite material, preparation method thereof and application of composite material in sodium ion battery |
| CN114506841A (en) * | 2022-04-19 | 2022-05-17 | 中科南京绿色制造产业创新研究院 | Biomass-graphene composite electrode material and preparation method and application thereof |
| CN114506841B (en) * | 2022-04-19 | 2022-07-08 | 中科南京绿色制造产业创新研究院 | Biomass-graphene composite electrode material with controllable interlayer structure and preparation method and application thereof |
| CN114873579A (en) * | 2022-05-10 | 2022-08-09 | 山东能源集团有限公司 | Composite carbon microsphere, preparation method and application thereof |
| CN115020668A (en) * | 2022-06-27 | 2022-09-06 | 广州鹏辉能源科技股份有限公司 | Carbon-based negative electrode for sodium/potassium ion battery and preparation method thereof |
| CN115974045A (en) * | 2022-12-06 | 2023-04-18 | 江西师范大学 | Method for preparing hard carbon by chemical gel synergistic basic metal oxide template method and application thereof |
| CN115974045B (en) * | 2022-12-06 | 2024-02-13 | 江西师范大学 | Method for preparing hard carbon by chemical gel synergistic alkaline metal oxide template method and application thereof |
| CN116845222A (en) * | 2023-08-16 | 2023-10-03 | 湖南金阳烯碳新材料股份有限公司 | Hard carbon/graphene composite anode material for sodium ion battery and preparation method thereof |
| CN116845222B (en) * | 2023-08-16 | 2024-02-20 | 湖南金阳烯碳新材料股份有限公司 | Hard carbon/graphene composite anode material for sodium ion battery and preparation method thereof |
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