CN104600292A - Preparation method for carbon-graphene doubly modified lithium iron phosphate anode material - Google Patents
Preparation method for carbon-graphene doubly modified lithium iron phosphate anode material Download PDFInfo
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- CN104600292A CN104600292A CN201310524401.2A CN201310524401A CN104600292A CN 104600292 A CN104600292 A CN 104600292A CN 201310524401 A CN201310524401 A CN 201310524401A CN 104600292 A CN104600292 A CN 104600292A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention a discloses a preparation method for a carbon-graphene doubly modified lithium iron phosphate anode material. The method includes the two steps of: first spray drying for preparation of an inner core and second spray drying for preparation of a core-shell structure anode material. The invention adopts a liquid phase method, ensures mixing of raw materials at the molecular level, and overcomes the problem of uneven component mixing in solid phase ball-milling method. By adopting the spray drying method, the problem of uneven product components caused by gel segregation during conventional drying is also overcome. The lithium iron phosphate particles prepared by the method are modified by carbon-graphene doubly, are uniformly dispersed in a carbon conductive network, and have excellent electron conductivity and excellent electrochemical performance. The spray drying method product is spherical, has high tap density up to 1.5-2.0g/cm<3>, and good processability, thus being suitable for preparation of high power type lithium ion power batteries.
Description
Technical field
The invention belongs to anode material for lithium-ion batteries technical field, be specifically related to a kind of preparation method with the dual modification lithium iron phosphate positive material of carbon-graphite alkene of high-tap density.
Background technology
Lithium ion battery is widely applied in telecommunications fields such as mobile phone, notebook computer, video cameras and occupies leading position.Positive electrode occupies critical role in lithium ion battery, is the emphasis of lithium ion battery development.Wherein, the LiFePO4 with olivine-type structure is to have that discharge platform is stable, cycle performance is good, fail safe is high and the feature such as low price and be subject to extensive concern.But the shortcoming that this material electronics conductivity is low and lithium ion diffusion velocity is slow have impact on its chemical property greatly.Therefore, conventionally control the bulk phase-doped and finishing of crystallite dimension, ion etc. and solve this problem.At lithium iron phosphate particles coated with carbon, the conductivity between particle can not only be strengthened, reduce polarization, and can particle growth be hindered, micronized particles.But LiFePO4 coated with carbon, the chemical property being conducive to material improves, and but significantly reduce the tap density of material, processing characteristics is poor.
Graphene is a kind of by sp
2the carbon atom that hybrid form exists is tightly packed forms the new carbon with two alveolate textures, has excellent conductivity, structural stability and higher specific area, is extensively studied in field of lithium ion battery.Adopt Graphene to improve LiFePO4 also to have been reported, as application number 201010146161.3 and 201110083171.1 adopts LiFePO4 and Graphene to be raw material, physical mixed prepares LiFePO4/graphene composite material, but this simple physical mixed is difficult to ensure Graphene being uniformly distributed between lithium iron phosphate particles.Application number 200910155316.7 and J.Mater.Chem.21 (2011) 3353-3358 with nano-scale lithium iron phosphate and graphene oxide for raw material, spray drying process is adopted to build a kind of micron ball particle of graphene-coated lithium iron phosphate, but employing nano-scale lithium iron phosphate is raw material, the aggregate of nano-grade lithium iron phosphate is unavoidably there is in raw material, Graphene only can form good conductive network on aggregate surface, and can not improve the conductivity between nano particle.
Summary of the invention
The object of this invention is to provide a kind of preparation method with the dual modification lithium iron phosphate positive material of carbon-graphite alkene of high-tap density.
To achieve these goals, technical scheme of the present invention is, the preparation method of the dual modification lithium iron phosphate positive material of a kind of carbon-graphite alkene, specifically comprises the following steps:
A. a spraying dry prepares kernel: take source of iron, phosphorus source and lithium source by the stoichiometric proportion of LiFePO4, be placed in graphene oxide dispersion, graphene oxide amount is 0.5% ~ 10% of LiFePO4 quality, adding citric acid is complexant, mix, adjust ph is between 2 ~ 6, at 100 ~ 250 DEG C after spraying dry in non-oxidizing atmosphere 550 ~ 900 DEG C sintering 1 ~ 20 hour, cooling porphyrize, obtains the LiFePO4 kernel of graphene modified;
B. two spraying dry prepare the positive electrode of nucleocapsid structure: take the LiFePO4 kernel that a certain amount of step a is obtained, take water-soluble organic carbon source, and it takes by carbonaceous amount contained by it is that 0.5 ~ 20% of nuclear mass in LiFePO4 calculates; Carbon source is dissolved in deionized water, add the LiFePO4 inner nuclear material of the graphene modified that step a obtains, dispersed, after 100 ~ 250 DEG C of spraying dry in non-oxidizing atmosphere 400 ~ 850 DEG C of sintering 30 ~ 300 minutes, obtain the LiFePO 4 material of the dual modification of carbon-graphite alkene with stove cooling.
Described lithium source is the one in lithium carbonate, lithium hydroxide, lithium acetate, lithium nitrate and lithium oxalate.
Described source of iron is the one in di-iron trioxide, ferric phosphate, ferrous oxalate, ferrous acetate and ferric nitrate.
Described phosphorus source is the one in triammonium phosphate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, lithium dihydrogen phosphate and phosphoric acid.
Described carbon source is one or more in glucose, polyethylene glycol, sucrose, fructose and salicylic acid.
Described non-oxidizing atmosphere is argon gas atmosphere or argon hydrogen mixed atmosphere.
The present invention adopts liquid phase method can ensure the mixing of raw material at molecular level, overcomes composition in solid-phase ball milling method and mixes uneven problem; The product component problem of non-uniform that when adopting spray drying process to also overcome conventional drying, gel segregation causes.Lithium iron phosphate particles prepared by the method is by the dual modification of carbon-graphite alkene, and LiFePO4 uniform particle is dispersed in carbonaceous conductive network, has excellent electron conduction and excellent chemical property; Spray drying process product is spherical, has higher tap density, and tap density can reach 1.5 ~ 2.0g/cm
3, processing characteristics is good, is applicable to prepare high power type lithium ion electrokinetic cell.
Accompanying drawing explanation
Fig. 1 is the XRD figure preparing sample according to embodiment 1 method.
Fig. 2 is the SEM figure preparing sample according to embodiment 1 method.
Fig. 3 is the charging and discharging curve under different multiplying preparing sample according to embodiment 1 method.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described further.
Embodiment 1:
A. a spraying dry prepares inner nuclear material: with lithium hydroxide, ferrous oxalate, ammonium dihydrogen phosphate for raw material, prepare burden according to stoichiometric proportion, be placed in graphene oxide dispersion (wherein graphene oxide amount is 3% of LiFePO4 quality), adding citric acid is complexant (its mole is 1 times of metal ion integral molar quantity), adjust ph is 4, stir after 5 hours, spraying dry at 120 DEG C, then gained powder is calcined 12 hours in 700 DEG C in argon gas atmosphere, cooling porphyrize, obtains the LiFePO4 inner nuclear material of graphene modified;
B. two spraying dry prepare the positive electrode of nucleocapsid structure: be dissolved in deionized water by appropriate glucose (quality of its carbon containing is 5% of inner nuclear material quality), add inner nuclear material, 120 DEG C of spraying dry are carried out after ultrasonic disperse is even, gained powder in argon gas 850 DEG C calcining 30 minutes, obtain the lithium iron phosphate positive material of the dual modification of carbon-graphite alkene with stove cooling, its tap density reaches 1.94g/cm
3.
Embodiment 2:
A. a spraying dry prepares inner nuclear material: with lithium acetate, ferric phosphate, diammonium hydrogen phosphate for raw material, prepare burden according to stoichiometric proportion, be placed in graphene oxide dispersion (wherein include 1% that graphene oxide amount is LiFePO4 quality), adding citric acid is complexant (its mole is 1 times of metal ion integral molar quantity), adjust ph is 2, stir after 3 hours, spraying dry at 100 DEG C, then gained powder is calcined 15 hours in 680 DEG C in argon gas atmosphere, cooling porphyrize, obtains the LiFePO4 inner nuclear material of graphene modified.
B. two spraying dry prepare the positive electrode of nucleocapsid structure: be dissolved in deionized water by appropriate polyethylene glycol (quality of its carbon containing is 10% of inner nuclear material quality), add inner nuclear material, 100 DEG C of spraying dry are carried out after ultrasonic disperse is even, gained powder in argon gas 800 DEG C calcining 60 minutes, obtain the lithium iron phosphate positive material of the dual modification of carbon-graphite alkene with stove cooling, its tap density reaches 1.75g/cm
3.
Embodiment 3:
A. a spraying dry prepares inner nuclear material: with lithium nitrate, ferrous acetate, lithium dihydrogen phosphate for raw material, prepare burden according to stoichiometric proportion, be placed in graphene oxide dispersion (wherein include 7% that graphene oxide amount is LiFePO4 quality), adding citric acid is complexant (its mole is 1 times of metal ion integral molar quantity), adjust ph is 4, stir after 5 hours, spraying dry at 150 DEG C, then gained powder is calcined 10 hours in 750 DEG C in argon gas atmosphere, cooling porphyrize, obtains the LiFePO4 inner nuclear material of graphene modified.
B. two spraying dry prepare the positive electrode of nucleocapsid structure: be dissolved in deionized water by appropriate bigcatkin willow sugar (quality of its carbon containing is 8% of inner nuclear material quality), add inner nuclear material, 150 DEG C of spraying dry are carried out after ultrasonic disperse is even, gained powder in argon gas 500 DEG C calcining 300 minutes, obtain the lithium iron phosphate positive material of the dual modification of carbon-graphite alkene with stove cooling, its tap density reaches 1.71g/cm
3.
Embodiment 4:
A. a spraying dry prepares inner nuclear material: with lithium oxalate, ferric nitrate, triammonium phosphate for raw material, prepare burden according to stoichiometric proportion, be placed in graphene oxide dispersion (wherein include 10% that graphene oxide amount is LiFePO4 quality), adding citric acid is complexant (its mole is 1 times of metal ion integral molar quantity), adjust ph is 6, stir after 2 hours, spraying dry at 250 DEG C, then gained powder is calcined 3 hours in 900 DEG C in argon gas atmosphere, cooling porphyrize, obtains the LiFePO4 inner nuclear material of graphene modified.
B. two spraying dry prepare the positive electrode of nucleocapsid structure: be dissolved in deionized water by appropriate fructose (quality of its carbon containing is 20% of inner nuclear material quality), add inner nuclear material, 250 DEG C of spraying dry are carried out after ultrasonic disperse is even, gained powder in argon gas 600 DEG C calcining 240 minutes, obtain the lithium iron phosphate positive material of the dual modification of carbon-graphite alkene with stove cooling, its tap density reaches 1.52g/cm3.
Embodiment 5:
A. a spraying dry prepares inner nuclear material: with lithium carbonate, di-iron trioxide, phosphoric acid for raw material, prepare burden according to stoichiometric proportion, be placed in graphene oxide dispersion (wherein graphene oxide amount is 5% of LiFePO4 quality), adding citric acid is complexant (its mole is 1 times of metal ion integral molar quantity), adjust ph is 3, stir 5 hours, spraying dry at 200 DEG C, then gained powder is calcined 6 hours in 800 DEG C in argon gas atmosphere, cooling porphyrize, obtains the LiFePO4 inner nuclear material of graphene modified.
B. two spraying dry prepare the positive electrode of nucleocapsid structure: be dissolved in deionized water by suitable amount of sucrose (quality of its carbon containing is 15% of inner nuclear material quality), add inner nuclear material, 200 DEG C of spraying dry are carried out after ultrasonic disperse is even, gained powder in argon gas 750 DEG C calcining 180 minutes, obtain the lithium iron phosphate positive material of the dual modification of carbon-graphite alkene with stove cooling, its tap density reaches 1.66g/cm
3.
The dual modification lithium iron phosphate positive material of the carbon-graphite alkene with high-tap density utilizing said method to obtain, its positive electrode has coreshell type structure, and kernel is the lithium iron phosphate particles of graphene modified, and shell is amorphous carbon.
Above embodiments of the invention are explained in detail, above-mentioned execution mode is only optimum embodiment of the present invention, but the present invention is not limited to above-described embodiment, in the ken that those of ordinary skill in the art possess, various change can also be made under the prerequisite not departing from present inventive concept.
Claims (6)
1. a preparation method for the dual modification lithium iron phosphate positive material of carbon-graphite alkene, is characterized in that comprising the following steps:
A. a spraying dry prepares kernel: take source of iron, phosphorus source and lithium source by the stoichiometric proportion of LiFePO4, be placed in graphene oxide dispersion, graphene oxide amount is 0.5% ~ 10% of LiFePO4 quality, adding citric acid is complexant, mix, adjust ph is between 2 ~ 6, at 100 ~ 250 DEG C after spraying dry in non-oxidizing atmosphere 550 ~ 900 DEG C sintering 1 ~ 20 hour, cooling porphyrize, obtains the LiFePO4 kernel of graphene modified;
B. two spraying dry prepare the positive electrode of nucleocapsid structure: take the LiFePO4 kernel that a certain amount of step a is obtained, take water-soluble organic carbon source, and it takes by carbonaceous amount contained by it is that 0.5 ~ 20% of nuclear mass in LiFePO4 calculates; Carbon source is dissolved in deionized water, add the LiFePO4 inner nuclear material of the graphene modified that step a obtains, dispersed, after 100 ~ 250 DEG C of spraying dry in non-oxidizing atmosphere 400 ~ 850 DEG C of sintering 30 ~ 300 minutes, obtain the LiFePO 4 material of the dual modification of carbon-graphite alkene with stove cooling.
2. the preparation method of the dual modification lithium iron phosphate positive material of a kind of carbon-graphite alkene as claimed in claim 1, is characterized in that lithium source is the one in lithium carbonate, lithium hydroxide, lithium acetate, lithium nitrate and lithium oxalate.
3. the preparation method of the dual modification lithium iron phosphate positive material of a kind of carbon-graphite alkene as claimed in claim 1, is characterized in that source of iron is the one in di-iron trioxide, ferric phosphate, ferrous oxalate, ferrous acetate and ferric nitrate.
4. the preparation method of the dual modification lithium iron phosphate positive material of a kind of carbon-graphite alkene as claimed in claim 1, is characterized in that phosphorus source is the one in triammonium phosphate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, lithium dihydrogen phosphate and phosphoric acid.
5. the preparation method of the dual modification lithium iron phosphate positive material of a kind of carbon-graphite alkene as claimed in claim 1, the carbon source that it is characterized in that is one or more in glucose, polyethylene glycol, sucrose, fructose and salicylic acid.
6. the preparation method of the dual modification lithium iron phosphate positive material of a kind of carbon-graphite alkene as claimed in claim 1, the non-oxidizing atmosphere that it is characterized in that is argon gas atmosphere or argon hydrogen mixed atmosphere.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104868121A (en) * | 2015-05-07 | 2015-08-26 | 天津大学 | Graphene-and-carbon-coated lithium iron phosphate lithium ion battery positive electrode material and production method thereof |
| CN105047919A (en) * | 2015-06-25 | 2015-11-11 | 中国航空工业集团公司北京航空材料研究院 | Preparation method for cathode material of lithium iron phosphate battery |
| CN105322145A (en) * | 2015-09-25 | 2016-02-10 | 复旦大学 | Lithium ferric manganese phosphate/graphene/ carbon composite material and preparation method and application |
| CN106784724A (en) * | 2017-01-12 | 2017-05-31 | 吉林大学 | A kind of LiFePO4The solvent heat assistant preparation method of@C/rGO multistage composite microballoons |
| CN107316976A (en) * | 2017-05-27 | 2017-11-03 | 广东烛光新能源科技有限公司 | A kind of anode material for lithium-ion batteries and preparation method thereof |
| CN107742714A (en) * | 2017-10-31 | 2018-02-27 | 湖南国盛石墨科技有限公司 | Preparation method for LiFePO4/expansion micro crystal graphite/carbon composite of lithium ion battery |
| CN109686962A (en) * | 2019-01-21 | 2019-04-26 | 新奥石墨烯技术有限公司 | Prepare method, the anode, battery of iron phosphate compound anode material of lithium |
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| CN102299326A (en) * | 2011-08-04 | 2011-12-28 | 浙江工业大学 | Graphene modified lithium iron phosphate/carbon composite material and its application |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104868121A (en) * | 2015-05-07 | 2015-08-26 | 天津大学 | Graphene-and-carbon-coated lithium iron phosphate lithium ion battery positive electrode material and production method thereof |
| CN105047919A (en) * | 2015-06-25 | 2015-11-11 | 中国航空工业集团公司北京航空材料研究院 | Preparation method for cathode material of lithium iron phosphate battery |
| CN105047919B (en) * | 2015-06-25 | 2020-08-04 | 中国航空工业集团公司北京航空材料研究院 | Preparation method of lithium iron phosphate battery positive electrode material |
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| CN106784724A (en) * | 2017-01-12 | 2017-05-31 | 吉林大学 | A kind of LiFePO4The solvent heat assistant preparation method of@C/rGO multistage composite microballoons |
| CN106784724B (en) * | 2017-01-12 | 2020-08-07 | 吉林大学 | L iFePO4Solvothermal assisted preparation method of @ C/rGO multistage composite microspheres |
| CN107316976A (en) * | 2017-05-27 | 2017-11-03 | 广东烛光新能源科技有限公司 | A kind of anode material for lithium-ion batteries and preparation method thereof |
| CN107316976B (en) * | 2017-05-27 | 2019-11-05 | 广东烛光新能源科技有限公司 | A kind of anode material for lithium-ion batteries and preparation method thereof |
| CN107742714A (en) * | 2017-10-31 | 2018-02-27 | 湖南国盛石墨科技有限公司 | Preparation method for LiFePO4/expansion micro crystal graphite/carbon composite of lithium ion battery |
| CN109686962A (en) * | 2019-01-21 | 2019-04-26 | 新奥石墨烯技术有限公司 | Prepare method, the anode, battery of iron phosphate compound anode material of lithium |
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