CN107611357A - A kind of graphene-coated lithium iron phosphate preparation method - Google Patents
A kind of graphene-coated lithium iron phosphate preparation method Download PDFInfo
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- CN107611357A CN107611357A CN201710594025.2A CN201710594025A CN107611357A CN 107611357 A CN107611357 A CN 107611357A CN 201710594025 A CN201710594025 A CN 201710594025A CN 107611357 A CN107611357 A CN 107611357A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 38
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 26
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002002 slurry Substances 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 229910052742 iron Inorganic materials 0.000 claims abstract description 13
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 13
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 12
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 11
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 11
- 239000011574 phosphorus Substances 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 8
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 7
- 239000002244 precipitate Substances 0.000 claims abstract description 5
- 235000015112 vegetable and seed oil Nutrition 0.000 claims abstract description 5
- 239000008158 vegetable oil Substances 0.000 claims abstract description 5
- 239000012298 atmosphere Substances 0.000 claims abstract description 4
- 230000001681 protective effect Effects 0.000 claims abstract description 4
- 238000009413 insulation Methods 0.000 claims abstract description 3
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 10
- 229910019142 PO4 Inorganic materials 0.000 claims description 8
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 claims description 6
- 229910000399 iron(III) phosphate Inorganic materials 0.000 claims description 6
- 229910000904 FeC2O4 Inorganic materials 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000001694 spray drying Methods 0.000 claims description 4
- 229910010951 LiH2 Inorganic materials 0.000 claims description 3
- 229910017677 NH4H2 Inorganic materials 0.000 claims description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 3
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 3
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 3
- 229910003002 lithium salt Inorganic materials 0.000 claims description 3
- 159000000002 lithium salts Chemical class 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims 1
- 239000000243 solution Substances 0.000 description 24
- 229910052493 LiFePO4 Inorganic materials 0.000 description 10
- 239000013074 reference sample Substances 0.000 description 9
- 239000006258 conductive agent Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000005955 Ferric phosphate Substances 0.000 description 3
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 229940032958 ferric phosphate Drugs 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- QSNQXZYQEIKDPU-UHFFFAOYSA-N [Li].[Fe] Chemical compound [Li].[Fe] QSNQXZYQEIKDPU-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000004513 sizing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- LLYXJBROWQDVMI-UHFFFAOYSA-N 2-chloro-4-nitrotoluene Chemical compound CC1=CC=C([N+]([O-])=O)C=C1Cl LLYXJBROWQDVMI-UHFFFAOYSA-N 0.000 description 1
- 239000006245 Carbon black Super-P Substances 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 1
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 1
- 229910001290 LiPF6 Inorganic materials 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000005030 aluminium foil Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Classifications
-
- 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
Landscapes
- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention provides a kind of graphene-coated lithium iron phosphate preparation method, comprises the following steps：1) a certain amount of lithium source is dissolved in deionized water and forms solution A, a certain amount of source of iron is dissolved in the deionized water after heating and forms solution B, a certain amount of phosphorus source is added in solution A and stirring disappears to form solution C to white precipitate；2) solution B is added after solution C being stirred into a period of time, then continues stirring at a certain temperature and obtains colloidal sol for a period of time；3) colloidal sol is filtered, be spray-dried after be made presoma；4) presoma and vegetable oil are configured to slurry according to certain solid content, then slurry is coated uniformly on nickel strap and is put into tube furnace with certain thickness, rapid cool obtains material D after tube furnace rises to 700 900 DEG C and insulation 3min in a short time；5) material D after 300 500 DEG C of high temperature pre-burning and 700 900 DEG C of high-temperature calcination is cooled to room temperature under protective atmosphere.
Description
【Technical field】
The invention belongs to power battery anode material technical field, more particularly to a kind of graphene-coated lithium iron phosphate to prepare
Method.
【Background technology】
LiFePO4 because its have it is safe, have extended cycle life, operating temperature range is wide, abundant raw material, clean environment firendly
Etc. the positive electrode that advantage is widely used as electrokinetic cell.But LiFePO4 self-conductive poor performance, cause lithium ion diffusion system
Number is relatively low, has a strong impact on the high rate performance of electrokinetic cell.Current corrective measure is to add conductive agent in LiFePO4 slurry,
Such as conductive black, electrically conductive graphite, CNT, graphene, but whole structure is poor, because conductive agent specific surface area is big,
Surface energy is big, easily reunites during slurry is configured, the performance of electric conductivity is affected.
【The content of the invention】
The present invention proposes the graphene coated phosphoric acid of a kind of electric conductivity that can improve LiFePO 4 material and high rate performance
Iron lithium preparation method.
The present invention provides a kind of graphene-coated lithium iron phosphate preparation method, comprises the following steps：
1) a certain amount of lithium source is dissolved in deionized water and forms solution A, by a certain amount of source of iron be dissolved in heating go from
Solution B is formed in sub- water, a certain amount of phosphorus source is added in the solution A and stirring disappears to form solution C to white precipitate；
2) solution B is added after the solution C being stirred into a period of time, then continues one section of stirring at a certain temperature
Time obtains colloidal sol；
3) presoma will be made after colloidal sol filtering, spray drying；
4) presoma and vegetable oil are configured to slurry according to certain solid content, then the slurry with certain
Thickness be coated uniformly on nickel strap and be put into tube furnace, the tube furnace rise in a short time 700-900 DEG C and be incubated
Rapid cooling obtains material D after 3min；
5) by material D under protective atmosphere after 300-500 DEG C of high temperature pre-burning and 700-900 DEG C of high-temperature calcination it is cold
But to room temperature.
In a preferred embodiment, the molar ratio of the lithium source, the source of iron and phosphorus source is (1-1.8):
(1-1.8):(1-1.8)。
In a preferred embodiment, the lithium source is soluble lithium salt, preferably Li2CO3, LiOH or LiH2PO4In
One kind or any mixing.
In a preferred embodiment, the source of iron is preferably FePO4、Fe2O3And FeC2O4In one kind or any mixed
Close.
In a preferred embodiment, phosphorus source is preferably NH4H2PO4And/or H3PO4。
In a preferred embodiment, in step 1), source of iron is dissolved in 90 DEG C of deionized water and forms solution B；Step
It is rapid 2) in, will the solution C stir 1-6h after add the solution B, then continue at a temperature of 80-95 DEG C stir 8-12h.
In a preferred embodiment, in step 2), by pH value control between 3-8.
In a preferred embodiment, in step 4), the solid content of the slurry is 50-80%, the thickness of the nickel strap
It is 10-100mm coated in the thickness on the nickel strap to spend for 1-10mm, the slurry.
In a preferred embodiment, in step 4), the tube furnace rises to 700-900 DEG C in 30min；Step 5)
In, the high temperature pre-burning is to rise to 300-500 DEG C with 1-8 DEG C/min heating rate and be incubated 2-6h, and the high-temperature calcination is
700-900 DEG C is continuously heating to 1-8 DEG C/min heating rate and is incubated 4-10h.
The graphene-coated lithium iron phosphate that graphene-coated lithium iron phosphate preparation method provided by the present invention obtains can
Positive electrode as electrokinetic cell, and the electrokinetic cell prepared has more preferable high rate performance and cycle performance.In addition, should
Preparation method technique is simple, does not produce harmful substance, is adapted to production in enormous quantities.
【Brief description of the drawings】
Fig. 1 is that the graphene-coated lithium iron phosphate that embodiment obtains and the XRD spectrum of LiFePO4 reference sample contrast.
Fig. 2 is the graphene-coated lithium iron phosphate and the SEM micro-structure diagrams of LiFePO4 reference sample that embodiment obtains
Contrast.
Fig. 3 is the TEM figures for the graphene-coated lithium iron phosphate that embodiment obtains.
Fig. 4 is the graphene-coated lithium iron phosphate and LiFePO4 reference sample obtained respectively using embodiment as positive electrode
The cycle performance test curve of the battery of preparation.
【Embodiment】
In order that purpose, technical scheme and the advantageous effects of invention become apparent from understanding, below in conjunction with accompanying drawing and tool
Body embodiment, the present invention will be described in further detail.It should be appreciated that the specific embodiment party described in this specification
Formula is not intended to limit the present invention just for the sake of explaining the present invention.
The present invention provides a kind of graphene-coated lithium iron phosphate preparation method, comprises the following steps：
1) a certain amount of lithium source is dissolved in deionized water and forms solution A, by a certain amount of source of iron be dissolved in heating go from
Solution B is formed in sub- water, a certain amount of phosphorus source is added in the solution A and stirring disappears to form solution C to white precipitate；
2) solution B is added after the solution C being stirred into a period of time, then continues one section of stirring at a certain temperature
Time obtains colloidal sol；
3) presoma will be made after colloidal sol filtering, spray drying；
4) presoma and vegetable oil are configured to slurry according to certain solid content, then the slurry with certain
Thickness be coated uniformly on nickel strap and be put into tube furnace, the tube furnace rise in a short time 700-900 DEG C and be incubated
Rapid cooling obtains material D after 3min；
5) by material D under protective atmosphere after 300-500 DEG C of high temperature pre-burning and 700-900 DEG C of high-temperature calcination it is cold
But to room temperature.
Specifically, the lithium source is soluble lithium salt, preferably Li2CO3, LiOH or LiH2PO4In one kind or any mixed
Close.The source of iron is preferably FePO4、Fe2O3And FeC2O4In one kind or any mixing.Phosphorus source is preferably NH4H2PO4Or/
And H3PO4.The molar ratio of the lithium source, the source of iron and phosphorus source is (1-1.8):(1-1.8):(1-1.8).
In step 1), source of iron is dissolved in 90 DEG C of deionized water and forms solution B.In step 2), the solution C is stirred
The solution B is added after 1-6h, then continues to stir 8-12h at a temperature of 80-95 DEG C.Further, in step 2), by pH
Value control is between 3-8.In step 4), the solid content of the slurry is 50-80%, and the thickness of the nickel strap is 1-10mm, institute
It is 10-100mm that slurry, which is stated, coated in the thickness on the nickel strap；The tube furnace rises to 700-900 DEG C in 30min.Step
5) in, the high temperature pre-burning is to rise to 300-500 DEG C with 1-8 DEG C/min heating rate and be incubated 2-6h, the high-temperature calcination
It is to be continuously heating to 700-900 DEG C with 1-8 DEG C/min heating rate and be incubated 4-10h.
Embodiment
A certain amount of LiOH is dissolved in deionized water and forms solution A, by a certain amount of FeC2O4It is dissolved in 90 DEG C of deionization
Solution B is formed in water, by a certain amount of H3PO4Add in the solution A and stir and disappear to form solution C, this reality to white precipitate
Apply in example, LiOH, FeC2O4And H3PO4Molar ratio be 1:1:1.The solution B is added after the solution C is stirred into 2h, so
Continue stirring 12h at a temperature of 90 DEG C afterwards and obtain colloidal sol, during this period, pH value is controlled 6 or so.Next will be described molten
Presoma is made after glue filtering, spray drying.The presoma and vegetable oil are configured to the slurry that solid content is 60%, then
The slurry is coated uniformly on thick 5mm nickel strap and is put into tube furnace according to 100mm thickness, in the tube furnace
Rapid cooling obtains material D after temperature rises to 800 DEG C and insulation 3min in 26min.Material D is heated under an argon atmosphere
450 DEG C and 6h is incubated, continues to be heated to 700 DEG C and be cooled to room temperature after being incubated 10h, you can obtain graphene coated ferric phosphate
Lithium.
Electrokinetic cell is prepared as positive electrode using the graphene-coated lithium iron phosphate that the present embodiment obtains.Specifically, by institute
Positive electrode, conductive agent (Super-P) and binding agent (Kynoar) are stated according to 96.5:1:2.5 mass ratio is dissolved in organic
Stirring prepares anode sizing agent in solvent (1-METHYLPYRROLIDONE), and the anode sizing agent is coated on aluminium foil and prepares positive pole
Piece.Meanwhile using Delanium as negative material, with conductive agent (conductive carbon black) and binding agent (LA133) according to 95:2:3 matter
Amount prepares cathode size than being dissolved in stirring in deionized water, and the cathode size is coated on copper foil and prepares negative plate.So
The positive plate and the negative plate are separated with barrier film afterwards and are wound making core, volume is used in the electrolyte of injection
Than for 1:1:1 ethylene carbonate, diethyl carbonate and dimethyl carbonate and LiPF6Concentration be 1mol/L, be assembled into 32650
Type battery A.
As a comparison, using the LiFePO4 commonly used in the prior art without graphene coated as reference sample, compare by
The graphene-coated lithium iron phosphate that embodiment obtains and the XRD spectrum and the micro- knots of SEM of the LiFePO4 reference sample
Structure.In addition, using the LiFePO4 reference sample as positive electrode, battery is prepared according to the process meanses prepared needed for battery A
B, and battery A and battery B are subjected to electric performance test after preliminary filling, high temperature ageing, partial volume, wherein, voltage range is
2.0-3.6V environment temperature is 25 DEG C.
Referring to Fig. 1, by the graphene-coated lithium iron phosphate that embodiment obtains and the LiFePO4 reference sample
XRD spectrum analytic explanation：Both diffraction maximum positions do not have notable difference, graphene coated ferric phosphate provided by the invention
Lithium preparation method does not have the crystal structure for changing LiFePO 4 material.
Referring to Fig. 2, upper figure represents the graphene-coated lithium iron phosphate obtained by embodiment, figure below represents the phosphorus
Sour iron lithium reference sample, observation SEM microstructures are understood：The granular size of the graphene-coated lithium iron phosphate be more uniformly distributed and
Particle diameter is smaller, and such characteristic is more beneficial for improving the high rate performance of electrokinetic cell.In addition, also referring to Fig. 3, described in observation
The TEM image of graphene-coated lithium iron phosphate is understood：Obtained using graphene-coated lithium iron phosphate preparation method provided by the invention
The product obtained is one layer of class graphene film Rotating fields of cladding around lithium iron phosphate particles, and such graphene film Rotating fields energy
It is enough to strengthen the electric conductivity of LiFePO 4 material and lithium ion mobility ability.
Fig. 4 and following table are referred to, the graphene-coated lithium iron phosphate and the ferric phosphate obtained respectively with embodiment
Lithium reference sample is that battery A prepared by positive electrode and battery B electric performance test result is shown：The battery A's fills first
Discharging efficiency, constant current are filled with ratio, capacity and positive pole gram volume and are above the battery B；The internal resistance of the battery A is less than the electricity
Pond B；The cycle performance of the battery A is better than the battery B.
| Species | Efficiency/% first | Internal resistance/m Ω | Constant current is filled with ratio/% | Capacity/mAh | Positive pole gram volume mAh/g |
| Battery A | 89.63% | 5.2 | 98.61% | 6056 | 142.8 |
| Battery B | 87.21% | 7.5 | 96.72% | 5905 | 140.2 |
The graphene-coated lithium iron phosphate that graphene-coated lithium iron phosphate preparation method provided by the present invention obtains can
Positive electrode as electrokinetic cell, and the electrokinetic cell prepared has more preferable high rate performance and cycle performance.In addition, should
Preparation method technique is simple, does not produce harmful substance, is adapted to production in enormous quantities.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is to combine specific preferred embodiment to institute of the present invention
The further description of work, it is impossible to assert that the specific implementation of the present invention is confined to these explanations.It is all the present invention spirit and
All any modification, equivalent and improvement made within principle etc., should be included within the scope of the present invention.
Claims (9)
- A kind of 1. graphene-coated lithium iron phosphate preparation method, it is characterised in that：Comprise the following steps：1) a certain amount of lithium source is dissolved in deionized water and forms solution A, a certain amount of source of iron is dissolved in the deionized water of heating Middle formation solution B, a certain amount of phosphorus source is added in the solution A and stirring disappears to form solution C to white precipitate；2) solution B is added after the solution C being stirred into a period of time, then continues stirring a period of time at a certain temperature Obtain colloidal sol；3) presoma will be made after colloidal sol filtering, spray drying；4) presoma and vegetable oil are configured to slurry according to certain solid content, then the slurry with certain thickness Degree is coated uniformly on nickel strap and is put into tube furnace, and the tube furnace rises to 700-900 DEG C and insulation 3min in a short time Rapid cooling obtains material D afterwards；5) material D is cooled to after 300-500 DEG C of high temperature pre-burning and 700-900 DEG C of high-temperature calcination under protective atmosphere Room temperature.
- 2. graphene-coated lithium iron phosphate preparation method as claimed in claim 1, it is characterised in that：The lithium source, the iron The molar ratio of source and phosphorus source is (1-1.8):(1-1.8):(1-1.8).
- 3. graphene-coated lithium iron phosphate preparation method as claimed in claim 1, it is characterised in that：The lithium source is solubility Lithium salts, preferably Li2CO3, LiOH or LiH2PO4In one kind or any mixing.
- 4. graphene-coated lithium iron phosphate preparation method as claimed in claim 1, it is characterised in that：The source of iron is preferably FePO4、Fe2O3And FeC2O4In one kind or any mixing.
- 5. graphene-coated lithium iron phosphate preparation method as claimed in claim 1, it is characterised in that：Phosphorus source is preferably NH4H2PO4And/or H3PO4。
- 6. graphene-coated lithium iron phosphate preparation method as claimed in claim 1, it is characterised in that：In step 1), by source of iron It is dissolved in 90 DEG C of deionized water and forms solution B；In step 2), the solution B is added after the solution C is stirred into 1-6h, so Continue to stir 8-12h at a temperature of 80-95 DEG C afterwards.
- 7. graphene-coated lithium iron phosphate preparation method as claimed in claim 1, it is characterised in that：In step 2), by pH value Control is between 3-8.
- 8. graphene-coated lithium iron phosphate preparation method as claimed in claim 1, it is characterised in that：In step 4), the slurry The solid content of material is 50-80%, and the thickness of the nickel strap is 1-10mm, and the slurry is coated in the thickness on the nickel strap 10-100mm。
- 9. graphene-coated lithium iron phosphate preparation method as claimed in claim 1, it is characterised in that：In step 4), the pipe Formula stove rises to 700-900 DEG C in 30min；In step 5), the high temperature pre-burning is risen to 1-8 DEG C/min heating rate 300-500 DEG C and 2-6h is incubated, the high-temperature calcination is to be continuously heating to 700-900 DEG C simultaneously with 1-8 DEG C/min heating rate It is incubated 4-10h.
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| CN113363463A (en) * | 2021-06-02 | 2021-09-07 | 湖北亿纬动力有限公司 | Sludge/biomass co-pyrolysis coke-coated lithium iron phosphate cathode material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113363463A (en) * | 2021-06-02 | 2021-09-07 | 湖北亿纬动力有限公司 | Sludge/biomass co-pyrolysis coke-coated lithium iron phosphate cathode material and preparation method and application thereof |
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Application publication date: 20180119 |