CN106450223A - Fluorine-doped and carbon-coated lithium iron phosphate and preparation and application thereof - Google Patents
Fluorine-doped and carbon-coated lithium iron phosphate and preparation and application thereof Download PDFInfo
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- CN106450223A CN106450223A CN201611020407.6A CN201611020407A CN106450223A CN 106450223 A CN106450223 A CN 106450223A CN 201611020407 A CN201611020407 A CN 201611020407A CN 106450223 A CN106450223 A CN 106450223A
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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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
- H01M4/621—Binders
- H01M4/622—Binders being polymers
- H01M4/623—Binders being polymers fluorinated polymers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides fluorine-doped and carbon-coated lithium iron phosphate, a preparation preparation and application of the fluorine-doped and carbon-coated lithium iron phosphate as a lithium ion battery anode material, and the preparation method comprises the following steps that (1) pure phase lithium iron phosphate is obtained; (2) the pure phase lithium iron phosphate and a fluorine-containing organic matter are mixed, ground for several hours and dried, and a mixture is obtained; (3) the mixture is calcined under the atmosphere of protective gas, a fluorine-doped and carbon-coated lithium iron phosphate material is obtained after cooling, different from villiaumite doping for conventional fluorine doping, F-C in the fluorine-containing organic matter is used for fluorine doping and carbon coating which are performed by one step, the performance of the modified material is improved remarkably, and the specific discharge capacity can reach 150 mAh/g; (2) the preparation method is simple, the grain diameter of the spherical lithium iron phosphate obtained with a solvothermal method is about 40-50 nm, and the surface of the lithium iron phosphate is uniformly coated with one layer of F-containing organic matter.
Description
Technical field
The present invention relates to a kind of carbon-coated LiFePO 4 for lithium ion batteries of Fluorin doped and its preparation method and application, category energy storage material and electricity
Technical field of chemistry.
Background technology
Used as most promising anode material for lithium-ion batteries, LiFePO4 has lot of advantages：Cheap, theoretical appearance
Amount is high, have extended cycle life, cycle performance is excellent, the structure thermal stability during lithium ion deintercalation is good etc., is most to be hopeful to answer
High-power lithium ion battery positive electrode for high-power electric appliance and hybrid vehicle.But the limit due to crystal structure itself
System, the electronic conductivity of pure phase LiFePO4 and lithium ion diffusion rate are very low, cause the not high and high magnification of its actual specific capacity
Poor performance, significantly limit large-scale application of the electrode material in electrokinetic cell field.
So far, people have done numerous studies work at the aspect such as LiFePO 4 material nanorize, cladding and doping vario-property
Make, good achievement is achieved, LiFePO 4 material has gradually moved towards practical application.But from the point of view of actual service condition,
LiFePO 4 material and its battery performance still need and are continuously improved and are improved, to meet need of the market to LiFePO4
Ask.
Content of the invention
The shortcoming of prior art in view of the above, it is an object of the invention to provide a kind of carbon coating is uniform, structure is steady
High carbon-coated nano-grade lithium iron phosphate of Fluorin doped of fixed, good conductivity, specific capacity and its preparation method and application.
For achieving the above object, technical solution of the present invention is as follows：
A kind of preparation method of the carbon-coated LiFePO 4 for lithium ion batteries of Fluorin doped, comprises the steps：
(1) pure phase LiFePO4 is obtained；
(2) pure phase LiFePO4 is mixed with organic fluorocompound, a few hours post-drying is ground, obtain mixture；
(3) mixture is calcined under protective gas atmosphere, after cooling, obtains final product the carbon-coated nano iron phosphate of Fluorin doped
Lithium material.
It is preferred that, in step (1), pure phase LiFePO4 is using coprecipitation, hydro-thermal method, solvent-thermal method or colloidal sol
Prepared by gel method.
It is preferred that, in step (2) organic fluorocompound be Kynoar (PVDF), politef (PTFE),
The copolymer (PFA) of fluorinated ethylene propylene copolymer (FEP), perfluoro propyl perfluoroalkyl vinyl ether and politef, ethylene-four
The mixture of one or more in fluoride copolymers (ETFE).
It is preferred that, in step (2), LiFePO4 is 10 with the mass ratio of organic fluorocompound:(0.5～4).
It is preferred that, when organic fluorocompound is solid in step (2), add organic solvent to make during mixing fluorine-containing organic
Thing fully dissolves, and described organic solvent is N-Methyl pyrrolidone (NMP), dimethyl phthalate (DMP), dimethyl sulfoxide
(DMSO), dimethyl fumarate (DMF) one kind therein.
It is preferred that, in step (2), milling time is 1～4 hour.
It is preferred that, in step (3), protective gas is nitrogen, argon, helium or neon one kind therein.
It is preferred that, in step (3), calcining heat is 600～900 DEG C, and calcination time is 3～5h.
For achieving the above object, the present invention also provides a kind of fluorine for obtaining according to any one preparation method above-mentioned and mixes
Miscellaneous carbon-coated LiFePO 4 for lithium ion batteries.
For achieving the above object, the present invention also provide a kind of carbon-coated LiFePO 4 for lithium ion batteries of above-mentioned Fluorin doped as lithium from
The application of sub- cell positive material.
The present invention has the effect that：
(1) different with villiaumite doping from conventional Fluorin doped, the present invention is with the F-C in organic fluorocompound, LiFePO4 to be entered
Row Fluorin doped carbon coating, fluorine doped and one step of bag carbon are carried out, and the material property after modification is significantly improved, specific discharge capacity
Up to 150mAh/g；
(2) preparation method is simple, and the particle diameter of obtained spherical LiFePO 4 is about 40～50nm, its coated with uniform
There is one layer of Organic substance containing F.
Description of the drawings
Fig. 1 is the XRD spectrum of pure phase LiFePO4 in the embodiment of the present invention 1.
Fig. 2 is the SEM figure of pure phase LiFePO4 in the embodiment of the present invention 1.
Fig. 3 is the XRD spectrum of the carbon-coated LiFePO 4 for lithium ion batteries of Fluorin doped obtained in the embodiment of the present invention 1.
Fig. 4 is schemed for the SEM of the carbon-coated LiFePO 4 for lithium ion batteries of Fluorin doped obtained in the embodiment of the present invention 1.
Fig. 5 is schemed for the XPS of the carbon-coated LiFePO 4 for lithium ion batteries of Fluorin doped obtained in the embodiment of the present invention 1.
Fig. 6 is the charging and discharging curve of the carbon-coated LiFePO 4 for lithium ion batteries of Fluorin doped obtained in the embodiment of the present invention 1.
Fig. 7 is the charging and discharging curve of pure phase LiFePO4 obtained in the embodiment of the present invention 1.
Fig. 8 is the CV curve of the carbon-coated LiFePO 4 for lithium ion batteries of Fluorin doped obtained in the embodiment of the present invention 2.
Fig. 9 is the multiplying power property curve of the carbon-coated LiFePO 4 for lithium ion batteries of Fluorin doped obtained in the embodiment of the present invention 3.
Specific embodiment
Below by way of specific instantiation, embodiments of the present invention are described, those skilled in the art can be by this specification
Disclosed content understands other advantages of the present invention and effect easily.The present invention can also pass through in addition different concrete realities
The mode of applying is carried out or applies, and the every details in this specification can also be based on different viewpoints and application, without departing from
Various modifications and changes are carried out under the spirit of the present invention.
Embodiment 1
(1) nanoscale pure phase LiFePO4 is prepared using solvent-thermal method
A. Lithium hydroxide monohydrate (LiOH H is measured2O) 0.015mol, phosphoric acid (H3PO4) 0.005mol, ferrous sulfate heptahydrate
(FeSO4·7H2O) 0.005mol, ethylene glycol 40mL and ascorbic acid 0.0016mol；
B. Lithium hydroxide monohydrate is added in the mixed solution of phosphoric acid and ethylene glycol, after stirring 30min, adds Vitamin C
Acid and ferrous sulfate heptahydrate, are stirred for 30min, are subsequently poured in reactor；
C. reactor being put in baking oven, 10h is heated at 150 DEG C；
D. sample is taken out, room temperature is naturally cooled to, be subsequently poured into 9000r/min centrifugation 10min in test tube；
E. the upper solution in test tube is outwelled, with ethanol solution and deionized water cleaning sample (each 3 times) in turn, is centrifuged
Till upper solution is limpid, 60 DEG C of drying in vacuum drying oven is then placed in, obtains nanoscale pure phase iron phosphate powder；
LiFePO4 will be obtained carries out X-ray diffraction (XRD) component analyses, and is entered by scanning electron microscope (SEM)
Row observation, as can be seen from Figure 1, the XRD spectrum of pure phase LiFePO4 and standard diagram (JCPDS PDF 40-1499) basic
Cause, and without obvious miscellaneous peak, illustrate that proportioning is suitable, reaction is complete, and impurity is less, and main component is olivine-type crystal structure
LiFePO 4 material.As can be seen from Figure 2, LiFePO 4 material outward appearance is in uniformly spherical, and its grain diameter is 30-40nm；
(2) in molar ratio 10:0.5 takes above-mentioned nanoscale pure phase LiFePO4 and Kynoar (PVDF) is put into mortar
In, appropriate NMP mixing is subsequently adding, after grinding 1h, is put in vacuum drying oven and dries, obtain mixture；
(3) mixture being put in tube furnace, 3h is calcined in 600 DEG C under the atmosphere of nitrogen, obtain final product Fluorin doped after cooling
Carbon-coated nano level LiFePO4.
The carbon-coated nano level LiFePO4 sample of Fluorin doped obtained above is carried out X-ray diffraction (XRD) component divide
Analysis and X-ray photoelectron spectroscopic analysis, and observed by scanning electron microscope (SEM), its interpretation of result is as follows：
A.XRD component analyses there are not noise spike as shown in figure 3, sample is more conform with standard diagram, and image stabilization is in baseline
Near, after high-temperature process, degree of crystallinity improves a lot；
B.SEM photo is as shown in figure 4, the shape of sample particle remains as spherical, uniformity and pure phase phosphoric acid shown in Fig. 2
Ferrum lithium is basically identical, and grain diameter is 40-50nm, compared to the particle diameter of the pure phase LiFePO4 without carbon coating shown in Fig. 2
Increase；
C.XPS collection of illustrative plates is as shown in figure 5, in figure 285.6eV corresponds to C1s, 683.2eV pair in upper right corner illustration (enlarged drawing)
Should be in F1sTrack, shows the presence of fluorine element and carbon in sample.We can see that from master map in sample containing O, Fe,
The elements such as C, F, P, correspond respectively to LiFePO4Each element in@C/F, shows that the sample for preparing is LiFePO4@C/F, and no miscellaneous
Matter.
Using the carbon-coated nano level LiFePO4 of Fluorin doped manufactured in the present embodiment as positive active material, conductive black
(SP) it is conductive agent, Kynoar (PVDF) is binding agent, by positive active material：Conductive agent：The mass ratio 80 of binding agent:
10:10 mixing add appropriate NMP to be coated on aluminium foil after grinding two hours in mortar, then 120 DEG C of bakings in an oven
4h, the tabletting punching after roll squeezer upper roller is pressed through by dried smear, being assembled into battery carries out electrochemical property test.Fig. 6
The charging and discharging curve of Fluorin doped carbon-coated LiFePO 4 for lithium ion batteries and pure phase LiFePO4 under 0.5C multiplying power is respectively with shown in Fig. 7,
It can be seen that first three under 0.5C multiplying power cycle charge-discharge specific capacity of pure phase ferric phosphate lithium cell is respectively
142.5mAh/g, 141.7mAh/g, 141.4mAh/g and 127.3mAh/g, 127.7mAh/g, 126.8mAh/g, efficiency for charge-discharge
Respectively 89.33%, 90.12%, 89.67%, show that the charge/discharge capacity of pure phase ferric phosphate lithium cell is low, this be due to pure
The electronic conductivity of phase lithium iron phosphate and lithium ion diffusion rate be relatively low to be caused.Three circulations of Fluorin doped carbon-coated LiFePO 4 for lithium ion batteries
Charging and discharging capacity be respectively 153.2mAh/g, 154.6mAh/g, 155.4mAh/g and 141.2mAh/g, 142.5mAh/g,
141.0mAh/g, efficiency for charge-discharge is respectively 92.17%, 92.17%, 90.73%.Compared to pure phase LiFePO4, Fluorin doped
Carbon-coated LiFePO 4 for lithium ion batteries (LiFePO4@C/F) charging and discharging curve capacity is higher, and repeatability is more preferable, while also more stable.
Embodiment 2
(1) nanoscale pure phase LiFePO4 is prepared using hydro-thermal method
A. lithium chloride (0.015mol, phosphoric acid 0.005mol, ferrous chloride 0.005mol, deionized water 40mL and anti-are measured
Bad hematic acid 0.0016mol)；
B. lithium chloride is added in the solution of phosphoric acid and deionized water, after stirring 30min, adds ascorbic acid and chlorination
Ferrous iron, is stirred for 30min, is subsequently poured in reactor；
C. reactor being put in baking oven, 5h is heated at 180 DEG C；
D. sample is taken out, room temperature is naturally cooled to, be subsequently poured into 8000r/min centrifugation 20min in test tube；
E. the upper solution in test tube is outwelled, with ethanol solution and deionized water cleaning sample (each 3 times) in turn, is centrifuged
Till upper solution is limpid, 60 DEG C of drying in vacuum drying oven is then placed in, obtains nanoscale pure phase iron phosphate powder；
(2) in mass ratio 10:4 take nanoscale pure phase LiFePO4 and politef (PTFE) is put in mortar, then
After the appropriate DMSO mixing of addition, grinding 4h, it is put in vacuum drying oven and dries, obtain mixture；
(3) mixture being put in tube furnace, 5h is calcined in 900 DEG C under the atmosphere of helium, obtain final product Fluorin doped after cooling
Carbon-coated nano level LiFePO4.
Using the carbon-coated nano level LiFePO4 of Fluorin doped manufactured in the present embodiment as positive active material, conductive black
(SP) it is conductive agent, Kynoar (PVDF) is binding agent, by positive active material：Conductive agent：The mass ratio 80 of binding agent:
10:10 mixing, being assembled into battery carries out electrochemical property test.
Fig. 8 is the CV curve of the carbon-coated LiFePO 4 for lithium ion batteries of Fluorin doped obtained in the embodiment of the present invention 2.Upper left side oxygen in Fig. 8
The peak current density for changing peak is about 1.37A/g, and the peak current density of lower right reduction peak is about -2.08A/g, and figure is basic
Symmetrically.LiFePO4The redox peaks of@C/F are obvious, and peak current is with respect to pure phase LiFePO4Increased, show Fluorin doped carbon
Cladding can improve the diffusion rate of lithium ion.And LiFePO4The oxidoreduction peak position of@C/F is for pure phase LiFePO4Also have
It is obviously reduced, shows that doping can reduce polarization, improve the electrochemical reversibility of material.
Embodiment 3
(1) nanoscale pure phase LiFePO4 is prepared using coprecipitation
A. lithium chloride 0.03mol, phosphoric acid 0.01mol, ferrous chloride 0.01mol, glycerol 60mL and ascorbic acid are measured
0.0032mol；
B. ferrous chloride and ascorbic acid is added in the mixed solution of phosphoric acid and glycerol (30ml), 30min is stirred,
As solution a, lithium chloride is added in the ethylene glycol solution of 30ml, as solution b；
C. with peristaltic pump, solution a, b are mixed, after 1h, reacts complete；
D. sample is poured into 8000r/min in test tube and is centrifuged 20min；
E. the upper solution in test tube is outwelled, with ethanol solution and deionized water cleaning sample (each 3 times) in turn, is centrifuged
Till upper solution is limpid, 60 DEG C of drying in vacuum drying oven is then placed in, obtains nanoscale pure phase iron phosphate powder；
(2) in mass ratio 10:2 take nanoscale pure phase LiFePO4 and fluorinated ethylene propylene copolymer (FEP) is put into mortar
In, appropriate DMF mixing is subsequently adding, after grinding 3h, is put in vacuum drying oven and dries, obtain mixture；
(3) mixture being put in tube furnace, 4h is calcined in 800 DEG C under the atmosphere of argon, obtain final product Fluorin doped after cooling
Carbon-coated nano level LiFePO4.
Using the carbon-coated nano level LiFePO4 of Fluorin doped manufactured in the present embodiment as positive active material, conductive black
(SP) it is conductive agent, Kynoar (PVDF) is binding agent, by positive active material：Conductive agent：The mass ratio 80 of binding agent:
10:10 mixing, being assembled into battery carries out electrochemical property test.
Fig. 9 is the multiplying power property curve of the carbon-coated LiFePO 4 for lithium ion batteries of Fluorin doped obtained in the embodiment of the present invention 3.As a result show
LiFePO4Discharge capacity of/C the battery in 0.1C, 0.5C, 1C, 2C respectively 147,142.5,130,126.1mAh/g, 1C is put
It is the 85.78% of 0.1C that capacitance is 88.46%, the 2C discharge capacity of 0.1C, shows after Fluorin doped carbon coating,
LiFePO4Multiplying power property be obviously improved.
Above-described embodiment only principle of the illustrative present invention and its effect, not for the restriction present invention.Any ripe
The personage for knowing this technology all can carry out modifications and changes without prejudice under the spirit and the scope of the present invention to above-described embodiment.Cause
This, all those of ordinary skill in the art are completed under without departing from disclosed spirit and technological thought
All equivalent modifications or change, must be covered by the claim of the present invention.
Claims (10)
1. a kind of preparation method of the carbon-coated LiFePO 4 for lithium ion batteries of Fluorin doped, it is characterised in that comprise the steps：
(1) pure phase LiFePO4 is obtained；
(2) pure phase LiFePO4 is mixed with organic fluorocompound, a few hours post-drying is ground, obtain mixture；
(3) mixture is calcined under protective gas atmosphere, after cooling, obtains final product the carbon-coated nano-grade lithium iron phosphate material of Fluorin doped
Material.
2. the preparation method of the carbon-coated LiFePO 4 for lithium ion batteries of Fluorin doped according to claim 1, it is characterised in that：Step (1)
Middle pure phase LiFePO4 is prepared using coprecipitation, hydro-thermal method, solvent-thermal method or sol-gal process.
3. the preparation method of the carbon-coated LiFePO 4 for lithium ion batteries of Fluorin doped according to claim 1, it is characterised in that：Step (2)
Middle organic fluorocompound is Kynoar (PVDF), politef (PTFE), fluorinated ethylene propylene copolymer (FEP), perfluor
One kind in the copolymer (PFA) of propyl group perfluoroalkyl vinyl ether and politef, ethylene-tetrafluoroethylene copolymer (ETFE) or
Several mixture.
4. the preparation method of the carbon-coated LiFePO 4 for lithium ion batteries of Fluorin doped according to claim 1, it is characterised in that：Step (2)
Middle LiFePO4 is 10 with the mass ratio of organic fluorocompound:(0.5～4).
5. the preparation method of the carbon-coated LiFePO 4 for lithium ion batteries of Fluorin doped according to claim 1, it is characterised in that：Step (2)
When middle organic fluorocompound is solid, organic solvent during mixing, is added so that organic fluorocompound is fully dissolved, the organic solvent is N-
Methyl pyrrolidone (NMP), dimethyl phthalate (DMP), dimethyl sulfoxide (DMSO), dimethyl fumarate (DMF) its
In one kind.
6. the preparation method of the carbon-coated LiFePO 4 for lithium ion batteries of Fluorin doped according to claim 1, it is characterised in that：Step (2)
Middle milling time is 1～4 hour.
7. the preparation method of the carbon-coated LiFePO 4 for lithium ion batteries of Fluorin doped according to claim 1, it is characterised in that：Step (3)
Middle protective gas is nitrogen, argon, helium or neon one kind therein.
8. the preparation method of the carbon-coated LiFePO 4 for lithium ion batteries of Fluorin doped according to claim 1, it is characterised in that：Step (3)
Middle calcining heat is 600～900 DEG C, and calcination time is 3～5h.
9. a kind of carbon-coated LiFePO 4 for lithium ion batteries of the Fluorin doped for being obtained according to any one preparation method in claim 1～8.
10. the carbon-coated LiFePO 4 for lithium ion batteries of Fluorin doped according to claim 9 is used as the application of anode material for lithium-ion batteries.
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Cited By (10)
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| CN107195901A (en) * | 2017-05-27 | 2017-09-22 | 中国科学院物理研究所 | Perfluorocarbon acid salt material and preparation method thereof, anode pole piece and battery |
| CN107994223A (en) * | 2017-12-11 | 2018-05-04 | 广东工业大学 | A kind of composite material of the fluorin-doped modification of aluminium and its preparation method and application |
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