CN110098407A - Carbon-based storage sodium negative electrode material, its application and preparation method - Google Patents
Carbon-based storage sodium negative electrode material, its application and preparation method Download PDFInfo
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- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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Abstract
The invention discloses a kind of carbon-based storage sodium negative electrode material, its application and preparation methods, carbon-based storage sodium negative electrode material is made of biomass-based hard carbon material, the interlamellar spacing of hard carbon is not less than 0.37nm, the hard carbon interlamellar spacing much larger than graphite layers away from, the deintercalation gap structure of sodium ion is formed, realization reversibly stores sodium ion.The preparation method of biomass-based anode material of lithium-ion battery includes: that will clean containing tea polyphenols and polyhydroxy aldehyde/ketone biomass material；Then the raw material after vacuum drying cleaning；It grinds the raw material after drying to obtain granular precursor again；Then under inert gas protection, granular precursor is subjected to high temperature cabonization processing, it is cooling up to carbon-based storage sodium negative electrode material.The present invention selects biological material to carry out above-mentioned process, and raw material sources are extensive, environmental-friendly, and gained hard carbon cathode material has excellent sodium insertion and abjection ability, good cycling stability, reversible specific capacity high.
Description
Technical field
The present invention relates to a kind of sodium-ion battery, its application and preparation methods, more particularly to a kind of sodium-ion battery
Electrode material, its application and preparation method, are applied to storage sodium material and sodium-ion battery technical field.
Background technique
Currently, global warming, air pollution and the exhaustion of fossil fuel bring huge challenge to the whole mankind, seek
Looking for the energy storage system of safety and long-life just becomes extremely urgent.Currently, sodium-ion battery is considered as before one kind has very much
The material on way, because global resources distribution is abundant, and cost of material is low, and the aluminum that can be used compared with lithium ion battery
Collector cost is also low, is particularly suitable for extensive energy storage.The nearest research hotspot of sodium-ion battery is concentrated mainly on negative electrode material
On, because sodium ion cannot be embedded in graphite linings by graphite as most widely used lithium ion battery negative material.Therefore,
Scientists find negative electrode material that is low in cost and haveing excellent performance in urgent.Currently, mainly there is the cathode material of following classification
Material: carbon material, metal oxide and organic compound.Wherein, amorphous hard carbon seemingly most promising material, due to its nothing
Existing defects and gap in sequence structure, it can reversibly store sodium atom.This makes hard carbon have high reversible capacity, low sodium storage
Deposit voltage and excellent cyclical stability.
Although hard carbon material, which is used as anode material of lithium-ion battery, has high chemical property, realizing that its industry is raw
There are still two huge obstructions before producing application: cost of material height and first all low efficiencys.Because hard carbon cathode surface defect is more,
It will form fine and close SEI when it is contacted with electrolyte, cause polarization very big, therefore first all coulombic efficiencies rarely exceed 70%.
The synthesis procedures such as hard carbon material such as phenolic resin traditional simultaneously are complicated, generally need complicated pre-treatment, cost of material is high, high temperature
Carbon low yield is cracked, the first all coulombic efficiencies of traditional hard carbon material are low, and cyclical stability and specific capacity are lower, technique controlling difficulty
Greatly, it is unfavorable for industrial applications and implementation.
Summary of the invention
In order to solve prior art problem, it is an object of the present invention to overcome the deficiencies of the prior art, and to provide one kind
Carbon-based storage sodium negative electrode material, its application and preparation method, prepare sodium ion hard carbon cathode material using biological material, can
It is low with first all coulombic efficiencies to solve the problems, such as existing cost of material height, while ensure that excellent cyclical stability and high ratio
Capacity is suitable for large-scale production.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A kind of carbon-based storage sodium negative electrode material, is made, the interlamellar spacing of hard carbon is not less than of biomass-based hard carbon material
0.37nm, the hard carbon interlamellar spacing is much larger than graphite layers away from forming the deintercalation gap structure of sodium ion, realization reversibly stores sodium
Ion.Preferably hard carbon material is made using containing tea polyphenols and polyhydroxy aldehyde/ketone biomass material in biomass-based hard carbon material.
As currently preferred technical solution, reversible specific capacity is not less than the 0.1C of carbon-based storage sodium negative electrode material for the first time
227.1mAh/g, coulombic efficiency is not less than 79.3% for the first time.
A kind of application of the carbon-based storage sodium negative electrode material of the present invention, is used to prepare sodium-ion battery, battery includes based on biology
The anode material of lithium-ion battery and electrolyte of matter, the electrolyte contain sodium salt NaPF6、NaClO4With in NaTFSI at least
One kind, and the electrolyte also contains selected from nonaqueous solvents ethylene carbonate, diethyl carbonate, propene carbonate, diethylene glycol (DEG)
At least one of dimethyl ether, glycol dimethyl ether and dimethyl carbonate.
As currently preferred technical solution, the application of above-mentioned carbon-based storage sodium negative electrode material, by biomass-based hard carbon material
Material is used as negative electrode active material, is uniformly mixed with sodium alginate according to the mass ratio of 9.5:0.5, negative electrode slurry is made, is coated in
On aluminium foil, it is put into vacuum oven to be not less than at 100 DEG C and dry at least 12h to get hard carbon cathode pole piece.As the present invention
Further preferred technical solution is to use to electrode with metallic sodium piece using the hard carbon cathode pole piece as working electrode
The mixed liquor that EC/DEC is 1:1 and electrolyte concentration is 1.0mol/L is electrolyte, is assembled into sodium under inert gas atmosphere
Ion battery.
A kind of preparation method of the carbon-based storage sodium negative electrode material of the present invention, includes the following steps:
A. pretreatment of raw material:
It is 100% calculating, biological material with the gross mass percentage of biological material using biological material as raw material
Tea polyphenols containing the 20wt% not less than biological material total amount in material, also containing not less than biological material total amount
20wt% polyhydroxy aldehyde or polyhydroxyketone；Biological material is impregnated in deionized water after at least 2 hours, cleans, obtains clean
Net raw material；Above-mentioned biological material preferably uses the blade-section of Theaceae Camellia Plants；
B. the raw material drying obtained after being pre-processed in the step a, and be cooled to room temperature, dry raw material is obtained,
It is spare；As currently preferred technical solution, above-mentioned drying means be vacuum drying mode, drying temperature section be 60~
100 DEG C, being dried the time is 12~24 hours；
C. dry raw material obtained in the step b is ground, obtains hard carbon granular precursor powder；
It is preferred that the particle size interval of above-mentioned granular precursor is 200~500 mesh；
D. under inert protective atmosphere, to be not less than the heating rate of 5 DEG C/min, from room temperature to heat treatment temperature
1200~1600 DEG C of temperature range, and 0.5~10 hour is kept the temperature under temperature condition of heat treatment, it will be obtained in the step c
The hard carbon granular precursor powder arrived carries out high temperature cabonization processing, then cools to room temperature with the furnace, to obtain biomass-based hard
Carbon material has high reversible capacity with hard carbon, has low sodium stored voltage and excellent cyclical stability.
The present invention compared with prior art, has following obvious prominent substantive distinguishing features and remarkable advantage:
1. the method for the present invention selects biological material to carry out high temperature cabonization process, biomass material source used is wide
General, process flow is simple, environmental-friendly, without complicated pre-treatment, has greatly saved production cost；
2. hard carbon cathode material of the present invention has excellent sodium insertion and abjection ability, it is used as sodium-ion battery cathode, it is first
All coulombic efficiencies are high, good cycling stability, and reversible specific capacity is high, are suitble in industrial circle large-scale application.
Detailed description of the invention
Fig. 1 is the SEM photograph of biomass-based anode material of lithium-ion battery made from the embodiment of the present invention one.
Fig. 2 is the XRD diagram of biomass-based anode material of lithium-ion battery made from the embodiment of the present invention one.
Fig. 3 is all charging and discharging curves of head of the biomass-based anode material of lithium-ion battery of the embodiment of the present invention one.
Fig. 4 is the cycle performance curve of the biomass-based anode material of lithium-ion battery of the embodiment of the present invention one.
Specific embodiment
Above scheme is described further below in conjunction with specific implementation example, the preferred embodiment of the present invention is described in detail such as
Under:
Embodiment one:
In the present embodiment, a kind of carbon-based storage sodium negative electrode material, with former containing tea polyphenols and polyhydroxy aldehyde/ketone biomass
Material is made hard carbon material, and the interlamellar spacing of hard carbon is not less than 0.37nm, the hard carbon interlamellar spacing much larger than graphite layers away from, formed sodium from
The deintercalation gap structure of son, realization reversibly store sodium ion, and reversible specific capacity is not less than 245.3mAh/g to 0.1C for the first time,
Coulombic efficiency is not less than 80.8% for the first time.
In the present embodiment, the preparation method of the carbon-based storage sodium negative electrode material of a kind of the present embodiment, includes the following steps:
A. pretreatment of raw material:
Using Green tea biological material as raw material, Green tea biological material is the blade part of Theaceae Camellia Plants
Point, it is 100% calculating with the gross mass percentage of Green tea biological material, contains in Green tea biological material raw not less than green tea
The tea polyphenols of the 20wt% of material total amount, also containing not less than Green tea biological material total amount 20wt% polyhydroxy aldehyde or
Polyhydroxyketone；At room temperature, Green tea biological material is put into container, deionized water is added, immersion treatment 2 hours, cleans
For several times, clean raw material is obtained；
B. obtained raw material is put into vacuum oven after pre-processing in the step a, using vacuum drying mode,
Controlling drying temperature is 100 DEG C, and being dried the time is 12 hours, is dried, and be cooled to room temperature, and obtains dry original
Material, it is spare；
C. dry raw material obtained in the step b is put into agate mortar, is ground, makes presoma
The partial size of particle reaches 200~500 mesh, obtains hard carbon granular precursor powder；
D. the hard carbon granular precursor powder obtained in the step c is put into crucible, then crucible is placed in vacuum
In tube furnace, under inert protective atmosphere, with the heating rate of 5 DEG C/min, from room temperature to 1400 DEG C of heat treatment temperature, and
2 hours are kept the temperature under constant temperature condition of heat treatment, hard carbon granular precursor powder is subjected to high temperature cabonization processing, then with furnace
Cooled to room temperature is taken out biomass-based hard carbon material, to obtain biomass-based hard carbon material as sample.
A kind of application of the carbon-based storage sodium negative electrode material of the present invention, is used to prepare sodium-ion battery, battery includes based on biology
The anode material of lithium-ion battery and electrolyte of matter, the electrolyte contain NaClO4, from nonaqueous solvents ethylene carbonate EC, carbon
Diethyl phthalate DEC.
Using biomass-based hard carbon material as negative electrode active material, mixed with sodium alginate according to the mass ratio of 9.5:0.5
Uniformly, negative electrode slurry is made, is coated on aluminium foil, is put into vacuum oven with 12h dry at 100 DEG C to get hard carbon cathode
Pole piece.
Using the hard carbon cathode pole piece as working electrode, with metallic sodium piece be to electrode, use EC/DEC for 1:1 and
Electrolyte NaClO4The mixed liquor that concentration is 1.0mol/L is electrolyte, is assembled into sodium-ion battery under an argon atmosphere.
Experimental test and analysis:
The SEM figure of biomass-based hard carbon cathode material obtained by the present embodiment is as shown in Figure 1, the interlayer of hard carbon forms sodium ion
Deintercalation gap structure, realization reversibly store sodium ion.The XRD diagram of biomass-based hard carbon cathode material obtained by the present embodiment is such as
Shown in Fig. 2.The position at d (002) peak is at 23.93 ° as can be seen from Figure 2.According to Bragg equation d (002)=λ/2sin θ
(002), d (002)=0.37nm is calculated in wavelength of the λ for incident X-ray radiation, λ=0.154056nm, 2 θ=23.93 °,
For persursor material after carrying out high temperature carbonization, the interlamellar spacing of hard carbon is 0.37nm, the hard carbon interlamellar spacing much larger than graphite layers away from
(0.335nm) is suitble to the deintercalation of sodium ion, improves reversible specific capacity.
Biomass-based hard carbon material prepared by the present embodiment is negative electrode active material, with sodium alginate according to 9.5:
0.5 mass ratio is uniformly mixed, and negative electrode slurry is made, and is coated on aluminium foil, is put into 100 DEG C of dry 12h in vacuum oven, i.e.,
Obtain hard carbon cathode pole piece.Using the pole piece as working electrode, metallic sodium piece is to use concentration for the NaClO of 1mol/L at electrode4's
The mixed liquor of mixed solvent EC:DEC=1:1 is that electrolyte is assembled into button cell, and survey in the glove box of argon atmosphere
Try its chemical property.As shown in figure 3, the reversible specific capacity of material is 245mAh/g under 0.1C current density.Shown in Fig. 4,
Under 0.1C current density, after circulating battery 200 weeks, specific capacity remains at 225mAh/g.
Embodiment two:
The present embodiment is basically the same as the first embodiment, and is particular in that:
In the present embodiment, the preparation method of the carbon-based storage sodium negative electrode material of a kind of the present embodiment, includes the following steps:
A. pretreatment of raw material:
Using Green tea biological material as raw material, Green tea biological material is the blade part of Theaceae Camellia Plants
Point, it is 100% calculating with the gross mass percentage of Green tea biological material, contains in Green tea biological material raw not less than green tea
The tea polyphenols of the 20wt% of material total amount, also containing not less than Green tea biological material total amount 20wt% polyhydroxy aldehyde or
Polyhydroxyketone；At room temperature, Green tea biological material is put into container, deionized water is added, immersion treatment 2 hours, cleans
For several times, clean raw material is obtained；
B. obtained raw material is put into vacuum oven after pre-processing in the step a, using vacuum drying mode,
Controlling drying temperature is 100 DEG C, and being dried the time is 12 hours, is dried, and be cooled to room temperature, and obtains dry original
Material, it is spare；
C. dry raw material obtained in the step b is put into agate mortar, is ground, makes presoma
The partial size of particle reaches 200~500 mesh, obtains hard carbon granular precursor powder；
D. the hard carbon granular precursor powder obtained in the step c is put into crucible, then crucible is placed in vacuum
In tube furnace, under inert protective atmosphere, with the heating rate of 5 DEG C/min, from room temperature to 1200 DEG C of heat treatment temperature, and
2 hours are kept the temperature under constant temperature condition of heat treatment, hard carbon granular precursor powder is subjected to high temperature cabonization processing, then with furnace
Cooled to room temperature is taken out biomass-based hard carbon material, to obtain biomass-based hard carbon material as sample.In addition to
Biomass-based carbon material resulting in the present embodiment is used as except the negative electrode material of sodium-ion battery, is the same as example 1
Mode assembled battery and test its chemical property.Experimental test and analysis result is shown in the following table 1.
Embodiment three:
The present embodiment is substantially the same as in the previous example, and is particular in that:
In the present embodiment, the preparation method of the carbon-based storage sodium negative electrode material of a kind of the present embodiment, includes the following steps:
A. pretreatment of raw material:
Using Green tea biological material as raw material, Green tea biological material is the blade part of Theaceae Camellia Plants
Point, it is 100% calculating with the gross mass percentage of Green tea biological material, contains in Green tea biological material raw not less than green tea
The tea polyphenols of the 20wt% of material total amount, also containing not less than Green tea biological material total amount 20wt% polyhydroxy aldehyde or
Polyhydroxyketone；At room temperature, Green tea biological material is put into container, deionized water is added, immersion treatment 2 hours, cleans
For several times, clean raw material is obtained；
B. obtained raw material is put into vacuum oven after pre-processing in the step a, using vacuum drying mode,
Controlling drying temperature is 100 DEG C, and being dried the time is 12 hours, is dried, and be cooled to room temperature, and obtains dry original
Material, it is spare；
C. dry raw material obtained in the step b is put into agate mortar, is ground, makes presoma
The partial size of particle reaches 200~500 mesh, obtains hard carbon granular precursor powder；
D. the hard carbon granular precursor powder obtained in the step c is put into crucible, then crucible is placed in vacuum
In tube furnace, under inert protective atmosphere, with the heating rate of 5 DEG C/min, from room temperature to 1600 DEG C of heat treatment temperature, and
2 hours are kept the temperature under constant temperature condition of heat treatment, hard carbon granular precursor powder is subjected to high temperature cabonization processing, then with furnace
Cooled to room temperature is taken out biomass-based hard carbon material, to obtain biomass-based hard carbon material as sample.In addition to
Biomass-based carbon material resulting in the present embodiment is used as except the negative electrode material of sodium-ion battery, is the same as example 1
Mode assembled battery and test its chemical property.Experimental test and analysis result is shown in the following table 1.
The electrochemical property test result after sodium-ion battery is made in 1. the above embodiment of the present invention material of table
It can be seen that the biomass hard carbon cathode material first charge-discharge of the above embodiment of the present invention from table 1 and Fig. 3, Fig. 4
Efficiency is up to 80% or more, and good cycling stability, reversible specific capacity has good chemical property in 240mAh/g or more.
The present invention selects biological material to carry out above-mentioned process, and raw material sources are extensive, environmental-friendly, gained hard carbon cathode material tool
There are excellent sodium insertion and abjection ability, good cycling stability, reversible specific capacity high.
Combination attached drawing of the embodiment of the present invention is illustrated above, but the present invention is not limited to the above embodiments, it can be with
The purpose of innovation and creation according to the present invention makes a variety of variations, under the Spirit Essence and principle of all technical solutions according to the present invention
Change, modification, substitution, combination or the simplification made, should be equivalent substitute mode, as long as meeting goal of the invention of the invention,
Without departing from the technical principle and inventive concept of the carbon-based storage sodium negative electrode material of the present invention, its application and preparation method, belong to
Protection scope of the present invention.
Claims (9)
1. a kind of carbon-based storage sodium negative electrode material, which is characterized in that contain tea polyphenols and polyhydroxy aldehyde/ketone biomass material system
At hard carbon material, the interlamellar spacing of hard carbon is not less than 0.37nm, and the hard carbon interlamellar spacing is much larger than graphite layers away from forming sodium ion
Deintercalation gap structure, realization reversibly store sodium ion.
2. carbon-based storage sodium negative electrode material according to claim 1, which is characterized in that reversible specific capacity is not less than its 0.1C for the first time
227.1mAh/g, coulombic efficiency is not less than 79.3% for the first time.
3. the application of carbon-based storage sodium negative electrode material described in a kind of claim 1, which is characterized in that it is used to prepare sodium-ion battery,
Battery includes anode material of lithium-ion battery and electrolyte based on biomass, and the electrolyte contains sodium salt NaPF6、NaClO4
At least one of with NaTFSI, and the electrolyte also contains selected from nonaqueous solvents ethylene carbonate, diethyl carbonate, carbon
At least one of acid propylene ester, diethylene glycol dimethyl ether, glycol dimethyl ether and dimethyl carbonate.
4. the application of carbon-based storage sodium negative electrode material according to claim 3, it is characterised in that: make biomass-based hard carbon material
It for negative electrode active material, is uniformly mixed with sodium alginate according to the mass ratio of 9.5:0.5, negative electrode slurry is made, be coated in aluminium foil
On, it is put into vacuum oven to be not less than at 100 DEG C and dry at least 12h to get hard carbon cathode pole piece.
5. the application of carbon-based storage sodium negative electrode material according to claim 4, it is characterised in that: make the hard carbon cathode pole piece
It is to use EC/DEC for 1:1 and mixed liquor that electrolyte concentration is 1.0mol/L at electrode with metallic sodium piece for working electrode
For electrolyte, it is assembled into sodium-ion battery under inert gas atmosphere.
6. the preparation method of carbon-based storage sodium negative electrode material described in a kind of claim 1, which comprises the steps of:
A. pretreatment of raw material:
It using biological material as raw material, is calculated with the gross mass percentage of biological material for 100%, in biological material
Tea polyphenols containing the 20wt% not less than biological material total amount are also more containing the 20wt% not less than biological material total amount
Hydroxy aldehyde or polyhydroxyketone；Biological material is impregnated in deionized water after at least 2 hours, is cleaned, clean raw material is obtained；
B. the raw material drying obtained after being pre-processed in the step a, and be cooled to room temperature, dry raw material is obtained, it is spare；
C. dry raw material obtained in the step b is ground, obtains hard carbon granular precursor powder；
D. under inert protective atmosphere, to be not less than the heating rate of 5 DEG C/min, from room temperature to heat treatment temperature 1200~
1600 DEG C of temperature range, and 0.5~10 hour is kept the temperature under temperature condition of heat treatment, it will be hard obtained in the step c
Carbon matrix precursor particle powder carries out high temperature cabonization processing, room temperature is then cooled to the furnace, to obtain biomass-based hard carbon material.
7. the preparation method of carbon-based storage sodium negative electrode material according to claim 6, it is characterised in that: in the step a, institute
State the blade-section that biological material is selected from Theaceae Camellia Plants.
8. the preparation method of carbon-based storage sodium negative electrode material according to claim 6, it is characterised in that: in the step b, institute
Stating drying means is vacuum drying mode, and drying temperature section is 60~100 DEG C, and being dried the time is 12~24 hours.
9. the preparation method of carbon-based storage sodium negative electrode material according to claim 6, it is characterised in that: in the step c, institute
The particle size interval for stating granular precursor is 200~500 mesh.
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| CN110867578A (en) * | 2019-11-21 | 2020-03-06 | 江苏理工学院 | Sodium ion battery and preparation method and application thereof |
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| CN114436237A (en) * | 2021-12-21 | 2022-05-06 | 华中科技大学 | Hard carbon material and preparation method and application thereof |
| CN114725378A (en) * | 2022-04-22 | 2022-07-08 | 湖南钠方新能源科技有限责任公司 | Negative electrode slurry and preparation method thereof, negative electrode plate and secondary battery |
| CN114804064A (en) * | 2022-04-14 | 2022-07-29 | 福建师范大学 | Method for preparing starch-based biomass hard carbon by yeast fermentation and application thereof |
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| CN116022769A (en) * | 2023-02-24 | 2023-04-28 | 蜂巢能源科技股份有限公司 | Hard carbon negative electrode material of sodium ion battery and preparation method thereof |
| CN116344803A (en) * | 2023-04-10 | 2023-06-27 | 吉安冠佳新能源开发有限公司 | Hard carbon negative electrode material for sodium ion battery and preparation method thereof |
| CN117303345A (en) * | 2023-09-06 | 2023-12-29 | 同济大学 | Negative electrode material of sodium ion battery, preparation method of negative electrode material and sodium ion battery |
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