CN106654186A - Large-scale preparation and lithium battery application of vanadium pentoxide and carbon nano composite thereof - Google Patents

Large-scale preparation and lithium battery application of vanadium pentoxide and carbon nano composite thereof Download PDF

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CN106654186A
CN106654186A CN201610898017.2A CN201610898017A CN106654186A CN 106654186 A CN106654186 A CN 106654186A CN 201610898017 A CN201610898017 A CN 201610898017A CN 106654186 A CN106654186 A CN 106654186A
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vanadium pentoxide
preparation
vanadic anhydride
solution
powder
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朱纪欣
黄维
马中原
黄晓
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Nanjing Tech University
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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
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/362Composites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/058Construction or manufacture
    • 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
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/483Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • 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
    • 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
    • H01M4/583Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries
    • 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention discloses large-scale preparation and lithium battery application of vanadium pentoxide and carbon nano composite thereof, and belongs to the technical field of functional nano material preparation. The preparation method comprises the following steps: dissolving vanadium pentoxide solid powder in pure water, mixing with hydrogen peroxide, obtaining a scarlet solution, and preserving the temperature of the solution for a period of time to become a colloidal sol; carrying out freeze drying treatment on the colloidal sol to obtain a three-dimensional self-supporting solid; and taking partial solid to be calcinated under nitrogen atmosphere so as to obtain a vanadium pentoxide nano material. The corresponding solid is added into composite carbon nano tube and graphene as long as the scarlet solution is obtained, and the mixture is dispersed uniformly without changing remaining operation. The lithium battery positive electrode material prepared in the method is long in service life, high in capacity and stable in cycle performance. The whole technological process is simple, the price of raw materials is low, no toxic product is generated, the energy consumption is low, and the material is green and environmentally-friendly, so that the disadvantage that existing lithium battery materials are high in production cost, complex in process and great in byproduct toxicity is overcome, and the material is applicable to industrial large-scale production.

Description

Vanadium pentoxide and its carbon nano-complex prepare with scale and lithium battery applications
Technical field
The present invention relates to a kind of vanadic anhydride that can be used as anode material for lithium-ion batteries and its carbon-based composite nanometer The large-scale preparation method of material, belongs to the preparing technical field of function nano material.
Background technology
With the sharp increase of the growing and size of population of global economy, the mankind are increasing to the demand of the energy, Therefore energy problem has become the problem that a whole mankind is badly in need of facing and solving.Fossil energy it is non-renewable and increasingly withered Exhaust and force us to need to research and develop new forms of energy., with having extended cycle life, energy density is high, stable performance for lithium battery, environmental friendliness etc. Feature gets more and more people's extensive concerning and uses, and is that a kind of most ripe and most widely used energy of technology turns in new energy field Change technology.
Lithium battery has been widely used in electric automobile, mobile phone, in computer and some wearable devices, as new forms of energy are produced The continuous development of industry, the market demand of lithium battery can further expand.And present lithium battery generally existing production cost is higher, The shortcomings of capacity is relatively low.Research and development battery capacity is high, and extensively, the simple lithium battery of production technology is particularly important raw material sources.
Vanadic anhydride raw material sources are extensive, with low cost, are adapted to large-scale production anode material of lithium battery, what it had Layer structure causes lithium ion easier to insert positive pole, increases these advantages such as reactivity, high theoretical capacity and causes it Become one of optimal material of magnanimity preparation and low cost production lithium battery anode.But the vanadic anhydride of bulk does not have Larger specific surface area, and limit its further business the shortcomings of bad electric conductivity and poor ion transport capability Using.For this purpose, the vanadic anhydride material of the three-dimensional self-supporting of preparation structure nanosizing is increasing its specific surface area and active sites The pliability of point and material, combined conductive agent is strengthening its electronics and ion transport capability is improve its lithium electrical property important Measure.
CNT is a kind of high-end conductive agent, in one-dimentional structure, by carbon atom hydridization one or more are coaxial Carbon pipe is constituted.CNT is spread out, the conductive network being cross-linked with each other can be formed, greatly improve the conduction of material Property.And CNT itself is lightweight, other elements are practically free of, industrialized production is had been carried out now, be a kind of ten sub-argument The conductive additive thought.
Redox graphene be graphene oxide is reduced obtained from, compared with Graphene, its surface is contained on a small quantity Oxygen-containing functional group, similar to Graphene in performance.Graphene is honeybee of the carbon atom through the tight periodic arrangement of sp2 hydridization Nest shape two-dimensional material.Since finding Graphene from 2004, Graphene just receives the extensive concern of people.Graphene is known Most thin, most tough material, almost fully transparent, heat conduction, electric conductivity is very excellent.The Graphene preparation cost of individual layer compared with Height, can prepare redox graphene by thermal reduction graphene oxide under inert atmosphere, to reduce production cost, be adapted to work Industry metaplasia is produced.
The content of the invention
It is an object of the invention to provide a kind of low in raw material price, technical process is simple and environmentally-friendly, excellent performance function The synthetic method of nanometer anode material of lithium battery, to overcome battery material complex manufacturing instantly, high energy consumption, with high costs etc. Shortcoming.
A kind of vanadic anhydride of the present invention and its complex nano material, are realized by following experimental program:
First, the preparation method of vanadium pentoxide nanometer material:
Vanadium pentoxide powder is dissolved in ultra-pure water;Add hydrogen peroxide solution (ratio 0.3- that mass fraction is 30% 2g V2O5:25mL H2O:5mL 30%H2O2), 45~90min is placed at ambient temperature, obtain the clear solution of redness;Will The solution for obtaining is positioned over 12~24h of insulation in 40~60 degree of insulating boxs, obtains collosol substance russet.
Vanadium pentoxide sol is put in liquid nitrogen and freezes 10min, be put into immediately after in freeze dryer carry out vacuumizing it is dry It is dry, the solid of the three-dimensional self supporting structure of puffy is obtained after 48h.
Take fraction solids to calcine in a nitrogen atmosphere, be warmed up to 300~600 DEG C, 0.5~3h of time, heating rate 2-10 DEG C/min, you can obtain vanadium pentoxide nanometer material.
2nd, the preparation method of vanadic anhydride composite carbon nanometer tube nano material
Vanadium pentoxide powder is dissolved in ultra-pure water, hydrogen peroxide solution is added, 1h is placed at ambient temperature, obtain red The clear solution of color;Add CNT pressed powder (ratio 0.3-2g V2O5:25mL H2O:5mL 30%H2O2:0.06- 0.4g CNTs), and ultrasonic disperse 30min;The solution for obtaining is positioned in 50 degree of insulating boxs and is incubated 24h, obtained reddish brown The collosol substance of color.
Vanadium pentoxide sol is put in liquid nitrogen and freezes 10min, be put into immediately after in freeze dryer carry out vacuumizing it is dry It is dry, obtain the solid of the three-dimensional self supporting structure of puffy.
Resulting solid is calcined in a nitrogen atmosphere, vanadic anhydride composite carbon nanometer tube nanometer material is obtained Material.
3rd, the preparation method of vanadic anhydride composite graphite alkene nano material
Vanadium pentoxide powder is dissolved in ultra-pure water, hydrogen peroxide solution is added, 1h is placed at ambient temperature, obtain red The clear solution of color;Add graphene oxide solid (ratio 0.3-2g V2O5:25mL H2O:5mL30%H2O2:0.06-0.4g Graphene), and ultrasonic disperse 30min;The solution for obtaining is positioned in 50 degree of insulating boxs and is incubated 24h, obtain pitchy reddish brown The collosol substance of color.
Vanadium pentoxide sol is put in liquid nitrogen and freezes 10min, be put into immediately after in freeze dryer carry out vacuumizing it is dry It is dry, obtain the solid of the three-dimensional self supporting structure of puffy.
Resulting solid is calcined in a nitrogen atmosphere, vanadic anhydride composite graphite alkene nano material is obtained.
Compared with other prepare vanadic anhydride and its related complex MATERIALS METHODS, the present invention prepare vanadic anhydride and The method of its composite nano materials is simple, vanadic anhydride wide material sources, easily obtains, and vanadic anhydride reacts with hydrogen peroxide During only oxygen release, without noxious gas emission to air in, meet the theory of Green Chemistry.Insulation, freezes, calcined Journey is all low energy consumption, takes short, the shirtsleeve operation stage, can be produced on a large scale, is adapted to industrial applications.Additionally, with activity The quality of material vanadic anhydride is effective mass, and in the case where current density is 150A/Kg, three kinds of positive electrodes show Preferable data result.Single component vanadic anhydride charging and discharging capacity is up to 165Ah/Kg, close business application LiFePO4Battery, higher than general LiCoO2The 140Ah/Kg and LiMn of battery2O4The 148Ah/Kg of battery.Vanadic anhydride is answered Compound/carbon nano pipe charging and discharging capacity is up to 385Ah/Kg, and discharge and recharge specific energy reaches 1143Wh/Kg, and discharge and recharge 100 is enclosed Afterwards capacity is still maintained at more than 200Ah/Kg, and vanadic anhydride composite graphite alkene charging and discharging capacity then reaches 287Ah/Kg. These performances meet the practical application of material low cost production.
4th, the lithium battery energy storage battery application of vanadic anhydride and its carbon-based composite nano material and using vanadic anhydride and The preparation method that its carbon-based composite nano material is used as the lithium battery of anode material of lithium battery.
Vanadium pentoxide nanometer material, vanadic anhydride composite carbon nanometer tube nano material, vanadic anhydride composite graphite Alkene nano material can be used as anode material for lithium-ion batteries.
The method for preparing lithium battery, is first according to active material:Conductive agent:Binding agent mass ratio is 7:2:1 by positive pole material Material, acetylene black, polyvinylidene fluoride is well mixed material in the presence of solvent N-methyl pyrilidone, obtains dispersion equal One slurry, is then uniformly applied in aluminum foil current collector.Then working electrode is dried in 60 degree of vacuum drying chambers 24h.With metal lithium sheet as negative pole, 1.0M LiPF6in EC:DMC:EMC=1:1:1Vol% is electrolyte, with polypropylene screen work For barrier film, battery case model 2032, the assembling button cell in glove box (nine, Nanjing).
Battery carries out perseverance after being completed on cell tester (the new prestige battery testing cabinet CT-4008-5V5mA in Shenzhen) Stream charge and discharge cycles test, 2~4V of operating voltage, data acquisition is painted after completing by origin data processing softwares Figure, analysis.
The vanadic anhydride and its complex nano material of preparation has layer structure feature, be adapted to lithium ion insertion and Abjection, improves the reactivity of vanadium and lithium.Nanostructured increases the specific surface area of material so that reactivity site increases significantly Plus, it is also beneficial to improve the contact area of material and electrolyte, strengthen the conducting power of ion-electron.The structure of three-dimensional self-supporting So that material is more fluffy, and it is flexible, it is adapted to prepare variously-shaped electrode, range of application is wider, and the potential value of business is bigger.
Anode material of lithium battery prepared by the method has higher capacity, and cycle life is longer, stable discharge and recharge effect Rate, in addition raw material be easy to get and low cost, the simplicity of production technology, course of reaction is innoxious, and these advantages are conducive to the party Method is applied to industrialize actual production.
Description of the drawings
Fig. 1 is vanadic anhydride X-ray diffractogram.
Fig. 2 is the electron microscope of vanadium pentoxide nanometer material.
Fig. 3 is the electron microscope of vanadic anhydride composite carbon nanometer tube nano material.
Fig. 4 is the electron microscope of vanadic anhydride composite graphite alkene nano material.
Specific embodiment
Below in conjunction with being embodied as example, it is intended to further illustrate the present invention and the unrestricted present invention.
Embodiment 1
0.364g vanadic anhydride pressed powders are dissolved in 25ml pure water, the dioxygen that 5ml mass fractions are 30% is added The aqueous solution, places 1h under room temperature environment, obtains wine-colored solution.The solution is positioned in 50 DEG C of insulating box and is incubated 24h, solution becomes colloidal sol.Colloidal sol is placed in liquid nitrogen and freezes 10min, put into immediately after carry out in freeze dryer vacuumize it is dry It is dry, fluffy solid is obtained after 48h.Take fraction solids to calcine in a nitrogen atmosphere, be warmed up to 400 DEG C, time 0.5h heats up 10 DEG C/min of speed, you can obtain vanadium pentoxide nanometer material.Fig. 1 is shown five oxidations after the calcining in embodiment 1 Two vanadium XRD spectras, spectrogram and standard card JCPDS card no:41-1426 matches, and belongs to rhombic system, Pmmn spaces Group.
Embodiment 2
1.092g vanadic anhydride pressed powders are dissolved in 25ml pure water, the dioxygen that 5ml mass fractions are 30% is added The aqueous solution, places 1h under room temperature environment, obtains wine-colored solution.The solution is positioned in 50 DEG C of insulating box and is incubated 24h, solution becomes colloidal sol.Colloidal sol is placed in liquid nitrogen and freezes 10min, put into immediately after carry out in freeze dryer vacuumize it is dry It is dry, fluffy solid is obtained after 48h.Take fraction solids to calcine in a nitrogen atmosphere, be warmed up to 400 DEG C, time 0.5h heats up 10 DEG C/min of speed, you can obtain vanadium pentoxide nanometer material.
Embodiment 3
1.82g vanadic anhydride pressed powders are dissolved in 25ml pure water, the hydrogen peroxide that 5ml mass fractions are 30% is added Solution, places 1h under room temperature environment, obtains wine-colored solution.The solution is positioned in 50 DEG C of insulating box and is incubated 24h, Solution becomes colloidal sol.Colloidal sol is placed in liquid nitrogen and freezes 10min, to be put into carried out in freeze dryer immediately after and vacuumize drying, 48h Fluffy solid is obtained afterwards.Take fraction solids to calcine in a nitrogen atmosphere, be warmed up to 400 DEG C, time 0.5h, heating rate 10 DEG C/min, you can obtain vanadium pentoxide nanometer material.
Embodiment 4
0.364g vanadic anhydride pressed powders are dissolved in 25ml pure water, the dioxygen that 5ml mass fractions are 30% is added The aqueous solution, places 1h under room temperature environment, obtains wine-colored solution.145.6mg CNTs are added in dark red solution The solution is positioned in 50 DEG C of insulating box and is incubated 24h by pressed powder, ultrasonic disperse 30min, and solution becomes colloidal sol.Will be molten Glue is placed in liquid nitrogen and freezes 10min, to put into carried out in freeze dryer immediately after and vacuumizes drying, and fluffy consolidating is obtained after 48h Body.Take fraction solids to calcine in a nitrogen atmosphere, be warmed up to 400 DEG C, time 0.5h, 10 DEG C/min of heating rate, you can obtain Vanadic anhydride composite carbon nanometer tube nano material.
Embodiment 5
0.364g vanadic anhydride pressed powders are dissolved in 25ml pure water, the dioxygen that 5ml mass fractions are 30% is added The aqueous solution, places 1h under room temperature environment, obtains wine-colored solution.145.6mg graphite oxides are added in dark red solution The solution is positioned in 50 DEG C of insulating box and is incubated 24h by alkene solid, ultrasonic disperse 30min, and solution becomes colloidal sol.By colloidal sol It is placed in liquid nitrogen and freezes 10min, to put into carried out in freeze dryer immediately after and vacuumize drying, fluffy solid is obtained after 48h. Take fraction solids to calcine in a nitrogen atmosphere, be warmed up to 400 DEG C, time 0.5h, 10 DEG C/min of heating rate, you can obtain five oxygen Change two vanadium composite graphite alkene nano materials.
Embodiment 6
Vanadic anhydride and its carbon-based composite nano material prepared by the present invention is used as anode material of lithium battery, presses first According to active material:Conductive agent:Binding agent mass ratio is 7:2:1 by positive electrode, acetylene black, and polyvinylidene fluoride is in solvent N- first In the presence of base pyrrolidones, material is well mixed, obtains the homogeneous slurry of dispersion, be then uniformly applied to aluminium foil afflux On body.Then working electrode is dried into 24h in 60 degree of vacuum drying chambers.With metal lithium sheet as negative pole, 1.0M LiPF6in EC:DMC:EMC=1:1:1Vol% is electrolyte, using polypropylene screen as barrier film, battery case model 2032, in glove box Assembling button cell in (nine, Nanjing).Battery be completed after in cell tester (the new prestige battery testing cabinet CT- in Shenzhen Constant current charge-discharge loop test, 2~4V of operating voltage are carried out on 4008-5V5mA), data acquisition passes through origin after completing Data processing software is drawn, analysis.

Claims (10)

1. a kind of preparation method of vanadium pentoxide nanometer material, it is characterised in that the preparation method is comprised the following steps:
A. vanadium pentoxide powder is dissolved in ultra-pure water;Add 30% hydrogen peroxide solution;Vanadium pentoxide powder, ultra-pure water with The ratio of 30% hydrogen peroxide solution is 0.3-2g V2O5:25mL H2O:5mL 30%H2O2, obtain the clear solution of redness;Will To solution be positioned in 40~60 degree of insulating boxs 12~24h of insulation, obtain V russet2O5Collosol substance;
B. vanadium pentoxide sol is put in liquid nitrogen and freezes 10min, being put into immediately after in freeze dryer carries out vacuumizing drying, Obtain the V of the three-dimensional self supporting structure of puffy2O5Three-dimensional manometer pressed powder;
C. resulting solid is calcined in a nitrogen atmosphere, is obtained vanadium pentoxide nanometer material.
2. a kind of preparation method of vanadium pentoxide nanometer material as claimed in claim 1, it is characterised in that used by step a Vanadium pentoxide powder quality be 0.364-2g, hydrogen peroxide mass fraction be 30%, 5mL.
3. a kind of preparation method of vanadium pentoxide nanometer material as claimed in claim 1, it is characterised in that:In step b Vacuum drying time is 10-48h.
4. a kind of preparation method of vanadium pentoxide nanometer material as claimed in claim 1, it is characterised in that:In step c Heating rate is 2-10 DEG C/min, and speed is warmed up to 300-600 DEG C, and calcination time is 0.5-3h.
5. a kind of preparation method of vanadic anhydride composite carbon nanometer tube nano material, it is characterised in that the preparation method includes Following steps:
A. vanadium pentoxide powder is dissolved in ultra-pure water, adds 30% hydrogen peroxide solution, 1h is placed at ambient temperature, obtained Red clear solution;Add CNT pressed powder;Vanadium pentoxide powder, ultra-pure water, 30% hydrogen peroxide solution and carbon The ratio of nanotube solids powder is 0.3-2g V2O5:25mL H2O:5mL30%H2O2:0.06-0.4g CNT, and ultrasonic disperse 30min;The solution for obtaining is positioned in 50 degree of insulating boxs and is incubated 24h, obtain the V of black2O5/ CNT collosol substances;
B. the colloidal sol of vanadic anhydride composite carbon nanometer tube is put in liquid nitrogen and freezes 10min, be put into immediately after in freeze dryer Carry out vacuumizing drying, obtain the V of the three-dimensional self supporting structure of puffy2O5/ CNT nano-solid powder;
C. resulting solid is calcined in a nitrogen atmosphere, is obtained vanadic anhydride/carbon nano tube composite nano material.
6. a kind of preparation method of vanadic anhydride composite carbon nanometer tube nano material as claimed in claim 5, its feature exists In:Carbon nanotube mass ratio used is 10%-40%.
7. a kind of preparation method of vanadic anhydride composite graphite alkene nano material, it is characterised in that the preparation method include with Lower step:
A. vanadium pentoxide powder is dissolved in ultra-pure water, adds 30% hydrogen peroxide solution, 1h is placed at ambient temperature, obtained Red clear solution;Add graphene oxide;Vanadium pentoxide powder, ultra-pure water, 30% hydrogen peroxide solution and Graphene Ratio is 0.3-2g V2O5:25mL H2O:5mL 30%H2O2:0.06-0.4g Graphenes, and ultrasonic disperse 30min;To obtain Solution be positioned in 50 degree of insulating boxs and be incubated 24h, obtain the V of pitchy2O5/ GO collosol substances;
B. the colloidal sol of vanadic anhydride composite graphite alkene is put in liquid nitrogen and freezes 10min, be put in freeze dryer immediately after Row vacuumizes drying, obtains the V of the three-dimensional self supporting structure of puffy2O5/ GO nano-solid powder;
C. resulting solid is calcined in a nitrogen atmosphere, is obtained vanadic anhydride/graphene composite nano material.
8. a kind of preparation method of vanadic anhydride composite graphite alkene nano material as claimed in claim 7, it is characterised in that: Graphene oxide mass ratio used is 10%-40%.
9. the lithium battery energy storage battery application of vanadic anhydride and its complex nano material, it is characterised in that vanadic anhydride nanometer Material, vanadic anhydride composite carbon nanometer tube nano material, vanadic anhydride composite graphite alkene nano material can be used as lithium ion Cell positive material.
10. the vanadic anhydride for being prepared using the present invention and its complex nano material are used as the lithium battery of anode material of lithium battery Preparation method, it is characterised in that
A. according to active material:Conductive agent:Binding agent mass ratio is 7:2:1 exists positive electrode, acetylene black, polyvinylidene fluoride In the presence of solvent N-methyl pyrilidone, material is well mixed, obtains the homogeneous slurry of dispersion, be then uniformly applied to In aluminum foil current collector;
B. working electrode is dried into 24h in 60 degree of vacuum drying chambers;
C. with metal lithium sheet as negative pole, 1.0M LiPF6in EC:DMC:EMC=1:1:1Vol% is electrolyte, with polypropylene screen As barrier film, button cell is assembled in glove box.
CN201610898017.2A 2016-10-14 2016-10-14 Large-scale preparation and lithium battery application of vanadium pentoxide and carbon nano composite thereof Pending CN106654186A (en)

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CN107482195A (en) * 2017-08-04 2017-12-15 郴州国盛新材科技有限公司 A kind of button cell and its preparation method and application
CN107611410A (en) * 2017-09-30 2018-01-19 湖南国盛石墨科技有限公司 V2o5/ graphene composite materials preparation method and anode
CN107665982A (en) * 2017-08-04 2018-02-06 郴州国盛新材科技有限公司 A kind of vanadic anhydride/graphene composite material and preparation method thereof
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CN112993217A (en) * 2019-12-13 2021-06-18 中国科学院大连化学物理研究所 Preparation method of organic-inorganic hybrid material based on vanadium pentoxide and application of organic-inorganic hybrid material in zinc ion battery
CN115064684A (en) * 2022-07-18 2022-09-16 陕西科技大学 Vanadium oxide/reduced graphene oxide composite material and preparation method and application thereof
CN115520897A (en) * 2022-10-28 2022-12-27 江苏大学 Preparation method of high-rate low-temperature-resistant nano lithium vanadate anode material

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Application publication date: 20170510