CN108899487A - A kind of high conductivity lithium ion battery negative material and preparation method thereof - Google Patents
A kind of high conductivity lithium ion battery negative material and preparation method thereof Download PDFInfo
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- CN108899487A CN108899487A CN201810619274.7A CN201810619274A CN108899487A CN 108899487 A CN108899487 A CN 108899487A CN 201810619274 A CN201810619274 A CN 201810619274A CN 108899487 A CN108899487 A CN 108899487A
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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
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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
- H01M4/48—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
- H01M4/62—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
- 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
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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
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- 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 kind of preparation methods of high conductivity lithium ion battery negative material, including：Molysite, mantoquita, conducting polymer are added in n,N-Dimethylformamide, heating stirring to transparence obtains spinning solution；Spinning solution is subjected to electrostatic spinning injection, obtains film after dry；Carburizing reagent is carried out after film is activated, and obtains the high conductivity lithium ion battery negative material；Wherein, the temperature of activation is 260-300 DEG C, and the time of activation is 2-4h；The temperature of carburizing reagent is 570-630 DEG C, and the time of carburizing reagent is 2-4h.The preparation method of high conductivity lithium ion battery negative material proposed by the present invention is safe and non-toxic, and preparation is simple, and yield is high, preparation parameter controllability is strong, the lithium ion battery negative material electric conductivity being prepared is high, specific capacity with higher, good high rate performance and cyclical stability.
Description
Technical field
The present invention relates to technical field of lithium ion battery negative more particularly to a kind of high conductivity lithium ion battery are negative
Pole material and preparation method thereof.
Background technique
Lithium ion battery by its high-energy-density, high voltage, have extended cycle life, green non-pollution the advantages that, 3C electricity
Sub- product scope is widely used.But at present electric automobile market fast development LIBs performance is proposed it is higher
Requirement, the especially charge-discharge magnification performance under its high current.At present high rate performance LIBs not fully up to expectations mainly by
In electrochemical reaction and charge and discharge process slower on electrode-electrolyte interface caused by poor lithium-ion-conducting.But
It is that there is drawbacks in terms of electric conductivity for the carbon based negative electrodes material of mainstream currently on the market, limits performance of lithium ion battery into one
The key factor promoted is walked, the lithium ion battery negative material for seeking high conductivity is of great practical significance.
Summary of the invention
Technical problems based on background technology, the invention proposes a kind of high conductivity lithium ion battery negative materials
And preparation method thereof, the preparation method is safe and non-toxic, and preparation is simple, and yield is high, and preparation parameter controllability is strong, system
Standby obtained lithium ion battery negative material electric conductivity is high, specific capacity with higher, good high rate performance and stable circulation
Property.
A kind of preparation method of high conductivity lithium ion battery negative material proposed by the present invention, includes the following steps：
S1, molysite, mantoquita, conducting polymer are added in n,N-Dimethylformamide, heating stirring to transparence obtains
Spinning solution；
S2, spinning solution is subjected to electrostatic spinning injection, obtains film after dry；
S3, carburizing reagent is carried out after activating film, obtains the high conductivity lithium ion battery negative material；Wherein,
The temperature of activation is 260-300 DEG C, and the time of activation is 2-4h；The temperature of carburizing reagent be 570-630 DEG C, carburizing reagent when
Between be 2-4h.
Preferably, in S1, molysite, mantoquita mass ratio be 1-4：5-1.
Preferably, molysite, mantoquita mass ratio be 2：1.
Preferably, in S1, the molysite is the mixed of one or more of ferric nitrate, iron chloride, ferric acetyl acetonade
Close object.
Preferentially, the molysite selects ferric nitrate.
Preferably, in S1, the mantoquita is copper acetate.
Preferably, in S1, the conducting polymer is one of polyacrylonitrile, polyaniline, polyvinylpyrrolidone
Or a variety of mixture.
Preferably, in S1, the temperature of heating stirring is 55-65 DEG C.
Preferably, the temperature of heating stirring is 60 DEG C.
Preferably, in S2, in electrostatic spinning course of injection, spinning voltage 12-18kV, the promotion speed of electrostatic spinning
Degree is 1.0-2.0mL/h；The spacing of spray head to receiver board is 8-16cm；Ambient humidity is 35%-50%.
Preferably, spinning voltage 12-14kV, the driving velocity of electrostatic spinning are 1.0-1.3mL/h；Spray head is to receiver board
Spacing be 14-16cm；Ambient humidity is 40%-45%.
Preferably, spinning voltage 12kV, the driving velocity of electrostatic spinning are 1.0mL/h；Spacing of the spray head to receiver board
For 12cm；Ambient humidity is 43%.
Preferably, in S3, the carburizing reagent carries out in an inert atmosphere.
Preferably, the concrete technology of S3 is：Film is placed in Muffle furnace, in air atmosphere, with 1.5-2.5 DEG C/min
Heating rate be warming up to 260-300 DEG C of activation 2-4h, be subsequently placed in tube furnace, in an inert atmosphere, with 4-6 DEG C/min's
Heating rate is warming up to 570-630 DEG C of carbonization 2-4h, cools down after reaction, obtains the high conductivity negative electrode of lithium ion battery
Material.
Preferably, the concrete technology of S3 is：Film is placed in Muffle furnace, in air atmosphere, with the heating of 2 DEG C/min
Rate is warming up to 280 DEG C of activation 3h, is subsequently placed in tube furnace, in argon atmosphere, is warming up to the heating rate of 5 DEG C/min
600 DEG C of carbonization 2h, cooling obtains the high conductivity lithium ion battery negative material after reaction.
Preferably, in S2, the drying carries out in a vacuum drying oven.
A kind of high conductivity lithium ion battery negative material that the present invention also proposes, using the high conductivity lithium-ion electric
The preparation method of pond negative electrode material is prepared.
In the preparation method of high conductivity lithium ion battery negative material of the present invention, obtained first by electrospinning device
It is carbonized by precursor after activation in high temperature inert atmosphere, is specially 570-630 DEG C by adjusting carburizing temperature, utilizes carbon
On carbon nano-fiber, ferroso-ferric oxide, iron, copper and carbon nano-fiber has been made in conducting medium growth in situ by thermal reduction mechanism
Composite material, i.e. Fe3O4/ Fe/Cu/CNFs composite material；During preparation, pass through control electrostatic spinning and subsequent thermal
The technological parameter of processing, and the iron and copper in situ of introducing has the simple substance of ultra-high conductivity in the process, prepares resulting material
With two-dimensional structure, wherein the introducing of metal simple-substance effectively increases the electric conductivity of composite material, is conducive to the quick transmitting of electronics,
Certain supporting role is provided simultaneously for the shape holding of material；Using obtained composite material as negative electrode of lithium ion battery material
Material shows higher specific capacity, good high rate performance and cyclical stability.When current density is 500mAg-1And 1000mAg-1, reversible capacity of the electrode after circulation 50 weeks is respectively 618mAhg-1And 493mAhg-1, especially when charging and discharging currents increase
To 5000mAg-1, still there is 321mAg-1Reversible discharge capacity, superior high rate performance is shown under high current charge-discharge；
The preparation method is safe and non-toxic, and preparation is simple, and yield is high, and preparation parameter controllability is strong.
Detailed description of the invention
Fig. 1 is the XRD diagram of material prepared by the embodiment of the present invention 1, comparative example 1 and comparative example 2；
Fig. 2 is the SEM figure of negative electrode material prepared by the embodiment of the present invention 1；
Fig. 3 is the multiplying power figure of negative electrode material prepared by the embodiment of the present invention 1.
Specific embodiment
In the following, technical solution of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of preparation method of high conductivity lithium ion battery negative material proposed by the present invention, includes the following steps：
S1,2g ferric nitrate, 1g copper acetate and 2g polyacrylonitrile (PAN) are added in 20mL N,N-dimethylformamide
(DMF) in, heating stirring 12h obtains spinning solution to form homogeneous and transparent solution at 60 DEG C；
S2, the spinning solution of above-mentioned preparation is placed in the syringe with metal needle, then this syringe is fixed on electrostatic
The anode of device for spinning, and the anode of electrostatic spinning apparatus power supply is clipped on metal needle, aluminium film is laid in electrostatic spinning
On the collecting board of device, and adjusting collecting board at a distance from metal needle is 14cm, and the voltage of electrostatic spinning apparatus power supply is
The speed that pushes away of 15kV, syringe are 1.0mL/h, carry out electrostatic spinning injection, obtain film after dry；
S3, film is placed in Muffle furnace, in air atmosphere, 280 DEG C of activation is warming up to the heating rate of 2 DEG C/min
3h, then the product after activation is placed in tube furnace, in an inert atmosphere, 600 DEG C of carbon are warming up to the heating rate of 5 DEG C/min
Change 2h, obtains the high conductivity lithium ion battery negative material, as Fe3O4/ Fe/Cu/CNFs composite material.
The high conductivity lithium ion battery negative material being prepared is subjected to charging and discharging capacity and cycle performance test：
The electrode slice that the high conductivity lithium ion battery negative material being prepared and conductive agent, binder are mixed is as work
Electrode, wherein the weight ratio of high conductivity lithium ion battery negative material and conductive agent, binder is 8：1：1, it is gold to electrode
Belong to lithium, electrolyte 1molL-1LiF6/ EC-DMC (volume ratio 1：1), simulated battery is assembled into argon atmosphere glove box.
Charge-discharge test is carried out to simulated battery, voltage range is 0.01~2.5V (vs.Li+/ Li), current density 500mAg-1、
1000mAg-1And 5000mAg-1。
Embodiment 2
A kind of preparation method of high conductivity lithium ion battery negative material proposed by the present invention, includes the following steps：
S1,4g ferric nitrate, 1g copper acetate and 2g polyacrylonitrile (PAN) are added in 20mL N,N-dimethylformamide
(DMF) in, heating stirring 12h obtains spinning solution to form homogeneous and transparent solution at 60 DEG C；
S2, the spinning solution of above-mentioned preparation is placed in the syringe with metal needle, then this syringe is fixed on electrostatic
The anode of device for spinning, and the anode of electrostatic spinning apparatus power supply is clipped on metal needle, aluminium film is laid in electrostatic spinning
On the collecting board of device, and adjusting collecting board at a distance from metal needle is 14cm, and the speed that pushes away of syringe is 1.0mL/h, electrostatic
The voltage of device for spinning power supply is 15kV, carries out electrostatic spinning injection, obtains film after dry；
S3, film is placed in Muffle furnace, in air atmosphere, 280 DEG C of activation is warming up to the heating rate of 2 DEG C/min
3h, then the product after activation is placed in tube furnace, in an inert atmosphere, 600 DEG C of carbon are warming up to the heating rate of 5 DEG C/min
Change 2h, obtains the high conductivity lithium ion battery negative material.
Obtained high conductivity lithium ion battery negative material is subjected to charging and discharging capacity and cycle performance test, height is led
The electrode slice that electrical lithium ion battery negative material and conductive agent, binder are mixed is as working electrode, wherein highly conductive
Property lithium ion battery negative material and conductive agent, binder weight ratio be 8：1：1, it is lithium metal to electrode, electrolyte is
1molL-1LiF6/ EC-DMC (volume ratio 1：1), simulated battery is assembled into argon atmosphere glove box.To simulated battery into
Row charge-discharge test, voltage range are 0.01~2.5V (vs.Li+/ Li), current density 500mAg-1、1000mAg-1With
5000mAg-1。
Embodiment 3
A kind of preparation method of high conductivity lithium ion battery negative material proposed by the present invention, includes the following steps：
S1,2g ferric nitrate, 1g copper acetate and 2g polyaniline are added in 20mL n,N-Dimethylformamide (DMF), 60
Heating stirring 12h obtains spinning solution to form homogeneous and transparent solution at DEG C；
S2, the spinning solution of above-mentioned preparation is placed in the syringe with metal needle, then this syringe is fixed on electrostatic
The anode of device for spinning, and the anode of electrostatic spinning apparatus power supply is clipped on metal needle, aluminium film is laid in electrostatic spinning
On the collecting board of device, and adjusting collecting board at a distance from metal needle is 14cm, and the voltage of electrostatic spinning apparatus is 15kV, note
The speed that pushes away of emitter is 1.0mL/h, carries out electrostatic spinning injection, obtains film after dry；
S3, film is placed in Muffle furnace, in air atmosphere, 280 DEG C of activation is risen to the heating rate of 2 DEG C/min
3h, then the product after activation is placed in tube furnace, in an inert atmosphere, 600 DEG C of carbonizations are risen to the heating rate of 5 DEG C/min
2h obtains the high conductivity lithium ion battery negative material.
The high conductivity lithium ion battery negative material being prepared is subjected to charging and discharging capacity and cycle performance test,
The electrode slice that high conductivity lithium ion battery negative material and conductive agent, binder are mixed is as working electrode, wherein
The weight ratio of high conductivity lithium ion battery negative material and conductive agent, binder is 8：1：1, it is lithium metal, electrolysis to electrode
Liquid is 1molL-1LiF6/ EC-DMC (volume ratio 1：1), simulated battery is assembled into argon atmosphere glove box.To simulation electricity
Pond carries out charge-discharge test, and voltage range is 0.01~2.5V (vs.Li+/ Li), current density 500mAg-1、1000mAg-1With
5000mAg-1。
Embodiment 4
A kind of preparation method of high conductivity lithium ion battery negative material proposed by the present invention, includes the following steps：
S1, molysite, mantoquita, conducting polymer are added in n,N-Dimethylformamide, heating stirring to transparence obtains
Spinning solution；
S2, spinning solution is subjected to electrostatic spinning injection, obtains film after dry；
S3, carburizing reagent is carried out after activating film, obtains the high conductivity lithium ion battery negative material；Wherein,
The temperature of activation is 300 DEG C, and the time of activation is 2h；The temperature of carburizing reagent is 630 DEG C, and the time of carburizing reagent is 2h.
Embodiment 5
A kind of preparation method of high conductivity lithium ion battery negative material proposed by the present invention, includes the following steps：
S1, molysite, mantoquita, conducting polymer are added in n,N-Dimethylformamide, heating stirring to transparence obtains
Spinning solution；
S2, spinning solution is subjected to electrostatic spinning injection, obtains film after dry；
S3, carburizing reagent is carried out after activating film, obtains the high conductivity lithium ion battery negative material；Wherein,
The temperature of activation is 260 DEG C, and the time of activation is 4h；The temperature of carburizing reagent is 570 DEG C, and the time of carburizing reagent is 4h.
Embodiment 6
A kind of preparation method of high conductivity lithium ion battery negative material proposed by the present invention, includes the following steps：
S1, molysite, mantoquita, conducting polymer are added in n,N-Dimethylformamide, heating stirring to transparence obtains
Spinning solution；Wherein, molysite, mantoquita mass ratio be 4：5；The molysite is ferric acetyl acetonade；The mantoquita is copper acetate；It is described
Conducting polymer is polyvinylpyrrolidone；The temperature of heating stirring is 65 DEG C；
S2, spinning solution is subjected to electrostatic spinning injection, obtains film after dry；Wherein, in electrostatic spinning course of injection,
Spinning voltage is 18kV, and the driving velocity of electrostatic spinning is 1.0mL/h；The spacing of spray head to receiver board is 16cm；Ambient humidity
It is 35%；The drying carries out in a vacuum drying oven；
S3, film is placed in Muffle furnace, in air atmosphere, 260 DEG C of work is warming up to the heating rate of 2.5 DEG C/min
Change 4h, be subsequently placed in tube furnace, in an inert atmosphere, 630 DEG C of carbonization 2h be warming up to the heating rate of 4 DEG C/min, reacts
After it is cooling, obtain the high conductivity lithium ion battery negative material.
A kind of high conductivity lithium ion battery negative material that the present invention also proposes, using the high conductivity lithium-ion electric
The preparation method of pond negative electrode material is prepared.
Embodiment 7
A kind of preparation method of high conductivity lithium ion battery negative material proposed by the present invention, includes the following steps：
S1, molysite, mantoquita, conducting polymer are added in n,N-Dimethylformamide, heating stirring to transparence obtains
Spinning solution；Wherein, molysite, mantoquita mass ratio be 1：1；The molysite be ferric nitrate, iron chloride mixture, and ferric nitrate,
The weight ratio of iron chloride is 2：1；The mantoquita is copper acetate；The conducting polymer is the mixture of polyacrylonitrile, polyaniline,
And the weight ratio of polyacrylonitrile, polyaniline is 3：2；The temperature of heating stirring is 55 DEG C；
S2, spinning solution is subjected to electrostatic spinning injection, obtains film after dry；Wherein, in electrostatic spinning course of injection,
Spinning voltage is 12kV, and the driving velocity of electrostatic spinning is 2.0mL/h；The spacing of spray head to receiver board is 8cm；Ambient humidity is
50%；The drying carries out in a vacuum drying oven；
S3, film is placed in Muffle furnace, in air atmosphere, 300 DEG C of work is warming up to the heating rate of 1.5 DEG C/min
Change 2h, be subsequently placed in tube furnace, in an inert atmosphere, 600 DEG C of carbonization 4h be warming up to the heating rate of 6 DEG C/min, reacts
After it is cooling, obtain the high conductivity lithium ion battery negative material.
A kind of high conductivity lithium ion battery negative material that the present invention also proposes, using the high conductivity lithium-ion electric
The preparation method of pond negative electrode material is prepared.
Embodiment 8
A kind of preparation method of high conductivity lithium ion battery negative material proposed by the present invention, includes the following steps：
S1, molysite, mantoquita, conducting polymer are added in n,N-Dimethylformamide, heating stirring to transparence obtains
Spinning solution；Wherein, molysite, mantoquita mass ratio be 2：1；The molysite selects ferric nitrate；The mantoquita is copper acetate；It is described to lead
Electric polymer is polyaniline；The temperature of heating stirring is 60 DEG C；
S2, spinning solution is subjected to electrostatic spinning injection, obtains film after dry；Wherein, in electrostatic spinning course of injection,
Spinning voltage is 12kV, and the driving velocity of electrostatic spinning is 1.0mL/h；The spacing of spray head to receiver board is 12cm；Ambient humidity
It is 43%；The drying carries out in a vacuum drying oven；
S3, film is placed in Muffle furnace, in air atmosphere, 280 DEG C of activation is warming up to the heating rate of 2 DEG C/min
3h is subsequently placed in tube furnace, in argon atmosphere, is warming up to 600 DEG C of carbonization 2h, reaction knot with the heating rate of 5 DEG C/min
Cooling obtains the high conductivity lithium ion battery negative material after beam.
A kind of high conductivity lithium ion battery negative material that the present invention also proposes, using the high conductivity lithium-ion electric
The preparation method of pond negative electrode material is prepared.
Comparative example 1
A kind of preparation method of lithium ion battery negative material, includes the following steps：
S1,2g ferric nitrate, 1g copper acetate and 2g polyacrylonitrile (PAN) are added in 20mLN, dinethylformamide
(DMF) in, heating stirring 12h is at 60 DEG C to form homogeneous and transparent solution；
S2, the solution of above-mentioned preparation is placed in the syringe with metal needle, then this syringe is fixed on Static Spinning
The anode of silk device, and the anode of electrostatic spinning apparatus power supply is clipped on metal needle, aluminium film is laid in electrostatic spinning dress
On the collecting board set, and adjusting collecting board at a distance from metal needle is 14cm, and electrostatic spinning apparatus supply voltage is 15kV, note
The speed that pushes away of emitter is 1.0mL/h, carries out electrostatic spinning injection, obtains film after dry；
S3, film is placed in Muffle furnace, in air atmosphere, 280 DEG C of activation is risen to the heating rate of 2 DEG C/min
3h, then the product after activation is placed in tube furnace, 550 DEG C of carbonizations are risen to the heating rate of 5 DEG C/min in an inert atmosphere
2h obtains lithium ion battery negative material.
Comparative example 2
A kind of preparation method of lithium ion battery negative material, includes the following steps：
S1,2g ferric nitrate, 1g copper acetate and 2g polyacrylonitrile (PAN) are added in 20mLN, dinethylformamide
(DMF) in, heating stirring 12h is at 60 DEG C to form homogeneous and transparent solution；
S2, the solution of above-mentioned preparation is placed in the syringe with metal needle, then this syringe is fixed on Static Spinning
The anode of silk device, and the anode of electrostatic spinning apparatus power supply is clipped on metal needle, aluminium film is laid in electrostatic spinning dress
On the collecting board set, and adjusting collecting board at a distance from metal needle is 14cm, and the speed that pushes away of voltage 15kV, syringe are
1.0mL/h carries out drying after electrostatic spinning, obtains film；
S3, film is placed in Muffle furnace, in air atmosphere, rises to 280 DEG C with the heating rate of 2 DEG C/min, activation
3h, then the product after activation is placed in tube furnace, in an inert atmosphere, 700 DEG C of carbonizations are risen to the heating rate of 5 DEG C/min
2h。
Fig. 1 is the XRD diagram of material prepared by the embodiment of the present invention 1, comparative example 1 and comparative example 2, as shown in Figure 1, carbonization temperature
Different its of degree ultimately generates product difference, is carbonized at 600 DEG C in embodiment 1, obtain be ferroso-ferric oxide, iron,
Copper and carbon nano-fiber composite material, i.e. Fe3O4/ Fe/Cu/CNFs composite material；And it is carried out at 550 DEG C in comparative example 1
Carbonization, obtains being ferroso-ferric oxide, copper and carbon nano-fiber composite material, i.e. Fe3O4/ Cu/CNFs composite material；And
When being carbonized at 700 DEG C in comparative example 2, obtain being cementite, copper, carbon nano-fiber composite material, i.e. Fe3C/Cu/CNFs is multiple
Condensation material.
Fig. 2 is the SEM figure of negative electrode material prepared by the embodiment of the present invention 1, and as shown in Figure 2, fiber is presented in the product of generation
Shape, diameter is in 250nm or so.
Fig. 3 is the multiplying power figure of negative electrode material prepared by the embodiment of the present invention 1, from the figure 3, it may be seen that negative electrode material is carrying out multiplying power
Performance is very outstanding when charge-discharge test.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of high conductivity lithium ion battery negative material, which is characterized in that include the following steps：
S1, molysite, mantoquita, conducting polymer are added in n,N-Dimethylformamide, heating stirring to transparence obtains spinning
Liquid；
S2, spinning solution is subjected to electrostatic spinning injection, obtains film after dry；
S3, carburizing reagent is carried out after activating film, obtains the high conductivity lithium ion battery negative material；Wherein, it activates
Temperature be 260-300 DEG C, time of activation is 2-4h；The temperature of carburizing reagent is 570-630 DEG C, and the time of carburizing reagent is
2-4h。
2. the preparation method of high conductivity lithium ion battery negative material according to claim 1, which is characterized in that in S1
In, molysite, mantoquita mass ratio be 1-4：5-1；Preferably, molysite, mantoquita mass ratio be 2：1.
3. the preparation method of high conductivity lithium ion battery negative material according to claim 1 or claim 2, which is characterized in that
In S1, the molysite is the mixture of one or more of ferric nitrate, iron chloride, ferric acetyl acetonade；Preferentially, the iron
Salt selects ferric nitrate.
4. the preparation method of high conductivity lithium ion battery negative material described in any one of -3 according to claim 1, feature
It is, in S1, the mantoquita is copper acetate.
5. the preparation method of high conductivity lithium ion battery negative material described in any one of -4 according to claim 1, feature
It is, in S1, the conducting polymer is one or more of polyacrylonitrile, polyaniline, polyvinylpyrrolidone
Mixture.
6. the preparation method of high conductivity lithium ion battery negative material described in any one of -5 according to claim 1, feature
It is, in S1, the temperature of heating stirring is 55-65 DEG C；Preferably, the temperature of heating stirring is 60 DEG C.
7. the preparation method of high conductivity lithium ion battery negative material described in any one of -6 according to claim 1, feature
It is, in S2, in electrostatic spinning course of injection, spinning voltage 12-18kV, the driving velocity of electrostatic spinning is 1.0-
2.0mL/h；The spacing of spray head to receiver board is 8-16cm；Ambient humidity is 35%-50%；Preferably, spinning voltage 12-
14kV, the driving velocity of electrostatic spinning are 1.0-1.3mL/h；The spacing of spray head to receiver board is 14-16cm；Ambient humidity is
40%-45%；Preferably, spinning voltage 12kV, the driving velocity of electrostatic spinning are 1.0mL/h；Spray head is between receiver board
Away from for 12cm；Ambient humidity is 43%.
8. the preparation method of high conductivity lithium ion battery negative material described in any one of -7 according to claim 1, feature
It is, in S3, the carburizing reagent carries out in an inert atmosphere.
9. the preparation method of high conductivity lithium ion battery negative material described in any one of -8 according to claim 1, feature
It is, the concrete technology of S3 is：Film is placed in Muffle furnace, in air atmosphere, with the heating rate of 1.5-2.5 DEG C/min
It is warming up to 260-300 DEG C of activation 2-4h, is subsequently placed in tube furnace, in an inert atmosphere, with the heating rate liter of 4-6 DEG C/min
Temperature cools down after reaction to 570-630 DEG C of carbonization 2-4h, obtains the high conductivity lithium ion battery negative material；It is preferred that
The concrete technology on ground, S3 is：Film is placed in Muffle furnace, in air atmosphere, is warming up to the heating rate of 2 DEG C/min
280 DEG C of activation 3h, are subsequently placed in tube furnace, in argon atmosphere, are warming up to 600 DEG C of carbonizations with the heating rate of 5 DEG C/min
2h, cooling obtains the high conductivity lithium ion battery negative material after reaction.
10. a kind of high conductivity lithium ion battery negative material, which is characterized in that using such as any one of claim 1-9 institute
The preparation method for stating high conductivity lithium ion battery negative material is prepared.
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