CN108642606A - Cobaltosic oxide/carbon nano-fiber composite material and its preparation method and application - Google Patents
Cobaltosic oxide/carbon nano-fiber composite material and its preparation method and application Download PDFInfo
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
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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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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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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
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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
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- 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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- 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
- H01M4/62—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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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- H01M4/00—Electrodes
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The present invention relates to cobaltosic oxide/carbon nano-fiber composite materials and its preparation method and application, wherein described method includes following steps：(1) electrostatic spinning process prepares the high molecular polymer nanofiber containing cobalt and the dry high molecular polymer nanofiber containing cobalt；And (2) heat treatment process, cobaltosic oxide/carbon nano-fiber composite material is made.Cobaltosic oxide/carbon nano-fiber composite material of the present invention can be used for lithium ion battery negative material, have high capacity and good electric conductivity, while inhibiting volume expansion so that the cycle performance of lithium ion battery is good.
Description
Technical field
The present invention relates to nanometer composite technology fields, and in particular to cobaltosic oxide/carbon nano-fiber composite material and its
Preparation method and application.
Background technology
It is mainly carbon material that lithium ion battery, which is commercialized negative material, and carbon material has as lithium ion battery negative material
Electrode potential is low, and cycle efficieny is high, has extended cycle life, and security performance is high, it is cheap the advantages that.But carbon material theoretical capacity
Low, specific capacity is only 200-400mAh/g, and for current potential close to lithium metal, when charging is easy to happen the precipitation of Li dendrite, without
Method meets demand of the growing electrical equipment for lithium ion cell high-capacity.
So far, other negative materials in research mainly have alloy material and metal oxide-type cathode material
Material.The discharge platform of metal oxide is generally higher than carbon material, can inhibit the generation of Li dendrite to a certain extent, be conducive to
Improve battery security.Cobaltosic oxide is wherein typical a kind of, its theoretical capacity is far above carbon material, but as negative
Material volume expansion in charge and discharge process in pole is larger, and poorly conductive.Therefore, the embedded cobaltosic oxide nano in carbon material
Particle is a kind of high efficiency method preparing lithium ion battery negative material so that the existing very high capacity of material, and have good
Electric conductivity, while volume expansion is also inhibited, cycle performance is good.
Rarely have in carbon material embedded cobaltosic oxide nano particle in the prior art, is that a kind of to prepare lithium ion battery negative
The high efficiency method of pole material, the present inventor pass through creative work invention cobaltosic oxide/carbon nano-fiber composite wood
Material and preparation method, and applied to the remarkable result acquired by lithium ion battery negative material.
Invention content
The object of the present invention is to provide cobaltosic oxide/carbon nano-fiber composite materials and its preparation method and application.
What the technology of the present invention was realized in：Cobaltosic oxide/carbon nano-fiber composite material, preparation method and application.First, originally
Invention provides the preparation method of cobaltosic oxide/carbon nano-fiber composite material, and described method includes following steps：(1) electrostatic
Spinning process prepares the high molecular polymer nanofiber containing cobalt and the dry high molecular polymer Nanowire containing cobalt
Dimension；And (2) heat treatment process, the cobaltosic oxide/carbon nano-fiber composite material is made.
In one aspect of the invention, in step (1), spinning precursor solution is prepared, by the precursor solution
Electrostatic spinning is carried out by certain Parameter Conditions, the high molecular polymer nanofiber containing cobalt is obtained, described in obtaining
High molecular polymer nanofiber is dried in vacuo.
In the present invention, the preparation spinning precursor solution refers to：By cobalt salt with organic high molecular polymer with certain
Ratio is dissolved in solvent, is performed under heating conditions and is stirred until homogeneous, and forms precursor solution.
In another aspect of this invention, in step (2), the heat treatment process includes three steps：
The high molecular polymer nanofiber containing cobalt after drying is heated to certain temperature heat preservation by (2-1) in air
A few hours, and be slowly cooled to room temperature；
(2-2), which is placed under inert gas shielding, to be heated to high temperature and keeps the temperature a few hours, and the carbon nano-fiber containing cobalt is obtained；
Carbon nano-fiber containing cobalt is thermally treated resulting in the cobaltosic oxide/carbon nano-fiber by (2-3) in air again
Composite material.
In one aspect of the invention, in step (1), the organic high molecular polymer be polyvinylpyrrolidone,
One or both of polyacrylonitrile, polyvinyl alcohol are a variety of, and the solvent is deionized water, absolute ethyl alcohol, N, N- dimethyl
One or both of amide is a variety of, cobalt salt be selected as cabaltous nitrate hexahydrate, four acetate hydrate cobalts, Cobalt monosulfate heptahydrate one
Kind or two or more.
Further, a concentration of 8wt%-12wt% of the organic high molecular polymer；Cobalt salt and high molecular polymer
Mass ratio is 1: 10-1: 1.
In the above embodiment of the present invention, applied field intensity is 0.5-2kv/cm during the electrostatic spinning.
Preferably, the present invention step (2-1) in, when aoxidizing in air, heating temperature between 150-300 DEG C,
Heating time is between 1-5h；In step (2-2), inert gas is in argon gas or nitrogen, and heating temperature is in 700-1200
DEG C, heating time is between 1-5h；In step (2-3), heat treatment is to carry out oxidizing thermal treatment, the oxidation in the air
The temperature of heat treatment is between 200 DEG C -400 DEG C, and heating time is between 1-10h.
The present invention also provides the above methods, and cobaltosic oxide/carbon nano-fiber composite material is prepared, it is preferred that institute
The specific surface area and thermal stability for stating cobaltosic oxide/carbon nano-fiber composite material are improved.
The present invention also provides the above methods, and cobaltosic oxide/carbon nano-fiber composite material is prepared, it is preferred that institute
Cobaltosic oxide/carbon nano-fiber composite material rough surface is stated, cobaltosic oxide nano is particle studded in carbon nano-fiber
Portion and surface, cobaltosic oxide nano particle size is between 10-220hm, and carbon nano-fiber diameter is between 80-250nm.
Four oxygen that the cobaltosic oxide/carbon nano-fiber composite material or the above method of the present invention of the present invention is prepared
Change three cobalts/carbon nano-fiber composite material and is used as lithium ion battery negative material.
The pattern of cobaltosic oxide/carbon nano-fiber composite material of the present invention is uniform, has very high specific surface area, heat
Stability is good and a kind of good cycle, the high lithium ion battery negative material of capacity.The technology for having filled up this field is empty
In vain, a kind of technology path efficiently preparing excellent lithium ion battery negative material is provided.
The positive effect of the present invention is that the small size of nano material significantly increases lithium ion deintercalation rate, therefore lithium ion
Transmission range in electrode material reduces, while material specific surface area is big, is provided in charge and discharge process more for material
Embedding lithium space, the good cycle of material, capacity is high.
Description of the drawings
Fig. 1 is the scanning electron microscope schematic diagram of cobaltosic oxide/carbon nano-fiber composite material of the present invention.
Specific embodiment party French
The preparation method of above-mentioned cobaltosic oxide/carbon nano-fiber composite material of the invention, the method includes as follows
Step：(1) electrostatic spinning process prepares the high molecular polymer nanofiber containing cobalt and the dry macromolecule containing cobalt
Polymer nanofiber；And (2) heat treatment process, the cobaltosic oxide/carbon nano-fiber composite material is made.
In one aspect of the invention, in step (1), spinning precursor solution is prepared, by the precursor solution
Electrostatic spinning is carried out by certain Parameter Conditions, the high molecular polymer nanofiber containing cobalt is obtained, described in obtaining
High molecular polymer nanofiber is dried in vacuo.
In the present invention, the preparation spinning precursor solution refers to：By cobalt salt with organic high molecular polymer with certain
Ratio is dissolved in solvent, is performed under heating conditions and is stirred until homogeneous, and forms precursor solution.
In another aspect of this invention, in step (2), the heat treatment process includes three steps：
The high molecular polymer nanofiber containing cobalt after drying is heated to certain temperature heat preservation by (2-1) in air
A few hours, and be slowly cooled to room temperature；
(2-2), which is placed under inert gas shielding, to be heated to high temperature and keeps the temperature a few hours, and the carbon nano-fiber containing cobalt is obtained；
Carbon nano-fiber containing cobalt is thermally treated resulting in the cobaltosic oxide/carbon nano-fiber by (2-3) in air again
Composite material.
In one aspect of the invention, in step (1), the organic high molecular polymer be polyvinylpyrrolidone,
One or both of polyacrylonitrile, polyvinyl alcohol are a variety of, and the solvent is deionized water, absolute ethyl alcohol, N, N- dimethyl
One or both of amide is a variety of, cobalt salt be selected as cabaltous nitrate hexahydrate, four acetate hydrate cobalts, Cobalt monosulfate heptahydrate one
Kind or two or more.
Further, a concentration of 8wt%-12wt% of the organic high molecular polymer；Cobalt salt and high molecular polymer
Mass ratio is 1: 10-1: 1.
In the above embodiment of the present invention, applied field intensity is 0.5kv-2kv during the electrostatic spinning.
Preferably, the present invention step (2-1) in, when aoxidizing in air, heating temperature between 150-300 DEG C,
Heating time is between 1-5h；In step (2-2), inert gas is in argon gas or nitrogen, and heating temperature is in 700-1200
DEG C, heating time is between 1-5h；In step (2-3), heat treatment is to carry out oxidizing thermal treatment, the oxidation in the air
The temperature of heat treatment is between 200 DEG C -400 DEG C, and heating time is between 1-10h.
The present invention also provides the above methods, and cobaltosic oxide/carbon nano-fiber composite material is prepared, it is preferred that institute
Cobaltosic oxide/carbon nano-fiber composite material rough surface is stated, cobaltosic oxide nano is particle studded in carbon nano-fiber
Portion and surface, cobaltosic oxide nano particle size is between 10-220nm, and carbon nano-fiber diameter is between 80-250nm.
The present invention is described further below in conjunction with drawings and examples：
Embodiment 1
Tetra- acetate hydrate cobalts of 0.5g are mixed with 1g polyacrylonitrile (PAN), 9gN is added, N- dimethylformamides carry out magnetic force
Stirring, whipping temp are 70 DEG C, time 2h.12h is stood after stirring evenly, and is configured to presoma.Colloidal sol is packed into plastic needle
Cylinder carries out Electrospun, electric field strength 1kv/cm, ambient humidity 20%RH, and fiber is collected with aluminium foil, and that has spun contains
The high molecular polymer nanofiber of cobalt is put into vacuum tank and is preserved for 24 hours.Then fiber is placed in tube furnace into pre- oxygen
Change, temperature is 250 DEG C, keeps the temperature furnace cooling after 3h, 5 DEG C/min of heating rate, obstructed protection gas.Fiber after pre-oxidation is placed
It is sintered in tube furnace, temperature is 1000 DEG C, keeps the temperature 1h, leads to argon gas protection, the carbon nano-fiber containing cobalt is obtained after furnace cooling.
Carbon nano-fiber containing cobalt is placed in tube furnace and carries out secondary oxidation, temperature is 300 DEG C, keeps the temperature 5h, four are obtained after furnace cooling
Co 3 O/carbon nano-fiber composite material.The specific surface area and heat of the cobaltosic oxide/carbon nano-fiber composite material are steady
It is qualitative to be improved.Fig. 1 is cobaltosic oxide/carbon nano-fiber scanning electron microscope schematic diagram of embodiment one, wherein described four
The rough surface of Co 3 O/carbon nano-fiber composite material, cobaltosic oxide nano are particle studded inside carbon nano-fiber
And surface, cobaltosic oxide nano particle size is between 80-220nm, and carbon nano-fiber diameter is between 80-200nm.
Embodiment 2
Tetra- acetate hydrate cobalts of 0.5g are mixed with 1g polyacrylonitrile (PAN), 9gN is added, N- dimethylformamides carry out magnetic force
Stirring, whipping temp are 70 DEG C, time 2h.12h is stood after stirring evenly, and is configured to presoma.Colloidal sol is packed into plastic needle
Cylinder carries out Electrospun, electric field strength 1kv/cm, ambient humidity 20%RH, and fiber is collected with aluminium foil, and that has spun contains
The high molecular polymer nanofiber of cobalt is put into vacuum tank and is preserved for 24 hours.Then fiber is placed in tube furnace into pre- oxygen
Change, temperature is 250 DEG C, keeps the temperature furnace cooling after 3h, 5 DEG C/min of heating rate, obstructed protection gas.Fiber after pre-oxidation is placed
It is sintered in tube furnace, temperature is 700 DEG C, keeps the temperature 1h, leads to nitrogen protection, the carbon nano-fiber containing cobalt is obtained after furnace cooling.
Carbon nano-fiber containing cobalt is placed in tube furnace and carries out secondary oxidation, temperature is 300 DEG C, keeps the temperature 5h, four are obtained after furnace cooling
Co 3 O/carbon nano-fiber composite material.The rough surface of the cobaltosic oxide/carbon nano-fiber composite material, four oxygen
Change three cobalt nano-particles to be embedded in inside carbon nano-fiber and surface, cobaltosic oxide nano particle size between 10-30nm,
Carbon nano-fiber diameter is between 60-130nm.
Four oxygen that the cobaltosic oxide/carbon nano-fiber composite material or the above method of the present invention of the present invention is prepared
Change three cobalts/carbon nano-fiber composite material and is used as lithium ion battery negative material.
Cobaltosic oxide prepared by the present invention/carbon nano-fiber composite material pattern is uniform, has very high specific surface area,
Thermal stability is good and a kind of good cycle, the high lithium ion battery negative material of capacity.
The positive effect of the present invention is that the small size of nano material significantly increases lithium ion deintercalation rate, therefore lithium ion
Transmission range in electrode material reduces, while material specific surface area is big, is provided in charge and discharge process more for material
Embedding lithium space, the good cycle of material, capacity is high.
The above is only presently preferred embodiments of the present invention.It will be appreciated by those skilled in the art that the present invention is not limited to here
The specific embodiment, can carry out for a person skilled in the art it is various it is apparent variation, readjust and substitute and
Without departing from the scope of protection of the present invention.Therefore, although being described in further detail to the present invention by above example,
But the present invention is not limited only to above example, can also include more other without departing from the inventive concept
Equivalent embodiment, and the scope of the present invention is determined by scope of the appended claims.
Claims (10)
1. the preparation method of cobaltosic oxide/carbon nano-fiber composite material, which is characterized in that the method includes walking as follows
Suddenly：
(1) electrostatic spinning process prepares the high molecular polymer nanofiber containing cobalt and the dry macromolecule containing cobalt
Polymer nanofiber；And
(2) cobaltosic oxide/carbon nano-fiber composite material is made in heat treatment process.
2. according to the method described in claim 1, it is characterized in that, preferred,
In step (1), spinning precursor solution is prepared, the precursor solution is quiet by certain Parameter Conditions progress
Electrospun obtains the high molecular polymer nanofiber containing cobalt, the high molecular polymer nanofiber vacuum that will be obtained
It is dry.
3. according to the method described in claim 2, it is characterized in that,
The preparation spinning precursor solution refers to：Cobalt salt and organic high molecular polymer are dissolved in solvent with certain proportion,
It is stirred under heating condition to uniform, formation precursor solution.
4. according to the method described in claim 1, it is characterized in that,
In step (2), the heat treatment process includes three steps：
(2-1) by the high molecular polymer nanofiber containing cobalt after drying be heated in air certain temperature heat preservation number it is small
When, and be slowly cooled to room temperature；
(2-2), which is placed under inert gas shielding, to be heated to high temperature and keeps the temperature a few hours, and the carbon nano-fiber containing cobalt is obtained；
(2-3) heat treatment certain time obtains the cobaltosic oxide/carbon nanometer in air again by the carbon nano-fiber containing cobalt
Fibrous composite.
5. according to the method described in claim 3, it is characterized in that,
In step (1), the organic high molecular polymer is one in polyvinylpyrrolidone, polyacrylonitrile, polyvinyl alcohol
Kind or two or more, the solvent be deionized water, absolute ethyl alcohol, N, one or both of N- dimethylformamides or more
Kind, cobalt salt is selected as the one or two or more of cabaltous nitrate hexahydrate, four acetate hydrate cobalts, Cobalt monosulfate heptahydrate.
6. according to the method described in claim 5, it is characterized in that,
A concentration of 8wt%-12wt% of organic high molecular polymer；The mass ratio of cobalt salt and high molecular polymer is 1: 10-1
∶1。
7. according to claim 1-3,5-6 any one of them method, which is characterized in that
Applied field intensity is 0.5-2kv/cm during the electrostatic spinning.
8. according to the method described in claim 4, it is characterized in that,
In step (2-1), when aoxidizing in air, heating temperature is between 150-300 DEG C, and heating time is between 1-5h；
In step (2-2), inert gas is in argon gas or nitrogen, and heating temperature is at 700-1200 DEG C, and heating time is in 1-
Between 5h；
In step (2-3), heat treatment is to carry out oxidizing thermal treatment in the air, and the temperature of the oxidizing thermal treatment is 200
Between DEG C -400 DEG C, heating time is between 1-10h.
9. according to cobaltosic oxide/carbon nano-fiber composite material, feature made from any one of claim 1-8 the methods
It is, the cobaltosic oxide/carbon nano-fiber composite material rough surface, cobaltosic oxide nano is particle studded in carbon nanometer
Fibrous inside and surface, cobaltosic oxide nano particle size is between 10-220nm, and carbon nano-fiber diameter is in 80-250nm
Between.
10. according to cobaltosic oxide/carbon nano-fiber composite material or root made from any one of claim 1-8 the methods
According to the purposes of cobaltosic oxide/carbon nano-fiber composite material described in claim 9, which is characterized in that
Cobaltosic oxide/the carbon nano-fiber composite material is used for lithium ion battery negative material.
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Cited By (9)
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| CN109755033A (en) * | 2019-03-08 | 2019-05-14 | 桂林电子科技大学 | A kind of carbon fiber loaded cobalt/cobalt oxide composite material and preparation method and application |
| CN110137461A (en) * | 2019-05-10 | 2019-08-16 | 陕西科技大学 | Lithium ion battery cobalt/cobalt oxide carbon nano-fiber flexible electrode material and preparation method thereof derived from MOF |
| CN110311116A (en) * | 2019-07-08 | 2019-10-08 | 西安交通大学 | A kind of Co2AlO4The preparation method of/C nano fiber |
| CN110707307A (en) * | 2019-10-22 | 2020-01-17 | 西京学院 | Hollow nanofiber Co3O4/S composite material, preparation method and application |
| CN111063888A (en) * | 2019-12-11 | 2020-04-24 | 肇庆市华师大光电产业研究院 | Preparation method of modified carbon nanofiber lithium-sulfur battery positive electrode material |
| CN111554892A (en) * | 2020-04-24 | 2020-08-18 | 宁波大学 | Lithium battery negative electrode material Co3O4Preparation method of nano-fiber |
| CN113644263A (en) * | 2021-07-26 | 2021-11-12 | 西北工业大学 | Preparation method and application of flexible carbon nanofiber framework coated with ultra-uniform lithium-philic sites |
| CN114245941A (en) * | 2021-03-31 | 2022-03-25 | 宁德新能源科技有限公司 | Negative electrode sheet, electrochemical device, and electronic device |
| CN115020707A (en) * | 2022-06-09 | 2022-09-06 | 中南大学 | Flexible lithium metal battery lithium-philic carbon nanofiber framework material and preparation method and application thereof |
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Application publication date: 20181012 |