CN107123805A - A kind of nano-silicone wire/carbon composite material and preparation method thereof - Google Patents

A kind of nano-silicone wire/carbon composite material and preparation method thereof Download PDF

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CN107123805A
CN107123805A CN201710515424.5A CN201710515424A CN107123805A CN 107123805 A CN107123805 A CN 107123805A CN 201710515424 A CN201710515424 A CN 201710515424A CN 107123805 A CN107123805 A CN 107123805A
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parts
nano
mixture
composite material
carbon composite
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程三岗
李宝玉
陈枫
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In Guosheng Battery Technology (beijing) Co Ltd
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In Guosheng Battery Technology (beijing) Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • 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
    • 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
    • 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
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/386—Silicon or alloys based on silicon
    • 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
    • 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 kind of nano-silicone wire/carbon composite material, it is made up of the raw material below according to parts by weight：65 70 parts of nano silica fume, 100 110 parts of graphite, 6 10 parts of sodium methyl silicate, 35 parts of TBAB, 18 22 parts of triphenylphosphine radium chloride, 210 230 parts of dimethyl ether, 30 35 parts of maleimide, 23 27 parts of polyvinylpyrrolidone.The invention also discloses the preparation method of the nano-silicone wire/carbon composite material.Nano-silicone wire/carbon composite material prepared by the present invention has good charge/discharge capacity and excellent cycle performance, market is disclosure satisfy that to the higher and higher performance requirement of nano-silicone wire/carbon composite material, with wide market prospects.

Description

A kind of nano-silicone wire/carbon composite material and preparation method thereof
Technical field
The present invention relates to technical field of lithium batteries, specifically a kind of nano-silicone wire/carbon composite material and preparation method thereof.
Background technology
With the development of society and science and technology, people propose higher requirement to the performance of lithium ion battery, and electrode material Material plays key effect in battery performance improvement.Currently, commercialized lithium ion battery generally uses graphite-like carbon material As anode material, due to the electrode relatively low theoretical electrochemistry capacity (theoretical capacity 372m Ah/g) limitation in itself, by changing Enter battery preparation technique and be difficult to make a breakthrough to improve battery performance, the lithium ion cell electrode of Novel high-specific capacity flexible The great urgency of exploitation of material.The metals such as Si, Sn and Sb are that people study more high-capacity anode materials, and wherein silicon has There are the theoretical electrochemistry capacity (theoretical capacity 4200m Ah/g) more than 10 times higher than now widely used carbon material, low embedding lithium Voltage (is less than 0.5V), and the common insertion of solvent molecule is not present in telescopiny, turns into the earth's crust the advantages of rich content One of preferred negative pole of high specific energy electrokinetic cell of future generation.But it is in addition embedding de- in electrochemistry because silicon materials electric conductivity itself is poor Serious bulk effect (the volume change produced during lithium：280%~310%), the destruction and mechanical efflorescence of material structure are caused, Cause between electrode material and electrode material and collector separation, and then lose electrical contact, cause the cycle performance of electrode drastically Decline.
At present it has been proposed that solving the method for this problem mainly has two kinds：One of method is exactly by silicon nanosizing.Because With the reduction of particle, the Volume Changes of silicon can be reduced to a certain extent, reduce electrode interior stress.But nano material exists Easily reunite in cyclic process, be insufficient to allow the performance improvement of battery to practical.Second, using nano-silicone wire/carbon composite material, i.e., Nano-silicon with electro-chemical activity or silicon alloy material are embedded in or loaded in carbon material, on the one hand carbon material can improve The electric conductivity of active silicon materials, another aspect carbon material can disperse as " cushioning frame " and buffer silicon materials in discharge and recharge During electrode interior stress caused by Volume Changes, the cyclical stability with nano-silicone wire/carbon composite material.
With the development of science and technology, market proposes higher and higher performance requirement to nano-silicone wire/carbon composite material, it is existing Nano-silicone wire/carbon composite material can not gradually meet the market demand in terms of capacity and cycle performance.Research and development capacity is higher, cyclicity Nano-silicone wire/carbon composite material that can be more excellent is by with important market value and social value.
The content of the invention
It is an object of the invention to provide a kind of nano-silicone wire/carbon composite material and preparation method thereof, to solve above-mentioned background skill The problem of being proposed in art.
To achieve the above object, the present invention provides following technical scheme：
A kind of nano-silicone wire/carbon composite material, is made up of the raw material below according to parts by weight：65-70 parts of nano silica fume, graphite 100-110 parts, 6-10 parts of sodium methyl silicate, 3-5 parts of TBAB, 18-22 parts of triphenylphosphine radium chloride, DPG two 210-230 parts of methyl ether, 30-35 parts of maleimide, 23-27 parts of polyvinylpyrrolidone.
It is used as further scheme of the invention：It is made up of the raw material below according to parts by weight：66-69 parts of nano silica fume, stone Black 102-108 parts, 7-9 parts of sodium methyl silicate, 3.5-4.5 parts of TBAB, 19-21 parts of triphenylphosphine radium chloride, dipropyl 215-225 parts of glycol dimethyl ether, 31-34 parts of maleimide, 24-26 parts of polyvinylpyrrolidone.
It is used as further scheme of the invention：It is made up of the raw material below according to parts by weight：67 parts of nano silica fume, graphite 105 parts, 8 parts of sodium methyl silicate, 4 parts of TBAB, 20 parts of triphenylphosphine radium chloride, 220 parts of dimethyl ether, horse Come 33 parts of acid imide, 25 parts of polyvinylpyrrolidone.
The preparation method of the nano-silicone wire/carbon composite material, step is as follows：
1) graphite and triphenylphosphine radium chloride are weighed, after merging, using ethanol as lapping liquid, ball milling mixing 2-3h is obtained Mixture A；
2) mixture A is put into the mix acid liquor of the concentrated sulfuric acid and concentrated nitric acid, in 50-55 DEG C, 150-200rpm bar Stir process 1-2h under part, then ultrasonication 40-45min, then reclaims ethanol at 75-80 DEG C, obtains mixture B；
3) mixture B is centrifuged, and the solid matter of acquisition is washed 3-4 times, dried at 80-90 DEG C It is dry, obtain mixture C；
4) nano silica fume, TBAB, dimethyl ether and polyvinylpyrrolidone are weighed, after merging, plus Enter mixture C, ball milling mixing 3-4h, then ultrasonication 1-2h, obtains mixture D；
5) mixture D is centrifuged, and the solid matter of acquisition is dried at 100-110 DEG C, obtained Mixture E；
6) sodium methyl silicate and maleimide are weighed, after merging, mixture E is added, adds mixture E gross mass 35-40% deionized water, then puts into super shearing dispersion machine, handles 1-2h, obtain mixture F together；
7) mixture F is subjected to vacuum revolving, then dried at 100-110 DEG C, obtain mixture G；
8) mixture G is put into microwave treater, 8-10min is handled under 2460-2480Mhz frequency, then The deionized water of 5-8 times of weight is added, ultrasonication 40min stands 24h, centrifuged, and to the solid matter water of acquisition Wash 3-4 times, dried at 80-90 DEG C, you can.
It is used as further scheme of the invention：Step 1) in, the consumption of the ethanol is graphite and triphenylphosphine chlorination 2-3 times of rhodium gross weight.
It is used as further scheme of the invention：Step 2) in, the ultrasonication frequency is 60-80KHz.
It is used as further scheme of the invention：Step 2) in, the mass fraction of the concentrated sulfuric acid is 98%, concentrated nitric acid Mass fraction is 70%.
It is used as further scheme of the invention：Step 2) in, the volume ratio of the concentrated sulfuric acid and concentrated nitric acid is 2:1.
It is used as further scheme of the invention：Step 4) in, the ultrasonication frequency is 100-120KHz.
It is used as further scheme of the invention：Step 8) in, the ultrasonication frequency is 90KHz.
Compared with prior art, the beneficial effects of the invention are as follows：
Nano-silicone wire/carbon composite material prepared by the present invention has good charge/discharge capacity and excellent cycle performance, energy Market is enough met to the higher and higher performance requirement of nano-silicone wire/carbon composite material, with wide market prospects.
Embodiment
Technical scheme is described in more detail with reference to embodiment.
Embodiment 1
A kind of nano-silicone wire/carbon composite material, is made up of the raw material below according to parts by weight：65 parts of nano silica fume, graphite 100 Part, 6 parts of sodium methyl silicate, 3 parts of TBAB, 18 parts of triphenylphosphine radium chloride, 210 parts of dimethyl ether, Malaysia 30 parts of acid imide, 23 parts of polyvinylpyrrolidone.
In the present embodiment, the preparation method of the nano-silicone wire/carbon composite material, step is as follows：
1) graphite and triphenylphosphine radium chloride are weighed, after merging, using ethanol as lapping liquid, ball milling mixing 2h is mixed Compound A, wherein, the consumption of the ethanol is 2 times of graphite and triphenylphosphine radium chloride gross weight；
2) mixture A is put into the mix acid liquor of the concentrated sulfuric acid and concentrated nitric acid, stirred under conditions of 50 DEG C, 150rpm 1h is handled, then ultrasonication 40min, ethanol is then reclaimed at 75 DEG C, obtain mixture B, wherein, at the ultrasonic wave Reason frequency is 60KHz, and the mass fraction of the concentrated sulfuric acid is 98%, and the mass fraction of concentrated nitric acid is 70%, the concentrated sulfuric acid and The volume ratio of concentrated nitric acid is 2:1；
3) mixture B is centrifuged, and the solid matter of acquisition is washed 3 times, dried, obtained at 80 DEG C Obtain mixture C；
4) nano silica fume, TBAB, dimethyl ether and polyvinylpyrrolidone are weighed, after merging, plus Enter mixture C, ball milling mixing 3h, then ultrasonication 1h, obtains mixture D, wherein, the ultrasonication frequency is 100KHz；
5) mixture D is centrifuged, and the solid matter of acquisition is dried at 100 DEG C, mixed Thing E；
6) sodium methyl silicate and maleimide are weighed, after merging, mixture E is added, adds mixture E gross mass 35% deionized water, then puts into super shearing dispersion machine, handles 1h, obtain mixture F together；
7) mixture F is subjected to vacuum revolving, then dried at 100 DEG C, obtain mixture G；
8) mixture G is put into microwave treater, 8min is handled under 2460Mhz frequency, then add 5 times of weights The deionized water of amount, ultrasonication 40min stands 24h, centrifuges, and the solid matter of acquisition is washed 3 times, 80 Dried at DEG C, you can, wherein, the ultrasonication frequency is 90KHz.
Embodiment 2
A kind of nano-silicone wire/carbon composite material, is made up of the raw material below according to parts by weight：66 parts of nano silica fume, graphite 102 Part, 9 parts of sodium methyl silicate, 4.5 parts of TBAB, 19 parts of triphenylphosphine radium chloride, 215 parts of dimethyl ether, horse Come 34 parts of acid imide, 26 parts of polyvinylpyrrolidone.
In the present embodiment, the preparation method of the nano-silicone wire/carbon composite material, step is as follows：
1) graphite and triphenylphosphine radium chloride are weighed, after merging, using ethanol as lapping liquid, ball milling mixing 2.5h is obtained Mixture A, wherein, the consumption of the ethanol is 2.3 times of graphite and triphenylphosphine radium chloride gross weight；
2) mixture A is put into the mix acid liquor of the concentrated sulfuric acid and concentrated nitric acid, stirred under conditions of 51 DEG C, 160rpm 1h is handled, then ultrasonication 42min, ethanol is then reclaimed at 75 DEG C, obtain mixture B, wherein, at the ultrasonic wave Reason frequency is 70KHz, and the mass fraction of the concentrated sulfuric acid is 98%, and the mass fraction of concentrated nitric acid is 70%, the concentrated sulfuric acid and The volume ratio of concentrated nitric acid is 2:1；
3) mixture B is centrifuged, and the solid matter of acquisition is washed 4 times, dried, obtained at 85 DEG C Obtain mixture C；
4) nano silica fume, TBAB, dimethyl ether and polyvinylpyrrolidone are weighed, after merging, plus Enter mixture C, ball milling mixing 3h, then ultrasonication 1.5h, obtains mixture D, wherein, the ultrasonication frequency is 100KHz；
5) mixture D is centrifuged, and the solid matter of acquisition is dried at 100 DEG C, mixed Thing E；
6) sodium methyl silicate and maleimide are weighed, after merging, mixture E is added, adds mixture E gross mass 37% deionized water, then puts into super shearing dispersion machine, handles 1.5h, obtain mixture F together；
7) mixture F is subjected to vacuum revolving, then dried at 100 DEG C, obtain mixture G；
8) mixture G is put into microwave treater, 8min is handled under 2460Mhz frequency, then add 6 times of weights The deionized water of amount, ultrasonication 40min stands 24h, centrifuges, and the solid matter of acquisition is washed 3 times, 85 Dried at DEG C, you can, wherein, the ultrasonication frequency is 90KHz.
Embodiment 3
A kind of nano-silicone wire/carbon composite material, is made up of the raw material below according to parts by weight：67 parts of nano silica fume, graphite 105 Part, 8 parts of sodium methyl silicate, 4 parts of TBAB, 20 parts of triphenylphosphine radium chloride, 220 parts of dimethyl ether, Malaysia 33 parts of acid imide, 25 parts of polyvinylpyrrolidone.
In the present embodiment, the preparation method of the nano-silicone wire/carbon composite material, step is as follows：
1) graphite and triphenylphosphine radium chloride are weighed, after merging, using ethanol as lapping liquid, ball milling mixing 2.5h is obtained Mixture A, wherein, the consumption of the ethanol is 2.5 times of graphite and triphenylphosphine radium chloride gross weight；
2) mixture A is put into the mix acid liquor of the concentrated sulfuric acid and concentrated nitric acid, stirred under conditions of 52 DEG C, 170rpm 1.5h is handled, then ultrasonication 42min, ethanol is then reclaimed at 78 DEG C, obtain mixture B, wherein, the ultrasonic wave Processing frequency is 70KHz, and the mass fraction of the concentrated sulfuric acid is 98%, and the mass fraction of concentrated nitric acid is 70%, the concentrated sulfuric acid Volume ratio with concentrated nitric acid is 2:1；
3) mixture B is centrifuged, and the solid matter of acquisition is washed 4 times, dried, obtained at 85 DEG C Obtain mixture C；
4) nano silica fume, TBAB, dimethyl ether and polyvinylpyrrolidone are weighed, after merging, plus Enter mixture C, ball milling mixing 3.5h, then ultrasonication 1.5h, obtains mixture D, wherein, the ultrasonication frequency For 11KHz；
5) mixture D is centrifuged, and the solid matter of acquisition is dried at 105 DEG C, mixed Thing E；
6) sodium methyl silicate and maleimide are weighed, after merging, mixture E is added, adds mixture E gross mass 38% deionized water, then puts into super shearing dispersion machine, handles 1.5h, obtain mixture F together；
7) mixture F is subjected to vacuum revolving, then dried at 105 DEG C, obtain mixture G；
8) mixture G is put into microwave treater, 9min is handled under 2470Mhz frequency, then add 6 times of weights The deionized water of amount, ultrasonication 40min stands 24h, centrifuges, and the solid matter of acquisition is washed 4 times, 85 Dried at DEG C, you can, wherein, the ultrasonication frequency is 90KHz.
Embodiment 4
A kind of nano-silicone wire/carbon composite material, is made up of the raw material below according to parts by weight：69 parts of nano silica fume, graphite 108 Part, 7 parts of sodium methyl silicate, 3.5 parts of TBAB, 21 parts of triphenylphosphine radium chloride, 225 parts of dimethyl ether, horse Come 31 parts of acid imide, 24 parts of polyvinylpyrrolidone.
In the present embodiment, the preparation method of the nano-silicone wire/carbon composite material, step is as follows：
1) graphite and triphenylphosphine radium chloride are weighed, after merging, using ethanol as lapping liquid, ball milling mixing 2.5h is obtained Mixture A, wherein, the consumption of the ethanol is 3 times of graphite and triphenylphosphine radium chloride gross weight；
2) mixture A is put into the mix acid liquor of the concentrated sulfuric acid and concentrated nitric acid, stirred under conditions of 55 DEG C, 180rpm 1.5h is handled, then ultrasonication 45min, ethanol is then reclaimed at 80 DEG C, obtain mixture B, wherein, the ultrasonic wave Processing frequency is 70KHz, and the mass fraction of the concentrated sulfuric acid is 98%, and the mass fraction of concentrated nitric acid is 70%, the concentrated sulfuric acid Volume ratio with concentrated nitric acid is 2:1；
3) mixture B is centrifuged, and the solid matter of acquisition is washed 3 times, dried, obtained at 85 DEG C Obtain mixture C；
4) nano silica fume, TBAB, dimethyl ether and polyvinylpyrrolidone are weighed, after merging, plus Enter mixture C, ball milling mixing 3.5h, then ultrasonication 2h, obtains mixture D, wherein, the ultrasonication frequency is 110KHz；
5) mixture D is centrifuged, and the solid matter of acquisition is dried at 110 DEG C, mixed Thing E；
6) sodium methyl silicate and maleimide are weighed, after merging, mixture E is added, adds mixture E gross mass 40% deionized water, then puts into super shearing dispersion machine, handles 1.5h, obtain mixture F together；
7) mixture F is subjected to vacuum revolving, then dried at 110 DEG C, obtain mixture G；
8) mixture G is put into microwave treater, 9min is handled under 2480Mhz frequency, then add 7 times of weights The deionized water of amount, ultrasonication 40min stands 24h, centrifuges, and the solid matter of acquisition is washed 4 times, 85 Dried at DEG C, you can, wherein, the ultrasonication frequency is 90KHz.
Embodiment 5
A kind of nano-silicone wire/carbon composite material, is made up of the raw material below according to parts by weight：70 parts of nano silica fume, graphite 110 Part, 10 parts of sodium methyl silicate, 5 parts of TBAB, 22 parts of triphenylphosphine radium chloride, 230 parts of dimethyl ether, Malaysia 35 parts of acid imide, 27 parts of polyvinylpyrrolidone.
In the present embodiment, the preparation method of the nano-silicone wire/carbon composite material, step is as follows：
1) graphite and triphenylphosphine radium chloride are weighed, after merging, using ethanol as lapping liquid, ball milling mixing 3h is mixed Compound A, wherein, the consumption of the ethanol is 3 times of graphite and triphenylphosphine radium chloride gross weight；
2) mixture A is put into the mix acid liquor of the concentrated sulfuric acid and concentrated nitric acid, stirred under conditions of 55 DEG C, 200rpm 2h is handled, then ultrasonication 45min, ethanol is then reclaimed at 80 DEG C, obtain mixture B, wherein, at the ultrasonic wave Reason frequency is 80KHz, and the mass fraction of the concentrated sulfuric acid is 98%, and the mass fraction of concentrated nitric acid is 70%, the concentrated sulfuric acid and The volume ratio of concentrated nitric acid is 2:1；
3) mixture B is centrifuged, and the solid matter of acquisition is washed 4 times, dried, obtained at 90 DEG C Obtain mixture C；
4) nano silica fume, TBAB, dimethyl ether and polyvinylpyrrolidone are weighed, after merging, plus Enter mixture C, ball milling mixing 4h, then ultrasonication 2h, obtains mixture D, wherein, the ultrasonication frequency is 120KHz；
5) mixture D is centrifuged, and the solid matter of acquisition is dried at 110 DEG C, mixed Thing E；
6) sodium methyl silicate and maleimide are weighed, after merging, mixture E is added, adds mixture E gross mass 40% deionized water, then puts into super shearing dispersion machine, handles 2h, obtain mixture F together；
7) mixture F is subjected to vacuum revolving, then dried at 110 DEG C, obtain mixture G；
8) mixture G is put into microwave treater, 10min is handled under 2480Mhz frequency, then add 8 times The deionized water of weight, ultrasonication 40min stands 24h, centrifuges, and the solid matter of acquisition is washed 4 times, Dried at 90 DEG C, you can, wherein, the ultrasonication frequency is 90KHz.
Electrode of lithium cell is made in nano-silicone wire/carbon composite material prepared by 1-5 of the embodiment of the present invention：With obtained nanometer Si-C composite material is active material, and Super-P carbon blacks are conductive agent, and PVDF is binding agent, and in mass ratio 7: 2: 1 are well mixed Afterwards, it is that solvent is sized mixing with 1-METHYLPYRROLIDONE, slurry is coated in the pole that 1.0cm × 1.5cm is made on the copper foil of 8 μ m-thicks Piece, the thickness needed for 70 DEG C of dry back rollers are depressed into pole piece dries 12h under 120 DEG C of vacuum, standby.Using metal lithium sheet as to electricity Pole, the films of Celgard 2300 are barrier film, 1mol/L LiPF6/ EC+DEC+DMC (volume ratio 1: 1: 1) is that electrolyte assembles experiment Battery (designed, designed, diameter of phi=30mm, long L=100mm).Test real with indigo plant electricity battery test system CT2001A testers The charge-discharge performance in electrical verification pond.Charging/discharging voltage scope is 0.005-2.0V, charging and discharging currents density 80mA/g, and test battery is followed The ring capability retention of 100 weeks.
Test result is as follows：Discharge capacity is 968.2-983.6mAh/g first, and coulombic efficiency is 90.5- first 92.7%, capability retention is 95.3-98.5% after circulation in 100 weeks.
Nano-silicone wire/carbon composite material prepared by the present invention has good charge/discharge capacity and excellent cycle performance, energy Market is enough met to the higher and higher performance requirement of nano-silicone wire/carbon composite material, with wide market prospects.
The better embodiment to the present invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment party , can also be on the premise of present inventive concept not be departed from formula, the knowledge that one skilled in the relevant art possesses Various changes can be made.

Claims (10)

1. a kind of nano-silicone wire/carbon composite material, it is characterised in that be made up of the raw material below according to parts by weight：Nano silica fume 65- 70 parts, 100-110 parts of graphite, 6-10 parts of sodium methyl silicate, 3-5 parts of TBAB, 18-22 parts of triphenylphosphine radium chloride, 210-230 parts of dimethyl ether, 30-35 parts of maleimide, 23-27 parts of polyvinylpyrrolidone.
2. nano-silicone wire/carbon composite material according to claim 1, it is characterised in that by below according to the raw material system of parts by weight Into：66-69 parts of nano silica fume, 102-108 parts of graphite, 7-9 parts of sodium methyl silicate, 3.5-4.5 parts of TBAB, triphenyl 19-21 parts of phosphine radium chloride, 215-225 parts of dimethyl ether, 31-34 parts of maleimide, polyvinylpyrrolidone 24-26 Part.
3. nano-silicone wire/carbon composite material according to claim 2, it is characterised in that by below according to the raw material system of parts by weight Into：67 parts of nano silica fume, 105 parts of graphite, 8 parts of sodium methyl silicate, 4 parts of TBAB, 20 parts of triphenylphosphine radium chloride, two 220 parts of Propylene Glycol Dimethyl Ether, 33 parts of maleimide, 25 parts of polyvinylpyrrolidone.
4. the preparation method of a kind of nano-silicone wire/carbon composite material as described in claim 1-3 is any, it is characterised in that step is such as Under：
1) graphite and triphenylphosphine radium chloride are weighed, after merging, using ethanol as lapping liquid, ball milling mixing 2-3h is mixed Thing A；
2) mixture A is put into the mix acid liquor of the concentrated sulfuric acid and concentrated nitric acid, under conditions of 50-55 DEG C, 150-200rpm Stir process 1-2h, then ultrasonication 40-45min, then reclaims ethanol at 75-80 DEG C, obtains mixture B；
3) mixture B is centrifuged, and the solid matter of acquisition is washed 3-4 times, dried at 80-90 DEG C, Obtain mixture C；
4) nano silica fume, TBAB, dimethyl ether and polyvinylpyrrolidone are weighed, after merging, is added mixed Compound C, ball milling mixing 3-4h, then ultrasonication 1-2h, obtains mixture D；
5) mixture D is centrifuged, and the solid matter of acquisition is dried at 100-110 DEG C, mixed Thing E；
6) sodium methyl silicate and maleimide are weighed, after merging, mixture E is added, adds mixture E gross mass 35- 40% deionized water, then puts into super shearing dispersion machine, handles 1-2h, obtain mixture F together；
7) mixture F is subjected to vacuum revolving, then dried at 100-110 DEG C, obtain mixture G；
8) mixture G is put into microwave treater, 8-10min is handled under 2460-2480Mhz frequency, is then added The deionized water of 5-8 times of weight, ultrasonication 40min stands 24h, centrifuges, and washes 3- to the solid matter of acquisition 4 times, dried at 80-90 DEG C, you can.
5. the preparation method of nano-silicone wire/carbon composite material according to claim 4, it is characterised in that step 1) in, it is described The consumption of ethanol is 2-3 times of graphite and triphenylphosphine radium chloride gross weight.
6. the preparation method of nano-silicone wire/carbon composite material according to claim 4, it is characterised in that step 2) in, it is described Ultrasonication frequency is 60-80KHz.
7. the preparation method of nano-silicone wire/carbon composite material according to claim 4, it is characterised in that step 2) in, it is described The mass fraction of the concentrated sulfuric acid is 98%, and the mass fraction of concentrated nitric acid is 70%.
8. the preparation method of nano-silicone wire/carbon composite material according to claim 7, it is characterised in that step 2) in, it is described The volume ratio of the concentrated sulfuric acid and concentrated nitric acid is 2:1.
9. the preparation method of nano-silicone wire/carbon composite material according to claim 4, it is characterised in that step 4) in, it is described Ultrasonication frequency is 100-120KHz.
10. the preparation method of nano-silicone wire/carbon composite material according to claim 4, it is characterised in that step 8) in, it is described Ultrasonication frequency is 90KHz.
CN201710515424.5A 2017-06-29 2017-06-29 A kind of nano-silicone wire/carbon composite material and preparation method thereof Pending CN107123805A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103050668A (en) * 2012-12-24 2013-04-17 中南大学 Method for preparing Si/C composite cathode material for lithium ion battery
CN104362300A (en) * 2014-12-02 2015-02-18 南京工业大学 Preparation method of silicon-carbon composite negative electrode material of lithium ion battery and application of silicon-carbon composite negative electrode material
CN105355870A (en) * 2015-10-22 2016-02-24 清华大学深圳研究生院 Expanded graphite and nano-silicon composite material, preparation method thereof, electrode plate and battery

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103050668A (en) * 2012-12-24 2013-04-17 中南大学 Method for preparing Si/C composite cathode material for lithium ion battery
CN104362300A (en) * 2014-12-02 2015-02-18 南京工业大学 Preparation method of silicon-carbon composite negative electrode material of lithium ion battery and application of silicon-carbon composite negative electrode material
CN105355870A (en) * 2015-10-22 2016-02-24 清华大学深圳研究生院 Expanded graphite and nano-silicon composite material, preparation method thereof, electrode plate and battery

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