CN106207175A - A kind of preparation method of LiFePO4/graphene composite material - Google Patents
A kind of preparation method of LiFePO4/graphene composite material Download PDFInfo
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- CN106207175A CN106207175A CN201610804294.2A CN201610804294A CN106207175A CN 106207175 A CN106207175 A CN 106207175A CN 201610804294 A CN201610804294 A CN 201610804294A CN 106207175 A CN106207175 A CN 106207175A
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- roasting
- lifepo4
- composite material
- graphene composite
- dried
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 34
- 239000002131 composite material Substances 0.000 title claims abstract description 22
- 229910052493 LiFePO4 Inorganic materials 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 45
- 238000000498 ball milling Methods 0.000 claims abstract description 18
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 16
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910010707 LiFePO 4 Inorganic materials 0.000 claims abstract description 10
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 claims abstract description 9
- 239000002699 waste material Substances 0.000 claims abstract description 8
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 7
- 239000010439 graphite Substances 0.000 claims abstract description 7
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 7
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002270 dispersing agent Substances 0.000 claims abstract description 6
- 238000007654 immersion Methods 0.000 claims abstract description 6
- 235000010344 sodium nitrate Nutrition 0.000 claims abstract description 6
- 239000004317 sodium nitrate Substances 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 11
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 11
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 229910052744 lithium Inorganic materials 0.000 claims description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 229910052698 phosphorus Inorganic materials 0.000 claims description 5
- 229910052700 potassium Inorganic materials 0.000 claims description 5
- 239000011591 potassium Substances 0.000 claims description 5
- 238000005245 sintering Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 7
- 238000010791 quenching Methods 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 abstract 1
- 239000012286 potassium permanganate Substances 0.000 abstract 1
- 230000000171 quenching effect Effects 0.000 abstract 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 239000005955 Ferric phosphate Substances 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229940032958 ferric phosphate Drugs 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 description 1
- 229910000399 iron(III) phosphate Inorganic materials 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- 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 the preparation method of a kind of LiFePO4/graphene composite material.The method mainly includes that by organic solvent immersion, ultrasonic Treatment, ball milling, roasting, quenching and conductive black is baking mixed obtains LiFePO 4 material by waste lithium iron phosphate battery positive plate；Then natural flake graphite and sodium nitrate are joined in sulfuric acid solution, obtain graphene oxide by oxidations such as potassium permanganate；Finally the LiFePO 4 material obtained and graphene oxide being mixed, with N methyl 2 ketopyrrolidine as dispersant, ball milling i.e. obtains LiFePO4/graphene composite material.The method using the present invention, method is simple, low cost, and the conductivity of composite material obtained can be excellent.
Description
Technical field
The present invention relates to technical field of composite preparation, particularly relate to a kind of LiFePO4/graphene composite material
Preparation method.
Background technology
Lithium ion battery has the features such as voltage height, specific energy height, non-environmental-pollution, is widely used in mobile phone etc. portable
Formula electronic equipment.Since Graphene is successfully prepared, its lamella has flexibility and controllability, it is possible to more effectively improve activity
The chemical property of material.Graphene is the lithium ion battery material that a class has application prospect.Ferric phosphate lithium cell has because of it
There are environmental friendliness, cheap, heat stability advantages of higher, are widely used in the field such as mobile phone, electric automobile.Waste and old
The recovery method of lithium iron phosphate battery positive material mainly has two big classes: a kind of wet method for the purpose of reclaiming precious metal is soaked
Go out, another kind of for regeneration lithium iron phosphate positive material.Graphene is suitable as covering material to strengthen LiFePO4 electric conductivity
And cycle performance.
Summary of the invention
The present invention is to solve problem of the prior art, it is provided that the preparation of a kind of LiFePO4/graphene composite material
Method.
The preparation method of a kind of LiFePO4/graphene composite material of the present invention, step is as follows:
(1) waste lithium iron phosphate battery positive plate is put in the mixed organic solvents of ethyl acetate and ethanol and soak, wherein, second
The volume ratio of acetoacetic ester and ethanol is 1～10 1, carries out ultrasonic Treatment during immersion, and supersonic frequency is 50～60kHz, with stirring
Device is stirred, and stir speed (S.S.) is 150～180r/min, and soak time is 0.5～3h, filter, in 30～90 DEG C be dried 1～
2h, obtains positive electrode；
(2) positive electrode ball milling 0.5～10h in planetary ball mill obtained by step (1) filtration drying, drum's speed of rotation is
50～1000r/min；
(3) positive electrode after step (2) ball milling being put into together with appropriate lithium carbonate roasting kiln roasting, sintering temperature is
500～850 DEG C, obtain roasting material, lithium carbonate by meet the mol ratio of Li, Fe and P in roasting material be 0.95～1.1 0.9～
The requirement of 1.1 0.9～1.1 is added；
(4) roasting material that step (3) obtains is put in the water of 0 ~ 50 DEG C and quenches, then in 30～120 DEG C be dried 0.5～
10h；
(5) step (4) dried material is mixed with conductive black, at 500～850 DEG C, the lower roasting 8～30h of nitrogen protection,
Obtaining LiFePO 4 material, the most dried material is 1 0.01 ~ 2 with the mass ratio of conductive black；
(6) natural flake graphite and sodium nitrate are joined in the sulfuric acid solution of 1 ~ 10mol/L, be stirred continuously lower addition Gao Meng
Acid potassium, react 80～90min, then control reaction temperature be 0～45 DEG C, continue reaction 30～800min, be slowly added to from
Sub-water, is then slowly added to a certain amount of 5～10% hydrogen peroxide of mass concentration, after reaction 40～60min at 80～90 DEG C
Washing by centrifugation, 30～100 DEG C of drying obtain graphene oxide；
(7) graphene oxide that LiFePO 4 material step (5) obtained and step (6) obtain is according to mass ratio 8 ~ 100 1
Mixing, with METHYLPYRROLIDONE as dispersant, planetary ball mill ball milling 1～8h, then 30～120 DEG C are dried 1～10h,
Again at 500～850 DEG C, the lower roasting 8～30h of nitrogen protection, obtain LiFePO4/graphene composite material.
In step (1), the volume ratio of ethyl acetate and ethanol is preferably 11.
In step (6), sulfuric acid concentration is preferably 2～5mol/L.
The present invention soaks positive plate by the mixed organic solvents of ethyl acetate and ethanol and carries out ultrasonic Treatment, makes
Obtain positive electrode to be more conducive to separate.Positive electrode after ball milling adds a certain amount of lithium carbonate and carries out roasting together so that final
Obtain LiFePO 4 material and meet the requirement of battery material.The present invention utilizes waste lithium iron phosphate material and natural flake graphite system
Standby LiFePO4/graphene composite material method is simple, low cost, and the conductivity of composite material obtained can be excellent.
Detailed description of the invention
Below in conjunction with instantiation, the present invention is described in detail.
Embodiment 1:
A kind of preparation method of LiFePO4/graphene composite material, step is as follows:
(1) waste lithium iron phosphate battery positive plate is put in the mixed organic solvents of ethyl acetate and ethanol and soak, wherein, second
The volume ratio of acetoacetic ester and ethanol is 11, carries out ultrasonic Treatment during immersion, and supersonic frequency is 50kHz, stirs with agitator
Mixing, stir speed (S.S.) is 150r/min, and soak time is 0.5h, filters, in 30 DEG C of dry 1h, obtains positive electrode；
(2) the positive electrode ball milling 0.5h in planetary ball mill obtained by step (1) filtration drying, drum's speed of rotation is 50r/
min；
(3) positive electrode after step (2) ball milling being put into together with appropriate lithium carbonate roasting kiln roasting, sintering temperature is
500 DEG C, obtaining roasting material, lithium carbonate adds by meeting the requirement that the mol ratio of Li, Fe and P in roasting material is 0.95 0.9 0.9
Add；
(4) roasting material that step (3) obtains is put in the water of 0 DEG C and quench, then in 30 DEG C of dry 0.5h；
(5) step (4) dried material is mixed with conductive black, at 500 DEG C, the lower roasting 8h of nitrogen protection, obtain phosphoric acid
Ferrum lithium material, the most dried material is 1 0.01 with the mass ratio of conductive black；
(6) natural flake graphite and sodium nitrate are joined in the sulfuric acid solution of 1mol/L, be stirred continuously lower addition permanganic acid
Potassium, reacts 80min, and then controlling reaction temperature is 0 DEG C, continues reaction 30min, is slowly added to deionized water, then at 80 DEG C
Under be slowly added to the hydrogen peroxide of a certain amount of 5% mass concentration, through centrifuge washing after reaction 40min, 30 DEG C of drying are aoxidized
Graphene；
(7) graphene oxide that LiFePO 4 material step (5) obtained and step (6) obtain mixes according to mass ratio 81,
With METHYLPYRROLIDONE as dispersant, planetary ball mill ball milling 1h, then 30 DEG C of dry 1h, then at 500 DEG C, nitrogen is protected
Protect lower roasting 8h, obtain LiFePO4/graphene composite material.
Embodiment 2:
A kind of preparation method of LiFePO4/graphene composite material, step is as follows:
(1) waste lithium iron phosphate battery positive plate is put in the mixed organic solvents of ethyl acetate and ethanol and soak, wherein, second
The volume ratio of acetoacetic ester and ethanol is 10 1, carries out ultrasonic Treatment during immersion, and supersonic frequency is 60kHz, carries out with agitator
Stirring, stir speed (S.S.) is 180r/min, and soak time is 3h, filters, in 90 DEG C of dry 2h, obtains positive electrode；
(2) the positive electrode ball milling 10h in planetary ball mill obtained by step (1) filtration drying, drum's speed of rotation is
1000r/min；
(3) positive electrode after step (2) ball milling being put into together with appropriate lithium carbonate roasting kiln roasting, sintering temperature is
850 DEG C, obtaining roasting material, lithium carbonate adds by meeting the requirement that the mol ratio of Li, Fe and P in roasting material is 111；
(4) roasting material that step (3) obtains is put in the water of 50 DEG C and quench, then in 120 DEG C of dry 10h；
(5) step (4) dried material is mixed with conductive black, at 850 DEG C, the lower roasting 30h of nitrogen protection, obtain phosphoric acid
Ferrum lithium material, the most dried material is 12 with the mass ratio of conductive black；
(6) natural flake graphite and sodium nitrate are joined in the sulfuric acid solution of 10mol/L, be stirred continuously lower addition permanganic acid
Potassium, reacts 90min, and then controlling reaction temperature is 45 DEG C, continues reaction 800min, is slowly added to deionized water, then 90
Being slowly added to the hydrogen peroxide of a certain amount of 10% mass concentration at DEG C, through centrifuge washing after reaction 60min, 100 DEG C of drying obtain
Graphene oxide；
(7) graphene oxide that LiFePO 4 material step (5) obtained and step (6) obtain mixes according to mass ratio 100 1
Close, with METHYLPYRROLIDONE as dispersant, planetary ball mill ball milling 8h, then 120 DEG C of dry 10h, then at 850 DEG C, nitrogen
Roasting 30h under gas shielded, obtains LiFePO4/graphene composite material.
Embodiment 3:
A kind of preparation method of LiFePO4/graphene composite material, step is as follows:
(1) waste lithium iron phosphate battery positive plate is put in the mixed organic solvents of ethyl acetate and ethanol and soak, wherein, second
The volume ratio of acetoacetic ester and ethanol is 51, carries out ultrasonic Treatment during immersion, and supersonic frequency is 55kHz, stirs with agitator
Mixing, stir speed (S.S.) is 160r/min, and soak time is 2h, filters, in 60 DEG C of dry 1.5h, obtains positive electrode；
(2) the positive electrode ball milling 5h in planetary ball mill obtained by step (1) filtration drying, drum's speed of rotation is 500r/
min；
(3) positive electrode after step (2) ball milling being put into together with appropriate lithium carbonate roasting kiln roasting, sintering temperature is
650 DEG C, obtaining roasting material, lithium carbonate adds by meeting the requirement that the mol ratio of Li, Fe and P in roasting material is 111；
(4) roasting material that step (3) obtains is put in the water of 20 DEG C and quench, then in 60 DEG C of dry 8h；
(5) step (4) dried material is mixed with conductive black, at 750 DEG C, the lower roasting 10h of nitrogen protection, obtain phosphoric acid
Ferrum lithium material, the most dried material is 1 0.5 with the mass ratio of conductive black；
(6) natural flake graphite and sodium nitrate are joined in the sulfuric acid solution of 2mol/L, be stirred continuously lower addition permanganic acid
Potassium, reacts 85min, and then controlling reaction temperature is 35 DEG C, continues reaction 60min, is slowly added to deionized water, then at 85 DEG C
Under be slowly added to the hydrogen peroxide of a certain amount of 8% mass concentration, through centrifuge washing after reaction 50min, 50 DEG C of drying are aoxidized
Graphene；
(7) graphene oxide that LiFePO 4 material step (5) obtained and step (6) obtain mixes according to mass ratio 91,
With METHYLPYRROLIDONE as dispersant, planetary ball mill ball milling 3h, then 70 DEG C of dry 5h, then at 650 DEG C, nitrogen is protected
Protect lower roasting 20h, obtain LiFePO4/graphene composite material.
Claims (3)
1. the preparation method of LiFePO4/graphene composite material, it is characterised in that step is as follows:
(1) waste lithium iron phosphate battery positive plate is put in the mixed organic solvents of ethyl acetate and ethanol and soak, wherein, second
The volume ratio of acetoacetic ester and ethanol is 1～10 1, carries out ultrasonic Treatment during immersion, and supersonic frequency is 50～60kHz, with stirring
Device is stirred, and stir speed (S.S.) is 150～180r/min, and soak time is 0.5～3h, filter, in 30～90 DEG C be dried 1～
2h, obtains positive electrode；
(2) positive electrode ball milling 0.5～10h in planetary ball mill obtained by step (1) filtration drying, drum's speed of rotation is
50～1000r/min；
(3) positive electrode after step (2) ball milling being put into together with appropriate lithium carbonate roasting kiln roasting, sintering temperature is
500～850 DEG C, obtain roasting material, lithium carbonate by meet the mol ratio of Li, Fe and P in roasting material be 0.95～1.1 0.9～
The requirement of 1.1 0.9～1.1 is added；
(4) roasting material that step (3) obtains is put in the water of 0 ~ 50 DEG C and quenches, then in 30～120 DEG C be dried 0.5～
10h；
(5) step (4) dried material is mixed with conductive black, at 500～850 DEG C, the lower roasting 8～30h of nitrogen protection,
Obtaining LiFePO 4 material, the most dried material is 1 0.01 ~ 2 with the mass ratio of conductive black；
(6) natural flake graphite and sodium nitrate are joined in the sulfuric acid solution of 1 ~ 10mol/L, be stirred continuously lower addition Gao Meng
Acid potassium, react 80～90min, then control reaction temperature be 0～45 DEG C, continue reaction 30～800min, be slowly added to from
Sub-water, is then slowly added to a certain amount of 5～10% hydrogen peroxide of mass concentration, after reaction 40～60min at 80～90 DEG C
Washing by centrifugation, 30～100 DEG C of drying obtain graphene oxide；
(7) graphene oxide that LiFePO 4 material step (5) obtained and step (6) obtain is according to mass ratio 8 ~ 100 1
Mixing, with METHYLPYRROLIDONE as dispersant, planetary ball mill ball milling 1～8h, then 30～120 DEG C are dried 1～10h,
Again at 500～850 DEG C, the lower roasting 8～30h of nitrogen protection, obtain LiFePO4/graphene composite material.
2. the preparation method of LiFePO4/graphene composite material as claimed in claim 1, it is characterised in that in step (1)
The volume ratio of ethyl acetate and ethanol is 11.
3. the preparation method of LiFePO4/graphene composite material as claimed in claim 1, it is characterised in that in step (6)
Sulfuric acid concentration is 2～5mol/L.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107123802A (en) * | 2017-05-25 | 2017-09-01 | 长沙理工大学 | A kind of preparation method of graphene modified phosphate iron lithium material |
| CN114824253A (en) * | 2022-04-24 | 2022-07-29 | 中南大学 | Method for granulating spherical particles of lithium ion battery cathode material |
| CN116495787A (en) * | 2023-03-22 | 2023-07-28 | 四川大学 | Manganese-based compound prepared based on waste lithium battery, preparation method of manganese-based compound and battery |
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| CN102208706A (en) * | 2011-05-04 | 2011-10-05 | 合肥国轩高科动力能源有限公司 | Recycling treatment method of waste and old lithium iron phosphate battery anode materials |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107123802A (en) * | 2017-05-25 | 2017-09-01 | 长沙理工大学 | A kind of preparation method of graphene modified phosphate iron lithium material |
| CN114824253A (en) * | 2022-04-24 | 2022-07-29 | 中南大学 | Method for granulating spherical particles of lithium ion battery cathode material |
| CN114824253B (en) * | 2022-04-24 | 2024-03-15 | 中南大学 | Granulating method for spherical particles of lithium ion battery anode material |
| CN116495787A (en) * | 2023-03-22 | 2023-07-28 | 四川大学 | Manganese-based compound prepared based on waste lithium battery, preparation method of manganese-based compound and battery |
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