CN106783218A - A kind of battery graphene complex material and preparation method thereof - Google Patents

A kind of battery graphene complex material and preparation method thereof Download PDF

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CN106783218A
CN106783218A CN201611248439.1A CN201611248439A CN106783218A CN 106783218 A CN106783218 A CN 106783218A CN 201611248439 A CN201611248439 A CN 201611248439A CN 106783218 A CN106783218 A CN 106783218A
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王维根
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Taizhou Dragon Valley Mdt InfoTech Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/32Carbon-based
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/32Carbon-based
    • H01G11/38Carbon pastes or blends; Binders or additives therein
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
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    • H01G11/48Conductive polymers
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
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    • H01M4/364Composites as mixtures
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/58Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624Electric conductive fillers
    • H01M4/625Carbon or graphite
    • YGENERAL 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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    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract

This application discloses a kind of battery graphene complex material and preparation method thereof, raw material is trimethylolpropane polyoxyethylene polyoxypropylene ether, hydrofluoric acid, nano-silicon, graphite, polytetrafluoroethylene (PTFE), absolute ethyl alcohol, cobalt acid lithium, sodium acid carbonate, titanium dioxide, 1,2 dichloroethanes, potassium nitrate, titanium carbide, acetone, octane, toluene, tetrahydrofuran and ethylenediamine tetra-acetic acid;Process is simple, mild condition, with good electric conductivity, capacity is big, energy density is high, good cycle;Low in raw material price, operation is simple, circulates 300 500 times, capacity 600mAh;Easy to operate, quality and yield are easy to control;Large-scale instrument and equipment is not relied on, high-quality battery Graphene is capable of achieving and is mass produced, can extensively produced and constantly replace current material.

Description

A kind of battery graphene complex material and preparation method thereof
Technical field
The application belongs to the preparation field of grapheme material, more particularly to a kind of battery with graphene complex material and its Preparation method.
Background technology
The researcher of nearest Univ California-Los Angeles USA just develops a kind of miniature based on Graphene Ultracapacitor, the capacitor not only low-profile, and also charging rate is 1000 times of common batteries, can be within the several seconds Mobile phone even automobile charges, while can be used to manufacture the device of small volume.
As the most strong a kind of novel nano-material of the most thin, maximum intensity, electrical and thermal conductivity performance that have now been found that, Graphene It is referred to as " dark fund ", is " king of new material ", scientist even foretells that Graphene " will thoroughly change 21 century ".Very likely lift Play a subversiveness new technology new industrial revolution have swept the globe.
Actually Graphene is inherently present in nature, is simply difficult to separate single layer structure.Graphene is folded from level to level It is exactly hydrofluoric acid to get up, and thick 1 millimeter hydrofluoric acid comprises about 3,000,000 layer graphenes.Pencil is gently streaked on paper, is left Vestige may be several layers of or even an only layer graphene.
Miniature Graphene super capacitor technology is broken through and can be described as bringing revolutionary development to battery.Main manufacture at present The method of button capacitor is lithographic printing, it is necessary to put into substantial amounts of manpower and cost, hinders the business application of product. And common DVD burner is now only needed, and even stay at home, 30 minutes just can be on a CD using cheap material Manufacture more than 100 miniature Graphene super capacitor.
The scientific circles that appear in of Graphene have evoked huge great waves.It has been found that Graphene has unusual leading Electrical property, beyond the intensity and fabulous translucency of steel decades of times, its appearance is expected to trigger in hyundai electronicses sciemtifec and technical sphere One wheel revolution.In Graphene, electronics can be migrated extremely efficiently, and traditional semiconductor and conductor, such as silicon and copper are remote There is no Graphene show must well.Due to the collision of electronics and atom, the form of traditional semiconductor and conductor heat releases one A little energy, general computer chip wastes the electric energy of 72%-81% by this way within 2013, and Graphene is then different, its electricity Sub- energy will not be depleted, and this makes it be provided with extraordinary good characteristic.
China also has unique advantage in Graphene research, from a manufacturing perspective, as Graphene raw materials for production Hydrofluoric acid, it is abundant in China's energy storage, it is cheap.In addition, mass production and large scale production are to hinder Graphene extensive Commercial main factor.And the newest achievement in research of China has successfully broken through this two hang-up, manufacturing cost from 5000 yuan/ Gram 3 yuan/gram are down to, solve the volume production problem of this material.Successfully it is manufactured that using chemical vapour deposition technique domestic first 15 inches of single-layer graphene, and successfully graphene transparent electrode is applied on electric resistance touch screen, prepare 7 inches of stones Black alkene touch-screen.
The application prospect of Graphene is exactly seen, many countries set up Graphene correlation technique research and development centre, taste one after another Examination is commercialized using Graphene, and then acquisition potentially applies patent in industry, technology and electronic correlation field.EU Committee Using Graphene as " following emerging flagship technological project ", set up and transferred in special research and development plan, coming 10 years 1000000000 Euros of warps Take.British government also invests in national Graphene research institute (NGI), tries hard to make this material can be from coming few decades Laboratory enters production line and market.
Chinese Graphene industrial technology innovation strategic alliances lead Bei Terui, Zheng Tai group, the hexa-atomic element in Changzhou, BOCO to collect Hispanic Graphene meeting has been participated in the representative of Tuan Dengsijia listed companies, and is signed with Italy, delegation of Sweden respectively Depth strategic cooperation agreement, is that " the Graphene whole world is merged, and China integrates " the first shot was fired for strategy.Additionally, the whole world at the beginning of 3 months First batch of 30,000 volume production Graphene mobile phones are issued in Chongqing, open the New Times of Graphene commercial application.Graphene is selected in The planning of " 13 " new material makes a decision substantially, it is contemplated that 2015 will be as the Chinese Graphene industry outburst first year, with society Can urbanization, technicalization, the development of hommization, design it is a kind of be difficult to be destroyed, yield is high and the battery that is produced on a large scale is used Graphene complex material and preparation method thereof, it is with low cost, to meet the market demand, it is very important.
Graphenano companies of Spain (company for producing Graphene on an industrial scale) are with more than Spain Cole watt University's joint study goes out the first Graphene polymeric material battery, and its reserve of electricity is three times of the best product of existing market, with this electricity The electric motor car most multipotency that pond provides electric power travels 1000 kilometers, and its charging interval was less than 8 minutes.Although this battery has various Excellent performance, but its cost is not high.The related responsible person of Graphenano companies, the cost of this battery will be lower than lithium battery 77%, completely within consumer's tolerance range.Additionally, in fields such as automotive fuel cells, Graphene is expected to bring revolutionary character It is progressive.
The content of the invention
The technical problem of solution:
The application is for existing graphene complex low yield, stability difference and the technical problem such as cost is high, there is provided a kind of battery With graphene complex material and preparation method thereof.
Technical scheme:
A kind of battery graphene complex material, the battery is matched with the raw materials by weight portion of graphene complex material It is as follows:100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, hydrofluoric acid 5-25 parts, nano-silicon 4-8 parts, graphite 20-60 Part, polytetrafluoroethylene (PTFE) 1-5 parts, absolute ethyl alcohol 6-10 parts, cobalt acid lithium 8-12 parts, sodium acid carbonate 3-7 parts, titanium dioxide 1-5 parts, 1, 2 dichloroethanes 3-7 parts, potassium nitrate 30-50 parts, titanium carbide 0.5-4.5 parts, acetone 2-6 parts, octane 1.5-5.5 parts, toluene 4.5- 8.5 parts, tetrahydrofuran 15-35 parts, ethylenediamine tetra-acetic acid 10-30 parts.
As a preferred technical solution of the present invention:The battery raw material of graphene complex material is by weight Number proportioning is as follows:100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, 5 parts of hydrofluoric acid, 4 parts of nano-silicon, 20 parts of graphite, 1 part of polytetrafluoroethylene (PTFE), 6 parts of absolute ethyl alcohol, 8 parts of cobalt acid lithium, 3 parts of sodium acid carbonate, 1 part of titanium dioxide, 1,23 parts of dichloroethanes, nitre 30 parts of sour potassium, 0.5 part of titanium carbide, 2 parts of acetone, 1.5 parts of octane, 4.5 parts of toluene, 15 parts of tetrahydrofuran, ethylenediamine tetra-acetic acid 10 Part.
As a preferred technical solution of the present invention:The battery raw material of graphene complex material is by weight Number proportioning is as follows:100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, 25 parts of hydrofluoric acid, 8 parts of nano-silicon, 60 parts of graphite, 5 parts of polytetrafluoroethylene (PTFE), 10 parts of absolute ethyl alcohol, 12 parts of cobalt acid lithium, 7 parts of sodium acid carbonate, 5 parts of titanium dioxide, 1,27 parts of dichloroethanes, 50 parts of potassium nitrate, 4.5 parts of titanium carbide, 6 parts of acetone, 5.5 parts of octane, 8.5 parts of toluene, 35 parts of tetrahydrofuran, ethylenediamine tetra-acetic acid 30 parts.
As a preferred technical solution of the present invention:The battery raw material of graphene complex material is by weight Number proportioning is as follows:100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, 10 parts of hydrofluoric acid, 5 parts of nano-silicon, 30 parts of graphite, 2 parts of polytetrafluoroethylene (PTFE), 7 parts of absolute ethyl alcohol, 9 parts of cobalt acid lithium, 4 parts of sodium acid carbonate, 2 parts of titanium dioxide, 1,24 parts of dichloroethanes, nitre 35 parts of sour potassium, 1.5 parts of titanium carbide, 3 parts of acetone, 2.5 parts of octane, 5.5 parts of toluene, 20 parts of tetrahydrofuran, ethylenediamine tetra-acetic acid 15 Part.
As a preferred technical solution of the present invention:The battery raw material of graphene complex material is by weight Number proportioning is as follows:100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, 20 parts of hydrofluoric acid, 7 parts of nano-silicon, 50 parts of graphite, 4 parts of polytetrafluoroethylene (PTFE), 9 parts of absolute ethyl alcohol, 11 parts of cobalt acid lithium, 6 parts of sodium acid carbonate, 4 parts of titanium dioxide, 1,26 parts of dichloroethanes, 45 parts of potassium nitrate, 3.5 parts of titanium carbide, 5 parts of acetone, 4.5 parts of octane, 7.5 parts of toluene, 30 parts of tetrahydrofuran, ethylenediamine tetra-acetic acid 25 parts.
As a preferred technical solution of the present invention:The battery raw material of graphene complex material is by weight Number proportioning is as follows:100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, 15 parts of hydrofluoric acid, 6 parts of nano-silicon, 40 parts of graphite, 3 parts of polytetrafluoroethylene (PTFE), 5 parts of absolute ethyl alcohol, 10 parts of cobalt acid lithium, 5 parts of sodium acid carbonate, 3 parts of titanium dioxide, 1,25 parts of dichloroethanes, 40 parts of potassium nitrate, 2.5 parts of titanium carbide, 4 parts of acetone, 3.5 parts of octane, 6.5 parts of toluene, 25 parts of tetrahydrofuran, ethylenediamine tetra-acetic acid 20 parts.
A kind of battery preparation method of graphene complex material, comprises the following steps:
The first step:Proportioning weighs trimethylolpropane polyoxyethylene polyoxypropylene ether, hydrofluoric acid, nano-silicon, stone by weight Ink, polytetrafluoroethylene (PTFE), absolute ethyl alcohol, cobalt acid lithium, sodium acid carbonate, titanium dioxide, 1,2 dichloroethanes, potassium nitrate, titanium carbide, third Ketone, octane, toluene, tetrahydrofuran and ethylenediamine tetra-acetic acid;
Second step:By in nano-silicon and graphite reactor of the input with agitator and thermometer, 450-550 DEG C is warming up to, stirred 30-40min is mixed, surplus stock is added, ground 30-50 minutes in grinder, dried at 65-75 DEG C of input after grinding is uniform 50-60min;
3rd step:Dried raw material is placed in ceramic crucible with cover, then ceramic crucible with cover is put into tube furnace 450-550 DEG C is first heated under high pure nitrogen protection, insulation reaction 1-3 hours, 700-800 is then further heated to DEG C, insulation reaction 2-4 hours, battery graphene complex material is obtained.
Beneficial effect:
A kind of battery of the present invention uses above technical scheme and existing skill with graphene complex material and preparation method thereof Art is compared, with following technique effect:1st, process is simple, mild condition, with good electric conductivity, capacity be big, energy density High, good cycle;2nd, low in raw material price, operation is simple, circulates 300-500 times, capacity 600mAh;It is 3rd, easy to operate, Quality and yield are easy to control;4th, large-scale instrument and equipment is not relied on, high-quality battery Graphene is capable of achieving and is mass produced, can With production extensively and constantly instead of current material.
Specific embodiment
Embodiment 1:
Proportioning weighs 100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, 5 parts of hydrofluoric acid, nano-silicon 4 by weight Part, 20 parts of graphite, 1 part of polytetrafluoroethylene (PTFE), 6 parts of absolute ethyl alcohol, 8 parts of cobalt acid lithium, 3 parts of sodium acid carbonate, 1 part of titanium dioxide, 1,2 two 3 parts of chloroethanes, 30 parts of potassium nitrate, 0.5 part of titanium carbide, 2 parts of acetone, 1.5 parts of octane, 4.5 parts of toluene, 15 parts of tetrahydrofuran, second 10 parts of ethylenediamine tetraacetic acid (EDTA).
By in nano-silicon and graphite reactor of the input with agitator and thermometer, 450 DEG C are warming up to, stir 30min, Surplus stock is added, is ground 30 minutes in grinder, 50min is dried at 65 DEG C of input after grinding is uniform.
Dried raw material is placed in ceramic crucible with cover, then ceramic crucible with cover is put into tube furnace in height 450 DEG C are first heated under purity nitrogen gas shielded, then insulation reaction 1 hour is further heated to 700 DEG C, and insulation reaction 2 is small When, battery graphene complex material is obtained.
Process is simple, mild condition, with good electric conductivity, capacity is big, energy density is high, good cycle;Raw material Cheap, operation is simple, circulates 300 times, capacity 600mAh;Easy to operate, quality and yield are easy to control;Do not rely on big Type instrument and equipment, is capable of achieving high-quality battery Graphene and mass produces, and can extensively produce and constantly replace current material.
Embodiment 2:
Proportioning weighs 100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, 25 parts of hydrofluoric acid, nano-silicon 8 by weight Part, 60 parts of graphite, 5 parts of polytetrafluoroethylene (PTFE), 10 parts of absolute ethyl alcohol, 12 parts of cobalt acid lithium, 7 parts of sodium acid carbonate, 5 parts of titanium dioxide, 1,2 7 parts of dichloroethanes, 50 parts of potassium nitrate, 4.5 parts of titanium carbide, 6 parts of acetone, 5.5 parts of octane, 8.5 parts of toluene, 35 parts of tetrahydrofuran, 30 parts of ethylenediamine tetra-acetic acid.
By in nano-silicon and graphite reactor of the input with agitator and thermometer, 550 DEG C are warming up to, stir 40min, Surplus stock is added, is ground 50 minutes in grinder, 60min is dried at 75 DEG C of input after grinding is uniform.
Dried raw material is placed in ceramic crucible with cover, then ceramic crucible with cover is put into tube furnace in height 550 DEG C are first heated under purity nitrogen gas shielded, then insulation reaction 3 hours is further heated to 800 DEG C, and insulation reaction 4 is small When, battery graphene complex material is obtained.
Process is simple, mild condition, with good electric conductivity, capacity is big, energy density is high, good cycle;Raw material Cheap, operation is simple, circulates 350 times, capacity 600mAh;Easy to operate, quality and yield are easy to control;Do not rely on big Type instrument and equipment, is capable of achieving high-quality battery Graphene and mass produces, and can extensively produce and constantly replace current material.
Embodiment 3:
Proportioning weighs 100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, 10 parts of hydrofluoric acid, nano-silicon 5 by weight Part, 30 parts of graphite, 2 parts of polytetrafluoroethylene (PTFE), 7 parts of absolute ethyl alcohol, 9 parts of cobalt acid lithium, 4 parts of sodium acid carbonate, 2 parts of titanium dioxide, 1,2 two 4 parts of chloroethanes, 35 parts of potassium nitrate, 1.5 parts of titanium carbide, 3 parts of acetone, 2.5 parts of octane, 5.5 parts of toluene, 20 parts of tetrahydrofuran, second 15 parts of ethylenediamine tetraacetic acid (EDTA).
By in nano-silicon and graphite reactor of the input with agitator and thermometer, 450 DEG C are warming up to, stir 30min, Surplus stock is added, is ground 30 minutes in grinder, 50min is dried at 65 DEG C of input after grinding is uniform.
Dried raw material is placed in ceramic crucible with cover, then ceramic crucible with cover is put into tube furnace in height 450 DEG C are first heated under purity nitrogen gas shielded, then insulation reaction 1 hour is further heated to 700 DEG C, and insulation reaction 2 is small When, battery graphene complex material is obtained.
Process is simple, mild condition, with good electric conductivity, capacity is big, energy density is high, good cycle;Raw material Cheap, operation is simple, circulates 400 times, capacity 600mAh;Easy to operate, quality and yield are easy to control;Do not rely on big Type instrument and equipment, is capable of achieving high-quality battery Graphene and mass produces, and can extensively produce and constantly replace current material.
Embodiment 4:
Proportioning weighs 100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, 20 parts of hydrofluoric acid, nano-silicon 7 by weight Part, 50 parts of graphite, 4 parts of polytetrafluoroethylene (PTFE), 9 parts of absolute ethyl alcohol, 11 parts of cobalt acid lithium, 6 parts of sodium acid carbonate, 4 parts of titanium dioxide, 1,2 6 parts of dichloroethanes, 45 parts of potassium nitrate, 3.5 parts of titanium carbide, 5 parts of acetone, 4.5 parts of octane, 7.5 parts of toluene, 30 parts of tetrahydrofuran, 25 parts of ethylenediamine tetra-acetic acid.
By in nano-silicon and graphite reactor of the input with agitator and thermometer, 550 DEG C are warming up to, stir 40min, Surplus stock is added, is ground 50 minutes in grinder, 60min is dried at 75 DEG C of input after grinding is uniform.
Dried raw material is placed in ceramic crucible with cover, then ceramic crucible with cover is put into tube furnace in height 550 DEG C are first heated under purity nitrogen gas shielded, then insulation reaction 3 hours is further heated to 800 DEG C, and insulation reaction 4 is small When, battery graphene complex material is obtained.
Process is simple, mild condition, with good electric conductivity, capacity is big, energy density is high, good cycle;Raw material Cheap, operation is simple, circulates 450 times, capacity 600mAh;Easy to operate, quality and yield are easy to control;Do not rely on big Type instrument and equipment, is capable of achieving high-quality battery Graphene and mass produces, and can extensively produce and constantly replace current material.
Embodiment 5:
Proportioning weighs 100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, 15 parts of hydrofluoric acid, nano-silicon 6 by weight Part, 40 parts of graphite, 3 parts of polytetrafluoroethylene (PTFE), 5 parts of absolute ethyl alcohol, 10 parts of cobalt acid lithium, 5 parts of sodium acid carbonate, 3 parts of titanium dioxide, 1,2 5 parts of dichloroethanes, 40 parts of potassium nitrate, 2.5 parts of titanium carbide, 4 parts of acetone, 3.5 parts of octane, 6.5 parts of toluene, 25 parts of tetrahydrofuran, 20 parts of ethylenediamine tetra-acetic acid.
By in nano-silicon and graphite reactor of the input with agitator and thermometer, 500 DEG C are warming up to, stir 35min, Surplus stock is added, is ground 40 minutes in grinder, 55min is dried at 70 DEG C of input after grinding is uniform.
Dried raw material is placed in ceramic crucible with cover, then ceramic crucible with cover is put into tube furnace in height 500 DEG C are first heated under purity nitrogen gas shielded, then insulation reaction 2 hours is further heated to 750 DEG C, and insulation reaction 3 is small When, battery graphene complex material is obtained.
Process is simple, mild condition, with good electric conductivity, capacity is big, energy density is high, good cycle;Raw material Cheap, operation is simple, circulates 500 times, capacity 600mAh;Easy to operate, quality and yield are easy to control;Do not rely on big Type instrument and equipment, is capable of achieving high-quality battery Graphene and mass produces, and can extensively produce and constantly replace current material.
All components in above example can be with commercially available.
The above embodiments are intended to illustrate the present invention, rather than limitation, therefore with it is of the invention Any change in claims suitable implication and scope, is all considered as being included within the scope of the claims.

Claims (7)

1. a kind of battery graphene complex material, it is characterised in that the battery raw material of graphene complex material Match by weight as follows:100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, hydrofluoric acid 5-25 parts, nano-silicon 4-8 Part, graphite 20-60 parts, polytetrafluoroethylene (PTFE) 1-5 parts, absolute ethyl alcohol 6-10 parts, cobalt acid lithium 8-12 parts, sodium acid carbonate 3-7 parts, dioxy Change 1-5 parts of titanium, 1,2 dichloroethanes 3-7 parts, potassium nitrate 30-50 parts, titanium carbide 0.5-4.5 parts, acetone 2-6 parts, octane 1.5- 5.5 parts, toluene 4.5-8.5 parts, tetrahydrofuran 15-35 parts, ethylenediamine tetra-acetic acid 10-30 parts.
2. a kind of battery graphene complex material according to claim 1, it is characterised in that:The battery graphite The raw materials by weight portion proportioning of alkene composite materials is as follows:100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, hydrogen fluorine 5 parts of acid, 4 parts of nano-silicon, 20 parts of graphite, 1 part of polytetrafluoroethylene (PTFE), 6 parts of absolute ethyl alcohol, 8 parts of cobalt acid lithium, 3 parts of sodium acid carbonate, dioxy Change 1 part of titanium, 1,23 parts of dichloroethanes, 30 parts of potassium nitrate, 0.5 part of titanium carbide, 2 parts of acetone, 1.5 parts of octane, 4.5 parts of toluene, four 15 parts of hydrogen furans, 10 parts of ethylenediamine tetra-acetic acid.
3. a kind of battery graphene complex material according to claim 1, it is characterised in that:The battery graphite The raw materials by weight portion proportioning of alkene composite materials is as follows:100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, hydrogen fluorine 25 parts of acid, 8 parts of nano-silicon, 60 parts of graphite, 5 parts of polytetrafluoroethylene (PTFE), 10 parts of absolute ethyl alcohol, 12 parts of cobalt acid lithium, 7 parts of sodium acid carbonate, 5 parts of titanium dioxide, 1,27 parts of dichloroethanes, 50 parts of potassium nitrate, 4.5 parts of titanium carbide, 6 parts of acetone, 5.5 parts of octane, toluene 8.5 Part, 35 parts of tetrahydrofuran, 30 parts of ethylenediamine tetra-acetic acid.
4. a kind of battery graphene complex material according to claim 1, it is characterised in that:The battery graphite The raw materials by weight portion proportioning of alkene composite materials is as follows:100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, hydrogen fluorine 10 parts of acid, 5 parts of nano-silicon, 30 parts of graphite, 2 parts of polytetrafluoroethylene (PTFE), 7 parts of absolute ethyl alcohol, 9 parts of cobalt acid lithium, 4 parts of sodium acid carbonate, two 2 parts of titanium oxide, 1,24 parts of dichloroethanes, 35 parts of potassium nitrate, 1.5 parts of titanium carbide, 3 parts of acetone, 2.5 parts of octane, 5.5 parts of toluene, 20 parts of tetrahydrofuran, 15 parts of ethylenediamine tetra-acetic acid.
5. a kind of battery graphene complex material according to claim 1, it is characterised in that:The battery graphite The raw materials by weight portion proportioning of alkene composite materials is as follows:100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, hydrogen fluorine 20 parts of acid, 7 parts of nano-silicon, 50 parts of graphite, 4 parts of polytetrafluoroethylene (PTFE), 9 parts of absolute ethyl alcohol, 11 parts of cobalt acid lithium, 6 parts of sodium acid carbonate, two 4 parts of titanium oxide, 1,26 parts of dichloroethanes, 45 parts of potassium nitrate, 3.5 parts of titanium carbide, 5 parts of acetone, 4.5 parts of octane, 7.5 parts of toluene, 30 parts of tetrahydrofuran, 25 parts of ethylenediamine tetra-acetic acid.
6. a kind of battery graphene complex material according to claim 1, it is characterised in that:The battery graphite The raw materials by weight portion proportioning of alkene composite materials is as follows:100 parts of trimethylolpropane polyoxyethylene polyoxypropylene ether, hydrogen fluorine 15 parts of acid, 6 parts of nano-silicon, 40 parts of graphite, 3 parts of polytetrafluoroethylene (PTFE), 5 parts of absolute ethyl alcohol, 10 parts of cobalt acid lithium, 5 parts of sodium acid carbonate, two 3 parts of titanium oxide, 1,25 parts of dichloroethanes, 40 parts of potassium nitrate, 2.5 parts of titanium carbide, 4 parts of acetone, 3.5 parts of octane, 6.5 parts of toluene, 25 parts of tetrahydrofuran, 20 parts of ethylenediamine tetra-acetic acid.
7. the preparation method of graphene complex material of battery described in a kind of claim 1, it is characterised in that including following step Suddenly:
The first step:Proportioning weighs trimethylolpropane polyoxyethylene polyoxypropylene ether, hydrofluoric acid, nano-silicon, stone by weight Ink, polytetrafluoroethylene (PTFE), absolute ethyl alcohol, cobalt acid lithium, sodium acid carbonate, titanium dioxide, 1,2 dichloroethanes, potassium nitrate, titanium carbide, third Ketone, octane, toluene, tetrahydrofuran and ethylenediamine tetra-acetic acid;
Second step:By in nano-silicon and graphite reactor of the input with agitator and thermometer, 450-550 DEG C is warming up to, stirred 30-40min is mixed, surplus stock is added, ground 30-50 minutes in grinder, dried at 65-75 DEG C of input after grinding is uniform 50-60min;
3rd step:Dried raw material is placed in ceramic crucible with cover, then ceramic crucible with cover is put into tube furnace 450-550 DEG C is first heated under high pure nitrogen protection, insulation reaction 1-3 hours, 700-800 is then further heated to DEG C, insulation reaction 2-4 hours, battery graphene complex material is obtained.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109003832A (en) * 2018-07-27 2018-12-14 福州大学 A kind of preparation method and application of three-dimensional porous graphene/nickel cobalt sulfide composite material

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101710617A (en) * 2009-05-12 2010-05-19 大连丽昌新材料有限公司 High-energy silicon-carbon composite negative electrode material for lithium ion battery and manufacturing process thereof
CN102496719A (en) * 2011-12-15 2012-06-13 中国科学院化学研究所 Silicon/graphene composite material, and preparation method and application of the same
CN104518207A (en) * 2013-09-27 2015-04-15 比亚迪股份有限公司 A lithium ion battery anode active material, a preparing method thereof, an anode and a lithium ion battery
CN105576242A (en) * 2016-03-08 2016-05-11 黑龙江聚拢华玺智能科技有限公司 Graphene battery
CN106129353A (en) * 2016-07-05 2016-11-16 苏州科淼新材料有限公司 A kind of lithium battery graphene complex and preparation method thereof
CN106257716A (en) * 2016-08-30 2016-12-28 浙江超威创元实业有限公司 The preparation method of a kind of silicon-carbon composite cathode material and lithium ion battery

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101710617A (en) * 2009-05-12 2010-05-19 大连丽昌新材料有限公司 High-energy silicon-carbon composite negative electrode material for lithium ion battery and manufacturing process thereof
CN102496719A (en) * 2011-12-15 2012-06-13 中国科学院化学研究所 Silicon/graphene composite material, and preparation method and application of the same
CN104518207A (en) * 2013-09-27 2015-04-15 比亚迪股份有限公司 A lithium ion battery anode active material, a preparing method thereof, an anode and a lithium ion battery
CN105576242A (en) * 2016-03-08 2016-05-11 黑龙江聚拢华玺智能科技有限公司 Graphene battery
CN106129353A (en) * 2016-07-05 2016-11-16 苏州科淼新材料有限公司 A kind of lithium battery graphene complex and preparation method thereof
CN106257716A (en) * 2016-08-30 2016-12-28 浙江超威创元实业有限公司 The preparation method of a kind of silicon-carbon composite cathode material and lithium ion battery

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109003832A (en) * 2018-07-27 2018-12-14 福州大学 A kind of preparation method and application of three-dimensional porous graphene/nickel cobalt sulfide composite material

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