CN104577120B - Phosphoric acid vanadium lithium and the preparation method of fluorinated phosphate vanadium lithium composite positive pole - Google Patents
Phosphoric acid vanadium lithium and the preparation method of fluorinated phosphate vanadium lithium composite positive pole Download PDFInfo
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—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
- H01M4/5805—Phosphides
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- H01—ELECTRIC ELEMENTS
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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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
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention discloses phosphoric acid vanadium lithium and the preparation method of fluorinated phosphate vanadium lithium composite positive pole, comprise the following steps: (1) prepares carbon pre-coated by the method for carbon thermal reduction, the V of metal ion mixing1‑mMmPO4/ C presoma, wherein M is Cr3+、Al3+、Y3+、Fe3+；(2) V that will be obtained1‑mMmPO4/ C presoma, carries out mixing dispersion with lithium source, fluorine source, phosphorus source and Graphene (FLG) the dispersion serosity of stoichiometric proportion under ethanol system and obtains mixed slurry；(3) by after above-mentioned obtained mixed slurry dried, carry out high temperature sintering process under inert gas shielding, i.e. obtain and there is metal ion mixing, Graphene and the phosphoric acid vanadium lithium of cracking carbon modification jointly and fluorinated phosphate vanadium lithium composite positive pole.Present invention process is simple, and the phosphoric acid vanadium lithium obtained and fluorinated phosphate vanadium lithium composite positive pole have multiplying power and the cycle performance of excellence, are with a wide range of applications in field of lithium ion battery.
Description
Technical field
The present invention relates to power lithium-ion battery, energy storage lithium ion battery technical field, particularly relate to a kind of phosphoric acid vanadium lithium and the preparation method of fluorinated phosphate vanadium lithium composite positive pole.
Background technology
Fossil fuel is the basis of the current economy of energy, but the lasting rising of global demand of petroleum, the continuous exhaustion of non-renewable resources, and the turbulent political situation of oil exporting country bring safely factor leading to social instability all to whole world new forms of energy.Therefore the exploitation of clean energy resource and use day by day urgent, and seem in energy storage field and field of traffic and be even more important.Lithium ion battery has been obtained for being widely applied and studying as a kind of energy storage instrument.The development of the development mainly positive electrode of lithium ion battery, current lithium ion anode material has respective defect to need further to overcome.Phosphate cathode material is a class positive electrode with fastest developing speed over nearly 10 years, and this kind of material has highly stable crystal structure and good safety.Wherein LiFePO4 (LiFePO4) it is current widely used positive electrode, but its running voltage 3.5V is relatively low, by contrast, and novel phosphate material phosphoric acid vanadium lithium (Li3V2(PO4)) be a kind of fast-ionic conductor, its can the lithium ion quantity of deintercalation more, there is more much higher change plateau potential 3.61,3.69,4.1,4.6V, the lithium ion deintercalation difficulty that wherein 4.6V platform is corresponding.Fluorinated phosphate vanadium lithium (LiVPO4F) due to the electronegativity that fluorion is strong, change metal oxidation reduction electricity to energy level, this material is to Li+The more a height of 4.2V of/Li current potential.Both poly-female lithium ion battery materials are as LiFePO4, and the native electronic electrical conductivity of phase pure material is the lowest, and material has certain polarization when discharge and recharge, and the average operation current potential of electrode material reduces, and can therefore lose a part of reversible capacity.In order to improve this defect, research worker has carried out multinomial modified work.(the Nonferrous Mel. Soc. such as Zhang Bao
China, 2010 (20): 619-623) with Al (NO3)3For aluminum source, phosphoric acid vanadium lithium is doped, it is achieved lithium vanadium phosphate material specific capacity, the reversible reaction of electrode, electron conductivity.(the Journal of Power Source such as Ren Manman
2006 (162): 1357-1362) with glucose as carbon source, phosphoric acid vanadium lithium is modified, and has synthesized the Li with nucleocapsid structure3V2(PO4)3/ C complex, this compound features with nucleocapsid structure has gone out good chemical property.Chen Meng etc. (battery industry, 2009,142 (2): 75-78) with Al to LiVPO4F is doped, and the discharge and recharge polarization of electrode material diminishes, and reversibility increases, and cyclicity gets a promotion.Although about Li3V2(PO4)3And LiVPO4The respective study on the modification of F electrode material is more, and the most single method of modifying could not enough be effectively improved Li3V2(PO4)3And LiVPO4The electric conductivity of F electrode material, and have no at present about Li3V2(PO4)3And LiVPO4The correlational study of F combination electrode material.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of phosphoric acid vanadium lithium and the preparation method of fluorinated phosphate vanadium lithium composite positive pole.
In order to solve above-mentioned technical problem, the technical solution used in the present invention is, phosphoric acid vanadium lithium and the preparation method of fluorinated phosphate vanadium lithium composite positive pole, comprises the following steps:
(1) carbothermic method prepares the V of carbon pre-coated metal ion mixing1-mMmPO4/ C presoma: be that 1-m:m:1:1.2～2.0 weighs vanadium source, doping metals source, phosphorus source, carbon source according to the mol ratio of V:M:P:C；After carrying out disperseing milled processed with dispersant, vacuum drying is placed under inert atmosphere and is sintered, and sintering temperature is 700～800 DEG C, and temperature retention time is 4～10h, i.e. obtains the V of carbon pre-coated metal ion mixing after Temperature fall1-mMmPO4/ C presoma；
(2) according to stoichiometric proportion V1-mMmPO4/ C:Li:F:P:C=(1+x): 3x:1-x:x:0.2～1.0 weighs the V obtained in step (1)1-mMmPO4/ C presoma, lithium source, fluorine source, phosphorus source and graphene conductive slurry, carry out ball milling dispersion process, sintering processes under inert atmosphere after vacuum drying equally in dispersant, sintering temperature is 650～750 degree, temperature retention time is 2～6h, i.e. obtains and have metal ion mixing after Temperature fall, Graphene and the phosphoric acid vanadium lithium of cracking carbon modification jointly and fluorinated phosphate vanadium lithium composite positive pole；
As preferably, described in step (1), vanadium source is V2O5、NH4VO3In one or a combination thereof, phosphorus source is the one in ammonium dihydrogen phosphate, diammonium phosphate, ammonium phosphate or a combination thereof, and described carbon source is the one in sucrose, glucose, phenolic resin, maltose, starch or a combination thereof.
As preferably, the doping metals source described in step (1) is the one in chromium, aluminum, yttrium, the nitrate of ferrum, chlorate, acetate or a combination thereof.
As preferably, described in step (2), lithium source is the one in lithium carbonate, Lithium hydrate, lithium acetate, lithium fluoride or a combination thereof；Phosphorus source is the one in ammonium dihydrogen phosphate, diammonium phosphate, ammonium phosphate or a combination thereof；Described fluorine source is lithium fluoride；Described graphene conductive slurry be weight/mass percentage composition be water system, ethanol system or the N-methyl ketopyrrolidine system dispersed paste of 2%～6%.
As preferably, described in step (1) and step (2), dispersant is ethanol, methanol or acetone solvent.
Phosphoric acid vanadium lithium and the structure of fluorinated phosphate vanadium lithium composite positive pole that the present invention prepares are x (Li3V2(1-m)M2m(PO4)3 ·(1-x)(LiV1-mMmPO4F), wherein x=0.1～0.9, m=0.01～0.15, M are the metal ion of doping, there is, between the crystal grain surface area crystal grain of material, the homogeneous conductive network being made up of carbon coating layer and Graphene.
Above-mentioned doped metal ion M is Cr3+、Al3+、Y3+、Fe3+。
The invention has the beneficial effects as follows:
This composite combines Li3V2(PO4)3And LiVPO4The advantage of F bi-material.The method introduces doped metal ion and organic carbon source, the V obtained during vanadium phosphate compounds is prepared in carbon thermal reduction1-xMPO4/ C presoma, sinters after carrying out with lithium source, fluorine source and the graphene dispersion serosity of stoichiometric proportion mixing dispersion under ethanol system, it is thus achieved that have the jointly modified phosphoric acid vanadium lithium of metal ion mixing, Graphene and cracking carbon and fluorinated phosphate vanadium lithium composite positive pole.The method carries out ion doping and carbon cladding to composite material precursor vanadium phosphate compounds, it is able to ensure that doped metal ion Effective Doping of vanadium position in vanadium phosphate compounds lattice, and owing to the pre-coated of vanadium phosphate compounds is processed, it is possible to realize in sintering process, effective suppression that crystal grain is grown up.
Accompanying drawing explanation
The present invention is further detailed explanation with detailed description of the invention below in conjunction with the accompanying drawings.
Fig. 1 is that the embodiment of the present invention 2 is obtained and has iron ion doping, Graphene and the jointly modified phosphoric acid vanadium lithium of cracking carbon and the X-ray diffractogram of fluorinated phosphate vanadium lithium composite positive pole.
Fig. 2 is that the embodiment of the present invention 2 is obtained and has iron ion doping, Graphene and the jointly modified phosphoric acid vanadium lithium of cracking carbon and the circulation performance of fluorinated phosphate vanadium lithium composite positive pole.
Detailed description of the invention
Embodiment 1
(1) it is that 0.95:0.05:1:2.0 weighs vanadic anhydride, aluminum nitrate, ammonium dihydrogen phosphate, sucrose according to the mol ratio of V:Al:P:C.After carrying out disperseing milled processed with ethanol, vacuum drying is placed under nitrogen atmosphere and is sintered, and sintering temperature is 700 DEG C, and temperature retention time is 10h, i.e. obtains carbon pre-coated, the V of Al ion doping after Temperature fall0.95AL0.05PO4/ C presoma；
(2) according to stoichiometric proportion V0.95M0.05PO4/ C:Li:F:P:C=1.2:0.6:0.8:0.2:0.2 weighs the V obtained in step (1)0.95AL0.05PO4/ C presoma, lithium carbonate, LiF, NH4H2PO4And graphene conductive slurry, ball milling dispersion process is carried out equally in ethanol, sintering processes under nitrogen atmosphere after vacuum drying, sintering temperature is 650 degree, temperature retention time is 6h, i.e. obtain after Temperature fall and there is Al-doping, Graphene and the phosphoric acid vanadium lithium of cracking carbon modification jointly and fluorinated phosphate vanadium lithium composite positive pole；
Embodiment 2
(1) it is that 0.85:0.15:1:1.5 weighs ammonium metavanadate, ferric nitrate, ammonium dihydrogen phosphate, phenolic resin according to the mol ratio of V:Fe:P:C.After carrying out disperseing milled processed with ethanol, vacuum drying is placed under nitrogen atmosphere and is sintered, and sintering temperature is 750 DEG C, and temperature retention time is 6h, i.e. obtains carbon pre-coated, the V of Fe ion doping after Temperature fall0.85Fe0.15PO4/ C presoma；
(2) according to stoichiometric proportion V0.85Fe0.15PO4/ C:Li:F:P:C=1.4:1.2:0.6:0.4:0.8 weighs the V obtained in step (1)0.85Fe0.15PO4/ C presoma, Lithium hydrate, LiF, NH4H2PO4And graphene conductive slurry, ball milling dispersion process is carried out equally in ethanol, sintering processes under nitrogen atmosphere after vacuum drying, sintering temperature is 700 degree, temperature retention time is 4h, i.e. obtain after Temperature fall and there is iron ion doping, Graphene and the phosphoric acid vanadium lithium of cracking carbon modification jointly and fluorinated phosphate vanadium lithium composite positive pole；
Embodiment 3
(1) it is that 0.9:0.1:1:1.2 weighs ammonium metavanadate, chromic nitrate, ammonium dihydrogen phosphate, glucose according to the mol ratio of V:Cr:P:C.After carrying out disperseing milled processed with methanol, vacuum drying is placed under nitrogen atmosphere and is sintered, and sintering temperature is 800 DEG C, and temperature retention time is 4h, i.e. obtains carbon pre-coated, the V of Cr ion doping after Temperature fall0.9Cr0.1PO4/ C presoma；
(2) according to stoichiometric proportion V0.9Cr0.1PO4/ C:Li:F:P:C=1.6:1.8:0.4:0.6:1.0 weighs the V obtained in step (1)0.9Cr0.1PO4/ C presoma, lithium acetate, LiF, NH4H2PO4And graphene conductive slurry, ball milling dispersion process is carried out equally in methanol, sintering processes under nitrogen atmosphere after vacuum drying, sintering temperature is 750 degree, temperature retention time is 2h, i.e. obtain after Temperature fall and there is Cr ion doping, Graphene and the phosphoric acid vanadium lithium of cracking carbon modification jointly and fluorinated phosphate vanadium lithium composite positive pole；
Embodiment 4
(1) it is that 0.98:0.02:1:1.4 weighs ammonium metavanadate, aluminum acetate, ammonium dihydrogen phosphate, glucose according to the mol ratio of V:Al:P:C.After carrying out disperseing milled processed with acetone, vacuum drying is placed under nitrogen atmosphere and is sintered, and sintering temperature is 700 DEG C, and temperature retention time is 4h, i.e. obtains carbon pre-coated, the V of Al ion doping after Temperature fall0.98Al0.01PO4/ C presoma；
(2) according to stoichiometric proportion V0.98Al0.02PO4/ C:Li:F:P:C=1.4:1.2:0.6:0.4:0.8 weighs the V obtained in step (1)0.98Al0.02PO4/ C presoma, lithium acetate, LiF, (NH4)2HPO4And graphene conductive slurry, ball milling dispersion process is carried out equally in acetone, sintering processes under nitrogen atmosphere after vacuum drying, sintering temperature is 700 degree, temperature retention time is 4h, i.e. obtain after Temperature fall and there is Al ion doping, Graphene and the phosphoric acid vanadium lithium of cracking carbon modification jointly and fluorinated phosphate vanadium lithium composite positive pole；
Button electricity makes and test
Composite obtained in embodiment 1～4 is all assembled into 2016 type button cells and carries out charge-discharge performance test.According to quality than active substance (positive electrode): acetylene black: binding agent (PVDF)=80:10:10, add NMP, prepare anode sizing agent, anode pole piece is obtained on even coating layer aluminium foil, employing metal lithium sheet is cathode pole piece, lithium hexafluoro phosphate is electrolyte, and Celgard2300 film is barrier film, assembles in argon glove box.Button electricity carries out multiplying power discharging test in 3.0V～4.4V voltage range.Fixing rate of charge is 0.5C, and discharge-rate is respectively 0.5C, 2.0C, 5.0C and 10.0C.
Invention described above embodiment, is not intended that limiting the scope of the present invention.Any amendment, equivalent and improvement etc. made within the spirit and principles in the present invention, within should be included in the claims of the present invention.
Claims (5)
1. phosphoric acid vanadium lithium and the preparation method of fluorinated phosphate vanadium lithium composite positive pole, comprises the following steps:
(1) carbothermic method prepares the V of carbon pre-coated metal ion mixing1-mMmPO4/ C presoma: be that 1-m:m:1:1.2～2.0 weighs vanadium source, doping metals source, phosphorus source, carbon source according to the mol ratio of V:M:P:C；After carrying out disperseing milled processed with dispersant, vacuum drying is placed under inert atmosphere and is sintered, and sintering temperature is 700～800 DEG C, and temperature retention time is 4～10h, i.e. obtains the V of carbon pre-coated metal ion mixing after Temperature fall1-mMmPO4/ C presoma；
(2) according to stoichiometric proportion V1-mMmPO4/ C:Li:F:P:C=(1+x): 3x:1-x:x:0.2～1.0 weighs the V obtained in step (1)1-mMmPO4/ C presoma, lithium source, fluorine source, phosphorus source and graphene conductive slurry, carry out ball milling dispersion process, sintering processes under inert atmosphere after vacuum drying equally in dispersant, sintering temperature is 650～750 degree, temperature retention time is 2～6h, i.e. obtains and have metal ion mixing after Temperature fall, Graphene and the phosphoric acid vanadium lithium of cracking carbon modification jointly and fluorinated phosphate vanadium lithium composite positive pole.
Preparation method the most according to claim 1, it is characterised in that described in step (1), vanadium source is V2O5、NH4VO3In one or a combination thereof, phosphorus source is the one in ammonium dihydrogen phosphate, diammonium phosphate, ammonium phosphate or a combination thereof, and described carbon source is the one in sucrose, glucose, phenolic resin, maltose, starch or a combination thereof.
Preparation method the most according to claim 1, it is characterised in that the doping metals source described in step (1) is the one in chromium, aluminum, yttrium, the nitrate of ferrum, chlorate, acetate or a combination thereof.
Preparation method the most according to claim 1, it is characterised in that described in step (2), lithium source is the one in lithium carbonate, Lithium hydrate, lithium acetate, lithium fluoride or a combination thereof；Phosphorus source is the one in ammonium dihydrogen phosphate, diammonium phosphate, ammonium phosphate or a combination thereof；Described fluorine source is lithium fluoride；Described graphene conductive slurry be weight/mass percentage composition be water system, ethanol system or the N-methyl ketopyrrolidine system dispersed paste of 2%～6%.
Preparation method the most according to claim 1, it is characterised in that described in step (1) and step (2), dispersant is ethanol, methanol or acetone solvent.
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| CN105702927B (en) * | 2016-02-15 | 2018-08-24 | 苏州大学 | A kind of compound porous anode material for lithium-ion batteries and preparation method thereof |
| CN108134077B (en) * | 2017-12-28 | 2020-08-11 | 清远佳致新材料研究院有限公司 | Preparation method of high-voltage lithium ion battery anode material with core-shell structure |
| CN108232168B (en) * | 2018-01-19 | 2020-06-09 | 河北力滔电池材料有限公司 | Modified lithium iron phosphate composite material and preparation method thereof |
| CN109935809A (en) * | 2019-02-28 | 2019-06-25 | 湖北锂诺新能源科技有限公司 | A kind of preparation method of aluminum fluoride cladding vanadium phosphate cathode material |
| JP7039524B2 (en) * | 2019-06-24 | 2022-03-22 | 本田技研工業株式会社 | Method for manufacturing positive electrode for lithium ion battery, positive electrode for lithium ion battery and positive electrode for lithium ion battery |
| CN110676455A (en) * | 2019-09-10 | 2020-01-10 | 浙江美都海创锂电科技有限公司 | Homogenizing process for nickel cobalt lithium manganate positive electrode material |
| CN111072004A (en) * | 2019-12-20 | 2020-04-28 | 大连博融新材料有限公司 | Sodium-doped lithium vanadium fluorophosphate material, and preparation method and application thereof |
| CN112018365B (en) * | 2020-09-08 | 2024-03-08 | 福建巨电新能源股份有限公司 | Aluminum-doped lithium vanadium fluorophosphate/phosphated graphene oxide composite material, preparation method thereof and application thereof in lithium ion battery |
| CN117819548A (en) * | 2024-03-01 | 2024-04-05 | 玖贰伍碳源科技（天津）有限公司 | Carbon material with parallel slit holes and preparation method and application thereof |
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