CN108054349A - A kind of carbon coating type phosphoric acid vanadium lithium and preparation method thereof - Google Patents
A kind of carbon coating type phosphoric acid vanadium lithium and preparation method thereof Download PDFInfo
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- CN108054349A CN108054349A CN201711104326.9A CN201711104326A CN108054349A CN 108054349 A CN108054349 A CN 108054349A CN 201711104326 A CN201711104326 A CN 201711104326A CN 108054349 A CN108054349 A CN 108054349A
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- 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
- H01M4/366—Composites as layered products
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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
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- H—ELECTRICITY
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- 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
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Abstract
The invention belongs to technical field of energy storage, disclose a kind of method for preparing carbon coating type phosphoric acid vanadium lithium, including：According to stoichiometric ratio, by Li2CO3、NH4H2PO4, citric acid and V2O5H2O hydrogels mix and are stirred at room temperature to obtain the first intermediate product；Carbon source and distilled water with first intermediate product are mixed, obtain the second intermediate product；Second intermediate product is heated using microwave heating, obtains the 3rd intermediate product；By the 3rd intermediate product be sealed at the first temperature at least 12 it is small when, obtain the 4th intermediate product；By the intermediate product at the second temperature, calcined in nitrogen atmosphere, obtain carbon coating type phosphoric acid vanadium lithium；Wherein, first temperature is more than or equal to 80 DEG C, and the second temperature is more than or equal to 350 DEG C.The present invention provides a kind of phosphoric acid vanadium lithium preparation method for promoting battery conductive.
Description
Technical field
The present invention relates to technical field of energy storage, more particularly to a kind of carbon coating type phosphoric acid vanadium lithium and preparation method thereof.
Background technology
At present, safety problem is increasingly becoming power lithium-ion battery in mixed power electric car and large-scale energy-storage system
(LIB) focus of future development.Monoclinic lithium vanadium phosphate (Li as one of most potential anode candidate3V2(PO4)3) by
In the PO of its covalent bonding4Group and the fast ionic diffusion coefficient being induced by it, show excellent thermal stability；With business
Transition metal oxide is compared, and has unique three-dimensional ion diffusion tunnel.However, when lithium ion passes through phase boundary diffusion, by
In separated VO6Octahedron causes Li3V2(PO4)3Electrical conductivity it is poor.
The content of the invention
The present invention provides a kind of carbon coating type phosphoric acid vanadium lithium and preparation method thereof, and it is conductive to solve phosphoric acid vanadium lithium in the prior art
The technical issues of property is poor.
In order to solve the above technical problems, the present invention provides a kind of method for preparing carbon coating type phosphoric acid vanadium lithium, including：
According to stoichiometric ratio, by Li2CO3、NH4H2PO4, citric acid and V2O5H2O hydrogels mix and at room temperature
Stir to get the first intermediate product；
Carbon source and distilled water with first intermediate product are mixed, obtain the second intermediate product；
Second intermediate product is heated using microwave heating, obtains the 3rd intermediate product；
By the 3rd intermediate product be sealed at the first temperature at least 12 it is small when, obtain the 4th intermediate product；
By the intermediate product at the second temperature, calcined in nitrogen atmosphere, obtain carbon coating type phosphoric acid vanadium lithium；
Wherein, first temperature is more than or equal to 80 DEG C, and the second temperature is more than or equal to 350 DEG C.
Further, the spy source uses polyethylene glycol PEG.
Further, during first intermediate product is prepared, mixing time is more than or equal to 30 minutes.
Further, when heating second intermediate product using microwave heating, using described in 320 watts of microwave irradiations
Second intermediate product at least 15 minutes.
Further, the phosphorus content of the carbon coating type phosphoric acid vanadium lithium is 7.69%.
A kind of carbon coating type phosphoric acid vanadium lithium, adopts and is prepared with the aforedescribed process.
A kind of preparation method of battery, using the above-mentioned carbon coating type phosphoric acid vanadium lithium stated；And using following steps：
Using n-methyl-2-pyrrolidone as solvent, by the carbon coating type phosphoric acid vanadium lithium, conductive black and Kynoar
PVDF, in mass ratio 8: 1: 1 are mixed and stirred for uniformly obtaining slurry；
The slurry is coated on aluminium foil, is then dried in vacuo in an oven, then suppresses and electrode slice to be measured is uniformly made,
And as anode；
Using lithium piece as to electrode, Celgard 2300 is membrane engagement electrolyte, is assembled into button cell.
Further, the electrolyte uses LiPF6For solute, the carbonic acid Asia second for 1: 1 mixing according to volume ratio is used
Ester and dimethyl carbonate mixed liquor are solvent；
Wherein, the concentration of electrolyte is 1mol/L.
Further, in the electrode slice quality control of carbon coating type phosphoric acid vanadium lithium in 1.2-1.5mg.
The one or more technical solutions provided in the embodiment of the present application, have at least the following technical effects or advantages：
The method of the preparation carbon coating type phosphoric acid vanadium lithium provided in the embodiment of the present application is situated between using polyethylene glycol as rheology
Matter and carbon matrix precursor successfully synthesize the good carbon coating type phosphoric acid vanadium lithium of high rate capability by rheology phase assisted microwave synthesis method and make
For positive electrode.Polyethylene glycol PEG is nonionic surface active agent, has preferable micelle formation and excellent scattered effect
Fruit, when preparing material, particle size can be reduced, subtract less granular reunion by adding in PEG；There is very strong configurational energy simultaneously
Power, oxygen atom and negative oxygen ion therein can form stable chelate with metal ion, can be efficiently against sintered
The particle agglomeration occurred in journey, and ethylene glycol also has coating material effect, can improve the crystallization degree of product, and
PEG is ordered into the carbon-coating of chain structure in the carbon that Pintsch process generates, and can improve the electrical conductivity of material, can improve the electricity of material
Conductance and cyclicity.Relatively uniform Li3V2(PO4)3Particle is encapsulated in amorphous carbon structure, is formed nucleocapsid structure, is provided
Effective electronics and ion transmission.When as cathode in lithium ion battery, composite material is shown under 50 DEG C of charge-discharge velocities
Show maximum discharge capacity for 101.8mAh g-1, and still there is 98.3% capacity retention ratio after 100 Xun Huans, show
Excellent high rate performance and excellent cyclical stability.Good chemical property be attributable to microwave Fast back-projection algorithm and
Even carbon coating, uniform coating carbon is from rheology phase precursor and small primary granule.
Description of the drawings
Fig. 1 is the small multiplying power 0.2C of carbon coating phosphoric acid vanadium lithium composite material provided by the invention, initial charge and discharge under 0.5C, 1C
Electric curve；
Fig. 2 is the small multiplying power 0.2C of carbon coating phosphoric acid vanadium lithium composite material provided by the invention, cycle performance under 0.5C, 1C
Schematic diagram；
Fig. 3 is the big multiplying power 5C of carbon coating phosphoric acid vanadium lithium composite material provided by the invention, and initial charge/discharge is bent under 10C
Line；
Fig. 4 is the big multiplying power 5C of carbon coating phosphoric acid vanadium lithium composite material provided by the invention, and cycle performance is illustrated under 10C
Figure；
Fig. 5 is the cyclic voltammetry curve of carbon coating phosphoric acid vanadium lithium composite material under the conditions of 0.1mV s-1 provided by the invention；
Fig. 6 is big multiplying power 5C provided by the invention, 10C, 20C, and carbon coating phosphoric acid vanadium lithium composite material follows under the conditions of 50C
Ring stability；Wherein, insertion is shown in the curve of the 5th, 25,50,75 and 100 circles under 50C multiplying powers.
Specific embodiment
The embodiment of the present application solves phosphoric acid in the prior art by carrying a kind of carbon coating type phosphoric acid vanadium lithium and preparation method thereof
The technical issues of vanadium lithium poorly conductive.
In order to better understand the above technical scheme, in conjunction with appended figures and specific embodiments to upper
It states technical solution to be described in detail, it should be understood that the specific features in the embodiment of the present invention and embodiment are to the application skill
The detailed description of art scheme rather than the restriction to technical scheme, in the case where there is no conflict, the embodiment of the present application
And the technical characteristic in embodiment can be mutually combined.
A kind of method for preparing carbon coating type phosphoric acid vanadium lithium, including：
According to stoichiometric ratio, by Li2CO3、NH4H2PO4, citric acid and V2O5H2O hydrogels mix and at room temperature
Stir to get the first intermediate product；
Carbon source and distilled water with first intermediate product are mixed, obtain the second intermediate product；
Second intermediate product is heated using microwave heating, obtains the 3rd intermediate product；
By the 3rd intermediate product be sealed at the first temperature at least 12 it is small when, obtain the 4th intermediate product；
By the intermediate product at the second temperature, calcined in nitrogen atmosphere, obtain carbon coating type phosphoric acid vanadium lithium；
Wherein, first temperature is more than or equal to 80 DEG C, and the second temperature is more than or equal to 350 DEG C.
Preferably, the spy source uses polyethylene glycol PEG.
In general, during first intermediate product is prepared, mixing time is more than or equal to 30 minutes.Using micro-
When Wave heating mode heats second intermediate product, using the second intermediate product at least 15 minutes described in 320 watts of microwave irradiations.
The phosphorus content of the carbon coating type phosphoric acid vanadium lithium is 7.69%.
The present embodiment also provides a kind of carbon coating type phosphoric acid vanadium lithium, adopts and is prepared with the aforedescribed process.
A kind of preparation method of battery, using the above-mentioned carbon coating type phosphoric acid vanadium lithium stated；And using following steps：
Using n-methyl-2-pyrrolidone as solvent, by the carbon coating type phosphoric acid vanadium lithium, conductive black and Kynoar
PVDF, in mass ratio 8: 1: 1 are mixed and stirred for uniformly obtaining slurry；
The slurry is coated on aluminium foil, is then dried in vacuo in an oven, then suppresses and electrode slice to be measured is uniformly made,
And as anode；
Using lithium piece as to electrode, Celgard 2300 is membrane engagement electrolyte, is assembled into button cell.
In general, the electrolyte uses LiPF6For solute, the carbonic acid Asia second for 1: 1 mixing according to volume ratio is used
Ester and dimethyl carbonate mixed liquor are solvent；Wherein, the concentration of electrolyte is 1mol/L.Carbon coating type phosphoric acid in the electrode slice
The quality control of vanadium lithium is in 1.2-1.5mg.
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with attached drawing to embodiment party of the present invention
Formula is described in further detail.
Embodiment one:Exemplified by using PEG-400 as carbon source：
An embodiment of the present invention provides a kind of preparation method of the negative material available for lithium ion battery, as shown in Figure 1,
This method includes：
(1) Li2CO3, NH4H2PO4, citric acid and V2O5H2O hydrogels are stoichiometrically weighed, is mixed and in room temperature
Lower stirring 30 minutes.
(2) PEG-400 of 1.5ml and suitable distilled water are added in mixture to obtain rheological body.PEG herein
As auxiliary rheological agents medium and carbon precursor.Then mixture is transferred in polytetrafluoroethylene (PTFE) (PTFE) container, and at 80 DEG C
Seal 12 it is small when.Obtained rheology presoma is calcined into 4h in 350 DEG C, N2 atmosphere.
(3) gained powder is worn into graininess again, be sealed in the crucible equipped with activated carbon, and in household microwave oven
With microwave (micro-wave oven is set, it means that has the non-microwave time during each irradiation) 15 minutes (frequencies of irradiation of 320W
Rate 2.45GHz, 800W).Carbon content in final products is determined as about 7.69%.
(4) by X-ray diffraction, the instruments such as scanning electron microscope and transmission electron microscope are to the physical property of product
It is characterized.The use of wavelength is 532nm, the WITEC α -300R Raman microscopes that surface sweeping scope is 50~1400cm-1 carry out
Raman spectrum analyses.
(5) material is made using suitable n-methyl-2-pyrrolidone as solvent, by Li3V2 (PO4) 3/C, conductive black
And PVDF, in mass ratio 80: 10: 10 are uniformly mixed, and stir 2h.Slurry is coated on aluminium foil, then the vacuum in 120 DEG C of baking ovens
Dry 12h, it is then uniform in being suppressed on tablet press machine, electrode slice to be measured is made.
(6) on each electrode the quality control of active material in 1.2-1.5mg.Using Li3V2 (PO4) 3/C as anode, lithium piece
For to electrode, Celgard 2300 is membrane, 1mol/L LiPF6/ (ethylene carbonate (EC) and dimethyl carbonate (DMC)=1：
1) solution is assembled into CR2032 types button cell and carries out charge-discharge test as electrolyte.
(7), referring to Fig. 1, Fig. 2, Fig. 3, Fig. 4, Fig. 5 and Fig. 6, constant current charge and discharge is carried out in multi-channel battery test system
Electrical measurement, potential range 3.0-4.3V, scope 0.2C, 0.5C, 1C, 5C, 10C, 20C to 50C.(1C is represented at room temperature
Current density is 133mAg-1).Cycling volt is carried out on Garmy PCI 4-750 electrochemical workstations between 3.0 and 4.3V
Peace method is tested, and sweep speed is 0.1mV s-1.
Embodiment two：Exemplified by using dodecyl sodium sulfonate lithium (SDS) as carbon source
An embodiment of the present invention provides a kind of preparation method of the negative material available for lithium ion battery, this method bags
It includes：
(1) Li2CO3, NH4H2PO4, citric acid and V2O5H2O hydrogels are stoichiometrically weighed, is mixed and in room temperature
Lower stirring 30 minutes.
(2) SDS of 2g and suitable distilled water are added in mixture to obtain rheological body.SDS is used as stream herein
Become auxiliary agent medium and carbon precursor.Then mixture is transferred in polytetrafluoroethylene (PTFE) (PTFE) container, and 12 is sealed at 80 DEG C
Hour.Obtained rheology presoma is calcined into 4h in 350 DEG C, N2 atmosphere.
(3) gained powder is worn into graininess again, be sealed in the crucible equipped with activated carbon, and in household microwave oven
With microwave (micro-wave oven is set, it means that has the non-microwave time during each irradiation) 5 minutes (frequencies of irradiation of 320W
2.45GHz, 800W).Carbon content in final products is determined as about 7.69%.
(4) by X-ray diffraction, the instruments such as scanning electron microscope and transmission electron microscope are to the physical property of product
It is characterized.The use of wavelength is 532nm, the WITEC α -300R Raman microscopes that surface sweeping scope is 50~1400cm-1 carry out
Raman spectrum analyses.
(5) material is made using suitable n-methyl-2-pyrrolidone as solvent, by Li3V2 (PO4) 3/C, conductive black
And PVDF, in mass ratio 80: 10: 10 are uniformly mixed, and stir 2h.Slurry is coated on aluminium foil, then the vacuum in 120 DEG C of baking ovens
Dry 12h, it is then uniform in being suppressed on tablet press machine, electrode slice to be measured is made.
(6) on each electrode the quality control of active material in 1.2-1.5mg.Using Li3V2 (PO4) 3/C as anode, lithium piece
For to electrode, Celgard 2300 is membrane, 1mol/L LiPF6/ (ethylene carbonate (EC) and dimethyl carbonate (DMC)=1：
1) solution is assembled into CR2032 types button cell and carries out charge-discharge test as electrolyte.
(7) constant current charge-discharge measurement, potential range 3.0-4.3V, scope are carried out in multi-channel battery test system
For 0.2C, 0.5C, 1C, 5C, 10C, 20C to 50C.(1C represents that current density is 133mAg-1) at room temperature.In 3.0 and 4.3V
Between Garmy PCI 4-750 electrochemical workstations on carry out cyclic voltammetry test, sweep speed be 0.1mV s-1.
Embodiment one, embodiment two difference lies in：By the use of different surfactants as carbon source, and it is successfully prepared carbon
Coat lithium vanadium phosphate material；Embodiment one, two is different difference lies in microwave treatment time.
The one or more technical solutions provided in the embodiment of the present application, have at least the following technical effects or advantages：
The method of the preparation carbon coating type phosphoric acid vanadium lithium provided in the embodiment of the present application is situated between using polyethylene glycol as rheology
Matter and carbon matrix precursor successfully synthesize the good carbon coating type phosphoric acid vanadium lithium of high rate capability by rheology phase assisted microwave synthesis method and make
For positive electrode.Polyethylene glycol PEG is nonionic surface active agent, has preferable micelle formation and excellent scattered effect
Fruit, when preparing material, particle size can be reduced, subtract less granular reunion by adding in PEG；There is very strong configurational energy simultaneously
Power, oxygen atom and negative oxygen ion therein can form stable chelate with metal ion, can be efficiently against sintered
The particle agglomeration occurred in journey, and ethylene glycol also has coating material effect, can improve the crystallization degree of product, and
PEG is ordered into the carbon-coating of chain structure in the carbon that Pintsch process generates, and can improve the electrical conductivity of material, can improve the electricity of material
Conductance and cyclicity.Relatively uniform Li3V2(PO4)3Particle is encapsulated in amorphous carbon structure, is formed nucleocapsid structure, is provided
Effective electronics and ion transmission.When as cathode in lithium ion battery, composite material is shown under 50 DEG C of charge-discharge velocities
Show maximum discharge capacity for 101.8mAh g-1, and still there is 98.3% capacity retention ratio after 100 Xun Huans, show
Excellent high rate performance and excellent cyclical stability.Good chemical property be attributable to microwave Fast back-projection algorithm and
Even carbon coating, uniform coating carbon is from rheology phase precursor and small primary granule.
It should be noted last that more than specific embodiment is merely illustrative of the technical solution of the present invention and unrestricted,
Although the present invention is described in detail with reference to example, it will be understood by those of ordinary skill in the art that, it can be to the present invention
Technical solution be modified or replaced equivalently, without departing from the spirit and scope of technical solution of the present invention, should all cover
Among scope of the presently claimed invention.
Claims (9)
- A kind of 1. method for preparing carbon coating type phosphoric acid vanadium lithium, which is characterized in that including：According to stoichiometric ratio, by Li2CO3、NH4H2PO4, citric acid and V2O5H2O hydrogels are mixed and are stirred at room temperature To the first intermediate product；Carbon source and distilled water with first intermediate product are mixed, obtain the second intermediate product；Second intermediate product is heated using microwave heating, obtains the 3rd intermediate product；By the 3rd intermediate product be sealed at the first temperature at least 12 it is small when, obtain the 4th intermediate product；By the intermediate product at the second temperature, calcined in nitrogen atmosphere, obtain carbon coating type phosphoric acid vanadium lithium；Wherein, first temperature is more than or equal to 80 DEG C, and the second temperature is more than or equal to 350 DEG C.
- 2. the method for carbon coating type phosphoric acid vanadium lithium is prepared as described in claim 1, it is characterised in that：The spy source uses poly- second Glycol PEG.
- 3. the method for carbon coating type phosphoric acid vanadium lithium is prepared as claimed in claim 2, it is characterised in that：It is preparing in described first Between during product, mixing time is more than or equal to 30 minutes.
- 4. the method for carbon coating type phosphoric acid vanadium lithium is prepared as claimed in claim 2, it is characterised in that：Using microwave heating When heating second intermediate product, using the second intermediate product at least 15 minutes described in 320 watts of microwave irradiations.
- 5. the method for carbon coating type phosphoric acid vanadium lithium is prepared as claimed in claim 2, it is characterised in that：The carbon coating type phosphoric acid The phosphorus content of vanadium lithium is 7.69%.
- 6. a kind of carbon coating type phosphoric acid vanadium lithium, which is characterized in that be prepared using method as claimed in claim 2.
- 7. a kind of preparation method of battery, which is characterized in that use carbon coating type phosphoric acid vanadium lithium as claimed in claim 6；And Using following steps：Using n-methyl-2-pyrrolidone as solvent, by the carbon coating type phosphoric acid vanadium lithium, conductive black and Kynoar PVDF, in mass ratio 8: 1: 1 are mixed and stirred for uniformly obtaining slurry；The slurry is coated on aluminium foil, is then dried in vacuo in an oven, then suppresses and electrode slice to be measured is uniformly made, and with This is anode；Using lithium piece as to electrode, Celgard 2300 is membrane engagement electrolyte, is assembled into button cell.
- 8. the preparation method of battery as claimed in claim 7, which is characterized in that the electrolyte uses LiPF6For solute, adopt It is solvent with according to the ethylene carbonate and dimethyl carbonate mixed liquor that volume ratio is 1: 1 mixing；Wherein, the concentration of electrolyte is 1mol/L.
- 9. the preparation method of battery as claimed in claim 7, which is characterized in that carbon coating type phosphoric acid vanadium lithium in the electrode slice Quality control in 1.2-1.5mg.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109755514A (en) * | 2018-12-27 | 2019-05-14 | 大连博融新材料有限公司 | A kind of carbon coating lithium vanadium fluorophosphates lithium ionic cell anode material and preparation method thereof |
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