CN110021746A - A kind of preparation method and lithium ion battery of carbon coating vanadium trioxide - Google Patents
A kind of preparation method and lithium ion battery of carbon coating vanadium trioxide Download PDFInfo
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- CN110021746A CN110021746A CN201910336935.XA CN201910336935A CN110021746A CN 110021746 A CN110021746 A CN 110021746A CN 201910336935 A CN201910336935 A CN 201910336935A CN 110021746 A CN110021746 A CN 110021746A
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- carbon coating
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- vanadium trioxide
- lithium ion
- ion battery
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- 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 the preparation methods and lithium ion battery of a kind of carbon coating vanadium trioxide, belong to field of lithium ion battery cathode material preparation.This method comprises the following steps: S1, and reducing agent and deionized water are configured to mixed solvent with the volume ratio of 1:1~9:1,70~80 DEG C is heated to, weighs vanadium source material, be dissolved in above-mentioned in the mixed solvent；Mixed solution in S1 is added in reaction kettle and seals, be heated to 110-160 DEG C and keep the temperature 10-18 hours by S2；S3 is cooled to room temperature after the hydro-thermal reaction to S2, the V for being coated with hydrocarbon is obtained after filtering2O3Nano material；S4, by V2O3Nano material dry 5-10h at 50-70 DEG C；The nano material powder that S4 is obtained is put into tube furnace by S5, is passed through inert gas or reducibility gas carries out atmosphere protection, be warming up to 350~450 DEG C with the rate of 3 DEG C/min, keep the temperature 3~8h, obtain carbon coating vanadium trioxide.Simple production process of the present invention；Hydro-thermal reaction required temperature condition is relatively low.
Description
Technical field
The present invention relates to field of lithium ion battery cathode material preparation, in particular to a kind of system of carbon coating vanadium trioxide
Preparation Method and lithium ion battery.
Background technique
With the enhancing of people's environmental consciousness and being continuously increased for energy demand, the development and utilization of new energy increasingly by
To the concern of countries in the world.Carrier of the lithium ion battery as energy storage, due to high-energy density, long circulation life,
The advantages that low self-discharge and small environmental pollution, has very big development potentiality.But with the development of other science and technology, to lithium ion
The performance requirement of battery is higher and higher.Lithium ion battery electrode material is the important component of lithium ion battery, is further
The performance for improving lithium ion battery, developing the electrode material haveing excellent performance becomes key.Charge and discharge of the vanadium trioxide in 0-3V
There is biggish theoretical specific capacity (about 1070mAh g-1) under voltage, be that a kind of lithium battery with larger application potential is negative
Pole material.However, poorly conductive restricts the performance of vanadium trioxide chemical property.In addition to this, the pattern of material is shadow
An important factor for ringing material electrochemical performance.Carbon coating is to improve a kind of effective method of material conductivity.To improve material
Chemical property, generally require the material for preparing three-dimensional or two-dimensional appearance with large specific surface area.Currently, preparation tool
In the method for having special appearance material, report that more is then to pass through higher temperature using high temperature hydro-thermal or solvent-thermal method
Calcination processing obtains final product.
Such as application No. is 201610179867.7 patents of invention to disclose a kind of carbon coating vanadium trioxide nano material
Preparation method, pass through high temperature mix hydro-thermal method synthesis the carbon-coated VO of different-shape2(B)(VO2(B)@C) nano material is
Then presoma carries out calcining to these presomas to obtain different-shape V2O3The method of nano material, including V2O3Nanometer
Particle and three-dimensional (3D) classifying porous V2O3@C micro-nano structure, the material being prepared can be used for lithium ion cell electrode material
Expect, wherein the classifying porous V of 3D2O3@C micro-nano structure presents extremely excellent chemical property, has very wide application
Prospect.
But higher heat treatment temperature not only consumes energy but also dangerous in above scheme.And complex process, cost compared with
It is high, it is difficult to industrialized production.
Summary of the invention
The present invention provides a kind of preparation method of carbon coating vanadium trioxide, simple process, low in cost and comparatively safe.
The present invention additionally provides a kind of lithium ion battery simultaneously.
A kind of preparation method of carbon coating vanadium trioxide, includes the following steps:
Reducing agent and deionized water are configured to mixed solvent with the volume ratio of 1:1~9:1, are heated to 70~80 DEG C by S1,
Vanadium source material is weighed, above-mentioned in the mixed solvent is dissolved in, wherein the concentration range of vanadium ion is 0.01-0.7mol/L；
Mixed solution that S1 is obtained is added in reaction kettle and is sealed by S2, is heated to 110-160 DEG C and to keep the temperature 10-18 small
When；
S3 is cooled to room temperature after the hydro-thermal reaction to S2, will obtain being coated with carbon after the substance filtering in reaction kettle
The V of hydrogen compound2O3Nano material；
S4, by the resulting V of S32O3Nano material dry 5-10h at 50-70 DEG C, obtains nano material powder；
The nano material powder that S4 is obtained is put into tube furnace by S5, is passed through inert gas or reducibility gas carries out gas
Atmosphere protection is warming up to 350~450 DEG C with the rate of 3 DEG C/min, keeps the temperature 3~8h, then cooled to room temperature, obtains carbon packet
Cover vanadium trioxide.
More preferably, the reducing agent is methanol, ethylene glycol, polyethylene glycol, oleyl amine, any one in hydrazine hydrate.
More preferably, the inert gas is any one of nitrogen or argon gas.
More preferably, the reducibility gas is argon hydrogen gaseous mixture.
More preferably, hydrogen volume accounts for volume of gas 3%-15% in argon hydrogen gaseous mixture.
A kind of lithium ion battery, the carbon that the lithium ion battery negative material uses above-mentioned any one the method to obtain
Cladding vanadium trioxide is lithium ion battery electrode material.
The present invention provides a kind of preparation method of carbon coating vanadium trioxide, has the following beneficial effects:
(1) intermediate steps that vanadium source is converted vanadium trioxide by the present invention are less, operate more convenient, produce work
Skill and operating process are relatively simple；
(2) hydro-thermal reaction required temperature condition of the present invention is relatively low, while guaranteeing that energy consumption reduces, also enhances behaviour
The safety coefficient of work, in addition also saves cost of manufacture.
(3) used reproducibility solvent can recycle in production process, and the waste material of generation is less, reduce environment
Pollution meets existing Materials rule.
Detailed description of the invention
Fig. 1 is hydrocarbon XRD spectrum of the gained containing Low Valent Vanadium after solvent thermal reaction at different temperatures；
Fig. 2 is hydrothermal temperature when being 125 DEG C and 160 DEG C, V prepared after 400 DEG C of calcinings under argon hydrogen gaseous mixture2O3/
The XRD spectrum of C；
Fig. 3 is hydrothermal temperature when being 125 DEG C and 160 DEG C, the synthesized V after 400 DEG C of calcinings2O3The scanning electron microscope of/C
Picture；
Fig. 4 is the material of method acquisition of the invention under 100mA/g current density, 200 charge and discharge cycles electric discharge ratios
Capacity Plan；
Fig. 5 is that in the prior art, hydro-thermal reaction is 160-260 DEG C of obtained carbon coating V2O3Cycle performance schematic diagram.
Specific embodiment
With reference to the accompanying drawing, the specific embodiment of the present invention is described in detail, it is to be understood that of the invention
Protection scope be not limited by the specific implementation.
Embodiment one:
Ethylene glycol and deionized water are mixed according to the volume ratio of 5:1, are configured to 65ml mixed solvent；
Above-mentioned mixed solvent is heated to 75 DEG C, weighs 0.02mol ammonium metavanadate, is dissolved in above-mentioned mixed solvent solution,
Stir 2 hours；
Above-mentioned solution is poured into 80ml ptfe autoclave liner, is put into baking oven and adds after reaction kettle is sealed
Heat keeps the temperature 14 hours at 125 DEG C；
It is cooled to room temperature after to hydro-thermal reaction, will obtain being coated with nytron after the substance filtering in reaction kettle
The V of object2O3Nano material；
Gained is coated with to the V of hydrocarbon2O3Nano material is put into baking oven, the dry 8h at 60 DEG C；
Mixing nano-powder after drying is put into tube furnace, it is more mixed than the argon hydrogen for 9:1 to be passed through argon gas and hydrogen volume
It closes gas and carries out atmosphere protection, be warming up to 400 DEG C with the rate of 3 DEG C/min, keep the temperature 5h, then cooled to room temperature, thus
To carbon-coated vanadium trioxide nano material.
Embodiment two:
Ethylene glycol and deionized water are mixed according to the volume ratio of 1:1, are configured to 65ml mixed solvent；
Above-mentioned mixed solvent is heated to 75 DEG C, weighs 0.02mol ammonium metavanadate, is dissolved in above-mentioned mixed solvent solution,
Stir 2 hours；
Above-mentioned solution is poured into 80ml ptfe autoclave liner, is put into baking oven and adds after reaction kettle is sealed
Heat keeps the temperature 18 hours at 110 DEG C；
It is cooled to room temperature after to hydro-thermal reaction, will obtain being coated with nytron after the substance filtering in reaction kettle
The V of object2O3Nano material；
Gained is coated with to the V of hydrocarbon2O3Nano material is put into baking oven, the dry 10h at 50 DEG C；
Mixing nano-powder after drying is put into tube furnace, it is more mixed than the argon hydrogen for 20:1 to be passed through argon gas and hydrogen volume
It closes gas and carries out atmosphere protection, be warming up to 350 DEG C with the rate of 3 DEG C/min, keep the temperature 8h, then cooled to room temperature, thus
To carbon-coated vanadium trioxide nano material.
Embodiment three:
Ethylene glycol and deionized water are mixed according to the volume ratio of 9:1, are configured to 65ml mixed solvent；
Above-mentioned mixed solvent is heated to 80 DEG C, weighs 0.02mol ammonium metavanadate, is dissolved in above-mentioned mixed solvent solution,
Stir 2 hours；
Above-mentioned solution is poured into 80ml ptfe autoclave liner, is put into baking oven and adds after reaction kettle is sealed
Heat keeps the temperature 10 hours at 160 DEG C；
It is cooled to room temperature after to hydro-thermal reaction, will obtain being coated with nytron after the substance filtering in reaction kettle
The V of object2O3Nano material；
Gained is coated with to the V of hydrocarbon2O3Nano material is put into baking oven, the dry 5h at 70 DEG C；
Mixing nano-powder after drying is put into tube furnace, it is more mixed than the argon hydrogen for 20:1 to be passed through argon gas and hydrogen volume
It closes gas and carries out atmosphere protection, be warming up to 350 DEG C with the rate of 3 DEG C/min, keep the temperature 8h, then cooled to room temperature, thus
To carbon-coated vanadium trioxide nano material.
As shown in Figure 1, which show hydrocarbon of the gained containing Low Valent Vanadium after solvent thermal reaction at different temperatures
XRD spectrum, shown in Fig. 2 illustrates, when hydrothermal temperature is 125 DEG C and 160 DEG C, under argon hydrogen gaseous mixture after 400 DEG C are calcined institute
The V of preparation2O3The XRD spectrum of/C, as seen from Figure 2, within the temperature range of technical scheme, obtained V2O3/
The pattern of C is close, and in situation similar in pattern, material has similar performance.
The performance detection of material:
Cycle performance test: by carbon-coated vanadium trioxide nano material, acetylene black, PVDF 8:1:1 in mass ratio into
Row is fully ground mixing, which is uniformly applied on copper foil and is dried, by the pole piece trimming after drying at diameter 12mm
Disk.Cathode uses metal lithium sheet, and diaphragm is Cdgard 2400, and 2032 type button cells are assembled into argon gas glove box,
Standing carries out electrochemical property test after a certain period of time.
Fig. 4 is illustrated under 100mA/g current density, 200 charge and discharge cycles specific discharge capacity figures.
Fig. 5 is that in the prior art, hydro-thermal reaction is 160-260 DEG C of obtained carbon coating V2O3Cycle performance schematic diagram.
By Fig. 4 and Fig. 5 compare it can be seen from the application using lower hydrothermal temperature three oxygen of carbon coating obtained
The circulation discharge performance for changing two vanadium aoxidizes two with higher hydrothermal temperature carbon coating three obtained is used in the prior art
The circulation discharge performance of vanadium is approximate.
Disclosed above is only several specific embodiments of the invention, and still, the embodiment of the present invention is not limited to this, is appointed
What what those skilled in the art can think variation should all fall into protection scope of the present invention.
Claims (6)
1. a kind of preparation method of carbon coating vanadium trioxide, which comprises the steps of:
Reducing agent and deionized water are configured to mixed solvent with the volume ratio of 1:1~9:1, are heated to 70~80 DEG C, weigh by S1
Vanadium source material is dissolved in above-mentioned in the mixed solvent, wherein the concentration range of vanadium ion is 0.01-0.7mol/L；
The mixed solution that S1 is obtained is added in reaction kettle and seals, be heated to 110-160 DEG C and keep the temperature 10-18 hours by S2；
S3 is cooled to room temperature after the hydro-thermal reaction to S2, will obtain being coated with hydrocarbonization after the substance filtering in reaction kettle
Close the V of object2O3Nano material；
S4, by the resulting V of S32O3Nano material dry 5-10h at 50-70 DEG C, obtains nano material powder；
The nano material powder that S4 is obtained is put into tube furnace by S5, is passed through inert gas or reducibility gas carries out atmosphere guarantor
Shield is warming up to 350~450 DEG C with the rate of 3 DEG C/min, keeps the temperature 3~8h, then cooled to room temperature, obtains carbon coating three
V 2 O.
2. a kind of preparation method of carbon coating vanadium trioxide as described in claim 1, which is characterized in that the reducing agent is
Methanol, ethylene glycol, polyethylene glycol, oleyl amine, any one in hydrazine hydrate.
3. a kind of preparation method of carbon coating vanadium trioxide as described in claim 1, which is characterized in that the inert gas
For any one of nitrogen or argon gas.
4. a kind of preparation method of carbon coating vanadium trioxide as described in claim 1, which is characterized in that the reproducibility gas
Body is argon hydrogen gaseous mixture.
5. a kind of preparation method of carbon coating vanadium trioxide as described in claim 1, which is characterized in that in argon hydrogen gaseous mixture
Hydrogen volume accounts for volume of gas 3%-15%.
6. a kind of lithium ion battery, which is characterized in that the lithium ion battery negative material is used as any in claim 1-5
The carbon coating vanadium trioxide that one the method obtains is lithium ion battery electrode material.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112210988A (en) * | 2020-10-16 | 2021-01-12 | 成都先进金属材料产业技术研究院有限公司 | Vanadium dioxide carbon fiber felt composite material and preparation method and application thereof |
| CN113555542A (en) * | 2021-09-18 | 2021-10-26 | 河南电池研究院有限公司 | Lithium ion battery cathode material and preparation method thereof |
| CN113912117A (en) * | 2021-11-15 | 2022-01-11 | 绍兴道普新材料科技有限公司 | Carbon bag V2O3Nano-rod composite material and preparation method and application thereof |
| CN113921805A (en) * | 2021-10-14 | 2022-01-11 | 合肥工业大学 | Preparation method of anion-doped vanadium trioxide positive electrode material for water-based zinc ion battery |
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| CN106025276A (en) * | 2016-08-18 | 2016-10-12 | 南京航空航天大学 | Carbon-coated vanadium trioxide nano material preparing method and lithium ion batteries |
| CN109292819A (en) * | 2018-11-12 | 2019-02-01 | 中国科学院上海硅酸盐研究所 | A kind of method that step hydro-thermal prepares vanadium trioxide powder |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112210988A (en) * | 2020-10-16 | 2021-01-12 | 成都先进金属材料产业技术研究院有限公司 | Vanadium dioxide carbon fiber felt composite material and preparation method and application thereof |
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| CN113555542A (en) * | 2021-09-18 | 2021-10-26 | 河南电池研究院有限公司 | Lithium ion battery cathode material and preparation method thereof |
| CN113921805A (en) * | 2021-10-14 | 2022-01-11 | 合肥工业大学 | Preparation method of anion-doped vanadium trioxide positive electrode material for water-based zinc ion battery |
| CN113912117A (en) * | 2021-11-15 | 2022-01-11 | 绍兴道普新材料科技有限公司 | Carbon bag V2O3Nano-rod composite material and preparation method and application thereof |
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Application publication date: 20190716 |