CN108539133A - Li3V2（PO4）3The preparation method of nanocrystalline/conducting polymer anode material for lithium-ion batteries - Google Patents
Li3V2（PO4）3The preparation method of nanocrystalline/conducting polymer anode material for lithium-ion batteries Download PDFInfo
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- CN108539133A CN108539133A CN201810156714.XA CN201810156714A CN108539133A CN 108539133 A CN108539133 A CN 108539133A CN 201810156714 A CN201810156714 A CN 201810156714A CN 108539133 A CN108539133 A CN 108539133A
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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
- H01M4/366—Composites as layered products
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01M10/052—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
- 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
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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 Li3V2(PO4)3The preparation method of the carbon-free anode material for lithium-ion batteries of nanocrystalline/conducting polymer (being abbreviated as LVP/CP), using phosphoric acid vanadium lithium and conducting polymer as main raw material(s), it is prepared for that phosphoric acid vanadium lithium is nanocrystalline using hydro-thermal method is improved, phosphoric acid vanadium lithium crystal grain nano effect is that the excellent anode material for lithium-ion batteries of processability is laid a good foundation；And microwave radiation technology hydro-thermal method is used, the self assembly Li of nucleocapsid3V2(PO4)3/ conductive polymer nanometer composite material, efficient, controllability is good, and the conducting polymer clad of gained provides Quick conductive network channel, makes Li3V2(PO4)3The chemical property of/conducting polymer combination electrode material significantly improves, which, which is assembled into battery, has excellent high rate performance and cyclical stability, and a kind of possibility is provided to prepare high-performance lithium ion battery cathode material.
Description
Technical field
The present invention relates to electrode material preparation fields, and in particular to a kind of Li3V2(PO4)3Nanocrystalline/conducting polymer lithium
The preparation method of ion battery positive electrode.
Background technology
Lithium ion battery (HEV) and electric vehicle (EVs) from small portable electronic device to mixed power electric car
Equal fields extensive use.Since the energy density of lithium ion battery is mainly determined by intercalation synthesis anode, have high theoretical
The positive electrode of capacity, high working voltage and low cost causes the great interest of researchers.In the positive material studied at present
In material, NASICON type monocrystalline Li3V2(PO4)3Due to theoretical capacity height, Environmental security and low cost, become the electricity of most foreground
One of pole material.Wherein, under 3.0~4.8V high working voltages, monocrystalline Li3V2(PO4)3In three lithium ions can all take off
Go out, theoretical capacity reaches 197mAh g-1.But lower electronic conductivity (about 2.4 × 10-7S cm-1) and lower lithium ion
Diffusion coefficient (10-10~10-9cm2s-1) lead to pure Li3V2(PO4)3Electrode capacitance amount is relatively low, practical is answered to limit its
With.To solve this defect, it is necessary to try to improve lithium ion and electronics shelves conductivity, be modified to material.Up to the present,
It can there are many methods come more than overcoming the problems, such as.Li3V2(PO4)3Internal lithium ion diffusion rate is mainly by crystal space structure
It is determined with crystallite dimension, synthesizing nanocrystalline grain regulates and controls ion diffusion path and diffusion interface, to effectively improve ion
Diffusion rate；It can also be by adulterating other ions (such as Mg2+, Fe3+, Nd3+, Na+Deng) continuous conductive path is formed on the electrode
Diameter, it is appropriate to improve in electrode in low conductivity.In addition, another feasible method for improving battery performance of surface cladding, passes through table
Face chemical modification provides being in direct contact between protective layer reduction active material and electrolyte, while improving electrode surface conductance
Rate.Wherein, conductive carbon coating layer can be used as Li3V2(PO4)3With the separation layer of electrolyte, while Li is overcome3V2(PO4)3Low
Surface conductivity.But the irregular carbon particle poor connectivity of carbon coating layer, leads to low electron-transport and capacitance loss.Conducting polymer
Object has excellent electric conductivity and electrochemical doping characteristic, can be used as conductive adhesive, surface functional material and electrode material, because
And have a wide range of applications in electrochemical energy storage field.Recently, conducting polymer is used as covering to improve electrode table
The electronic conductivity and electrochemistry in face.Health et al. effectively improves according to the report, can be coated by PEDOT under mild cryogenic conditions
Li3V2(PO4)3Battery performance is realized without carbon electrode material.Oxidation polymerization is obtained clad and is held with higher-wattage using electrode
Amount and excellent cyclical stability.However, Li in the synthesis process3V2(PO4)3Aoxidizing surface portion of the vanadium ion in particle
De- lithium, it is difficult to control Li3-xV2(PO4)3Composition.Therefore, a kind of simple and effective synthesis PEDOT of exploitation coats Li3V2(PO4)3At
To prepare the developing direction of excellent high rate performance and stable circulation positive electrode.
Invention content
To solve the above problems, the present invention provides a kind of Li3V2(PO4)3Nanocrystalline/conducting polymer compound lithium ion
The preparation method of cell positive material：By microwave heating assisting sol-gel method, the self assembly Li of nucleocapsid3V2
(PO4)3/ conductive polymer nanometer composite material.Method is easy to operate, gained positive electrode have good electronics and ion transmission,
Stable circulation and good chemical property can effectively promote lithium ion battery comprehensive performance, be suitble to energy industry industry metaplasia
The demand of production.
To achieve the above object, the technical solution that the present invention takes is：
Li3V2(PO4)3The preparation method of nanocrystalline/conducting polymer PEDOT anode material for lithium-ion batteries, including it is following
Step：
S1, appropriate CH is weighed by the stoichiometry formula of the ratio between amount of substance 3: 2: 3: 13COOLi·2H2O, NH4VO3、
NH4H2PO4And citric acid, the CH that will be weighed3COOLi·2H2O, NH4VO3、NH4H2PO4It is add to deionized water, it is fully molten
It solves, the aqueous citric acid solution that the mass concentration prepared is 27% is then added to above-mentioned by magnetic agitation after 30 minutes at room temperature
In solution, continuously stirs 2 hours, obtain mixture；
S2,70~80 DEG C will be warming up in the mixture half an hour of gained, remove extra water until forming gel；Then
180 DEG C of hydro-thermal reactions 24 hours in an oven, grind after taking-up, in nitrogen atmosphere 350 DEG C of microwave heating kept for 20 minutes, finally
It is roasted in 750 DEG C of nitrogen atmosphere under 6h and obtains pure Li3V2(PO4)3；
S3, CP monomers/Li is pressed3V2(PO4)3The mass percent of=5-20% weighs appropriate CP monomers, is added to 0.1M's
In HCl solution, it is sufficiently stirred under the conditions of ice-water bath 30 minutes, then add Li3V2(PO4)3Powder, sonic oscillation 10 minutes, makes
Li3V2(PO4)3After being uniformly dispersed, a concentration of 30% APS aqueous solutions are added dropwise, are dripped in 30~60 minutes, it is mono- by APS: CP
The proportioning of body (molar ratio)=1: 1.05 regulates and controls APS additions；After APS solution drips, continue stirring 10 hours, obtains powder production
Object；
S4, the powdered product of above-mentioned gained is filtered, with deionized water and absolute ethyl alcohol, repeatedly washing to filtrate is neutrality,
60 DEG C are dried in vacuo 24 hours to get Li3V2(PO4)3Nanocrystalline/conductive polymer composite.
The present invention is using phosphoric acid vanadium lithium and conducting polymer as main raw material(s), using microwave heating assisting sol-gel method
It is prepared for anode material for compound lithium ion battery, is had the following advantages that：
1, Li is prepared for using microwave heating assisting sol-gel method3V2(PO4)3It is nanocrystalline, Li3V2(PO4)3Crystal grain nanometer
Effect is that the excellent anode material for lithium-ion batteries of processability is laid a good foundation.
2, conducting polymer is coated using the method for in-situ polymerization self assembly, and efficient, controllability is good.
3, conducting polymer clad provides Quick conductive network channel, makes Li3V2(PO4)3/ conductive polymer electrodes material
There is material excellent high rate performance and cyclical stability, 10C charge-discharge cycles 500 times still to retain 87% capacitance.It is high to prepare
The anode material for lithium-ion batteries of ratio stable circulation provides a kind of possibility.
Description of the drawings
Fig. 1 is LVP/CP preparation flow figures.
The SEM photograph (a) and TEM photos (b) that Fig. 2 is LVP/CP
Fig. 3 is the multiplying power and stable circulation performance of LVP/CP anode lithium ion batteries.
Specific implementation mode
In order to make objects and advantages of the present invention be more clearly understood, the present invention is carried out with reference to embodiments further
It is described in detail.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to limit this hair
It is bright.
Embodiment
S1,5gCH is taken3COOLi·2H2O, 4.6g NH4VO3, 6.8g NH4H2PO4It is added in deionized water, at room temperature magnetic
After power stirs abundant dissolving in 30 minutes；3.8g citric acids are dissolved in 14ml deionized waters, are then added in above-mentioned solution, are continued
Stirring 2 hours.
S2,80 DEG C will be warming up in the mixture half an hour obtained by previous step, remove extra moisture content until forming brown
Gel；Then the gel is poured into closed in the hydrothermal reaction kettle of polytetrafluoroethylliner liner, 180 DEG C of hydro-thermal reactions 24 in an oven
Hour, mortar grinder after taking-up.It placing into ceramic crucible, 350 DEG C of microwave heating holding 20 minutes, takes out in nitrogen atmosphere,
Natural cooling.Finally 750 DEG C of roasting 6h obtain pure Li in nitrogen atmosphere tube furnace3V2(PO4)3；
S3,0.8gCP monomers are added in the HCl solution of 0.1M, are sufficiently stirred 30 minutes, make under the conditions of ice-water bath
CP monomers protonate, then add 8g Li3V2(PO4)3Powder, sonic oscillation 10 minutes, makes Li3V2(PO4)3It is uniformly dispersed.It weighs
2.05g APS are made into 30% aqueous solution, are added drop-wise in reaction solution, are dripped in 30 minutes.After APS solution drips, ice
Continue stirring 10 hours under water bath condition, obtains powdered product；
S4, the powdered product of above-mentioned gained is filtered, with deionized water and absolute ethyl alcohol, repeatedly washing to filtrate is neutrality,
60 DEG C of dryings 24 hours are to get Li in vacuum drying chamber3V2(PO4)3Nanocrystalline/conductive polymer composite.
S5, the storage lithium performance that obtained electrode material is assembled into CR2032 button cell Electrode materials.LVP/CP
Positive electrode, carbon black, Kynoar are uniformly mixed by 85: 10: 5 mass ratioes, on the aluminium flake coated in 1mm thickness, 1i0 DEG C of vacuum
It is cut after 6 hours dry and positive plate is made.Metal lithium sheet is as cathode, and Celgard2400 polypropylene is as diaphragm, LiPF6It is molten
In (1: 1) EC: DMC 1M mixed solutions as electrolyte.Each component is finally assembled into CR2032 button electricity in glove box
Pond.
S5, the microscopic appearance of SEM and tem observation product are utilized；Utilize Land loop tests instrument and CHI600A electrochemistry works
Make station to carry out, tests specific capacity, cyclical stability and the chemical property of lithium ion battery.Gained positive electrode is 200nm rulers
Very little hud typed LVP/CP composite materials, compared with Li3V2 (PO4) 3, high conductivity that LVP nano grain surfaces uniformly coat
The CP layers of significant chemical property for improving electrode.Obtained LVP/CP composite materials are initial under the conditions of 0.1C (3.0-4.3V)
Discharge capacity is 132.7mAhg-1.When with 10C rate charge-discharges, initial capacity can reach 103.5mAhg-1, 500 cycles
Capacity retention ratio is 87.3% afterwards, it is seen that it is with excellent high rate performance and cyclical stability.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the principle of the present invention, it can also make several improvements and retouch, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (1)
1.Li3V2(PO4)3The preparation method of nanocrystalline/conducting polymer anode material for lithium-ion batteries, which is characterized in that including
Following steps：
S1, appropriate CH is weighed by the stoichiometry formula of the ratio between amount of substance 3: 2: 3: 13COOLi·2H2O, NH4VO3、NH4H2PO4With
Citric acid, the CH that will be weighed3COOLi·2H2O, NH4VO3、NH4H2PO4It is add to deionized water, fully dissolves, at room temperature magnetic
After power stirs 30 minutes, then the aqueous citric acid solution that the mass concentration prepared is 27% is added in above-mentioned solution, continuously
Stirring 2 hours, obtains mixture；
S2,70~80 DEG C will be warming up in the mixture half an hour of gained, remove extra water until forming gel；Then it is drying
180 DEG C of hydro-thermal reactions 24 hours, grind after taking-up in case, in nitrogen atmosphere 350 DEG C of microwave heating kept for 20 minutes, last 750
In DEG C nitrogen atmosphere pure Li is obtained under roasting 6h3V2(PO4)3；
S3, CP monomers/Li is pressed3V2(PO4)3The mass percent of=5-20% weighs appropriate CP monomers, and the HCl for being added to 0.1M is molten
In liquid, it is sufficiently stirred under the conditions of ice-water bath 30 minutes, then add Li3V2(PO4)3Powder, sonic oscillation 10 minutes, makes Li3V2
(PO4)3After being uniformly dispersed, a concentration of 30% APS aqueous solutions are added dropwise, drips in 30~60 minutes, (rubs by APS: CP monomer
Your ratio)=1: 1.05 proportioning regulates and controls APS additions；After APS solution drips, continues stirring 10 hours, obtain powdered product；
S4, the powdered product of above-mentioned gained is filtered, it is neutral repeatedly to be washed to filtrate with deionized water and absolute ethyl alcohol, 60 DEG C
24 hours are dried in vacuo to get Li3V2(PO4)3Nanocrystalline/conductive polymer composite.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110224134A (en) * | 2019-07-24 | 2019-09-10 | 卢昌琴 | A kind of anode material for lithium-ion batteries and preparation method thereof |
| CN110364718A (en) * | 2019-07-24 | 2019-10-22 | 卢昌琴 | A kind of positive electrode and preparation method thereof with three-dimensional conductive structure for lithium ion battery |
| CN110676450A (en) * | 2019-10-16 | 2020-01-10 | 南昌工程学院 | Secondary battery anode material and battery thereof |
| CN112002902A (en) * | 2020-08-12 | 2020-11-27 | 中南大学 | Dual-modified ternary positive electrode material of lithium ion battery and preparation method of dual-modified ternary positive electrode material |
| CN112186163A (en) * | 2020-10-09 | 2021-01-05 | 西安交通大学 | Lithium vanadium fluorophosphate lithium-ion battery positive electrode material and synthesis method thereof |
| CN115954468A (en) * | 2023-03-15 | 2023-04-11 | 江苏蓝固新能源科技有限公司 | Cathode material, preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110224134A (en) * | 2019-07-24 | 2019-09-10 | 卢昌琴 | A kind of anode material for lithium-ion batteries and preparation method thereof |
| CN110364718A (en) * | 2019-07-24 | 2019-10-22 | 卢昌琴 | A kind of positive electrode and preparation method thereof with three-dimensional conductive structure for lithium ion battery |
| CN110676450A (en) * | 2019-10-16 | 2020-01-10 | 南昌工程学院 | Secondary battery anode material and battery thereof |
| CN112002902A (en) * | 2020-08-12 | 2020-11-27 | 中南大学 | Dual-modified ternary positive electrode material of lithium ion battery and preparation method of dual-modified ternary positive electrode material |
| CN112186163A (en) * | 2020-10-09 | 2021-01-05 | 西安交通大学 | Lithium vanadium fluorophosphate lithium-ion battery positive electrode material and synthesis method thereof |
| CN112186163B (en) * | 2020-10-09 | 2021-12-28 | 西安交通大学 | Lithium vanadium fluorophosphate lithium-ion battery positive electrode material and synthesis method thereof |
| CN115954468A (en) * | 2023-03-15 | 2023-04-11 | 江苏蓝固新能源科技有限公司 | Cathode material, preparation method and application thereof |
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Application publication date: 20180914 |