CN109037630B - A kind of phosphorus doping carbon coating Na3V2(PO4)2O2F positive electrode and preparation method thereof - Google Patents
A kind of phosphorus doping carbon coating Na3V2(PO4)2O2F positive electrode and preparation method thereof Download PDFInfo
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- CN109037630B CN109037630B CN201810827892.0A CN201810827892A CN109037630B CN 109037630 B CN109037630 B CN 109037630B CN 201810827892 A CN201810827892 A CN 201810827892A CN 109037630 B CN109037630 B CN 109037630B
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- H—ELECTRICITY
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- 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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- 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
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- 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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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- H—ELECTRICITY
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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
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Abstract
The present invention provides a kind of phosphorus doping carbon coating Na3V2(PO4)2O2F positive electrode and preparation method thereof, method are by ammonium metavanadate NH4VO3, ammonium dihydrogen phosphate NH4H2PO4, sodium fluoride NaF and sodium carbonate Na2CO3It is dissolved in deionized water, adds phytic acid and ethylene glycol, be transferred in reaction kettle after mixing, insulation reaction；Centrifugation, washing, obtain presoma after drying；Presoma is dispersed in alcohol, suitable glucose is added, is stirred to dry；Gained mixture is sintered in tube furnace finally, obtains the carbon-coated Na of phosphorus doping3V2(PO4)2O2F positive electrode.Carbon coating can significantly improve Na in technical solution of the present invention3V2(PO4)2O2The electronic conductivity of F positive electrode reduces polarization, improves the specific capacity and cyclical stability of material；The carbon-coated Na of the phosphorus doping of preparation3V2(PO4)2O2F positive electrode has good cycle performance and high rate performance.
Description
Technical field
The present invention relates to a kind of carbon-coated Na of phosphorus doping3V2(PO4)2O2F positive electrode and preparation method thereof, belongs to electrification
Learn power electrode Material Field.
Background technique
In recent years, lithium ion secondary battery because have high-energy density, high working voltage, memory-less effect, self discharge it is small,
It has extended cycle life, advantages of environment protection has become ideal energy accumulating device.As lithium ion battery is in portable electronic
The rapid development of the extensive use in market, especially electric automobile market, demand of the people to lithium ion battery are increasing.It is former
Therefore the lithium resource of this reserves limited (0.006%) is also largely consumed, and will face exhaustion.Therefore, with resourceful, cost
Cheap, widely distributed sodium is that the sodium-ion battery of basic raw material receives the extensive concern of people.Sodium and the same main group of lithium, physics
Chemical property is similar, from a wealth of sources, and content is higher in the earth's crust, and about 2.74%, the relative mass of sodium is bigger, can store more
Energy, the potential of sodium is higher, and selectable electrolyte range is wider, have more stable chemical property, make its safety
It is higher.Sodium-ion battery is similar with lithium ion battery working principle, is realized using embedding de- process of the sodium ion between positive and negative anodes
Charge and discharge.On long terms, the research and development of sodium-ion battery largely alleviate the battery development of lithium resource anxiety initiation
Limitation problem.Therefore, sodium-ion battery is considered as the next-generation battery for being most hopeful to substitute lithium ion battery.
As sodium-ion battery positive material, Na3V2(PO4)2O2F has open three dimensional NASICON structure, can generate very
It is special that dynamics of sodium ion during electrochemical migration can be improved in order to the fast transferring of sodium ion in big clearance space
Property；And Na3V2(PO4)2O2F also possesses the common feature of polyanionic material, and crystal structure is stablized, and stability of material is good.
However, Na3V2(PO4)2O2F also has the deficiency of all polyanionic material conductivity differences.Carbon coating is to have been found at present
Most effective and simplest one of the method for improving material conductivity.This patent modifies carbon coating layer by phosphorus source of phytic acid, right
Na3V2(PO4)2O2F positive electrode is modified, and for phytic acid as a kind of organic phosphorus sources, it has extremely strong complexing power, can make material
Material combination is closer, improves the structural stability of material.Na can not only be reduced by modifying carbon coating layer as phosphorus source using phytic acid3V2
(PO4)2O2Contact of the F positive electrode with electrolyte, the generation of side reaction, stabilizing material between inhibitory activity substance and electrolyte
Structure, to improve the cyclical stability of material；This phosphorus doping carbon coating layer can also further improve the conductivity of material,
Interface resistance between active material and electrolyte is effectively reduced, improves the deintercalation speed of sodium ion, to reduce active material in height
Polarization under multiplying power can effectively improve Na3V2(PO4)2O2The high rate performance of F.
Summary of the invention
The purpose of the present invention is to provide a kind of carbon-coated Na of phosphorus doping3V2(PO4)2O2F positive electrode (is labeled as
NVPOF/P-C, N, V, P, O, F, P, C respectively represent sodium, vanadium, phosphorus, oxygen, fluorine, phytic acid and carbon).Related NVPOF/P-C anode
Its synthesis material of material is ammonium metavanadate NH4VO3, ammonium dihydrogen phosphate NH4H2PO4, sodium fluoride NaF, sodium carbonate Na2CO3, phytic acid
C6H18O24P6, glucose C6H12O6With ethylene glycol (CH2OH)2。
The ammonium metavanadate, ammonium dihydrogen phosphate, sodium fluoride and sodium carbonate molal weight ratio be 2:2:1:1.
Ammonium metavanadate, sodium carbonate, sodium fluoride and glucose purity used is all larger than 99%, ammonium dihydrogen phosphate and ethylene glycol
Solution purity is all larger than 98%, and plant acid solution concentration is 60-80wt.%, further preferably 70wt.%.
Sodium source used can be sodium fluoride, sodium carbonate；Vanadium source can be ammonium metavanadate, vanadic anhydride；Phosphorus source can be phosphoric acid
Ammonium dihydrogen, diammonium hydrogen phosphate, phosphoric acid；Carbon source can be the carbon containing objects of organic or inorganics such as sucrose, glucose, carbon black, graphite, anthracite
Matter.
Solvent used can be any ratio of ethyl alcohol, ethylene glycol, polyethylene glycol, dimethylformamide and above-mentioned solvent and water
Mixed solution.
It is specific the preparation method comprises the following steps:
By ammonium metavanadate NH4VO3, ammonium dihydrogen phosphate NH4H2PO4, sodium fluoride NaF, sodium carbonate Na2CO3It is dissolved in deionized water
In, it is stirred 10 minutes at 75-80 DEG C, phytic acid and ethylene glycol is added, is transferred in reaction kettle after mixing, in 180-200 DEG C
Lower heat preservation 20-30h；After hydro-thermal process is completed and is cooled down, centrifuge washing is dried to obtain NVPOF forerunner in 80 DEG C of baking ovens
Body；It takes NVPOF presoma to be scattered in alcoholic solution, adds appropriate glucose and be dissolved in above-mentioned solution, heating water bath makes
Vaporized alcohol is placed in baking oven dry；By the mixture after above-mentioned drying in tube furnace under nitrogen atmosphere 500-600 DEG C guarantor
It is 1-2 hours warm, obtain the carbon-coated Na of phosphorus doping3V2(PO4)2O2F positive electrode (is labeled as NVPOF/P-C).By gained
NVPOF/P-C positive electrode stirs into slurry by 80:10:10 mass ratio with acetylene black, Kynoar (PVDF), is coated on aluminium
On foil, by drying, film is rushed and sodium-ion battery positive material pole piece is made in press mold.
Carbon coating can significantly improve Na in technical solution of the present invention3V2(PO4)2O2The electronic conductivity of F positive electrode,
Polarization is reduced, the specific capacity and cyclical stability of material are improved；Phytic acid acts not only as phosphorus source in the present invention, can also make
Carbon coating layer and Na can be improved due to the close coupling ability of it and metal ion for a part of carbon source3V2(PO4)2O2F matrix
Binding force, so as to improve the cycle performance of material, furthermore phosphorus doping can also increase the defects of carbon structure, more conducively conductivity of material
The raising of rate, to further improve the high rate performance of material.Equipment used in the present invention is simple, and process flow is easy to operate,
The carbon-coated Na of the phosphorus doping of preparation3V2(PO4)2O2F positive electrode has good cycle performance and high rate performance.
Detailed description of the invention
The X ray diffracting spectrum that Fig. 1 is sample NVPOF/P-C in sample NVPOF and embodiment 2 in comparative example 1.
Fig. 2 is charging and discharging curve of the sample NVPOF/P-C in 0.5C in embodiment 2.
Specific embodiment:
Below by the description of embodiment and comparative example, the substantive distinguishing features and advantage that the present invention is further explained.To retouch
It states conveniently, comparative example is described first, embodiment is then described again, compares therewith, shows effect of the invention.
Comparative example 1
By 1.1816g ammonium metavanadate NH4VO3, 1.1737g ammonium dihydrogen phosphate NH4H2PO4, 0.2121g sodium fluoride NaF,
0.5326g sodium carbonate Na2CO3It is dissolved in 15ml deionized water, is stirred 10 minutes in 80 DEG C, add 20ml ethylene glycol, after mixing
It is transferred in reaction kettle, is kept the temperature for 24 hours at 180 DEG C；After hydro-thermal process is completed and is cooled down, centrifuge washing, in 80 DEG C of baking ovens
It is dried to obtain NVPOF presoma；Take NVPOF presoma to be scattered in alcoholic solution, add appropriate glucose be dissolved in it is above-mentioned
In solution, after heating water bath makes vaporized alcohol, it is placed in baking oven dry；By the mixture after above-mentioned drying in tube furnace nitrogen
Lower 550 DEG C of atmosphere keep the temperature 1 hour, obtain NVPOF positive electrode.
Embodiment 1
By 1.1816g ammonium metavanadate NH4VO3, 1.1737g ammonium dihydrogen phosphate NH4H2PO4, 0.2121g sodium fluoride NaF,
0.5326g sodium carbonate Na2CO3It is dissolved in 15ml deionized water, is stirred 10 minutes in 80 DEG C, add 1ml phytic acid and 20ml ethylene glycol,
It is transferred in reaction kettle, is kept the temperature for 24 hours at 180 DEG C after mixing；After hydro-thermal process is completed and is cooled down, centrifuge washing,
NVPOF presoma is dried to obtain in 80 DEG C of baking ovens；It takes NVPOF presoma to be scattered in alcoholic solution, adds 15wt.% forerunner
The glucose of weight is dissolved in above-mentioned solution, after heating water bath makes vaporized alcohol, is placed in baking oven dry；By above-mentioned drying
Mixture afterwards in tube furnace under nitrogen atmosphere 550 DEG C keep the temperature 1 hour, obtain NVPOF/P-C positive electrode.
Embodiment 2
By 1.1816g ammonium metavanadate NH4VO3, 1.1737g ammonium dihydrogen phosphate NH4H2PO4, 0.2121g sodium fluoride NaF,
0.5326g sodium carbonate Na2CO3It is dissolved in 15ml deionized water, is stirred 10 minutes in 80 DEG C, add 1ml phytic acid and 20ml ethylene glycol,
It is transferred in reaction kettle, is kept the temperature for 24 hours at 180 DEG C after mixing；After hydro-thermal process is completed and is cooled down, centrifuge washing,
NVPOF presoma is dried to obtain in 80 DEG C of baking ovens；It takes NVPOF presoma to be scattered in alcoholic solution, adds 20wt.% forerunner
The glucose of weight is dissolved in above-mentioned solution, after heating water bath makes vaporized alcohol, is placed in baking oven dry；By above-mentioned drying
Mixture afterwards in tube furnace under nitrogen atmosphere 550 DEG C keep the temperature 1 hour, obtain NVPOF/P-C positive electrode.
Embodiment 3
By 1.1816g ammonium metavanadate NH4VO3, 1.1737g ammonium dihydrogen phosphate NH4H2PO4, 0.2121g sodium fluoride NaF,
0.5326g sodium carbonate Na2CO3It is dissolved in 15ml deionized water, is stirred 10 minutes in 80 DEG C, add 1ml phytic acid and 20ml ethylene glycol,
It is transferred in reaction kettle, is kept the temperature for 24 hours at 180 DEG C after mixing；After hydro-thermal process is completed and is cooled down, centrifuge washing,
NVPOF presoma is dried to obtain in 80 DEG C of baking ovens；It takes NVPOF presoma to be scattered in alcoholic solution, adds 25wt.% forerunner
The glucose of weight is dissolved in above-mentioned solution, after heating water bath makes vaporized alcohol, is placed in baking oven dry；By above-mentioned drying
Mixture afterwards in tube furnace under nitrogen atmosphere 550 DEG C keep the temperature 1 hour, obtain NVPOF/P-C positive electrode.
By NVPOF and NVPOF/P-C positive electrode obtained by comparative example 1 and embodiment 1-3 respectively with acetylene black, polyvinylidene fluoride
Alkene (PVDF) presses 80:10:10 mass ratio, and solvent is that N-Methyl pyrrolidone (NMP) stirs into slurry, is spread evenly across aluminium foil
On, by drying, rush film and sodium-ion battery positive material pole piece is made in press mold.It is to electrode with metallic sodium, GradeGF/D is
Diaphragm, the 1M NaClO containing 2wt.%FEC4/ (EC+DMC+EMC) (EC:DMC:EMC=1:1:1) is that electrolyte is assembled into electricity
Pond, carries out constant current charge-discharge test, and voltage range is 3.0~4.5V.
The capacity and capacity retention ratio of each example of table 1 charge-discharge test at 0.5C.
Claims (3)
1. a kind of prepare phosphorus doping carbon coating Na3V2(PO4)2O2The method of F positive electrode, which comprises the steps of:
(1) ammonium metavanadate, ammonium dihydrogen phosphate, sodium fluoride and sodium carbonate are dissolved in deionized water；
(2) phytic acid, ethylene glycol are added in the above solution, heats up, stir evenly；
(3) mixed solution obtained by (2) is transferred in reaction kettle, carries out hydro-thermal process；
(4) after step (3) hydro-thermal process is completed and cooled down, centrifuge washing is dried to obtain NVPOF forerunner in 80 DEG C of baking ovens
Body；
(5) it takes NVPOF presoma to be scattered in alcoholic solution, adds glucose and be dissolved in above-mentioned solution, heating water bath
It is dry in baking oven after making vaporized alcohol, obtain mixture；
(6) mixture after above-mentioned drying is sintered in tube furnace, obtains the carbon-coated Na of phosphorus doping3V2(PO4)2O2F
Positive electrode.
2. according to claim 1 prepare phosphorus doping carbon coating Na3V2(PO4)2O2The method of F positive electrode, feature exist
In: the sintering process of step (6) carries out in nitrogen or argon atmosphere.
3. according to claim 1 prepare phosphorus doping carbon coating Na3V2(PO4)2O2The method of F positive electrode, feature exist
In: step (2) is stirred 60 ~ 90 minutes at 75-80 DEG C；Step (3) is that heat preservation 20-30 is small at 180 ~ 200 DEG C
When；Step (6) is sintered 1 ~ 2 hour at 500 ~ 600 DEG C.
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| CN110518238B (en) * | 2019-08-27 | 2022-04-26 | 江苏大学 | Synthesis of sodium ion battery anode material Na based on organic phosphonic acid3V2(PO4)3Nitrogen-doped carbon and preparation method thereof |
| CN113224307A (en) * | 2021-05-11 | 2021-08-06 | 陈双强 | Preparation method of high-capacity high-magnification high-voltage sodium vanadium fluorophosphate doped material |
| CN113921795B (en) * | 2021-10-11 | 2023-08-22 | 广东工业大学 | Sodium ion battery positive electrode material, preparation method thereof and sodium ion battery |
| CN114639829A (en) * | 2022-03-01 | 2022-06-17 | 太原理工大学 | Metal-doped polyanion compound positive electrode material and preparation method thereof |
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| CN106328911A (en) * | 2016-11-30 | 2017-01-11 | 合肥工业大学 | Material with mixture of ions with sodium vanadium phosphate cathode material coated by carbon and preparing method thereof |
| CN106374104A (en) * | 2016-10-10 | 2017-02-01 | 济南大学 | Method for preparing sodium fluorine vanadium phosphate material in air atmosphere |
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| CN102509789A (en) * | 2011-10-17 | 2012-06-20 | 中南大学 | Method for preparing positive material fluorine-doped sodium vanadium phosphate of sodium-containing lithium ion battery |
| CN104733731B (en) * | 2015-03-25 | 2017-03-08 | 天津大学 | The method preparing uniform carbon coating vanadium phosphate sodium material |
| CN105932284B (en) * | 2016-07-13 | 2019-01-22 | 盐城工学院 | A kind of close cladded type composite material and preparation method of mesoporous carbon and application |
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| CN106374104A (en) * | 2016-10-10 | 2017-02-01 | 济南大学 | Method for preparing sodium fluorine vanadium phosphate material in air atmosphere |
| CN106328911A (en) * | 2016-11-30 | 2017-01-11 | 合肥工业大学 | Material with mixture of ions with sodium vanadium phosphate cathode material coated by carbon and preparing method thereof |
| CN107359340A (en) * | 2017-07-19 | 2017-11-17 | 广东迈纳科技有限公司 | A kind of preparation method of the compound micron ball of fluorophosphoric acid vanadyl sodium of three-dimensional grapheme network skeleton support |
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