CN105702930A - Preparation and application for Fe3O4-Cr2O3-graphene composite anode material of lithium ion battery - Google Patents
Preparation and application for Fe3O4-Cr2O3-graphene composite anode material of lithium ion battery Download PDFInfo
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- 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
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- H—ELECTRICITY
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- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H—ELECTRICITY
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
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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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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 discloses preparation and application for a Fe3O4-Cr2O3-graphene composite anode material of a lithium ion battery. The anode material is prepared by a hydrothermal method. The Fe3O4-Cr2O3-graphene composite anode material provided by the invention has excellent charging/discharging cycle performance, such performance can be related to the weight part ratio of ferric trichloride hexahydrate and potassium dichromate in the preparation method, and the performance is best when the weight part ratio of the ferric trichloride hexahydrate to the potassium dichromate is (4-6):1.
Description
Technical field
The invention belongs to energy field, relate to graphene battery material, be specifically related to a kind of lithium ion battery Fe3O4-Cr2O3The preparation of-Graphene composite anode materials and application。
Background technology
Cr2O3And Fe3O4Being respectively provided with high power capacity as lithium cell cathode material to be close to and be 2～3 times of business carbon negative pole material and obtain and pay close attention to widely, both materials also have a desirable substitution material that the advantages such as low, the environmental friendliness of cost were once considered as carbon, but Cr2O3Being easily generated dendrite in charge and discharge process and cause short circuit, safety issue constrains its application；Fe3O4Easy efflorescence in charge and discharge process and the reversible specific capacity rapid decrease that causes。In addition, Fe3O4Owing to by magnetic dipole graviational interaction, being prone between particle reunite, and chemical stability be not high, it is difficult to directly applying。Multimetal oxide is carried out recombination energy and effectively overcomes the defect between different metal-oxides by bibliographical information, it is thus achieved that the li-ion electrode materials of electrochemical performance。Therefore comprehensive Fe3O4And Cr2O3Two kinds of materials interact, bring it about positive cooperative effect, as some composites, there is many advantages in recent years in conjunction with Graphene, such as in energy storage, its huge specific surface area and good honeycomb mesoporous structure (> 1nm) are conducive to the abundant moistening Graphene body of solion in electrochemistry cyclic process, it is adsorbed on its surface to greatest extent, promotes energy storage density。The appearing as design and construct the material with new structure and special energy storage technology and provide probability and new thinking of Graphene and derivant thereof。
The electric conductivity of Graphene excellence and electron-transporting can significantly improve the electric conductivity of overall complex, are conducive to charge transfer in electrode/electrolyte, reduce solution resistance and charge transfer resistance；The specific surface area that Graphene is huge is conducive to controlling particle size and the dispersion of material, it is provided that better avtive spot, is conducive to electrolyte and electrode to be fully contacted；The good flexility of Graphene makes electrode material volumetric expansion/blockage effect in charge and discharge process be cushioned, thus improving the cyclicity of electrode。
Summary of the invention
It is an object of the invention to a kind of lithium ion battery Fe3O4-Cr2O3The preparation of-Graphene composite anode materials and application, for the battery preparing charging and discharging capacity height, good cycle。
The above-mentioned purpose of the present invention is achieved by the techniques below scheme:
A kind of lithium ion battery Fe3O4-Cr2O3The preparation method of-Graphene composite anode materials, including being made by step:
Step S1, weighs 70～90mg graphene oxide and 0.8～1.2g Polyethylene Glycol PEG-4000 puts in the beaker equipped with 80mL ethylene glycol, ultrasonic agitation 3～5h；
Step S2, adds the mixture of 0.5g Iron(III) chloride hexahydrate and potassium dichromate, adds 4.0g anhydrous sodium acetate, after ultrasonic agitation is uniform, regulates pH=10 with ammonia；The weight ratio of described Iron(III) chloride hexahydrate and potassium dichromate is 4～6:1；
Step S3, is placed in hydrothermal reaction kettle, 180～220 DEG C of reaction 8～12h；
Step S4, is cooled to room temperature, is sequentially added into deionized water and washes of absolute alcohol, centrifugation, and end product is placed in baking oven drying。
Further, described lithium ion battery Fe3O4-Cr2O3In the preparation method step S2 of-Graphene composite anode materials, the weight ratio of described Iron(III) chloride hexahydrate and potassium dichromate is 5:1。
Further, described lithium ion battery Fe3O4-Cr2O3The preparation process S1 of-Graphene composite anode materials is: weigh 80mg graphene oxide and 1g Polyethylene Glycol PEG-4000 puts in the beaker equipped with 80mL ethylene glycol, ultrasonic agitation 4h；
Further, described lithium ion battery Fe3O4-Cr2O3The preparation method step S3 of-Graphene composite anode materials is: be placed in hydrothermal reaction kettle, 200 DEG C of reaction 10h。
Above-mentioned Fe3O4-Cr2O3The application in the preparing lithium ion battery of-Graphene composite anode materials。
Advantages of the present invention:
Fe provided by the invention3O4-Cr2O3-graphene composite material has the charge-discharge performance of excellence, this performance is likely to relevant with the weight ratio of Iron(III) chloride hexahydrate in preparation method and potassium dichromate, when the weight ratio of Iron(III) chloride hexahydrate and potassium dichromate is between 4～6:1, performance is best。
Detailed description of the invention
Further illustrate the essentiality content of the present invention below in conjunction with embodiment, but do not limit scope with this。Although the present invention being explained in detail with reference to preferred embodiment, it will be understood by those within the art that, it is possible to technical scheme is modified or equivalent replacement, without deviating from the spirit and scope of technical solution of the present invention。
In the present invention, graphene oxide adopts the Hummers method of improvement to prepare, referring to document Hummers, W.S., Jr.；Offeman, R.E.J.Am.Chem.Soc.1958,80,1339。
Embodiment 1:Fe
3
O
4
-Cr
2
O
3
The preparation of-Graphene composite anode materials
Step S1, weighs 80mg graphene oxide and 1g Polyethylene Glycol PEG-4000 puts in the beaker equipped with 80mL ethylene glycol, ultrasonic agitation 4h；
Step S2, adds the mixture of 0.5g Iron(III) chloride hexahydrate and potassium dichromate, adds 4.0g anhydrous sodium acetate, after ultrasonic agitation is uniform, regulates pH=10 with ammonia；The weight ratio of described Iron(III) chloride hexahydrate and potassium dichromate is 5:1；
Step S3, is placed in hydrothermal reaction kettle, 200 DEG C of reaction 10h；
Step S4, is cooled to room temperature, is sequentially added into deionized water and washes of absolute alcohol, centrifugation, and end product is placed in baking oven drying。
Embodiment 2:Fe
3
O
4
-Cr
2
O
3
The preparation of-Graphene composite anode materials
Step S1, weighs 80mg graphene oxide and 1g Polyethylene Glycol PEG-4000 puts in the beaker equipped with 80mL ethylene glycol, ultrasonic agitation 4h；
Step S2, adds the mixture of 0.5g Iron(III) chloride hexahydrate and potassium dichromate, adds 4.0g anhydrous sodium acetate, after ultrasonic agitation is uniform, regulates pH=10 with ammonia；The weight ratio of described Iron(III) chloride hexahydrate and potassium dichromate is 4:1；
Step S3, is placed in hydrothermal reaction kettle, 200 DEG C of reaction 10h；
Step S4, is cooled to room temperature, is sequentially added into deionized water and washes of absolute alcohol, centrifugation, and end product is placed in baking oven drying。
Embodiment 3:Fe
3
O
4
-Cr
2
O
3
The preparation of-Graphene composite anode materials
Step S1, weighs 80mg graphene oxide and 1g Polyethylene Glycol PEG-4000 puts in the beaker equipped with 80mL ethylene glycol, ultrasonic agitation 4h；
Step S2, adds the mixture of 0.5g Iron(III) chloride hexahydrate and potassium dichromate, adds 4.0g anhydrous sodium acetate, after ultrasonic agitation is uniform, regulates pH=10 with ammonia；The weight ratio of described Iron(III) chloride hexahydrate and potassium dichromate is 6:1；
Step S3, is placed in hydrothermal reaction kettle, 200 DEG C of reaction 10h；
Step S4, is cooled to room temperature, is sequentially added into deionized water and washes of absolute alcohol, centrifugation, and end product is placed in baking oven drying。
Embodiment 4: the weight ratio of the contrast of embodiment 1, Iron(III) chloride hexahydrate and potassium dichromate is 3:1
Step S1, weighs 80mg graphene oxide and 1g Polyethylene Glycol PEG-4000 puts in the beaker equipped with 80mL ethylene glycol, ultrasonic agitation 4h；
Step S2, adds the mixture of 0.5g Iron(III) chloride hexahydrate and potassium dichromate, adds 4.0g anhydrous sodium acetate, after ultrasonic agitation is uniform, regulates pH=10 with ammonia；The weight ratio of described Iron(III) chloride hexahydrate and potassium dichromate is 3:1；
Step S3, is placed in hydrothermal reaction kettle, 200 DEG C of reaction 10h；
Step S4, is cooled to room temperature, is sequentially added into deionized water and washes of absolute alcohol, centrifugation, and end product is placed in baking oven drying。
Embodiment 5: the weight ratio of the contrast of embodiment 1, Iron(III) chloride hexahydrate and potassium dichromate is 7:1
Step S1, weighs 80mg graphene oxide and 1g Polyethylene Glycol PEG-4000 puts in the beaker equipped with 80mL ethylene glycol, ultrasonic agitation 4h；
Step S2, adds the mixture of 0.5g Iron(III) chloride hexahydrate and potassium dichromate, adds 4.0g anhydrous sodium acetate, after ultrasonic agitation is uniform, regulates pH=10 with ammonia；The weight ratio of described Iron(III) chloride hexahydrate and potassium dichromate is 7:1；
Step S3, is placed in hydrothermal reaction kettle, 200 DEG C of reaction 10h；
Step S4, is cooled to room temperature, is sequentially added into deionized water and washes of absolute alcohol, centrifugation, and end product is placed in baking oven drying。
Embodiment 6: effect example, battery assembles and test
Fe prepared by embodiment 1～53O4-Cr2O3-graphene composite material is as active substance, and acetylene black is as conductive agent, and Kynoar (PVDF) is as binding agent。Weigh active substance, acetylene black and PVDF, the said mixture ground and mixed in mortar that will weigh up according to 70:15:15 mass ratio, process of lapping drips a little NMP, after about grinding 1h, form pulpous state。Then being coated in equably on copper foil by slurry, in thermostatic drying chamber, 60 DEG C dry 24 hours, are cut into diameter 8mm sequin as active anode sheet with cutting machine。Do electrode slice by metal lithium sheet, in the glove box of full argon, be assembled into button cell。Adopt LandCT2001A battery test system, set certain charging/discharging voltage interval and carry out constant current charge-discharge test as 0～3V (vsLi+/Li) and charging and discharging currents。
Fe3O4-Cr2O3-graphene combination electrode is constant current charge-discharge (50mA g in 0～3V voltage range-1Electric current density), comparing result is as follows:
| Sample | First charge-discharge specific capacity (mAh g-1) | Capability retention (%) after 300 charge and discharge cycles |
| Embodiment 1 | 1299；1268 | 98.5 |
| Embodiment 2 | 1265；1234 | 96.5 |
| Embodiment 3 | 1257；1226 | 97.0 |
| Embodiment 4 | 725.51；904.43 | 74.5 |
| Embodiment 5 | 710.23；895.52 | 75.2 |
The above results shows, Fe provided by the invention3O4-Cr2O3-graphene composite material can obtain higher first charge-discharge specific capacity, and after 300 charge and discharge cycles, capability retention more than 95%, good stability。As can be seen here, Fe provided by the invention3O4-Cr2O3-graphene composite material has the charge-discharge performance of excellence, this performance is likely to relevant with the weight ratio of Iron(III) chloride hexahydrate in preparation method and potassium dichromate, when the weight ratio of Iron(III) chloride hexahydrate and potassium dichromate is between 4～6:1, performance is best。
The effect of above-described embodiment indicates that the essentiality content of the present invention, but does not limit protection scope of the present invention with this。It will be understood by those within the art that, it is possible to technical scheme is modified or equivalent replacement, without deviating from essence and the protection domain of technical solution of the present invention。
Claims (5)
1. a lithium ion battery Fe3O4-Cr2O3The preparation method of-Graphene composite anode materials, it is characterised in that include being made by step:
Step S1, weighs 70～90mg graphene oxide and 0.8～1.2g Polyethylene Glycol PEG-4000 puts in the beaker equipped with 80mL ethylene glycol, ultrasonic agitation 3～5h；
Step S2, adds the mixture of 0.5g Iron(III) chloride hexahydrate and potassium dichromate, adds 4.0g anhydrous sodium acetate, after ultrasonic agitation is uniform, regulates pH=10 with ammonia；The weight ratio of described Iron(III) chloride hexahydrate and potassium dichromate is 4～6:1；
Step S3, is placed in hydrothermal reaction kettle, 180～220 DEG C of reaction 8～12h；
Step S4, is cooled to room temperature, is sequentially added into deionized water and washes of absolute alcohol, centrifugation, and end product is placed in baking oven drying。
2. lithium ion battery Fe according to claim 13O4-Cr2O3The preparation method of-Graphene composite anode materials, it is characterised in that: in step S2, the weight ratio of described Iron(III) chloride hexahydrate and potassium dichromate is 5:1。
3. lithium ion battery Fe according to claim 1 and 23O4-Cr2O3The preparation method of-Graphene composite anode materials, it is characterised in that step S1 is: weigh 80mg graphene oxide and 1g Polyethylene Glycol PEG-4000 puts in the beaker equipped with 80mL ethylene glycol, ultrasonic agitation 4h；
4. lithium ion battery Fe according to claim 1 and 23O4-Cr2O3The preparation method of-Graphene composite anode materials, it is characterised in that step S3 is: be placed in hydrothermal reaction kettle, 200 DEG C of reaction 10h。
5. the Fe described in claim 1 or 23O4-Cr2O3The application in the preparing lithium ion battery of-Graphene composite anode materials。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109286010A (en) * | 2018-09-27 | 2019-01-29 | 河南大学 | A kind of growth in situ method of graphene coated nano chromium oxide negative electrode material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109286010A (en) * | 2018-09-27 | 2019-01-29 | 河南大学 | A kind of growth in situ method of graphene coated nano chromium oxide negative electrode material |
| CN109286010B (en) * | 2018-09-27 | 2020-12-11 | 河南大学 | In-situ growth method of graphene-coated nano chromium oxide negative electrode material |
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Application publication date: 20160622 |