CN109921001A - A kind of vanadium phosphate sodium/carbon composite anode material and its Microwave-assisted synthesis and application - Google Patents
A kind of vanadium phosphate sodium/carbon composite anode material and its Microwave-assisted synthesis and application Download PDFInfo
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Abstract
A kind of vanadium phosphate sodium/carbon composite anode material of the present invention and its Microwave-assisted synthesis and application, wherein method includes: that stoichiometrically mixed dissolution obtains mixed liquor one with ammonium metavanadate by sodium dihydrogen phosphate, then the glycerol that volume fraction is 30.0%~36.7% is added, it is uniformly mixed to obtain mixed liquor two, the concentration of sodium dihydrogen phosphate is 180~210mmol/L, and the concentration of ammonium metavanadate is 120~140mmol/L；Mixed liquor two is placed in microwave hydrothermal reactor, 15~90min of reaction at 175~185 DEG C is warming up to；After reaction, cooled to room temperature obtains celadon suspension precipitating；Be warming up to 700~800 DEG C after filtering, freeze-drying, calcine 6~10h to get.The present invention uses the compound of microwave-hydrothermal method energy rapid synthesis NVP presoma and glycerol, vanadium phosphate sodium/carbon complex positive electrode with three-dimensional plate floral structure is prepared through calcining again, the three-dimensional plate floral structure is made of two-dimensional nano thin slice, has excellent high rate performance and cycle performance as sodium-ion battery positive material.
Description
Technical field
The present invention relates to sodium ion battery electrode material technical field, in particular to a kind of vanadium phosphate sodium/carbon composite anode
Material and its Microwave-assisted synthesis and application.
Technical background
With the exhaustion of fossil resource and becoming increasingly conspicuous for problem of environmental pollution, energy problem has become today's society
Focus of attention.Increasingly serious energy challenge is coped with, is crucial using the power generation of sustainable clean energy resource.However, common can
Regeneration clean energy resource such as wind energy, solar energy, tide energy equistability and duration is poor, and generated electric energy can not be directly incorporated into electricity
It is used in net.Therefore, it urgently needs to develop safe and efficient, economic energy storage technology.Lithium ion battery because energy density is high,
Long service life, it is highly-safe the advantages that, widely studied and applied.However the reserves of lithium are limited (only takes up an area shell
0.0065%), expensive, limit its application in large area energy storage.There are many similar physical chemistry for sodium and lithium
Matter, and its rich reserves (account for about the earth's crust 2.86%), therefore the sodium-ion battery of sodium ion substitution lithium ion is by extensive
Concern.But sodium ion has biggish ionic radius and slower kinetic rate, constrains its commercialized process.
Rhombic vanadium phosphate sodium, molecular formula Na3V2(PO4)3(being abbreviated as NVP) has Fast ion conductor structure
(NASICON), there is very high sodium ion diffusion coefficient, and sodium ion insertion/embedding process volume change out is small, voltage platform is suitable
In (3.4V), theoretical specific energy high (400Wh/kg), thermal stability are good, therefore as very promising sodium-ion battery anode material
Material is paid close attention to by researchers.But the electric conductivity of vanadium phosphate sodium is poor, causes its practical storage sodium capacity lower, high rate performance compared with
Difference.Carbon coating is considered as two effective ways for improving vanadium phosphate sodium chemical property: carbon packet with multi-level nano-structure is constructed
Intergranular electron transfer rate can be effectively improved by covering；On the one hand multi-level nano-structure is capable of providing big specific surface area, mention
The haptoreaction area of high electrode material and electrolyte；On the other hand it can reduce electronics and ion inside vanadium phosphate sodium particle
Transmission range, and continuous electron-transport path is provided, to improve the overall transmission rate of electronics and ion.
Currently, researchers generally use template to synthesize vanadium phosphate sodium/carbon complex multilevel structure.Such as apply for public affairs
The patent document of cloth CN 108134082A discloses a kind of template and high energy ball milling method combines to synthesize vanadium phosphate sodium
Method, is prepared the NVP of nanometer sheet accumulation flower-like structure, and the interphase for utilizing raw material to synthesize in specific operation process is
Template, then ball milling interphase, high-temperature calcination obtain the NVP of the flower-like structure of nanometer sheet accumulation.But there are following for this application
Disadvantage: energy consumption is high, process is tediously long, and product is inhomogenous.The present invention is quasi-, and to provide a kind of microblogging auxiliary synthesis vanadium phosphate sodium/carbon compound just
The method of pole material and vanadium phosphate sodium/application of the carbon composite anode material in sodium-ion battery of synthesis.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of vanadium phosphate sodium/carbon composite anode material and its microwave-assisted conjunctions
At with application.
In order to solve the above-mentioned technical problem, the invention adopts the following technical scheme:
A kind of method of Microwave-assisted synthesis vanadium phosphate sodium/carbon composite anode material is provided, is specifically comprised the following steps:
(1) it prepares presoma reaction solution: sodium dihydrogen phosphate stoichiometrically (3:2) is mixed with ammonium metavanadate, and
It is dissolved in the mixed liquor one for forming sodium dihydrogen phosphate and ammonium metavanadate in deionized water, glycerol is then added into mixed liquor one and makees
For carbon source and Morphological control agent, it is uniformly mixed to obtain the mixed liquor two of sodium dihydrogen phosphate, ammonium metavanadate and glycerol, glycerol accounts for
The volume fraction of mixed liquor two is 30%~36.7%；, in mixed liquor two: phosphate dihydrogen sodium concentration is 180~210mmol/L,
Ammonium metavanadate concentration is 120~140mmol/L；Phosphate dihydrogen sodium concentration: ammonium metavanadate concentration is 3:2；
(2) Microwave-assisted synthesis precursor product: mixed liquor two obtained by step (1) is placed in microwave hydrothermal reactor,
15~90min is reacted at 175~185 DEG C；To after reaction, through cooled to room temperature, it is heavy obtain celadon suspension
It forms sediment (precursor product)；
(3) it prepares vanadium phosphate sodium/carbon composite anode material: after the precipitating directly freezed drying of step (2), being warming up to
700~800 DEG C, calcine 6~10h to get.
Further,
In step (2), the frequency of setting microwave hydrothermal reactor is 2450MHz.
Further,
In step (2), the power of setting microwave hydrothermal reactor is 800W.
Further,
The precipitating after freeze-drying is placed in tube furnace in step (3) and is heated to the heating rate of 1~2 DEG C/min
After 700~800 DEG C, calcine 6~10 hours.
Further,
In step (2), the volume ratio of mixed liquor two and microwave hydrothermal reactor is 57~65:100.
The present invention also provides the sodium of vanadium phosphate made from the above method/carbon complex positive electrode, the vanadium phosphate sodium/carbon is multiple
Closing object positive electrode has by the laminar three-dimensional flower-shaped structure of two-dimensional nano.
The present invention also provides application of the above method in sodium-ion battery preparation.
The present invention also provides the sodium of vanadium phosphate made from the above method/carbon complex positive electrode answering in sodium-ion battery
With.
Chemical reaction process of the present invention and reaction equation are as follows:
(1) glycerol is added in the aqueous solution of sodium dihydrogen phosphate and ammonium metavanadate as carbon source and Morphological control agent microblogging hydro-thermal
The compound (celadon suspension precipitating) that NVP amorphous precursors and glycerol are made is reacted, equation is as follows:
(2) NVP without
The compound of setting presoma and glycerol obtains vanadium phosphate sodium/carbon composite anode material through calcining
Beneficial effects of the present invention:
1, the present invention uses the compound of microwave-hydrothermal method rapid synthesis NVP presoma and glycerol, prepares one through calcining
Vanadium phosphate sodium/carbon complex sodium ion positive electrode NVP/C of kind of three-dimensional plate floral structure, the NVP/C of the three-dimensional plate floral structure by
Two-dimensional nano thin slice composition, has excellent high rate performance and cycle performance.
2, preparation method energy consumption provided by the invention is small, and easy to operate, process is shorter, and product is uniform controllable, specific surface area
Greatly, the chemical property of final preparation gained vanadium phosphate sodium/carbon composite anode material is effectively improved, can be in high-performance sodium
There is preferable development prospect in ion battery.
3, preparation method provided by the invention, is dried in the state of freezing, and makes the presoma of synthesis, by freezing
At solid, vacuumize at low temperature, so that the water in presoma micropore is directly distilled by solid is vaporous water, vaporous water is removed,
Due to being to be distilled to be dehydrated by ice when removing water, there is no the surface tension of water, so that the nanometer micropore of sample is not collapsed, to keep
Structure originally.So that final product form is uniform.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is the XRD diagram of the NVP/C-MW-01 and comparative example 1NVP/C-CH-01 of the embodiment of the present invention 1；
Fig. 2 be the embodiment of the present invention 1 NVP/C-MW-01 under different amplification (scale 1um) SEM figure.
Fig. 3 be the embodiment of the present invention 1 NVP/C-MW-01 under different amplification (scale 100nm) SEM figure.
Fig. 4 be the embodiment of the present invention 1 NVP/C-MW-01 under different amplification (scale 200nm) TEM figure.
Fig. 5 be comparative example 1 of the present invention NVP/C-CH-01 under different amplification (scale 1um) SEM scheme.
Fig. 6 be comparative example 1 of the present invention NVP/C-CH-01 under different amplification (scale 100nm) SEM scheme.
Fig. 7 be the embodiment of the present invention 2 NVP/C-MW-02 under different amplification (scale 1um) SEM figure.
Fig. 8 be the embodiment of the present invention 3 NVP/C-MW-03 under different amplification (scale 1um) SEM figure.
Fig. 9 be the embodiment of the present invention 4 NVP/C-MW-04 under different amplification (scale 200nm) SEM figure.
Figure 10 is high rate performance figure of the NVP/C-MW-01 of the embodiment of the present invention 1 under different current densities.
Figure 11 is cycle performance figure of the NVP/C-MW-01 of the embodiment of the present invention 1 under the current density of 10C.
Figure 12 is high rate performance figure of the NVP/C-CH-01 of comparative example 1 under different current densities.
Figure 13 is cycle performance figure of the NVP/C-CH-01 of comparative example 1 under the current density of 1C.
Specific embodiment
In order to preferably illustrate the content of the invention, below by specific embodiment to further verifying of the invention.It is special
Illustrate herein, embodiment is only that more directly description is of the invention, they are a part of the invention, cannot be to structure of the present invention
At any restrictions.
In order to avoid influence of the variation to reaction of reaction pressure in reactor caused by reaction solution volume change, with
The volume of reaction solution is arranged to identical, the microwave hydrothermal reactor conduct reaction appearance of simultaneous selection same volume by lower embodiment
Device, the volume of reaction solution (i.e. mixed liquor two) and the volume ratio of microwave hydrothermal reactor are controlled in (57~65): 100, preferably
60ml:100ml.
Embodiment 1
The present embodiment provides a kind of method of Microwave-assisted synthesis vanadium phosphate sodium/carbon composite anode material, specifically include as
Lower step:
(1) stoichiometrically 3:2 accurately weighs sodium dihydrogen phosphate and ammonium metavanadate mixing, is dissolved in deionized water and obtains
To mixed liquor one, it is 33.3% glycerol as carbon source and Morphological control agent that volume fraction is added into mixed liquor one, is then stirred
Mix uniformly mixed, forming concentration is respectively the mixed of the sodium dihydrogen phosphate of 200mmol/L and 133mmol/L, ammonium metavanadate and glycerol
Close liquid two.
(2) mixed liquor two is placed in microwave hydrothermal reactor, frequency 2450MHz, power 800W, 180 DEG C of hydro-thermals is set
React 1h；After reaction, through cooled to room temperature, celadon suspension precipitating (precursor product) is obtained.
(3) precipitating filtering, after freeze-drying, with the heating rate of 2 DEG C/min be warming up at 750 DEG C calcine 8h to get.Institute
It obtains product and is denoted as NVP/C-MW-01.
Embodiment 2
The present embodiment provides the methods of another Microwave-assisted synthesis vanadium phosphate sodium/carbon composite anode material, specifically include
Following steps:
(1) stoichiometrically 3:2 accurately weighs sodium dihydrogen phosphate and ammonium metavanadate mixing, is dissolved in deionized water and obtains
To mixed liquor one, it is 36.7% glycerol as carbon source and Morphological control agent that volume fraction is added into mixed liquor one, is then stirred
Mix uniformly mixed, forming concentration is respectively the mixed of the sodium dihydrogen phosphate of 210mmol/L and 140mmol/L, ammonium metavanadate and glycerol
Close liquid two.
(2) mixed liquor two is placed in microwave hydrothermal reactor, frequency 2450MHz, power 800W, 180 DEG C of hydro-thermals is set
React 30min；After reaction, through cooled to room temperature, celadon suspension precipitating (precursor product) is obtained.
(3) precipitating filtering, after freeze-drying, with the heating rate of 1 DEG C/min be warming up at 700 DEG C calcine 10h to get.
Products therefrom is denoted as NVP/C-MW-02.
Embodiment 3
The present embodiment provides the methods of another Microwave-assisted synthesis vanadium phosphate sodium/carbon composite anode material, specifically include
Following steps:
(1) stoichiometrically 3:2 weighs sodium dihydrogen phosphate and ammonium metavanadate mixing, is dissolved in deionized water and is mixed
Liquid one is closed, it is 30% glycerol as carbon source and Morphological control agent that volume fraction is added into mixed liquor one, is then stirred
Uniformly, the mixed liquor two that concentration is respectively the sodium dihydrogen phosphate of 180mmol/L and 120mmol/L, ammonium metavanadate and glycerol is formed.
(2) mixed liquor two is placed in microwave hydrothermal reactor, frequency 2450MHz, power 800W, 175 DEG C of hydro-thermals is set
React 90min；After reaction, through cooled to room temperature, celadon suspension precipitating (precursor product) is obtained.
(3) precipitating filtering, after freeze-drying, with the heating rate of 2 DEG C/min be warming up at 800 DEG C calcine 6h to get.Institute
It obtains product and is denoted as NVP/C-MW-03.
Embodiment 4
The present embodiment provides the methods of another Microwave-assisted synthesis vanadium phosphate sodium/carbon composite anode material, specifically include
Following steps:
(1) stoichiometrically 3:2 weighs sodium dihydrogen phosphate and ammonium metavanadate mixing, is dissolved in deionized water and is mixed
Liquid one is closed, it is 33.3% glycerol as carbon source and Morphological control agent that volume fraction is added into mixed liquor one, and then stirring is mixed
Close the mixed liquor for uniformly forming that concentration is respectively the sodium dihydrogen phosphate of 200mmol/L and 133mmol/L, ammonium metavanadate and glycerol
Two.
(2) in the microwave hydrothermal reactor for being placed in mixed liquor two, frequency 2450MHz, power 800W, 185 DEG C of water are set
Thermal response 15min；After reaction, through cooled to room temperature, celadon suspension precipitating (precursor product) is obtained.
(3) precipitating filtering, after freeze-drying, with the heating rate of 2 DEG C/min be warming up at 800 DEG C calcine 8h to get.Institute
It obtains product and is denoted as NVP/C-MW-04.
Comparative example 1
This comparative example the difference from embodiment 1 is that: step (2) using conventional hydrothermal method substitute microwave-hydrothermal method, reaction
12h.Products therefrom is denoted as NVP/C-CH-01.
Material morphology and storage sodium performance characterization analysis are carried out to product made from above-described embodiment:
1, the vanadium phosphate sodium positive electrode product prepared to above-described embodiment and comparative example 1 carries out morphology analysis:
(1) detection method:
Field emission scanning electron microscope (FESEM, Hitachi, S3400, Japan) and high resolution TEM (HRTEM,
JEOL, JEM-2010, Japan) under the pattern of above-mentioned product is detected respectively.X-ray diffraction diffractometer (XRD,
Haoyuan dx-2700, China) copper K α radiation 40kV and 30mA is used, for describing the crystal structure of NVP/C sample.
(2) Analysis of conclusion:
Fig. 1 is the XRD diagram of the product NVP/C-MW-01 of the embodiment of the present invention 1 and the product NVP-CH-01 of comparative example 1, by
Fig. 1 it can be seen that
1) the XRD peak intensity of the NVP/C-MW-01 of embodiment 1 is apparently higher than NVP/C-CH-01, illustrates using of the invention micro-
The obtained NVP/C product of wave hydro-thermal method has better crystallinity；
2) there are miscellaneous peak (grey iris out part in figure) in the XRD spectrum of the product NVP/C-CH-01 of Fig. 1 comparative example 1, and
Miscellaneous peak is not present in the XRD spectrum of the product NVP/C-MW-01 of the embodiment of the present invention 1, illustrates that microwave-hydrothermal method of the present invention is advantageous
In obtaining the higher vanadium phosphate sodium product of purity.
Fig. 2-3 be respectively the embodiment of the present invention 1 product NVP/C-MW-01 under different amplification (scale 1um,
SEM figure 100nm).By Fig. 2-3 it can be seen that the product NVP/C-MW-01 of the embodiment of the present invention 1 is two-dimensional nano thin slice group
At three-dimensional flower-shaped structure.Fig. 4 is TEM figure of the product NVP/C-MW-01 under 200nm scale, as seen from Figure 4 three-dimensional plate
Flower diameter about 250nm, only 10nm is thick for component units vanadium phosphate sodium two-dimensional slice, and the surface area of NVP/C-MW-01 is
119m2/g.Therefore, it can be seen that vanadium phosphate sodium product made from microwave-hydrothermal method of the invention is uniform from Fig. 2-4, specific surface area
Greatly.
Fig. 5-6 be comparative example 1 product NVP/C-CH-01 under different amplification (scale 1um, 100nm) SEM
Figure.The pattern of the product NVP/C-CH-01 of comparative example 1 is inhomogenous it can be seen from Fig. 5-6, is made of several nanometers of particle
Thin slice also has the bulky grain of about 200nm, and the NVP/C-CH surface area that comparative example 1 obtains is only 61m2/ g, specific surface area are small.
Fig. 7-9 is respectively the SEM figure of 2,3,4 product of embodiment.Image is shown: its vanadium phosphate sodium positive electrode obtained produces
Object all has the laminar three-dimensional flower-shaped structure of two-dimensional nano and biggish reference area.
2, the electrochemical measurement of vanadium phosphate sodium positive electrode product product prepared by embodiment 1 and comparative example 1
(1) experimental method
Using product NVP/C-CH-01 made from product NVP/C-MW-01 made from embodiment 1 and comparative example 1 as anode
Material, and be that 7:2:1 is mixed, while adjoining pyrrolidone with a certain amount of N- methyl according to mass ratio with conductive agent and binder
(NMP) solvent is ground into slurry.Then prepared thick slurry is coated uniformly on aluminium foil using coating equipment, will be made
The standby obtained aluminium foil for being coated with electrode material, which is put into 70 DEG C of vacuum drying ovens, dries.After being dried by the roll squeezer of suitable spacing
Aluminium foil compacting, obtained electrode film is then washed into sheet-punching machine a certain size disk.It weighs to obtain electricity with weighing balance
The weight of pole piece.It can be obtained by the quality of electrode material according to the quality that the weight of electrode slice cuts same size aluminium foil.?
It is 70% according to ratio of the active electrode material quality when smearing, so that active electrode material on electrode slice may finally be obtained
The quality of material.And as anode, metallic sodium piece is cathode, and glass fibre is as diaphragm, and sodium perchlorate is electrolyte, in gloves
It is assembled into sodium-ion battery in case, is applied in sodium-ion battery.
(2) results and discussion
Figure 10 is high rate performance figure of the NVP/C-MW-01 of the embodiment of the present invention 1 under different current densities.It can by Figure 10
To find out: NVP/C-MW-01 under 0.5C, 1C, 10C, 20C, 40C current density, specific discharge capacity is respectively 107,103,
101,97 and 93mAh/g, and when current density again returns to 0.5C, specific discharge capacity remains to reach 102mAh/g, capacity
Almost without decaying, excellent high rate performance is shown.
Figure 11 is cycle performance figure of the NVP/C-MW-01 of the embodiment of the present invention 1 under the current density of 10C.By Figure 11
It can be seen that it is excellent that there is the product NVP/C-MW-01 of three-dimensional plate floral structure to show obtained by embodiment 1 under 10C multiplying power
Cycle performance.
Figure 12 is high rate performance figure of the product NVP/C-CH-01 of comparative example 1 under different current densities.It can be with by Figure 12
Find out, for NVP/C-CH-01 under 0.1C, 0.5C, 1C, 5C, 10C current density, specific discharge capacity is respectively 71,49,46,27
And 10mAh/g, and when current density again returns to 5C, specific discharge capacity only has 28mAh/g, illustrates that comparative example 1 obtains
The performance of the product NVP/C-CH-01 high rate performance product NVP/C-MW-01 that compares the embodiment of the present invention 1 want far short of what is expected.
Figure 13 is cycle performance figure of the product NVP/C-CH-01 of comparative example 1 under the current density of 1C.It can be with by Figure 13
Find out: the cycle performance of the product NVP/C-CH-01 of comparative example 1 wants far short of what is expected compared to the product of the embodiment of the present invention.
In addition, preparation method energy consumption provided in an embodiment of the present invention is small, process is shorter, and the hydro-thermal method of comparative example needs
12h can just obtain NVP product, and the present invention is by the way of Microwave-assisted synthesis, it can will shorten to 15 the reaction time~
90min。
The above is a specific embodiment of the invention, but any restrictions cannot be constituted to the present invention, therefore need special
It points out, it is all based on the present invention, it is made any modification and is all fallen within the scope of the present invention with improvement.
Claims (6)
1. a kind of method of Microwave-assisted synthesis vanadium phosphate sodium/carbon composite anode material, which is characterized in that specifically include following step
It is rapid:
(1) prepare presoma reaction solution: sodium dihydrogen phosphate stoichiometrically mixed with ammonium metavanadate and be dissolved in from
The mixed liquor one of sodium dihydrogen phosphate and ammonium metavanadate is formed in sub- water, and glycerol is then added into mixed liquor one as carbon source and shape
Looks adjusting control agent is uniformly mixed to obtain the mixed liquor two of sodium dihydrogen phosphate, ammonium metavanadate and glycerol, and glycerol accounts for mixed liquor two
Volume fraction is 30%~36.7%；In mixed liquor two: the concentration of sodium dihydrogen phosphate is 180~210mmol/L, ammonium metavanadate
Concentration is 120~140mmol/L；Sodium dihydrogen phosphate: the concentration of ammonium metavanadate is 3:2；
(2) Microwave-assisted synthesis precursor product: mixed liquor two obtained by step (1) is placed in microwave hydrothermal reactor, in 175
15~90min is reacted at~185 DEG C；To after reaction, through cooled to room temperature, obtain celadon suspension precipitating；
(3) it prepares vanadium phosphate sodium/carbon composite anode material: the precipitating of step (2) is filtered, after freeze-drying, it is warming up to 700~
800 DEG C, calcine 6~10h to get.
2. the method for Microwave-assisted synthesis vanadium phosphate sodium/carbon composite anode material according to claim 1, feature exist
In,
In step (2), the frequency of setting microwave hydrothermal reactor is 2450MHz.
3. the method for Microwave-assisted synthesis vanadium phosphate sodium/carbon composite anode material according to claim 1 or 2, feature
It is,
The precipitating after freeze-drying is placed in tube furnace in step (3) and is heated to being warming up to the heating rate of 1~2 DEG C/min
700~800 DEG C, calcine 6~10h.
4. the method for Microwave-assisted synthesis vanadium phosphate sodium/carbon composite anode material according to claim 1 or 2, feature
It is,
In step (2), the volume ratio of mixed liquor two and microwave hydrothermal reactor is (57~65): 100.
5. vanadium phosphate made from the method for Microwave-assisted synthesis vanadium phosphate sodium/carbon composite anode material of any of claims 1 or 2
Sodium/carbon complex positive electrode, the vanadium phosphate sodium/carbon complex positive electrode have by the laminar three-dimensional of two-dimensional nano
Flower-like structure.
6. vanadium phosphate made from the method for Microwave-assisted synthesis vanadium phosphate sodium/carbon composite anode material of any of claims 1 or 2
Sodium/application of the carbon complex positive electrode in sodium-ion battery.
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| CN114221025A (en) * | 2021-12-15 | 2022-03-22 | 四川大学 | Sodium vanadium phosphate @ carbon core-shell nanorod, and preparation method and application thereof |
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