CN104577120A - Preparation method of lithium vanadium phosphate and fluorination lithium vanadium phosphate composite positive pole material - Google Patents
Preparation method of lithium vanadium phosphate and fluorination lithium vanadium phosphate composite positive pole material Download PDFInfo
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- CN104577120A CN104577120A CN201510001457.9A CN201510001457A CN104577120A CN 104577120 A CN104577120 A CN 104577120A CN 201510001457 A CN201510001457 A CN 201510001457A CN 104577120 A CN104577120 A CN 104577120A
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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
- H01M4/5805—Phosphides
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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
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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
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- 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
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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Abstract
The invention discloses a preparation method for a lithium vanadium phosphate and fluorination lithium vanadium phosphate composite positive pole material. The preparation method comprises the following steps: (1) preparing a V(1-m)MmPO4/C precursor pre-coated with carbon and mingled with metal ions by a carbon thermal reduction method, wherein the M is Cr<3+>, Al<3+>, Y<3+> and Fe<3+>; (2) performing mixed dispersion on the obtained V(1-m)MmPO4/C precursor and dispersion serosity in which a lithium source, a fluorine source, a phosphorus source and grapheme (FLG) are in a stoichiometric proportion under an alcohol system so as to obtain mixed pulp; (3) after performing drying treatment on the obtained mixed pulp, performing high-temperature sintering treatment under the protection of inert gas so as to obtain the lithium vanadium phosphate and fluorination lithium vanadium phosphate composite positive pole material mingled with the metal ions and jointly modified by the graphene and cracking carbon. According to the invention, the technology is simple, and the obtained lithium vanadium phosphate and fluorination lithium vanadium phosphate composite positive pole material has excellent multiplying power, an excellent cycle performance and a wide application prospect in the field of lithium ion batteries.
Description
Technical field
The present invention relates to power lithium-ion battery, energy storage lithium ion battery technical field, particularly relate to the preparation method of a kind of phosphoric acid vanadium lithium and 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 brings factor leading to social instability safely all to global new forms of energy.Therefore clean energy resource exploitation 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 widely used as a kind of energy storage instrument and has studied.The development of the development of lithium ion battery mainly positive electrode, current lithium ion anode material has respective defect to need to overcome further.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 fail safe.Wherein LiFePO4 (LiFePO
4) be current widely used positive electrode, but its operating voltage 3.5V is lower, by contrast, and novel phosphate material phosphoric acid vanadium lithium (Li
3v
2(PO
4)) 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 (LiVPO
4f) due to the electronegativity that fluorine ion is strong, change the energy level that metal oxidation reduction electricity is right, this material is to Li
+/ Li current potential is higher is 4.2V.These two kinds poly-female lithium ion battery materials are the same with LiFePO4, and the native electronic conductivity of phase pure material is very low, 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 modification work.Zhang Bao etc. (Nonferrous Mel. Soc. China, 2010 (20): 619-623) are with Al (NO
3)
3for adulterating to phosphoric acid vanadium lithium in aluminium source, realize lithium vanadium phosphate material specific capacity, the reversible reaction of electrode, electron conductivity.Ren Manman etc. (Journal of Power Source 2006 (162): 1357-1362) are carbon source with glucose, carry out modification, and synthesized the Li with nucleocapsid structure to phosphoric acid vanadium lithium
3v
2(PO
4)
3/ C compound, 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 LiVPO
4f adulterates, and the discharge and recharge polarization of electrode material diminishes, and invertibity increases, and cyclicity gets a promotion.Although about Li
3v
2(PO
4)
3and LiVPO
4f electrode material study on the modification is separately more, and comparatively single method of modifying could not reach and effectively improve Li
3v
2(PO
4)
3and LiVPO
4the conductivity of F electrode material, and have no at present about Li
3v
2(PO
4)
3and LiVPO
4the correlative study of F combination electrode material.
Summary of the invention
The technical problem to be solved in the present invention is to provide the preparation method of a kind of phosphoric acid vanadium lithium and fluorinated phosphate vanadium lithium composite positive pole.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is, the preparation method of phosphoric acid vanadium lithium and fluorinated phosphate vanadium lithium composite positive pole, comprises the following steps:
(1) carbothermic method prepares the V of carbon pre-coated metal ion mixing
1-mm
mpO
4/ C presoma: be that 1-m:m:1:1.2 ~ 2.0 take vanadium source, doping metals source, phosphorus source, carbon source according to the mol ratio of V:M:P:C; After carrying out dispersion grinding process with dispersant, vacuumize carries out sintering processes under being placed on inert atmosphere, and sintering temperature is 700 ~ 800 DEG C, and temperature retention time is 4 ~ 10h, namely obtains the V of carbon pre-coated metal ion mixing after Temperature fall
1-mm
mpO
4/ C presoma;
(2) according to stoichiometric proportion V
1-mm
mpO
4/ C:Li:F:P:C=(1+x): 3x:1-x:x:0.2 ~ 1.0 take the V obtained in step (1)
1-mm
mpO
4/ C presoma, lithium source, fluorine source, phosphorus source and graphene conductive slurry, carry out ball milling dispersion treatment equally in dispersant, sintering processes under inert atmosphere after vacuumize, sintering temperature is 650 ~ 750 degree, temperature retention time is 2 ~ 6h, namely obtains and have metal ion mixing, the phosphoric acid vanadium lithium of Graphene and the common modification of cracking carbon and fluorinated phosphate vanadium lithium composite positive pole after Temperature fall;
As preferably, described in step (1), vanadium source is V
2o
5, NH
4vO
3in one or its combination, described phosphorus source is one in ammonium dihydrogen phosphate, diammonium hydrogen phosphate, ammonium phosphate or its combination, and described carbon source is one in sucrose, glucose, phenolic resins, maltose, starch or its combination.
As preferably, the doping metals source described in step (1) is one in chromium, aluminium, yttrium, the nitrate of iron, chlorate, acetate or its combination.
As preferably, lithium source described in step (2) is one in lithium carbonate, lithium hydroxide, lithium acetate, lithium fluoride or its combination; Described phosphorus source is one in ammonium dihydrogen phosphate, diammonium hydrogen phosphate, ammonium phosphate or its combination; Described fluorine source is lithium fluoride; Described graphene conductive slurry to be mass percentage be 2% ~ 6% water system, alcohol system or nitrogen methyl pyrrolidone system dispersed paste.
As preferably, described in step (1) and step (2), dispersant is alcohol, methyl alcohol or acetone solvent.
The structure of the phosphoric acid vanadium lithium that the present invention prepares and fluorinated phosphate vanadium lithium composite positive pole is x (Li
3v
2 (1-m)m
2m(PO
4)
3(1-x) (LiV
1-mm
mpO
4f), wherein x=0.1 ~ 0.9, m=0.01 ~ 0.15, M is the metal ion of doping, there is the homogeneous conductive network be made up of carbon coating layer and Graphene between the crystal grain surface area crystal grain of material.
Above-mentioned doped metal ion M is Cr
3+, Al
3+, Y
3+, Fe
3+.
The invention has the beneficial effects as follows:
This composite material combines Li
3v
2(PO
4)
3and LiVPO
4the advantage of F bi-material.The method is prepared in the process of vanadium phosphate compounds in carbon thermal reduction and is introduced doped metal ion and organic carbon source, the V obtained
1-xmPO
4/ C presoma, carry out mixing with the lithium source of stoichiometric proportion, fluorine source and graphene dispersion slurries under alcohol system and disperse rear sintering, acquisition has metal ion mixing, the phosphoric acid vanadium lithium of Graphene and the common modification of cracking carbon and fluorinated phosphate vanadium lithium composite positive pole.The method ion doping is carried out to composite material precursor vanadium phosphate compounds and carbon coated, the Effective Doping of doped metal ion vanadium position in vanadium phosphate compounds lattice can be guaranteed, and due to the pre-coated process to vanadium phosphate compounds, can realize in sintering process, effective suppression that crystal grain is grown up.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Fig. 1 be the embodiment of the present invention 2 obtain and there is iron ion doping, the phosphoric acid vanadium lithium of Graphene and the common modification of cracking carbon and the X-ray diffractogram of fluorinated phosphate vanadium lithium composite positive pole.
Fig. 2 be the embodiment of the present invention 2 obtain and there is iron ion doping, the phosphoric acid vanadium lithium of Graphene and the common modification of cracking carbon and the circulation performance of fluorinated phosphate vanadium lithium composite positive pole.
Embodiment
Embodiment 1
(1) be that 0.95:0.05:1:2.0 takes vanadic oxide, aluminum nitrate, ammonium dihydrogen phosphate, sucrose according to the mol ratio of V:Al:P:C.After carrying out dispersion grinding process with alcohol, vacuumize carries out sintering processes under being placed on nitrogen atmosphere, and sintering temperature is 700 DEG C, and temperature retention time is 10h, namely obtains carbon pre-coated after Temperature fall, the V of Al ion doping
0.95aL
0.05pO
4/ C presoma;
(2) according to stoichiometric proportion V
0.95m
0.05pO
4/ C:Li:F:P:C=1.2:0.6:0.8:0.2:0.2 takes the V obtained in step (1)
0.95aL
0.05pO
4/ C presoma, lithium carbonate, LiF, NH
4h
2pO
4and graphene conductive slurry, ball milling dispersion treatment is carried out equally in alcohol, sintering processes under nitrogen atmosphere after vacuumize, sintering temperature is 650 degree, temperature retention time is 6h, namely obtain after Temperature fall and there is Al-doping, the phosphoric acid vanadium lithium of Graphene and the common modification of cracking carbon and fluorinated phosphate vanadium lithium composite positive pole;
Embodiment 2
(1) be that 0.85:0.15:1:1.5 takes ammonium metavanadate, ferric nitrate, ammonium dihydrogen phosphate, phenolic resins according to the mol ratio of V:Fe:P:C.After carrying out dispersion grinding process with alcohol, vacuumize carries out sintering processes under being placed on nitrogen atmosphere, and sintering temperature is 750 DEG C, and temperature retention time is 6h, namely obtains carbon pre-coated after Temperature fall, the V of Fe ion doping
0.85fe
0.15pO
4/ C presoma;
(2) according to stoichiometric proportion V
0.85fe
0.15pO
4/ C:Li:F:P:C=1.4:1.2:0.6:0.4:0.8 takes the V obtained in step (1)
0.85fe
0.15pO
4/ C presoma, lithium hydroxide, LiF, NH
4h
2pO
4and graphene conductive slurry, ball milling dispersion treatment is carried out equally in alcohol, sintering processes under nitrogen atmosphere after vacuumize, sintering temperature is 700 degree, temperature retention time is 4h, namely obtain after Temperature fall and there is iron ion doping, the phosphoric acid vanadium lithium of Graphene and the common modification of cracking carbon and fluorinated phosphate vanadium lithium composite positive pole;
Embodiment 3
(1) be that 0.9:0.1:1:1.2 takes ammonium metavanadate, chromic nitrate, ammonium dihydrogen phosphate, glucose according to the mol ratio of V:Cr:P:C.After carrying out dispersion grinding process with methyl alcohol, vacuumize carries out sintering processes under being placed on nitrogen atmosphere, and sintering temperature is 800 DEG C, and temperature retention time is 4h, namely obtains carbon pre-coated after Temperature fall, the V of Cr ion doping
0.9cr
0.1pO
4/ C presoma;
(2) according to stoichiometric proportion V
0.9cr
0.1pO
4/ C:Li:F:P:C=1.6:1.8:0.4:0.6:1.0 takes the V obtained in step (1)
0.9cr
0.1pO
4/ C presoma, lithium acetate, LiF, NH
4h
2pO
4and graphene conductive slurry, ball milling dispersion treatment is carried out equally in methyl alcohol, sintering processes under nitrogen atmosphere after vacuumize, sintering temperature is 750 degree, temperature retention time is 2h, namely obtain after Temperature fall and there is Cr ion doping, the phosphoric acid vanadium lithium of Graphene and the common modification of cracking carbon and fluorinated phosphate vanadium lithium composite positive pole;
Embodiment 4
(1) be that 0.98:0.02:1:1.4 takes ammonium metavanadate, aluminum acetate, ammonium dihydrogen phosphate, glucose according to the mol ratio of V:Al:P:C.After carrying out dispersion grinding process with acetone, vacuumize carries out sintering processes under being placed on nitrogen atmosphere, and sintering temperature is 700 DEG C, and temperature retention time is 4h, namely obtains carbon pre-coated after Temperature fall, the V of Al ion doping
0.98al
0.01pO
4/ C presoma;
(2) according to stoichiometric proportion V
0.98al
0.02pO
4/ C:Li:F:P:C=1.4:1.2:0.6:0.4:0.8 takes the V obtained in step (1)
0.98al
0.02pO
4/ C presoma, lithium acetate, LiF, (NH
4)
2hPO
4and graphene conductive slurry, ball milling dispersion treatment is carried out equally in acetone, sintering processes under nitrogen atmosphere after vacuumize, sintering temperature is 700 degree, temperature retention time is 4h, namely obtain after Temperature fall and there is Al ion doping, the phosphoric acid vanadium lithium of Graphene and the common modification of cracking carbon and fluorinated phosphate vanadium lithium composite positive pole;
Button electricity makes and test
The composite material 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 material (positive electrode): acetylene black: binding agent (PVDF)=80:10:10, add NMP, prepare anode sizing agent, even coating layer aluminium foil obtains anode pole piece, employing metal lithium sheet is cathode pole piece, lithium hexafluoro phosphate is electrolyte, and Celgard2300 film is barrier film, assembles in argon gas 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.
Above-described embodiment of the present invention, does not form limiting the scope of the present invention.Any amendment done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within claims of the present invention.
Claims (5)
1. the preparation method of phosphoric acid vanadium lithium and fluorinated phosphate vanadium lithium composite positive pole, comprises the following steps:
(1) carbothermic method prepares the V of carbon pre-coated metal ion mixing
1-mm
mpO
4/ C presoma: be that 1-m:m:1:1.2 ~ 2.0 take vanadium source, doping metals source, phosphorus source, carbon source according to the mol ratio of V:M:P:C; After carrying out dispersion grinding process with dispersant, vacuumize carries out sintering processes under being placed on inert atmosphere, and sintering temperature is 700 ~ 800 DEG C, and temperature retention time is 4 ~ 10h, namely obtains the V of carbon pre-coated metal ion mixing after Temperature fall
1-mm
mpO
4/ C presoma;
(2) according to stoichiometric proportion V
1-mm
mpO
4/ C:Li:F:P:C=(1+x): 3x:1-x:x:0.2 ~ 1.0 take the V obtained in step (1)
1-mm
mpO
4/ C presoma, lithium source, fluorine source, phosphorus source and graphene conductive slurry, carry out ball milling dispersion treatment equally in dispersant, sintering processes under inert atmosphere after vacuumize, sintering temperature is 650 ~ 750 degree, temperature retention time is 2 ~ 6h, namely obtains and have metal ion mixing, the phosphoric acid vanadium lithium of Graphene and the common modification of cracking carbon and fluorinated phosphate vanadium lithium composite positive pole after Temperature fall.
2. preparation method according to claim 1, is characterized in that, described in step (1), vanadium source is V
2o
5, NH
4vO
3in one or its combination, described phosphorus source is one in ammonium dihydrogen phosphate, diammonium hydrogen phosphate, ammonium phosphate or its combination, and described carbon source is one in sucrose, glucose, phenolic resins, maltose, starch or its combination.
3. preparation method according to claim 1, is characterized in that, the doping metals source described in step (1) is one in chromium, aluminium, yttrium, the nitrate of iron, chlorate, acetate or its combination.
4. preparation method according to claim 1, is characterized in that, lithium source described in step (2) is one in lithium carbonate, lithium hydroxide, lithium acetate, lithium fluoride or its combination; Described phosphorus source is one in ammonium dihydrogen phosphate, diammonium hydrogen phosphate, ammonium phosphate or its combination; Described fluorine source is lithium fluoride; Described graphene conductive slurry to be mass percentage be 2% ~ 6% water system, alcohol system or nitrogen methyl pyrrolidone system dispersed paste.
5. preparation method according to claim 1, is characterized in that, described in step (1) and step (2), dispersant is alcohol, methyl alcohol or acetone solvent.
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| CN105702927A (en) * | 2016-02-15 | 2016-06-22 | 苏州大学 | Composite porous cathode material for lithium-ion battery and preparation method of composite porous cathode material |
| CN108134077A (en) * | 2017-12-28 | 2018-06-08 | 清远佳致新材料研究院有限公司 | A kind of anode material for high-voltage lithium ion of nucleocapsid and preparation method thereof |
| CN108232168A (en) * | 2018-01-19 | 2018-06-29 | 河北力滔电池材料有限公司 | Modified phosphate iron lithium composite material and preparation method |
| 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 |
| 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 |
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| 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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