CN113184906A - One-step hydrothermal method for preparing V2O3Method of nanosphere - Google Patents
One-step hydrothermal method for preparing V2O3Method of nanosphere Download PDFInfo
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- CN113184906A CN113184906A CN202110522127.XA CN202110522127A CN113184906A CN 113184906 A CN113184906 A CN 113184906A CN 202110522127 A CN202110522127 A CN 202110522127A CN 113184906 A CN113184906 A CN 113184906A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
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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
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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 a one-step hydrothermal method for preparing V2O3The method for the nanosphere comprises the following steps: according to V (water): weighing 15-20 ml of water and 3-4 ml of ammonia water according to the volume ratio of V (ammonia water) to 5:1 to prepare a mixed solution, weighing a vanadium source, adding the vanadium source into the mixed solution, and stirring the mixed solution by using a magnetic stirrer at room temperature to obtain a solution A with the vanadium source concentration of 0.023-0.038 mol/L; step two: weighing a sulfur source, adding the sulfur source into the solution A, and stirring by using a magnetic stirrer at room temperature to obtain a solution B with the sulfur source concentration of 0.13-0.17 mol/L; step three: transferring the solution B into a polytetrafluoroethylene lining, putting the polytetrafluoroethylene lining into an oven, and carrying out solvothermal reaction at 160-200 ℃ for 18-24 h; step four: thermally reacting the solventCollecting the product by suction filtration, washing with a lotion, and freeze-drying to obtain V2O3An electrode material. The invention adopts a one-step hydrothermal method to prepare V2O3The method has the advantages of simple process, low energy consumption, high yield, suitability for large-scale production and low production cost; the product has high purity and crystallinity, uniform structure and beneficial performance.
Description
Technical Field
The invention belongs to the field of battery electrode materials, relates to preparation of electrode materials, and particularly relates to a method for preparing V by a one-step hydrothermal method2O3A method of nanospheres.
Background
In recent years, next-generation high-capacity, high-energy-density rechargeable batteries are continuously sought. Lithium ion batteries have been widely used in people's daily lives. Sodium Ion Batteries (SIBs) and Potassium Ion Batteries (PIBs) have recently attracted more and more attention due to their abundant resources and low cost. V2O3The open-air tunnel structure composed of three-dimensional V-V frames can effectively facilitate the insertion of alkali metal ions. A number of researchers have been extensively V2O3Will serve as the battery anode and cathode materials. (Mcnulty D, Buckley D N, O' Dwye C.V2O3 Polycrystalline Nanorod Cathodematerials for Li-Ion Batteries with Long Cycle Life and High Capacity Retention[J].ChemElectroChem,2017.)(Jin T,Li H,Li Y,et al.Intercalation pseudocapacitance in flexible and self-standing V2O3 porous nanofibers for high-rate and ultra-stable K ion storage[J]Nano Energy,2018,50:462-2O3Most of the synthesis methods are complicated, high-temperature calcination is needed, the process is complicated, and the energy consumption is high.
Disclosure of Invention
Based on the defects of the prior art, the invention aims to provide a one-step hydrothermal method for preparing V2O3The method of the nanosphere has simple preparation process and excellent product performance.
In order to achieve the purpose, the invention adopts the technical scheme that:
one-step hydrothermal method for preparing V2O3A method of nanospheres comprising the steps of:
the method comprises the following steps: according to V (water): weighing 15-20 ml of water and 3-4 ml of ammonia water according to the volume ratio of V (ammonia water) to 5:1 to prepare a mixed solution, weighing a vanadium source, adding the vanadium source into the mixed solution, and stirring the mixed solution by using a magnetic stirrer at room temperature to obtain a solution A with the vanadium source concentration of 0.023-0.038 mol/L;
step two: weighing a sulfur source, adding the sulfur source into the solution A, and stirring by using a magnetic stirrer at room temperature to obtain a solution B with the sulfur source concentration of 0.13-0.17 mol/L;
step three: transferring the solution B into a polytetrafluoroethylene lining, putting the polytetrafluoroethylene lining into an oven, and carrying out solvothermal reaction at 160-200 ℃ for 18-24 h;
step four: collecting the product of the solvothermal reaction in a suction filtration mode, and obtaining V after washing and freeze drying2O3An electrode material.
The invention also has the following technical characteristics:
preferably, the vanadium source is ammonium metavanadate.
Preferably, the sulfur source is thioacetamide.
Preferably, in the first step, the stirring time of the magnetic stirrer is 10-30 min, and the rotating speed is 500-700 r/min.
Preferably, the stirring time of the magnetic stirrer in the second step is 30-60 min, and the rotating speed is 500-700 r/min.
Preferably, the filling ratio of the polytetrafluoroethylene lining in the third step is 24-35%.
Preferably, the washing method in the fourth step is washing with water and ethanol alternately for three times.
Compared with the prior art, the invention has the following beneficial effects:
the invention adopts a one-step hydrothermal method to prepare V2O3Simple process, no need of high-temperature calcination, low energy consumption, high yield, and suitability for large-scale productionThe production cost is low;
v prepared by the invention2O3The nano-sphere self-assembled by nano particles is used as an electrode material, and has high purity, high crystallinity and uniform structure;
v prepared by the invention2O3The nanospheres have excellent performance in the anode material of the alkali metal ion battery.
Drawings
FIG. 1 is V prepared in example 22O3The XRD diffraction pattern of (1), wherein the abscissa is the angle of 2 theta and the ordinate is the intensity;
FIG. 2 is V prepared in example 22O3SEM picture of (1);
FIG. 3 is V prepared in example 22O3The graph of potassium rate performance in which the abscissa is the number of cycles and the ordinate is the capacity (mAh/g).
Detailed Description
Example 1:
the method comprises the following steps: weighing a certain amount of ammonium metavanadate, adding the ammonium metavanadate into a mixed solution of 15ml of water and 3ml of ammonia water, and stirring for 10min at room temperature by using a magnetic stirrer at the rotating speed of 500r/min to obtain a solution A with the concentration of 0.023 mol/l;
step two: weighing a certain amount of thioacetamide, adding the thioacetamide into the solution A, and stirring the thioacetamide for 30min at room temperature by using a magnetic stirrer at the rotating speed of 500r/min to obtain a solution B with the concentration of 0.13 mol/l;
step three: transferring the solution B into a polytetrafluoroethylene lining with a filling ratio of 24%; putting the mixture into an oven, and carrying out solvothermal reaction at 160 ℃ for 18 h;
step four: collecting the product of the solvothermal reaction in a suction filtration mode, alternately washing with water and ethanol for three times, and freeze-drying for 12 hours to obtain V2O3An electrode material.
Example 2:
the method comprises the following steps: weighing a certain amount of ammonium metavanadate, adding the ammonium metavanadate into a mixed solution of 15ml of water and 3ml of ammonia water, and stirring for 10min at room temperature by using a magnetic stirrer at the rotating speed of 500r/min to obtain a solution A with the concentration of 0.033 mol/l;
step two: weighing a certain amount of thioacetamide, adding the thioacetamide into the solution A, and stirring the thioacetamide for 40min at room temperature by using a magnetic stirrer at the rotating speed of 500r/min to obtain a solution B with the concentration of 0.15 mol/l;
step three: transferring the solution B into a polytetrafluoroethylene lining with a filling ratio of 28%; putting the mixture into an oven, wherein the solvothermal reaction temperature is 170 ℃, and the reaction time is 20 hours;
step four: collecting the product of the solvothermal reaction in a suction filtration mode, alternately washing with water and ethanol for three times, and freeze-drying for 12 hours to obtain V2O3An electrode material.
FIG. 1 is V prepared in example 22O3The XRD diffraction pattern of (1), wherein the abscissa is the angle of 2 theta and the ordinate is the intensity; as can be seen from FIG. 1, the diffraction peaks all point to JCPDS 71-0342V 2O3 PDF card, and the synthesis of pure phase V is proved2O3。
FIG. 2 is V prepared in example 22O3SEM picture of (1); it can be seen from fig. 2 that V2O3 is a nanosphere formed by self-assembly of nanoparticles, and has uniform size and uniform dispersion.
FIG. 3 is V prepared in example 22O3The graph of potassium rate performance in which the abscissa is the number of cycles and the ordinate is the capacity (mAh/g). From FIG. 3, it can be seen that the self-assembly V2O3The rate performance of the nanosphere potassium ion battery is good, and the nanosphere potassium ion battery can respectively maintain the capacities of 220, 250, 170, 150, 110 and 70mAh/g under the current densities of 0.1, 0.2, 0.5, 1, 2 and 5A/g. Example 3:
the method comprises the following steps: weighing a certain amount of ammonium metavanadate, adding the ammonium metavanadate into a mixed solution of 20ml of water and 4ml of ammonia water, and stirring the mixture for 30min at room temperature by using a magnetic stirrer at the rotating speed of 600r/min to obtain a solution A with the concentration of 0.025 mol/l;
step two: weighing a certain amount of thioacetamide, adding the thioacetamide into the solution A, and stirring the thioacetamide for 60min at room temperature by using a magnetic stirrer at the rotating speed of 650r/min to obtain a solution B with the concentration of 0.13 mol/l;
step three: transferring the solution B into a polytetrafluoroethylene lining with a filling ratio of 32%; putting the mixture into an oven, wherein the solvothermal reaction temperature is 160 ℃, and the reaction time is 24 hours;
step four: collecting the product of the solvothermal reaction in a suction filtration mode, alternately washing with water and ethanol for three times, and freeze-drying for 12 hours to obtain V2O3An electrode material.
Example 4:
the method comprises the following steps: weighing a certain amount of ammonium metavanadate, adding the ammonium metavanadate into a mixed solution of 18ml of water and 3.6ml of ammonia water, and stirring the mixture for 20min at room temperature by using a magnetic stirrer at the rotating speed of 500r/min to obtain a solution A with the concentration of 0.036 mol/l;
step two: weighing a certain amount of thioacetamide, adding the thioacetamide into the solution A, and stirring the thioacetamide for 30min at room temperature by using a magnetic stirrer at the rotating speed of 500r/min to obtain a solution B with the concentration of 0.17 mol/l;
step three: transferring the solution B into a polytetrafluoroethylene lining with a filling ratio of 30%; putting the mixture into an oven, wherein the solvothermal reaction temperature is 200 ℃, and the reaction time is 18 h;
step four: collecting the product of the solvothermal reaction in a suction filtration mode, alternately washing with water and ethanol for three times, and freeze-drying for 12 hours to obtain V2O3An electrode material.
Example 5:
the method comprises the following steps: weighing a certain amount of ammonium metavanadate, adding the ammonium metavanadate into a mixed solution of 15ml of water and 3ml of ammonia water, and stirring the mixture for 30min at room temperature by using a magnetic stirrer at the rotating speed of 700r/min to obtain a solution A with the concentration of 0.038 mol/l;
step two: weighing a certain amount of thioacetamide, adding the thioacetamide into the solution A, and stirring the thioacetamide for 60min at room temperature by using a magnetic stirrer at the rotating speed of 700r/min to obtain a solution B with the concentration of 0.16 mol/l;
step three: transferring the solution B into a polytetrafluoroethylene lining with a filling ratio of 35%; putting the mixture into an oven, wherein the solvothermal reaction temperature is 180 ℃, and the reaction time is 24 hours;
step four: collecting the product of the solvothermal reaction in a suction filtration mode, alternately washing with water and ethanol for three times, and freeze-drying for 12 hours to obtain V2O3An electrode material.
Claims (7)
1. One-step hydrothermal method for preparing V2O3A method of nanospheres comprising the steps of:
the method comprises the following steps: according to V (water): weighing 15-20 ml of water and 3-4 ml of ammonia water according to the volume ratio of V (ammonia water) to 5:1 to prepare a mixed solution, weighing a vanadium source, adding the vanadium source into the mixed solution, and stirring the mixed solution by using a magnetic stirrer at room temperature to obtain a solution A with the vanadium source concentration of 0.023-0.038 mol/L;
step two: weighing a sulfur source, adding the sulfur source into the solution A, and stirring by using a magnetic stirrer at room temperature to obtain a solution B with the sulfur source concentration of 0.13-0.17 mol/L;
step three: transferring the solution B into a polytetrafluoroethylene lining, putting the polytetrafluoroethylene lining into an oven, and carrying out solvothermal reaction at 160-200 ℃ for 18-24 h;
step four: and collecting the product of the solvothermal reaction in a suction filtration mode, washing the product, and freeze-drying the product to obtain the V2O3 electrode material.
2. The one-step hydrothermal process of claim 1 for preparing V2O3The method for preparing the nanosphere is characterized in that the vanadium source is ammonium metavanadate.
3. The one-step hydrothermal process of claim 1 for preparing V2O3A method of nanospheres characterized in that the source of sulfur is thioacetamide.
4. The one-step hydrothermal process of claim 1 for preparing V2O3The method for preparing the nanospheres is characterized in that in the step one, the stirring time of the magnetic stirrer is 10-30 min, and the rotating speed is 500-700 r/min.
5. The one-step hydrothermal process of claim 1 for preparing V2O3The method for preparing the nanospheres is characterized in that in the second step, the stirring time of the magnetic stirrer is 30-60 min, and the rotating speed is 500-700 r/min.
6. As claimed in claim1 the one-step hydrothermal method for preparing V2O3The method for preparing the nanosphere is characterized in that the filling ratio of the polytetrafluoroethylene lining in the step three is 24-35%.
7. The one-step hydrothermal process of claim 1 for preparing V2O3The method for washing the nanospheres is characterized in that the washing method in the fourth step is washing with water and ethanol alternately for three times.
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Citations (7)
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CN105621485A (en) * | 2015-12-30 | 2016-06-01 | 中国人民解放军国防科学技术大学 | Preparation method of vanadium trioxide powder |
CN105819507A (en) * | 2016-04-29 | 2016-08-03 | 陕西科技大学 | Preparation method and application of nanosheet self-assembled microflower-shaped VS2 |
US20170240752A1 (en) * | 2014-08-26 | 2017-08-24 | The Research Foundation For The State University Of New York | Vo2 and v2o5 nano- and micro-materials and processes of making and uses of same |
CN107840368A (en) * | 2017-11-21 | 2018-03-27 | 陕西科技大学 | A kind of nanometer sheet self assembly sub-micrometer flower-shape M-phase vanadium dioxide powder and preparation method thereof |
CN108117099A (en) * | 2017-12-22 | 2018-06-05 | 陕西科技大学 | A kind of spherical VOOH powders of stub self assembly and preparation method and application |
CN109772366A (en) * | 2019-03-18 | 2019-05-21 | 陕西科技大学 | A kind of preparation method of cuprous sulfide/vanadium trioxide as full PH elctro-catalyst |
CN111646509A (en) * | 2020-06-17 | 2020-09-11 | 广东工业大学 | Sodium-ion battery curled vanadium tetrasulfide nanosheet negative electrode material and preparation method and application thereof |
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2021
- 2021-05-13 CN CN202110522127.XA patent/CN113184906A/en active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
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US20170240752A1 (en) * | 2014-08-26 | 2017-08-24 | The Research Foundation For The State University Of New York | Vo2 and v2o5 nano- and micro-materials and processes of making and uses of same |
CN105621485A (en) * | 2015-12-30 | 2016-06-01 | 中国人民解放军国防科学技术大学 | Preparation method of vanadium trioxide powder |
CN105819507A (en) * | 2016-04-29 | 2016-08-03 | 陕西科技大学 | Preparation method and application of nanosheet self-assembled microflower-shaped VS2 |
CN107840368A (en) * | 2017-11-21 | 2018-03-27 | 陕西科技大学 | A kind of nanometer sheet self assembly sub-micrometer flower-shape M-phase vanadium dioxide powder and preparation method thereof |
CN108117099A (en) * | 2017-12-22 | 2018-06-05 | 陕西科技大学 | A kind of spherical VOOH powders of stub self assembly and preparation method and application |
CN109772366A (en) * | 2019-03-18 | 2019-05-21 | 陕西科技大学 | A kind of preparation method of cuprous sulfide/vanadium trioxide as full PH elctro-catalyst |
CN111646509A (en) * | 2020-06-17 | 2020-09-11 | 广东工业大学 | Sodium-ion battery curled vanadium tetrasulfide nanosheet negative electrode material and preparation method and application thereof |
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