CN110380031A - A kind of anode material of lithium-ion battery and preparation method thereof - Google Patents
A kind of anode material of lithium-ion battery and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of anode material of lithium-ion batteries and preparation method thereof.The negative electrode material is ZIF8/ zinc oxide/redox graphene trielement composite material, its preparation process includes, graphene oxide fiber is prepared using method of electrostatic spinning, reduction is carried out by strong reductant, and redox graphene fiber is prepared, zinc oxide and redox graphene fiber composite are obtained into zinc oxide/redox graphene composite material followed by hydro-thermal method, then ZIF8/ zinc oxide/redox graphene trielement composite material is prepared by inducing zinc.Zinc oxide electrode is compensated for the deficiency of electronics and sodium ion efficiency of transmission by introducing graphene, while the high specific area of ZIF8 improves the structural stability and ion adsorption capacity of material.Redox graphene fiber, zinc oxide, ZIF8 three's synergistic effect, the common chemical property for promoting sodium-ion battery.
Description
Technical field
The present invention relates to anode material of lithium-ion batteries of a kind of height ratio capacity and preparation method thereof, belong to materials chemistry neck
Domain.
Background technique
Since lithium ion battery successful commercialization in 1991, immense success has been achieved in terms of portable energy-storing.But
It is that the scarcity of lithium resource leads to continuing to increase for lithium ion battery cost.Sodium-ion battery has similar with lithium ion battery
Charge-discharge mechanism, and sodium resource wants relatively rich more than lithium, so sodium-ion battery is the ideal substitute of lithium ion battery.
However the commercialization graphite anode for lithium ion battery in sodium-ion battery and is not suitable for.Therefore, sodium-ion battery cathode
The research of material is of great significance to the exploitation of sodium-ion battery.
ZnO has rich reserves, low in cost, advantages of environment protection and excellent electricity as typical metal oxide
Chemical property has proved to be the very potential candidate of sodium-ion battery.But by simple zinc oxide be used for sodium from
When sub- cell negative electrode material, due in sodium-ion battery charge and discharge process repeatedly, sodium ion carries out insertion repeatedly and de-
Out, it will cause the huge volume expansion of anode material of lithium-ion battery and contraction, zinc oxide electrode material be easily damaged, therefore is single
Pure zinc oxide typically exhibits poor cyclical stability when as anode material of lithium-ion battery.In order to solve above-mentioned ask
It is a kind of promotion zinc oxide electrode stability that topic, which introduces various conductive carbon materials (including graphene, carbon nanotube, porous carbon etc.),
Effective ways.Graphene has proved to be a kind of very promising carbon material, large specific surface area, and conductivity is high, can be with
Effectively improve electron-transport speed.
Metal organic framework (Metal Organic Frameworks, MOFs) is emerging after zeolite molecular sieve development
A kind of porous material, surface can grafting and modifying ability, duct Modulatory character and the absorption screenings with organic zeolite membrane
Performance also becomes one of the hot spot of electrode material research field.MOFs material by metal center atom and organic ligand in conjunction with and
At, it is many kinds of, it is big that space may be selected；It can be applied to electrode material field, due to the spy of its porosity and high-specific surface area
Property, it can greatly promote the chemical property of electrode material.Wherein, the zeolite structured material (Zeolitic of imidazoles
Imidazolate Frameworks, ZIFs) it is a member in MOFs material, it is obtained due to the topological structure with zeolite molecular sieve
Name has excellent thermal stability and chemical stability.
Summary of the invention
Electric conductivity and structure are steady when the purpose of the invention is to overcome zinc oxide to be applied to anode material of lithium-ion battery
It is qualitatively insufficient, a kind of height ratio capacity anode material of lithium-ion battery and preparation method thereof is provided.By regulating and controlling the pattern of Zn0 simultaneously
It is compound with redox graphene with good conductivity, then one layer is generated in zinc oxide surface by inducing zinc
ZIF8, so as to improve the storage sodium chemical property of Zn0 negative electrode material, the problems such as alleviating the Zn0 volume expansion in cyclic process.
Specifically, the anode material of lithium-ion battery is a kind of ZIF8/ zinc oxide/redox graphene tri compound
The preparation process of material, the composite material includes preparing graphene oxide fiber using method of electrostatic spinning, passing through strong reductant
It carries out reduction and redox graphene fiber is prepared, followed by hydro-thermal method by zinc oxide and redox graphene fiber
It is compound to obtain zinc oxide/redox graphene composite material, then ZIF8/ zinc oxide/oxygen reduction is prepared by inducing zinc
Graphite alkene trielement composite material.
The preparation method of the anode material of lithium-ion battery, specifically includes the following steps:
(1) redox graphene fiber is prepared:
Graphene oxide water solution is prepared, ultrasonic disperse is uniform, and sodium hydroxide is added thereto, stirs at 60 DEG C -80 DEG C
Reaction 3-5h is mixed, drying is filtered, obtains solid powder.The solid powder is placed in and is configured to spin in N,N-dimethylformamide
Graphene oxide fiber is prepared by the method for wet spinning in silk stock solution.The graphene oxide fiber prepared is placed in
In reaction utensil, be added dropwise hydrazine hydrate, be placed in constant temperature oven, at 90~120 DEG C keep the temperature 6~12h, obtain reduction-oxidation graphite
Alkene fiber.
(2) zinc oxide/redox graphene fiber is prepared:
The redox graphene fiber prepared in step (1) is immersed in zinc acetate-ethanol solution, room temperature waits for
It after ethyl alcohol volatilizees, places it in Muffle furnace and is heat-treated, be warming up to 200~300 DEG C, keep the temperature 30~60min.It then will be hot
The redox graphene fiber of processing is placed in deionized water, adds suitable zinc chloride and hexa, stirring
Uniformly, in 60~90 DEG C heating water bath 6~12 hours, i.e., acquisition zinc oxide/redox graphene fiber.
(3) ZIF8/ zinc oxide/redox graphene trielement composite material is prepared:
Zinc oxide/redox graphene the fiber prepared in step (2) is placed in the methanol solution of methylimidazole,
2~5h of water bath with thermostatic control at 50 DEG C~80 DEG C, centrifuge separation collect product and obtain ZIF8/ zinc oxide/redox graphene
Trielement composite material.
Preferably, in the step (1), the concentration of the graphene oxide water solution is 0.1~2mg/mL, sodium hydroxide
With the solid-to-liquid ratio of graphene oxide water solution are as follows: 2~5:100g/mL.
Preferably, in the step (1), the solid-to-liquid ratio of the solid powder and n,N-Dimethylformamide is 0.1~2:
100g/mL,
Preferably, in the step (1), the dosage of hydrazine hydrate meets (0.1~0.5g) graphene oxide fiber: 0.1mL
The ratio of hydrazine hydrate.
Preferably, in step (2), the concentration of the zinc acetate-ethanol solution is 0.01~0.03mol/L；
Preferably, in step (2), the quality of the redox graphene fiber is 0.5~1g, and zinc acetate-ethyl alcohol is molten
The volume of liquid is 10~50mL.
Preferably, in step (2), the quality of the redox graphene fiber of the heat treatment is 0.5~1g, zinc chloride
Quality be 1~2g, the quality of hexa is 1~2g, and deionized water is 100~200mL.
Preferably, in step (3), the concentration of the methanol solution of the methylimidazole is 0.1~1mol/L.
Beneficial effects of the present invention are as follows:
Redox graphene fiber is prepared preparation method of the invention first, then grows one layer in fiber surface
Zinc bar array is aoxidized, finally wraps up one layer of ZIF8 on oxidation zinc bar surface again.Graphene is introduced in whole preparation process to be improved
Simple zinc oxide improves the efficiency of transmission of electronics and sodium ion, increases electricity as the insufficient defect of electrode material electric conductivity
Chemical property, while one layer of ZIF8 is coated on oxidation zinc bar surface again, this not only improves the structural stability of zinc oxide, but also
The specific surface area of ZIF8 is larger, convenient for adsorbing more sodium ions, accelerates the migration of sodium ion, to reach promotion electrochemistry
The effect of energy.In conclusion in the present invention, redox graphene fiber, zinc oxide, ZIF8 three's synergistic effect, jointly
Promote the chemical property of sodium-ion battery.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples:
Fig. 1 is ZIF8/ zinc oxide/compound anode material of lithium-ion battery of redox graphene obtained by embodiment 1
Specific discharge capacity recycle figure.
Fig. 2 is ZIF8/ zinc oxide/compound anode material of lithium-ion battery of redox graphene obtained by embodiment 1
High rate performance figure.
Specific embodiment
Embodiment 1:
(1) redox graphene fiber is prepared:
Take commercially available graphene oxide water solution (concentration 0.5mg/mL), ultrasonic 40min, in finely dispersed graphite oxide
It is added sodium hydroxide in aqueous solution, the solid-to-liquid ratio of sodium hydroxide and graphene oxide water solution is 3:100g/mL, at 70 DEG C
It is stirred to react 4h, then carries out filtering drying solid powder.Taking the solid powder for preparing according to solid-to-liquid ratio is 0.5:100g/mL
It is placed in n,N-Dimethylformamide and is configured to spinning solution, graphene oxide is then prepared by the method for wet spinning
Fiber.The graphene oxide fiber prepared is placed in reaction utensil, hydrazine hydrate, the dosage reference of the hydrazine hydrate is added dropwise to it
0.3g graphene oxide fiber: the ratio of 0.1mL hydrazine hydrate is added dropwise, and places it in constant temperature oven, 100 DEG C of heat preservation 8h react to obtain
Redox graphene fiber.
(2) zinc oxide/redox graphene fiber is prepared:
Zinc acetate-the ethanol solution for configuring 0.02mol/L, the redox graphene fiber that will be prepared in step (1)
0.8g is immersed in 40mL zinc acetate-ethanol solution, room temperature wait for ethyl alcohol volatilization after, place it in Muffle furnace
250 DEG C of heat preservations are heat-treated 40min.The redox graphene fiber 0.8g being heat-treated then is placed in 150mL deionized water
In, it adds 1.5g zinc chloride and is stirred evenly with 1.5g hexa, 80 DEG C of heating water baths, 8 hours acquisition zinc oxide/also
Former graphene oxide fiber.
(3) ZIF8/ zinc oxide/redox graphene is prepared:
The methanol solution for configuring the methylimidazole of 0.5mol/L, the zinc oxide/oxygen reduction fossil that will be prepared in step (2)
Black alkene fiber takes 0.8g to be placed in one, and 60 DEG C of heating water bath 4h are centrifugated later, collect product i.e. obtain ZIF8/ zinc oxide/
Redox graphene composite material.
Embodiment 2:
(1) redox graphene fiber is prepared:
Take commercially available graphene oxide water solution (concentration 0.1mg/mL), ultrasonic 30min, in finely dispersed graphite oxide
It is added sodium hydroxide in aqueous solution, the solid-to-liquid ratio of sodium hydroxide and graphene oxide water solution is 2:100g/mL, at 60 DEG C
It is stirred to react 3h, then carries out filtering drying solid powder.Taking the solid powder for preparing according to solid-to-liquid ratio is 0.1:100g/mL
It is placed in n,N-Dimethylformamide and is configured to spinning solution, graphene oxide is then prepared by the method for wet spinning
Fiber.The graphene oxide fiber prepared is placed in reaction utensil, hydrazine hydrate, the dosage reference of the hydrazine hydrate is added dropwise to it
0.1g graphene oxide fiber: the ratio of 0.1mL hydrazine hydrate is added dropwise, and places it in constant temperature oven, 90 DEG C of heat preservation 6h react to obtain
Redox graphene fiber.
(2) zinc oxide/redox graphene fiber is prepared:
Zinc acetate-the ethanol solution for configuring 0.01mol/L, the redox graphene fiber that will be prepared in step (1)
0.5g is immersed in 10mL zinc acetate-ethanol solution, after room temperature waits for ethyl alcohol volatilization, is placed it in 200 in Muffle furnace
DEG C heat preservation 30min.Then the redox graphene fiber 0.5g handled well is placed in 100mL deionized water, adds 1g
Zinc chloride is stirred evenly with 1g hexa, and 60 DEG C of heating water baths, 6 hours acquisition zinc oxide/redox graphene is fine
Dimension.
(3) ZIF8/ zinc oxide/redox graphene is prepared:
The methanol solution for configuring the methylimidazole of 0.1mol/L, the zinc oxide/oxygen reduction fossil that will be prepared in step (2)
Black alkene fiber takes 0.5g to be placed in one, and 50 DEG C of heating water bath 2h are centrifugated later, collect product i.e. obtain ZIF8/ zinc oxide/
Redox graphene composite material.
Embodiment 3:
(1) redox graphene fiber is prepared:
Take commercially available graphene oxide water solution (concentration 2mg/mL), ultrasonic 60min, in finely dispersed graphene oxide
It is added sodium hydroxide in aqueous solution, the solid-to-liquid ratio of sodium hydroxide and graphene oxide water solution is 5:100g/mL, is stirred at 80 DEG C
Reaction 5h is mixed, then carries out filtering drying solid powder.The solid powder prepared is taken to be placed according to solid-to-liquid ratio for 2:100g/mL
It is configured to spinning solution in n,N-Dimethylformamide, graphene oxide fibre is then prepared by the method for wet spinning
Dimension.The graphene oxide fiber prepared is placed in reaction utensil, hydrazine hydrate, the dosage reference of the hydrazine hydrate is added dropwise to it
0.5g graphene oxide fiber: the ratio of 0.1mL hydrazine hydrate is added dropwise, and places it in constant temperature oven, 120 DEG C of heat preservation 12h react
To redox graphene fiber.
(2) zinc oxide/redox graphene fiber is prepared:
Zinc acetate-the ethanol solution for configuring 0.03mol/L, the redox graphene fiber 1g that will be prepared in step (1)
It is immersed in 50mL zinc acetate-ethanol solution, after room temperature waits for ethyl alcohol volatilization, places it in 300 DEG C of guarantors in Muffle furnace
The redox graphene fiber 1g handled well is then placed in 200mL deionized water by warm 60min., adds 2g zinc chloride
It is stirred evenly with 2g hexa, 90 DEG C of heating water baths, 12 hours acquisition zinc oxide/redox graphene fibers.
(3) ZIF8/ zinc oxide/redox graphene is prepared:
The methanol solution for configuring the methylimidazole of 1mol/L, the zinc oxide/reduction-oxidation graphite that will be prepared in step (2)
Alkene fiber takes 1g to be placed in one, and 80 DEG C of heating water bath 5h are centrifugated later, collects product and obtains ZIF8/ zinc oxide/reduction
Graphene oxide composite material.
Claims (9)
1. a kind of anode material of lithium-ion battery, the negative electrode material is ZIF8/ zinc oxide/redox graphene tri compound
Material, which is characterized in that the preparation process of the ZIF8/ zinc oxide/redox graphene trielement composite material includes using
Method of electrostatic spinning prepares graphene oxide fiber, carries out reduction by strong reductant and redox graphene fiber is prepared,
Zinc oxide and redox graphene fiber composite are obtained into zinc oxide/redox graphene composite wood followed by hydro-thermal method
Material, then ZIF8/ zinc oxide/redox graphene trielement composite material is prepared by inducing zinc.
2. the preparation method of anode material of lithium-ion battery described according to claim 1, which is characterized in that specifically include following
Step:
(1) redox graphene fiber is prepared:
Graphene oxide water solution is prepared, ultrasonic disperse is uniform, and sodium hydroxide is added thereto, stirs at 60 DEG C -80 DEG C anti-
3-5h is answered, drying is filtered, obtains solid powder；The solid powder is placed in N,N-dimethylformamide and is configured to spinning original
Graphene oxide fiber is prepared by the method for wet spinning in liquid；The graphene oxide fiber prepared is placed in reaction
In ware, be added dropwise hydrazine hydrate, be placed in constant temperature oven, at 90~120 DEG C keep the temperature 6~12h, obtain redox graphene fibre
Dimension；
(2) zinc oxide/redox graphene fiber is prepared:
The redox graphene fiber prepared in step (1) is immersed in zinc acetate-ethanol solution, room temperature waits for ethyl alcohol
It after volatilization, places it in Muffle furnace and is heat-treated, be warming up to 200~300 DEG C, keep the temperature 30~60min, it then will heat treatment
Redox graphene fiber be placed in deionized water, add suitable zinc chloride and hexa, stir evenly,
In 60~90 DEG C heating water bath 6~12 hours, i.e., acquisition zinc oxide/redox graphene fiber；
(3) ZIF8/ zinc oxide/redox graphene trielement composite material is prepared:
Zinc oxide/redox graphene the fiber prepared in step (2) is placed in the methanol solution of methylimidazole, 50
DEG C~80 DEG C at 2~5h of water bath with thermostatic control, centrifuge separation collects product and obtains ZIF8/ zinc oxide/redox graphene ternary
Composite material.
3. preparation method according to claim 2, which is characterized in that in step (1), the graphene oxide water solution
Concentration is 0.1~2mg/mL, the solid-to-liquid ratio of sodium hydroxide and graphene oxide water solution are as follows: 2~5:100g/mL.
4. preparation method according to claim 2 or 3, which is characterized in that in the step (1), the solid powder with
The solid-to-liquid ratio of N,N-dimethylformamide is 0.1~2:100g/mL.
5. preparation method according to claim 2, which is characterized in that in step (1), the dosage of hydrazine hydrate meet (0.1~
0.5g) graphene oxide fiber: the ratio of 0.1mL hydrazine hydrate.
6. preparation method according to claim 2, which is characterized in that in step (2), the zinc acetate-ethanol solution
Concentration is 0.01~0.03mol/L.
7. the preparation method according to claim 2 or 6, which is characterized in that in step (2), the redox graphene
The quality of fiber is 0.5~1g, and zinc acetate-ethanol solution volume is 10~50mL.
8. preparation method according to claim 2, which is characterized in that in step (2), the oxygen reduction fossil of the heat treatment
The quality of black alkene fiber is 0.5~1g, and the quality of zinc chloride is 1~2g, and the quality of hexa is 1~2g, deionization
Water is 100~200mL.
9. preparation method according to claim 2, which is characterized in that in step (3), the methanol of the methylimidazole is molten
The concentration of liquid is 0.1~1mol/L.
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| CN114783782A (en) * | 2022-04-25 | 2022-07-22 | 武汉大学 | Three-dimensional graphene-metal organic framework electrode for 3D printing, and preparation method and application thereof |
| CN114783782B (en) * | 2022-04-25 | 2023-12-22 | 武汉大学 | Three-dimensional graphene-metal organic frame electrode for 3D printing, and preparation method and application thereof |
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