CN108832088A - A kind of biomass carbon/vanadium phosphate sodium combination electrode material and its preparation method and application - Google Patents
A kind of biomass carbon/vanadium phosphate sodium combination electrode material and its preparation method and application Download PDFInfo
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- CN108832088A CN108832088A CN201810584392.9A CN201810584392A CN108832088A CN 108832088 A CN108832088 A CN 108832088A CN 201810584392 A CN201810584392 A CN 201810584392A CN 108832088 A CN108832088 A CN 108832088A
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- biomass carbon
- vanadium phosphate
- electrode material
- combination electrode
- phosphate sodium
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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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- 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
- H01M4/58—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
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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 carbon/vanadium phosphate sodium combination electrode material and preparation method thereof and as the application of sodium-ion battery positive material, presoma is made by hydro-thermal process, then by obtaining biomass carbon/vanadium phosphate sodium combination electrode material after high-temperature heat treatment 8-10 hours, the vanadium phosphate sodium of composite material load is hollow near-spherical, with biggish specific surface area, more reactivity sites are provided for electrochemical reaction.Meanwhile the biological carbon matrix obtained after being carbonized by puffed rice improves the electron transfer rate of composite material, to accelerate the kinetics of the composite material, is highly suitable as sodium-ion battery positive material.For material of the invention while realizing high specific discharge capacity, obtaining has excellent high rate performance and cyclical stability, has vast potential for future development in fields such as mobile device, electric car, extensive energy storage.
Description
Technical field
The present invention relates to the positive electrode fields of sodium-ion battery, and in particular to a kind of biomass carbon/vanadium phosphate sodium is compound
Electrode material and its preparation method and application.
Background technique
Since twentieth century, with the continuous aggravation of world petroleum resource increasingly consumed with environmental pollution, green, cleaning
Secondary cell have been to be concerned by more and more people.In recent years, in numerous electrochemical energy storage systems, sodium-ion battery is at this moment
Come into the visual field of people.Firstly, sodium is tellurian the fourth-largest element, in the rich reserves of earth's crust reserves.Secondly, sodium source cost
Cheap, last sodium and lithium have similar chemical property, and the theory in lithium ion battery can be applied on sodium-ion battery.It is right
In sodium-ion battery, positive and negative pole material is the principal element for influencing its performance, and among the cost structure of sodium-ion battery, just
Pole material proportion highest (account for about battery cost 30~40%) is the key that restrict sodium-ion battery development, also very
Battery quality is decide in big degree.Therefore, especially urgent to the research of sodium-ion battery positive material.And numerous sodium from
In sub- cell positive material, fast-ionic conductor type Na3V2(PO4)3Anode has three-dimensional conductive network, and higher voltage platform is (about
3.4V) and theoretical specific capacity (about 117mAh g-1) and the advantages that good cyclical stability, make it in the great application of energy storage field
Potentiality.
But Na3V2(PO4)3Electronic conductivity it is poor, in charge and discharge process, capacity attenuation is obvious.Therefore, will
Na3V2(PO4)3Material is modified research and helps to improve its chemical property.Through studying, by active material and conductive carbon material
Expect that compound is maximally efficient modification strategies, therefore, biomass carbon/vanadium phosphate sodium combination electrode material can be used for sodium-ion battery
Positive electrode effectively improves material conductivity, obtains higher specific capacity and excellent performance.
Summary of the invention
It is an object of the invention to be directed to the defect of vanadium phosphate sodium electron conduction difference, a kind of biomass carbon/phosphorus is provided
Sour vanadium sodium combination electrode material and preparation method thereof and application as sodium-ion battery positive material, as made from this method
Biomass carbon/vanadium phosphate sodium combination electrode material is used as sodium-ion battery positive material, with high charge-discharge capacity, forthright again
Energy and cyclical stability.
Biomass carbon of the present invention/vanadium phosphate sodium combination electrode material preparation method, includes the following steps:
(1) puffed rice is placed in porcelain boat, be put into tube furnace under argon atmosphere carry out heat treatment be allowed to be carbonized, heat at
The reaction temperature of reason is 500 DEG C~700 DEG C, and the reaction time is 1~5 hour, is cooled to environment temperature, obtains biomass carbon materials
Material;
(2) vanadic anhydride and sodium dihydrogen phosphate is soluble in water, environment temperature stirs evenly to form mixed solution, then
Oxalic acid is dissolved in the mixed solution, it is lasting to stir, obtain stand-by solution;
(3) biomass carbon material prepared by step (1) is immersed in the stand-by solution that step (2) obtains, is allowed to abundant
Infiltration, is then added in polytetrafluoroethylene (PTFE) autoclave, seals and heat, obtain presoma;
(4) it by after presoma washing and drying made from step (3), is put into tube furnace under argon atmosphere and carries out high warm
Processing, reaction temperature are 700-900 DEG C, and the reaction time is 6-12 hours, are cooled to environment temperature, obtain target product biomass
Carbon/vanadium phosphate sodium combination electrode material.
In step (1), the condition of the heat treatment is:Reaction temperature be 550 DEG C~650 DEG C, the reaction time be 1.5~
3 hours, further preferably, reaction temperature was 600 DEG C, and the reaction time is 2 hours.
In step (2), the mass ratio of the vanadic anhydride, sodium dihydrogen phosphate and oxalic acid is 0.3~0.8:0.72~
1.44:0.6~4, it is 0.364~0.728 further preferably:0.72~1.44:0.756~3.78.
The ratio between quality and the volume of water of the vanadic anhydride are 0.3~0.8g:40mL~80mL;Further preferably
For 0.364~0.728g:50mL~70mL;Still more preferably 0.364~0.728g:60mL.
In step (3), the temperature of the heating is 160 DEG C~200 DEG C, and the time is 12~26 hours, further preferably,
The temperature of the heating is 170 DEG C~190 DEG C, and the time is 18~22 hours, and the temperature of the heating is 180 DEG C, the time
It is 20 hours.
In step (4), the reaction temperature of high-temperature heat treatment is 750-850 DEG C, and the reaction time is 8-10 hours,
In step (1), (2) and (4), the environment temperature is 10~40 DEG C, further preferably, the environment temperature
It is 20~30 DEG C.
The biomass carbon is from puffed rice carbonization, by puffed rice preparation process common in daily life
Inspire, by rice carry out expanding treatment, the biological carbon matrix with unique honeycomb macropore is obtained after carbonization, compare with
Other methods such as template, microfluid method, the carbon material of the preparations such as emulsion polymerization, expanding treatment is efficient, step simple possible,
Resulting rice has fabulous consistency, macroporsity, high-specific surface area and excellent electron conduction after carbonization, increases
The effective area of electrochemical reaction is added.The vanadium phosphate sodium loaded on the biomass carbon is hollow near-spherical, size about 5-
10μm.Biomass carbon prepared by the present invention/vanadium phosphate sodium combination electrode material, the vanadium phosphate sodium loaded are hollow near-spherical,
With biggish specific surface area, more reactivity sites are provided for electrochemical reaction.Meanwhile after being carbonized by puffed rice
To biological carbon matrix improve the electron transfer rate of composite material, it is non-to accelerate the kinetics of the composite material
Often it is suitable as sodium-ion battery positive material.
Compared with prior art, the invention has the advantages that:
The method of the present invention prepares biomass carbon/vanadium phosphate sodium combination electrode material presoma by hydro-thermal method, then passes through
High-temperature heat treatment obtains target product sodium-ion battery biomass carbon/vanadium phosphate sodium combination electrode material.The preparation method is simple
It is feasible, convenient for control.
Biomass carbon prepared by the present invention/vanadium phosphate sodium combination electrode material, the vanadium phosphate sodium loaded are hollow class ball
Shape has biggish specific surface area, provides more reactivity sites for electrochemical reaction.Meanwhile it being carbonized by puffed rice
The biological carbon matrix obtained afterwards improves the electron transfer rate of composite material, to accelerate the reaction power of the composite material
It learns.In the present invention, the electronic conductivity for effectively increasing vanadium phosphate sodium composite material is poor, thus realizing high specific discharge capacity
Meanwhile obtaining the novel sodium-ion battery positive material with excellent high rate performance and cyclical stability.In mobile device, electricity
The fields such as electrical automobile, extensive energy storage have broad application prospects.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of biomass carbon/vanadium phosphate sodium combination electrode material obtained in embodiment 1;
Fig. 2 is the scanning electron microscope (SEM) photograph of biomass carbon/vanadium phosphate sodium combination electrode material obtained in embodiment 2;
Fig. 3 is the scanning electron microscope (SEM) photograph of biomass carbon/vanadium phosphate sodium combination electrode material obtained in embodiment 3.
Specific embodiment
Below with reference to embodiment, the present invention will be described in detail, but the present invention is not limited to this.
Embodiment 1
Appropriate puffed rice is weighed to be placed in porcelain boat, be put into tube furnace under argon atmosphere carry out heat treatment be allowed to be carbonized,
Reaction temperature is 600 DEG C, and the reaction time is 2 hours, is slowly cooled to room temperature 25 DEG C, obtains biomass carbon material;By 0.364g
Vanadic anhydride and 0.72g sodium dihydrogen phosphate are placed in a beaker, and the deionized water of 60mL is added, and are stirred at room temperature and are formed uniformly mixing
Then solution weighs 0.756g oxalic acid and is dissolved in above-mentioned solution, lasting stirring a period of time, acquired solution is stand-by;By the suitable of preparation
The biomass carbon of amount is immersed in obtained mixed solution, is allowed to sufficiently infiltrate, is then added to polytetrafluoroethylene (PTFE) autoclave
In, it seals and heats, temperature is 180 DEG C, and the time is 20 hours, and 25 DEG C are cooled to room temperature after reaction, obtains presoma;It will be made
Presoma washing and drying after, be put into tube furnace under argon atmosphere and carry out high-temperature heat treatment, reaction temperature be 800 DEG C, instead
It is 10 hours between seasonable, is cooled to room temperature 25 DEG C, obtains target product biomass carbon/vanadium phosphate sodium combination electrode material.
The scanning electron microscope (SEM) photograph of biomass carbon/vanadium phosphate sodium combination electrode material obtained is as shown in Figure 1 in embodiment 1.
Embodiment 2
Appropriate puffed rice is weighed to be placed in porcelain boat, be put into tube furnace under argon atmosphere carry out heat treatment be allowed to be carbonized,
Reaction temperature is 600 DEG C, and the reaction time is 2 hours, is slowly cooled to room temperature 25 DEG C, obtains biomass carbon material;By 0.546g
Vanadic anhydride and 1.08g sodium dihydrogen phosphate are placed in a beaker, and the deionized water of 60mL is added, and are stirred at room temperature and are formed uniformly mixing
Then solution weighs 1.134g oxalic acid and is dissolved in above-mentioned solution, lasting stirring a period of time, acquired solution is stand-by;By the suitable of preparation
The biomass carbon of amount is immersed in obtained mixed solution, is allowed to sufficiently infiltrate, is then added to polytetrafluoroethylene (PTFE) autoclave
In, it seals and heats, temperature is 180 DEG C, and the time is 20 hours, and 25 DEG C are cooled to room temperature after reaction, obtains presoma;It will be made
Presoma washing and drying after, be put into tube furnace under argon atmosphere and carry out high-temperature heat treatment, reaction temperature be 800 DEG C, instead
It is 10 hours between seasonable, is cooled to room temperature 25 DEG C, obtains target product biomass carbon/vanadium phosphate sodium combination electrode material.
The scanning electron microscope (SEM) photograph of biomass carbon/vanadium phosphate sodium combination electrode material obtained is as shown in Figure 2 in embodiment 2.
Embodiment 3
Appropriate puffed rice is weighed to be placed in porcelain boat, be put into tube furnace under argon atmosphere carry out heat treatment be allowed to be carbonized,
Reaction temperature is 600 DEG C, and the reaction time is 2 hours, is slowly cooled to room temperature 25 DEG C, obtains biomass carbon material;By 0.728g
Vanadic anhydride and 1.44g sodium dihydrogen phosphate are placed in a beaker, and the deionized water of 60mL is added, and are stirred at room temperature and are formed uniformly mixing
Then solution weighs 3.78g oxalic acid and is dissolved in above-mentioned solution, lasting stirring a period of time, acquired solution is stand-by;By the appropriate of preparation
Biomass carbon be immersed in obtained mixed solution, be allowed to sufficiently infiltrate, be then added in polytetrafluoroethylene (PTFE) autoclave,
It seals and heats, temperature is 180 DEG C, and the time is 20 hours, and 25 DEG C are cooled to room temperature after reaction, obtains presoma;It will be obtained
It after presoma washing and drying, is put into tube furnace under argon atmosphere and carries out high-temperature heat treatment, reaction temperature is 800 DEG C, reaction
Time is 10 hours, is cooled to room temperature 25 DEG C, obtains target product biomass carbon/vanadium phosphate sodium combination electrode material.
The scanning electron microscope (SEM) photograph of biomass carbon/vanadium phosphate sodium combination electrode material obtained is as shown in Figure 3 in embodiment 3.
Performance test
Using biomass carbon made of above-described embodiment 1~3/vanadium phosphate sodium combination electrode material as sodium-ion battery anode
Active material presses 8 with Kynoar and conductive agent acetylene black:1:Appropriate N- methylpyrrole is added dropwise than mixed grinding in 1 quality
Alkanone is made into slurry, is coated on aluminium flake after being sufficiently stirred.Metallic sodium is cathode, and the sodium perchlorate that electrolyte is 1mol/L dissolves
Volume ratio is 1:1 ethylene carbonate and dimethyl carbonate.Button battery is assembled into glove box.The sodium that will be assembled
Ion half-cell carries out electrochemical property test after standing an evening, charging/discharging voltage range is 2.3V~3.9V.In room temperature environment
It is middle measurement biomass carbon/vanadium phosphate sodium combination electrode material as sodium-ion battery positive material reversible charging and discharging capacity,
Multiplying power property and charge-discharge performance.
The performance test results are as follows:
Current density of the biomass carbon of embodiment 1, the embodiment 2 and embodiment 3/vanadium phosphate sodium combination electrode material in 5C
Lower reversible discharge specific capacity is respectively 97mAh g-1、102mAh g-1With 108mAh g-1, and discharge after charge and discharge cycles 500 times
Specific capacity conservation rate is up to 90% or more.As it can be seen that biomass carbon obtained above/vanadium phosphate sodium combination electrode material is with higher
Charging and discharging capacity and excellent cyclical stability.
This is biomass carbon prepared by the present invention/vanadium phosphate sodium combination electrode material, and the vanadium phosphate sodium loaded is hollow
Near-spherical, size are about 5-10 μm, have biggish specific surface area, provide more reactivity sites for electrochemical reaction.
Meanwhile the biological carbon matrix obtained after being carbonized by puffed rice improves the electron transfer rate of composite material, so that accelerating should
The kinetics of composite material.In the present invention, the electronic conductivity for effectively increasing vanadium phosphate sodium composite material is poor, thus
While realizing high specific discharge capacity, the novel sodium-ion battery anode with excellent high rate performance and cyclical stability is obtained
Material.It has broad application prospects in fields such as mobile device, electric car, extensive energy storage.
Claims (10)
1. a kind of biomass carbon/vanadium phosphate sodium combination electrode material preparation method, which is characterized in that include the following steps:
(1) puffed rice is placed in porcelain boat, be put into tube furnace under argon atmosphere carry out heat treatment be allowed to be carbonized, heat treatment
Reaction temperature is 500 DEG C~700 DEG C, and the reaction time is 1~5 hour, is cooled to environment temperature, obtains biomass carbon material;
(2) vanadic anhydride and sodium dihydrogen phosphate is soluble in water, environment temperature stirs evenly to form mixed solution, then will be careless
Acid is dissolved in the mixed solution, lasting to stir, and obtains stand-by solution;
(3) biomass carbon material prepared by step (1) is immersed in the stand-by solution that step (2) obtains, is allowed to sufficiently infiltrate,
It is then added in polytetrafluoroethylene (PTFE) autoclave, seals and heats, obtain presoma;
(4) it by after presoma washing and drying made from step (3), is put into tube furnace and is carried out at high warm under argon atmosphere
Reason, reaction temperature are 700-900 DEG C, and the reaction time is 6-12 hours, are cooled to environment temperature, obtain target product biomass
Carbon/vanadium phosphate sodium combination electrode material.
2. biomass carbon according to claim 1/vanadium phosphate sodium combination electrode material preparation method, which is characterized in that
In step (1), the condition of the heat treatment is:Reaction temperature is 550 DEG C~650 DEG C, and the reaction time is 1.5~3 hours.
3. biomass carbon according to claim 1/vanadium phosphate sodium combination electrode material preparation method, which is characterized in that
In step (2), the mass ratio of the vanadic anhydride, sodium dihydrogen phosphate and oxalic acid is 0.3~0.8:0.72~1.44:0.6
~4.
4. biomass carbon according to claim 3/vanadium phosphate sodium combination electrode material preparation method, which is characterized in that
It is 0.364~0.728 in step (2):0.72~1.44:0.756~3.78.
5. biomass carbon according to claim 1/vanadium phosphate sodium combination electrode material preparation method, which is characterized in that
In step (2), the ratio between quality and the volume of water of the vanadic anhydride are 0.3~0.8g:40mL~80mL.
6. biomass carbon according to claim 1/vanadium phosphate sodium combination electrode material preparation method, which is characterized in that
In step (3), the temperature of the heating is 160 DEG C~200 DEG C, and the time is 12~26 hours.
7. biomass carbon according to claim 1/vanadium phosphate sodium combination electrode material preparation method, which is characterized in that
In step (4), the reaction temperature of high-temperature heat treatment is 750-850 DEG C, and the reaction time is 8-10 hours.
8. biomass carbon according to claim 1/vanadium phosphate sodium combination electrode material preparation method, which is characterized in that
In step (1), (2) and (4), the environment temperature is 10~40 DEG C.
9. biomass carbon/vanadium phosphate sodium combination electrode material of described in any item preparation method preparations according to claim 1~8
Material.
10. biomass carbon according to claim 9/vanadium phosphate sodium combination electrode material is as sodium-ion battery positive material
Application.
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CN111943161A (en) * | 2020-08-24 | 2020-11-17 | 西北大学 | Preparation method and application of vanadium sodium fluorophosphate and carbon compounded secondary battery positive electrode material |
CN113036103A (en) * | 2021-03-04 | 2021-06-25 | 哈尔滨工程大学 | Electrode material of vanadium sulfide composite carbonized common sow thistle for potassium ion battery |
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