CN104466168A - Preparation method of cobaltosic oxide-carbon porous nanofiber and application of cobaltosic oxide-carbon porous nanofiber to preparation of lithium ion battery - Google Patents
Preparation method of cobaltosic oxide-carbon porous nanofiber and application of cobaltosic oxide-carbon porous nanofiber to preparation of lithium ion battery Download PDFInfo
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- CN104466168A CN104466168A CN201410748139.4A CN201410748139A CN104466168A CN 104466168 A CN104466168 A CN 104466168A CN 201410748139 A CN201410748139 A CN 201410748139A CN 104466168 A CN104466168 A CN 104466168A
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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
- H01M4/48—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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01M4/62—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 discloses a preparation method of a cobaltosic oxide-carbon porous nanofiber and application of the cobaltosic oxide-carbon porous nanofiber to preparation of a lithium ion battery. The preparation method comprises the steps of dropwise adding a sol solution of soluble cobalt salt into a dimethylformamide solution of polyacrylonitrile and polymethyl methacrylate, continuously stirring, and keeping at the temperature of 80-100 DEG C for 24 hours; preparing a polymer/cobalt salt composite fiber supported on aluminum foil by using an electrostatic spinning process; heating the polymer/cobalt salt composite fiber to 280 DEG C at the rate of 2-4 DEG C/min in air, and keeping heating for 2 hours; and then, heating to 500 DEG C in the presence of inert atmosphere, keeping heating for 4 hours, and then, cooling to obtain the cobaltosic oxide-carbon porous nanofiber. The composite material has nano-scale size and high conductivity; when the cobaltosic oxide-carbon porous nanofiber is used as a negative electrode material of a lithium battery, the cycle life of the lithium battery can be prolonged, and the rate capability of the lithium battery can be improved; in addition, the preparation method is simple in process, good in repeatability, easy to implement and beneficial to industrial production.
Description
Technical field
The present invention relates to technical field of lithium ion battery negative, particularly relate to the preparation method of a kind of lithium ion cell cobaltic-cobaltous oxide-carbon porous nano-fibre.
Background technology
The advantage such as lithium ion battery has high voltage, high power capacity, volume is little, quality is light, memory-less effect, self discharge are little and have extended cycle life, becomes the mechanism of new electrochemical power sources of 21 century great potential.In current commercialization lithium battery, the theoretical capacity of negative material graphite only has 372mAh/g, can not meet the application demand of heavy-duty battery.Therefore, the negative material that exploitation has more high power capacity, long circulation life and a high rate capability becomes the target that domestic and international researcher chases.Wherein, transition metal oxide cobaltosic oxide (Co
3o
4) theoretical capacity (890mAh/g) is 2 ~ 3 times of graphite, have great application prospect; But there is the shortcoming that coulombic efficiency is first low, cycle life is poor and high rate performance is not high in it.
In order to improve Co
3o
4chemical property, mainly consider from following two aspects: (1) prepares Nano grade Co
3o
4material, can improve four cobalt oxides as the coulombic efficiency of negative material and cycle performance by this kind of method, (2) surface modification, as coated carbon-coating, doping metals etc., the conductivity of cobaltic-cobaltous oxide negative pole material can be increased by this kind of method, improve its high rate performance.And two kinds of methods combining are got up, designing a kind ofly has special appearance and has the cobaltosic oxide nano composite material of high conductivity, improves cycle life and the high rate performance of cobaltic-cobaltous oxide negative pole material, yet there are no relevant report.
Summary of the invention
In order to solve the technical problem of existing cobaltosic oxide and high rate performance difference low as lithium ion battery negative material cycle life, the invention provides the preparation method of a kind of cobaltosic oxide-carbon porous nano-fibre, the nano composite material diameter obtained is Nano grade, can improve its cycle life; Utilize poroid carbon nano-fiber as the conducting base of cobaltosic oxide, the conductance of cobaltosic oxide can be improved, thus improve its high rate performance.
In order to realize foregoing invention object, the present invention by the following technical solutions: a kind of lithium ion cell cobaltic-cobaltous oxide-carbon porous nano-fibre preparation method, step is as follows:
(1) polymer/inorganic spinning solution is prepared:
Under 80 ~ 100 DEG C of conditions, first distinguish the dimethyl formamide solution of polymer of preparation quality concentration 8 ~ 12% and dimethyl formamide (DMF) sol solutions of the soluble cobalt of mass concentration 15 ~ 22%; Again the dimethyl formamide sol solutions of soluble cobalt is mixed according to volume ratio 1:5 ~ 1:8 with the dimethyl formamide of polymer, then stir more than 20 hours at 80 ~ 100 DEG C, namely obtain polymer/cobalt salt spinning solution.
Described polymer be polyacrylonitrile and polymethyl methacrylate etc. mass mixing thing, the presoma of soluble cobalt adopt in acetylacetone cobalt, cobalt acetate, cobalt chloride or cobalt nitrate any one;
(2) polymer/cobalt salt composite fibre be carried on aluminium foil is prepared:
Be fixed to by aluminium foil as gathering-device on plastic plate, adopt electrostatic spinning process to prepare the polymer/cobalt salt composite fibre be carried on aluminium foil, the thickness controlling composite fibre is 0.1 ~ 0.5mm.
(3) cobaltosic oxide-carbon porous nano-fibre is prepared:
First polymer/cobalt salt composite fibre is at least kept 2 hours to 280 DEG C with the ramp of 2 ~ 4 DEG C/minute in atmosphere.At such a temperature, first polymethyl methacrylate liquefies, and polyacrylonitrile is still solid-state, and the polymethyl methacrylate of post liquefaction plays the effect of pore-creating, and composite material obtained like this has porousness, can improve the cycle performance of battery material; Then by polymer/cobalt salt composite fibre under argon shield, 500 DEG C at least keep 4 hours, namely obtain cobaltosic oxide-carbon porous nano-fibre, the diameter of gained fiber is about 90nm.The treatment temperature of 500 DEG C makes polyacrylonitrile carbonization, improves the conductivity of composite material.Thus cobaltosic oxide the method prepared-carbon porous nano-fibre composite material can be used as excellent lithium ion battery negative material, can improve cycle performance and the multiplying power property of lithium battery.
Cobaltosic oxide prepared by the application-carbon porous nano-fibre composite fibre, as lithium ion battery negative material, not only increases battery cycle life and high rate performance, and technique is simple, favorable reproducibility, easy to implement, be conducive to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the Technology Roadmap of preparation method of the present invention.
Fig. 2 is the X-ray diffraction result of cobaltosic oxide-carbon porous nano-fibre prepared by the embodiment of the present invention 1.Broad peak wherein between 26 ~ 28 ° corresponds to the amorphous carbon in cobaltosic oxide-carbon porous nano-fibre; Other peaks correspond respectively to the peak of pure Emission in Cubic cobaltosic oxide (JCPDS card: 03-065-3103).The result shows that the cobaltosic oxide-carbon porous nano-fibre composite material purity adopting this legal system standby is high, there is no other impurity.
Fig. 3 is the scanning electron microscope (SEM) photograph of cobaltosic oxide-carbon porous nano-fibre prepared by the embodiment of the present invention 1.
Fig. 4 is the lithium ion battery cycle performance curve under 0.1C of cobaltosic oxide-carbon porous nano-fibre as negative material of the embodiment of the present invention 1 preparation.Half-cell is carried out charge and discharge cycles under 0.1C multiplying power, cobaltosic oxide-carbon porous nano-fibre composite material demonstrates excellent chemical property, first charge-discharge specific capacity is respectively 1151.9mAh/g and 1561.7mAh/g, and first charge-discharge coulombic efficiency is 73.7%.After circulation 50 times, charge specific capacity remains on 1128.4mAh/g, and do not occur significantly decay, concrete data are shown in Fig. 4.
Fig. 5 is the change curve of cobaltosic oxide-carbon porous nano-fibre as lithium ion battery charging and discharging capacity under different current density of negative material of the embodiment of the present invention 1 preparation.Half-cell is carried out charge-discharge test with different multiplying, circulates 5 times under each multiplying power of 0.1C, 0.2C, 0.5C, 1C, 2C successively, as shown in Figure 5.It still keeps good chemical property in large multiplying power discharging situation, and under 1C, 2C discharge-rate, charge specific capacity reaches 804.5mAh/g and 598.8mAh/g respectively, still the obvious graphite cathode material far above Current commercial.After different multiplying charge-discharge test, under 0.1C multiplying power, this half-cell charge specific capacity is 1118.3mAh/g, and this composite material still can keep high specific capacity.
Embodiment
Further illustrate below in conjunction with drawings and Examples, following case does not produce restriction to the present invention.
Embodiment 1
(1) polymer/inorganic spinning solution is prepared: the polyacrylonitrile of 1g and the polymethyl methacrylate of 1g are joined 19ml dimethyl formamide (dimethyl formamide, density is 0.945g/ml) in, also constantly be stirred to 90 DEG C of heating and dissolve completely, obtain the dimethyl formamide solution of polymer; 0.6g acetylacetone cobalt is joined in the dimethyl formamide of 3.6ml, is constantly stirred to dissolving, obtain inorganic sol solution; Inorganic sol solution is added drop-wise in polymer solution, continues stirring 24 hours at 80 ~ 100 DEG C, namely obtain polymer/inorganic composite spinning solution.
(2) the polymer/inorganic composite nano fiber be carried on aluminium foil is prepared: be fixed to by aluminium foil on plastic plate as gathering-device, adopt electrostatic spinning process to prepare the polymer/inorganic composite nano fiber be carried on aluminium foil, the thickness controlling composite nano fiber is 0.1 ~ 0.5mm.
(3) prepare cobaltosic oxide-carbon porous nano-fibre: by polymer/inorganic nanometer composite fibre, first place 2 hours in 280 DEG C in atmosphere; Then, under inert gas argon shield, keep 4 hours at 500 DEG C, namely obtain cobaltosic oxide-carbon porous nano-fibre composite material, the diameter of gained composite material is about 90nm (as shown in Figure 3).
(4) assembling of lithium ion battery and performance test: composite porous for cobaltosic oxide-carbon, Kynoar binding agent and conductive agent Super P are mixed according to mass ratio 80:10:10, add nitrogen methyl pyrrolidone and mix, and be coated on Copper Foil, drying, slicing treatment, obtained lithium ion cell electrode sheet.Subsequently using lithium sheet as electrode anode sheet, microporous polypropylene membrane is barrier film, 1mol/L LiPF
6(solvent is isopyknic dimethyl carbonate and dipropyl carbonate) is electrolyte, and electrode slice assembles 2032CR button simulated battery in the glove box being full of argon gas therewith, with the sealing of battery packaging machine, obtains lithium ion battery.After lithium ion battery is left standstill 24 hours, under 0.1C electric current, carry out charge-discharge test respectively, charge and discharge voltage is between 0.01 ~ 3.0V; Under 0.1C and 2C electric current, carry out high rate performance test, charge and discharge voltage is between 0.01 ~ 3.0V.Embodiment 2:
(1) prepare polymer/inorganic spinning solution: join in 23ml dimethyl formamide by the polyacrylonitrile of 1g and the polymethyl methacrylate of 1g, be also constantly stirred to 90 DEG C of heating and dissolve completely, obtain the solution of polymer; 0.6g cobalt acetate is joined in the dimethyl formamide of 2.9ml, is constantly stirred to dissolving, obtain inorganic sol solution; Inorganic sol solution is added drop-wise in polymer solution, continues stirring 24 hours at 80 ~ 100 DEG C, namely obtain polymer/inorganic composite spinning solution.
Other steps are identical with embodiment 1, and gained composite fibre diameter is about 90nm.
Embodiment 3:
(1) prepare polymer/inorganic spinning solution: join in 15.5ml dimethyl formamide by the polyacrylonitrile of 1g and the polymethyl methacrylate of 1g, be also constantly stirred to 90 DEG C of heating and dissolve completely, obtain the dimethyl formamide solution of polymer; 0.6g cobalt chloride is joined in the dimethyl formamide of 2.2ml, is constantly stirred to dissolving, obtain inorganic sol solution; Inorganic sol solution is added drop-wise in polymer solution, continues stirring 24 hours at 80 ~ 100 DEG C, namely obtain polymer/inorganic composite spinning solution.
Other steps are identical with case study on implementation 1, and gained composite fibre diameter is about 95nm.
Embodiment 4:
(1) prepare polymer/inorganic spinning solution: join in 17ml dimethyl formamide by the polyacrylonitrile of 1g and the polymethyl methacrylate of 1g, be also constantly stirred to 90 DEG C of heating and dissolve completely, obtain the dimethyl formamide solution of polymer; 0.6g cobalt nitrate is joined in the dimethyl formamide of 2.6ml, is constantly stirred to dissolving, obtain inorganic sol solution; Inorganic sol solution is added drop-wise in polymer solution, continues stirring 24 hours at 80 ~ 100 DEG C, namely obtain polymer/inorganic composite spinning solution.
Other steps are identical with embodiment 1, and gained composite fibre diameter is about 100nm.
The lithium ion battery that table 1 is embodiment 1 ~ 4 carries out charge-discharge test first lap and the 50th and encloses the capacity obtained under 0.1C electric current.
Table 1
As can be seen from Table 1, after the cobaltosic oxide adopting this method to prepare-carbon porous nano-fibre composite material circulation 50 circle, capability retention is more than 94%, does not occur significantly decay, has good cycle performance.
The lithium ion battery that table 2 is embodiment 1 ~ 4 carries out the stored energy capacitance that charge-discharge test obtains under 0.1C and 2C electric current.
Table 2
| Embodiment | Charge specific capacity (0.1C) mAh/g | Charge specific capacity (2C) mAh/g |
| Embodiment 1 | 1151.9 | 598.8 |
| Embodiment 2 | 1123.5 | 592.3 |
| Embodiment 3 | 1101.3 | 590.1 |
| Embodiment 4 | 1086.8 | 562.4 |
As shown in Table 2, adopt cobaltosic oxide-carbon porous nano-fibre composite material of preparing of this method under 2C electric current during discharge and recharge specific capacity can remain on more than 562.4mAh/g, still far above the graphite cathode material of Current commercial.
Claims (5)
1. cobaltosic oxide-carbon porous nano-fibre preparation method, it is characterized in that, step is as follows:
(1) polymer/cobalt salt spinning solution is prepared:
Under 80 ~ 100 DEG C of heating conditions, first prepare the dimethyl formamide solution of polymer and the dimethyl formamide sol solutions of soluble cobalt respectively; Again the dimethyl formamide sol solutions of soluble cobalt is mixed with the dimethyl formamide of polymer, then stir more than 20 hours at 80 ~ 100 DEG C, namely obtain polymer/cobalt salt spinning solution;
(2) polymer/cobalt salt composite fibre be carried on aluminium foil is prepared:
Aluminium foil is fixed to as gathering-device on plastic plate, adopts electrostatic spinning process to prepare the polymer/cobalt salt composite fibre be carried on aluminium foil;
(3) cobaltosic oxide-carbon porous nano-fibre is prepared:
First polymer/cobalt salt composite fibre is at least kept 2 hours to 280 DEG C with the ramp of 2 ~ 4 DEG C/minute in atmosphere; Then by polymer/cobalt salt composite fibre under argon shield, 500 DEG C at least keep 4 hours, namely obtain cobaltosic oxide-carbon porous nano-fibre, the diameter of gained fiber is within the scope of 90nm-100nm.
2. cobaltosic oxide according to claim 1-carbon porous nano-fibre preparation method, it is characterized in that polymer described in step (1) be polyacrylonitrile and polymethyl methacrylate etc. mass mixing thing, the presoma of soluble cobalt is any one in acetylacetone cobalt, cobalt acetate, cobalt chloride or cobalt nitrate.
3. cobaltosic oxide according to claim 1-carbon porous nano-fibre preparation method, it is characterized in that in step (1), the mass concentration of polymer dimethyl formamide solution is 8 ~ 12%, soluble cobalt dimethyl formamide sol solutions mass concentration is 15 ~ 22%; The dimethyl formamide sol solutions of soluble cobalt mixes according to volume ratio 1:5 ~ 1:8 with the dimethyl formamide solution of polyacrylonitrile and polymethyl methacrylate.
4. cobaltosic oxide according to claim 1-carbon porous nano-fibre preparation method, is characterized in that in step (2), and the thickness controlling polymer/cobalt salt composite fibre is 0.1 ~ 0.5mm.
5. claim 1 gained cobaltosic oxide-carbon porous nano-fibre is used as the purposes of lithium ion battery.
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| CN105304873A (en) * | 2015-09-23 | 2016-02-03 | 南京理工大学 | Method for preparing cobaltosic oxide-carbon fiber composite material by using carbon fiber as template |
| CN105914359A (en) * | 2016-06-28 | 2016-08-31 | 王行柱 | Preparation method of flexible positive electrode of foldable lithium battery |
| CN108642606A (en) * | 2018-04-11 | 2018-10-12 | 西安交通大学 | Cobaltosic oxide/carbon nano-fiber composite material and its preparation method and application |
| CN108847492A (en) * | 2018-06-14 | 2018-11-20 | 北京航空航天大学 | A kind of N doping metals cobalt carbon nano-fiber composite material and its preparation method and application |
| CN109616625A (en) * | 2018-11-08 | 2019-04-12 | 华南理工大学 | A kind of one-dimensional porous carbon fiber of sulfur compound nano particle and preparation and application |
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| CN110854381A (en) * | 2019-11-27 | 2020-02-28 | 宁波大学 | Preparation method of carbon-doped tin-manganese composite oxide nanofiber modified by cobalt oxide |
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| CN114669319A (en) * | 2022-04-19 | 2022-06-28 | 南京航空航天大学 | Nano cobaltosic oxide-carbon nitrogen composite catalyst and preparation method and application thereof |
| CN114669319B (en) * | 2022-04-19 | 2023-06-23 | 南京航空航天大学 | Nanometer cobaltosic oxide-carbon nitrogen composite catalyst and preparation method and application thereof |
| CN115254147A (en) * | 2022-07-15 | 2022-11-01 | 苏州德亨节能环保科技有限公司 | Preparation method and application of indium zinc sulfide cobaltosic oxide composite material |
| CN116005299A (en) * | 2023-01-18 | 2023-04-25 | 安徽科技学院 | Porous carbon nanofiber material with parallel pore canal structure and preparation method thereof |
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Application publication date: 20150325 |