CN113264555A - Two-dimensional V6O13Preparation method and application of nanosheet - Google Patents
Two-dimensional V6O13Preparation method and application of nanosheet Download PDFInfo
- Publication number
- CN113264555A CN113264555A CN202110382706.9A CN202110382706A CN113264555A CN 113264555 A CN113264555 A CN 113264555A CN 202110382706 A CN202110382706 A CN 202110382706A CN 113264555 A CN113264555 A CN 113264555A
- Authority
- CN
- China
- Prior art keywords
- dimensional
- nanosheet
- preparation
- suspension
- lithium ion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000002135 nanosheet Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title abstract description 19
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 34
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 19
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000007774 positive electrode material Substances 0.000 claims abstract description 5
- 239000000725 suspension Substances 0.000 claims description 28
- 238000006243 chemical reaction Methods 0.000 claims description 23
- 239000011259 mixed solution Substances 0.000 claims description 14
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 claims description 13
- 229910001935 vanadium oxide Inorganic materials 0.000 claims description 12
- 238000005303 weighing Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- -1 polytetrafluoroethylene Polymers 0.000 claims description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 238000003760 magnetic stirring Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 13
- 238000003786 synthesis reaction Methods 0.000 abstract description 13
- 239000010405 anode material Substances 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract description 4
- 239000002243 precursor Substances 0.000 abstract description 4
- 238000004729 solvothermal method Methods 0.000 abstract description 4
- 239000003638 chemical reducing agent Substances 0.000 abstract 1
- 229910052720 vanadium Inorganic materials 0.000 abstract 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000004146 energy storage Methods 0.000 description 3
- 239000011888 foil Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 238000004108 freeze drying Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002121 nanofiber Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910032387 LiCoO2 Inorganic materials 0.000 description 1
- 229910052493 LiFePO4 Inorganic materials 0.000 description 1
- 229910001290 LiPF6 Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910002097 Lithium manganese(III,IV) oxide Inorganic materials 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 239000005486 organic electrolyte Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 229910001868 water Inorganic materials 0.000 description 1
Images
Classifications
-
- 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
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
-
- 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
-
- 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
- C01P2006/80—Compositional purity
-
- 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 two-dimensional V6O13Preparation method and application of nanosheet, wherein V is adopted in the method2O5Is a vanadium source, absolute ethyl alcohol and deionized water are mixed according to the volume ratio of 1:3 to be used as a reducing agent, and V with high purity and excellent electrochemical performance of the lithium ion battery is synthesized in one step by a simple constant-speed rotation hydrothermal method6O13And (3) a positive electrode material. The invention uses low-cost V2O5The two-dimensional V is synthesized by taking absolute ethyl alcohol as a raw material and adopting a constant-speed rotation hydrothermal method for the first time6O13The nano-sheet solves the problem that the synthesis of the precursor by the common standing hydrothermal method and the solvothermal method needs to be carried out by a complex process of heat treatment and the like. V synthesized by uniform speed rotation hydrothermal method6O13The powder is used as the lithium ion battery anode material, shows the advantages of high specific capacity, good cycle performance and the like, and has the advantages of simple synthesis process, low cost, high synthesis speed, low energy consumption, pure product, excellent performance, easiness in large-scale preparation and application and the like.
Description
Technical Field
The invention belongs to the technical field of energy storage materials, and particularly relates to a two-dimensional V6O13A preparation method and application of the nano-sheet.
Background
The rechargeable lithium ion battery has high energy density, high power density, long cycle performance and good safety performance, so that the rechargeable lithium ion battery becomes a key component in the fields of portable electronic equipment, power automobiles and large-scale energy storage. As is well known, the positive electrode material is the key to determine the energy density and cost of lithium ion batteries, and the currently commercially used positive electrode material of lithium ion batteries mainly comprises LiMn2O4、LiCoO2、LiFePO4And the theoretical specific capacities of the lithium ion batteries are lower (100-250 mAh/g), so that the further improvement of the energy density of the lithium ion batteries is greatly limited, and the wider application of the future energy storage technology is influenced. Vanadium Oxide (VO)2、V2O5、V3O7·H2O、V6O13、V2O3) Due to the advantages of various valence states, easy ion intercalation and deintercalation of the layered structure, rich reserve, environmental protection and the like, the layered structure becomes a potential electrode material in the lithium ion battery. Wherein V6O13Is a twisted VO formed by single and double layers alternately6The octahedrons are arranged in a zigzag manner in a common edge or common angle and belong to a monoclinic system. And delay [010]The crystal orientation forms an ion diffusion channel like a square pyramid, and the unit cell V6O13Can theoretically accommodate 8 Li ions and thus have a high theoretical specific capacity (417mAh/g) and energy density (890 Wh/Kg). In addition, V6O13Is metal at room temperatureAnd (3) state, good electronic conductivity. In 1979V was first identified in Murphy group6O13Used as a positive electrode material of a lithium ion battery, it was found to exhibit a good electrochemical performance. But because of V6O13Is vanadium oxide with mixed valence, the valence state of the vanadium oxide is difficult to control, the traditional solid phase method and the traditional gas phase method are difficult to synthesize pure phase, the traditional liquid phase hydrothermal method and the traditional solvothermal method are complex in synthesis process, and the product is impure to be not beneficial to V6O13The development of (1). Zhongguang et al synthesize V by solvothermal synthesis, freeze drying and calcining annealing treatment6O13/V6O13-y nanosheets. Huiqi Li et al synthesized V by sol-gel method combined with freeze-drying treatment2O5The nanofiber precursor is then calcined in argon to obtain V6O13And (3) nano fibers. Synthesis of NH by Xiaogong Tian et al by hydrothermal method4V4O10The precursor of the micro flower is combined with the heat treatment process to obtain V6O13Nanosheets. Synthesis of V6O13Most of the studies in (1) require a complicated and energy-consuming preparation process, which is very disadvantageous for industrialization, and it is important to explore a synthesis process with simple process, low energy consumption, time saving and high efficiency.
The hydrothermal method is used as a traditional liquid phase synthesis method, and the prepared powder has the advantages of good crystallization, purity, singleness, no agglomeration, superfine powder and the like, but a great amount of mesophase impurities are still inevitably generated in the synthesis process, which is very unfavorable for the purity of the product.
Disclosure of Invention
To overcome the disadvantages and shortcomings of the prior art and solve the problem of V with mixed valence6O13The invention provides a two-dimensional V, which has the problems of difficult synthesis, complex process and energy consumption6O13The preparation method and application of the nanosheet are characterized in that the two-dimensional V with high purity and good electrochemical performance is synthesized by a simple, efficient and low-consumption uniform-speed rotation hydrothermal method6O13Nanosheets.
The invention is realized by the following technical scheme:
two-dimensional V6O13A method of making nanoplatelets comprising the steps of:
step 1) mixing absolute ethyl alcohol and deionized water according to the volume ratio of 1:3 to prepare a mixed solution A;
step 2) weighing V2O5Adding raw materials into the mixed solution A prepared in the step 1), and magnetically stirring at room temperature to obtain a suspension B;
step 3) transferring the suspension B prepared in the step 2) into a high-pressure reaction kettle with a polytetrafluoroethylene lining, screwing the reaction kettle onto a middle rotating shaft of an oven, rotating at a constant speed of 360 degrees, carrying out hydrothermal reaction and preserving heat;
step 4), cooling to room temperature after the hydrothermal reaction is finished to obtain a suspension C;
step 5) washing the suspension C prepared in the step 4) by deionized water and absolute ethyl alcohol, and drying at 80 ℃ for 12h to obtain vanadium oxide powder with good dispersibility, namely the two-dimensional V6O13Nanosheets.
Preferably, the rotation speed of the magnetic stirring in the step 2) is 600r/min, and the time is 1.5 h.
Preferably, the rotating speed of the uniform rotation in the step 3) is 20-80 r/min.
Preferably, the temperature of the hydrothermal reaction in the step 3) is 200 ℃, and the heat preservation time is 4-6 h.
Two-dimensional V prepared by the preparation method6O13The nanosheet is applied to a lithium ion battery.
The lithium ion battery cathode material comprises the two-dimensional V prepared by the preparation method6O13Nanosheets.
The invention has the following beneficial effects:
1. the synthesis method is a constant-speed rotation hydrothermal method, and is a method for improving a common standing hydrothermal method. The invention uses low-cost V2O5The two-dimensional V is synthesized by adopting absolute ethyl alcohol as a raw material and adopting a constant-speed rotation hydrothermal method6O13The nanosheet is reacted, and the reaction kettle rotates at a constant speed of 360 degrees to ensure that the reaction is more uniform and sufficient,simultaneously quickens the reaction speed, greatly shortens the reaction time, and overcomes the defect that the traditional gas phase and solid phase method is difficult to synthesize V6O13The defect of pure phase, the obtained phase is purer, the subsequent calcination heat treatment process is not needed, the reaction process is simpler, the synthesis cost and the synthesis time are greatly saved, and the problem that the complex processes of the heat treatment process and the like are needed when the precursor is synthesized by the common standing hydrothermal method and the solvothermal method is solved.
2. The invention adopts a constant-speed rotation hydrothermal method to synthesize V6O13The powder is used as the lithium ion battery anode material, shows the advantages of high specific capacity, good cycle performance and the like, and has the advantages of simple synthesis process, low cost, high synthesis speed, low energy consumption, pure product, excellent performance, easiness in large-scale preparation and application and the like.
Drawings
FIG. 1 is a two-dimensional V6O13A flow diagram of nanosheet preparation;
FIG. 2 shows V obtained in example 16O13SEM atlas of the powder;
FIG. 3 is an XRD pattern of the products obtained in examples 1 to 3 and comparative examples 1 to 2;
FIG. 4 shows V in example 46O13The powder is used as a lithium ion battery anode material charge-discharge cycle performance diagram.
Detailed Description
The technical solution of the present invention is further described below with reference to the accompanying drawings, but the embodiments of the present invention are not limited thereto, and the process parameters not specifically mentioned may be performed by referring to the conventional techniques.
Example 1
Two-dimensional V6O13The preparation method of the nanosheet is shown in figure 1, and the nanosheet is prepared into V with high purity and good electrochemical performance through constant-speed rotation hydrothermal method6O13The nano-sheet comprises the following specific steps:
(1) and mixing absolute ethyl alcohol and deionized water according to the volume ratio of 1:3 to prepare 40mL of mixed solution A.
(2) Weighing 0.5g V2O5Adding the raw materials into the mixed solution A, and magnetically stirring for 1.5h at the room temperature at the rotating speed of 600r/min to obtain a suspension B.
(3) And transferring the suspension B into a high-pressure reaction kettle with a polytetrafluoroethylene lining, wherein the specification of the high-pressure reaction kettle is 70mL, screwing the reaction kettle onto a middle rotating shaft of an oven, rotating at a constant speed of 360 degrees at a rotating speed of 20r/min, setting the hydrothermal reaction temperature to be 200 ℃, and keeping the temperature for 5 hours.
(4) And cooling to room temperature after the hydrothermal reaction is finished to obtain a suspension C.
(5) Washing the suspension C with deionized water and absolute ethyl alcohol for 3 times respectively, and drying at 80 ℃ for 12 hours to obtain vanadium oxide powder with good dispersibility, namely the two-dimensional V6O13Nanosheets.
FIG. 2 shows V obtained in this example6O13As shown in fig. 2, most of the products obtained by the uniform-speed rotation hydrothermal method are two-dimensional nanosheets, and are uniformly distributed, and the surface of the synthesized nanosheet can be seen to be smooth and defect-free by higher-magnification SEM, which further indicates that the powder synthesized by the uniform-speed rotation hydrothermal method has good crystallinity.
Example 2
Two-dimensional V6O13The preparation method of the nanosheet comprises the following specific steps:
(1) and mixing absolute ethyl alcohol and deionized water according to the volume ratio of 1:3 to prepare 40mL of mixed solution A.
(2) Weighing 0.5g V2O5Adding the raw materials into the mixed solution A, and magnetically stirring for 1.5h at the room temperature at the rotating speed of 600r/min to obtain a suspension B.
(3) And transferring the suspension B into a high-pressure reaction kettle with a polytetrafluoroethylene lining, wherein the specification of the high-pressure reaction kettle is 70mL, screwing the reaction kettle onto a middle rotating shaft of an oven, rotating at a constant speed of 360 degrees at a rotating speed of 20r/min, setting the hydrothermal reaction temperature to be 200 ℃, and keeping the temperature for 4 hours.
(4) And cooling to room temperature after the hydrothermal reaction is finished to obtain a suspension C.
(5) Washing the suspension C with deionized water and anhydrous ethanol for 3 times respectively, and drying at 80 deg.C for 12 hr to obtain vanadium oxide powder with good dispersibilityThe two dimensions V6O13Nanosheets.
Example 3
Two-dimensional V6O13The preparation method of the nanosheet comprises the following specific steps:
(1) and mixing absolute ethyl alcohol and deionized water according to the volume ratio of 1:3 to prepare 40mL of mixed solution A.
(2) Weighing 0.5g V2O5Adding the raw materials into the mixed solution A, and magnetically stirring for 1.5h at the room temperature at the rotating speed of 600r/min to obtain a suspension B.
(3) And transferring the suspension B into a high-pressure reaction kettle with a polytetrafluoroethylene lining, wherein the specification of the high-pressure reaction kettle is 70mL, screwing the reaction kettle onto a middle rotating shaft of an oven, rotating at a constant speed of 360 degrees at a rotating speed of 80r/min, setting the hydrothermal reaction temperature to be 200 ℃, and keeping the temperature for 6 hours.
(4) And cooling to room temperature after the hydrothermal reaction is finished to obtain a suspension C.
(5) Washing the suspension C with deionized water and absolute ethyl alcohol for 3 times respectively, and drying at 80 ℃ for 12 hours to obtain vanadium oxide powder with good dispersibility, namely the two-dimensional V6O13Nanosheets.
Comparative example 1
A preparation method of vanadium oxide comprises the following specific steps:
(1) and mixing absolute ethyl alcohol and deionized water according to the volume ratio of 1:3 to prepare 40mL of mixed solution A.
(2) Weighing 0.5g V2O5Adding the raw materials into the mixed solution A, and magnetically stirring for 1.5h at the room temperature at the rotating speed of 600r/min to obtain a suspension B.
(3) And transferring the suspension B into a high-pressure reaction kettle with a polytetrafluoroethylene lining, wherein the specification of the high-pressure reaction kettle is 70mL, screwing the reaction kettle onto a middle rotating shaft of an oven, and keeping the temperature for 5 hours while setting the hydrothermal reaction temperature to be 200 ℃.
(4) And cooling to room temperature after the hydrothermal reaction is finished to obtain a suspension C.
(5) And washing the suspension C with deionized water and absolute ethyl alcohol for 3 times respectively, and drying at 80 ℃ for 12 hours to obtain vanadium oxide powder.
Comparative example 2
A preparation method of vanadium oxide comprises the following specific steps:
(1) and mixing absolute ethyl alcohol and deionized water according to the volume ratio of 1:1 to prepare 40mL of mixed solution A.
(2) Weighing 0.5g V2O5Adding the raw materials into the mixed solution A, and magnetically stirring for 1.5h at the room temperature at the rotating speed of 600r/min to obtain a suspension B.
(3) And transferring the suspension B into a high-pressure reaction kettle with a polytetrafluoroethylene lining, wherein the specification of the high-pressure reaction kettle is 70mL, screwing the reaction kettle onto a middle rotating shaft of an oven, rotating at a constant speed of 360 degrees at a rotating speed of 20r/min, setting the hydrothermal reaction temperature to be 200 ℃, and keeping the temperature for 5 hours.
(4) And cooling to room temperature after the hydrothermal reaction is finished to obtain a suspension C.
(5) And washing the suspension C with deionized water and absolute ethyl alcohol for 3 times respectively, and drying at 80 ℃ for 12 hours to obtain vanadium oxide powder.
Test example 1
The phase characterization of the products obtained in examples 1-3 and comparative examples 1-2 was carried out by XRD technique and comparison with V6O13The results are shown in figure 3 and table 1 below for the standard card.
TABLE 1 test results
From the XRD result in FIG. 3, it can be seen that when the volume ratio of the absolute ethyl alcohol to the deionized water is 1:3, the rotation speed of the hydrothermal reaction kettle is 20-80 r/min, and the reaction time is 4-6 h, relatively pure V can be obtained6O13Phase, when the hydrothermal kettle is in standing reaction or the volume ratio of the absolute ethyl alcohol to the deionized water is 1:1, the product generates more impure phase or does not generate V6O13. Thus, it can be confirmed that examples 1 to 3 successfully produced V6O13Pure phase.
Example 4
Two-dimensional V obtained in example 16O13The nano sheet is used as a lithium ion battery anode material, and the specific steps are as follows:
(1) weighing V prepared in example 1 according to the mass ratio of 7:2:16O13Adding a proper amount of N-methyl pyrrolidone solvent into the powder, acetylene black and pvdf, and fully and uniformly grinding.
(2) Uniformly coating the uniform slurry obtained in the step (1) on an Al foil by using a casting coating machine, and then placing the Al foil coated with the slurry in a vacuum drying oven for vacuum drying for 12 hours at the temperature of 80 ℃.
(3) The dried Al foil of (2) was taken out and punched out into a circular piece having a diameter of 12mm by a hand punch to obtain a working electrode.
(4) Using the 12mm disk electrode obtained in (3) as a working electrode, a metal lithium disk as a reference electrode, a Celgard disk as a diaphragm and containing 1M LiPF6The organic electrolyte (EC: DEC: DMC ═ 1:1:1) was used as a battery electrolyte. And assembling the button cell in a glove box filled with argon by adopting a 2016 type battery case, and carrying out electrochemical performance test after the button cell is placed for 24 hours.
Through the electrochemical performance cycle test, as shown in fig. 4, when the current density is 500mA/g, the initial discharge capacity is up to 199mAh/g, and after 100 cycles, the capacity retention rate is close to 87%. V illustrating constant speed rotation hydro-thermal synthesis6O13The two-dimensional nano-sheet has a relatively stable structure in Li+The agglomeration is not easy to occur in the transmission process, a better electrochemical performance is provided, and the lithium ion battery electrode material is very potential.
Claims (6)
1. Two-dimensional V6O13The preparation method of the nanosheet is characterized by comprising the following steps:
step 1) mixing absolute ethyl alcohol and deionized water according to the volume ratio of 1:3 to prepare a mixed solution A;
step 2) weighing V2O5Adding raw materials into the mixed solution A prepared in the step 1), and magnetically stirring at room temperature to obtain a suspension B;
step 3) transferring the suspension B prepared in the step 2) into a high-pressure reaction kettle with a polytetrafluoroethylene lining, screwing the reaction kettle onto a middle rotating shaft of an oven, rotating at a constant speed of 360 degrees, carrying out hydrothermal reaction and preserving heat;
step 4), cooling to room temperature after the hydrothermal reaction is finished to obtain a suspension C;
step 5) washing the suspension C prepared in the step 4) by deionized water and absolute ethyl alcohol, and drying at 80 ℃ for 12h to obtain vanadium oxide powder with good dispersibility, namely the two-dimensional V6O13Nanosheets.
2. A two-dimensional V according to claim 16O13The preparation method of the nanosheet is characterized in that the rotation speed of the magnetic stirring in the step 2) is 600r/min, and the time is 1.5 h.
3. A two-dimensional V according to claim 16O13The preparation method of the nanosheet is characterized in that the rotation speed of the uniform rotation in the step 3) is 20-80 r/min.
4. A two-dimensional V according to claim 16O13The preparation method of the nanosheet is characterized in that the temperature of the hydrothermal reaction in the step 3) is 200 ℃, and the heat preservation time is 4-6 h.
5. Two-dimensional V obtained by the production method according to any one of claims 1 to 46O13The nanosheet is applied to a lithium ion battery.
6. A lithium ion battery positive electrode material, characterized by comprising the two-dimensional V prepared by the preparation method of any one of claims 1 to 46O13Nanosheets.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110382706.9A CN113264555A (en) | 2021-04-09 | 2021-04-09 | Two-dimensional V6O13Preparation method and application of nanosheet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110382706.9A CN113264555A (en) | 2021-04-09 | 2021-04-09 | Two-dimensional V6O13Preparation method and application of nanosheet |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113264555A true CN113264555A (en) | 2021-08-17 |
Family
ID=77228622
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110382706.9A Pending CN113264555A (en) | 2021-04-09 | 2021-04-09 | Two-dimensional V6O13Preparation method and application of nanosheet |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113264555A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113929140A (en) * | 2021-09-15 | 2022-01-14 | 扬州大学 | Transition metal doped V6O13Nanobelt material and preparation method and application thereof |
| CN114804204A (en) * | 2022-06-07 | 2022-07-29 | 烟台大学 | Preparation of V by solvothermal-carbon reduction method 6 O 13 Method for preparing nano ball material |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090117464A1 (en) * | 2007-11-07 | 2009-05-07 | Korea Institute Of Science And Technology | Fabrication method for electrode active material and lithium battery comprising electrode active material fabricated therefrom |
| CN203525722U (en) * | 2013-09-13 | 2014-04-09 | 蚌埠市天星树脂有限责任公司 | Auto-rotation reaction kettle |
| CN104617264A (en) * | 2015-01-08 | 2015-05-13 | 南京航空航天大学 | Synthetic method of high-performance one-dimensional nanostructure vanadium oxide lithium ion battery electrode material |
| CN105540666A (en) * | 2015-12-21 | 2016-05-04 | 桂林理工大学 | Method for preparing nanofiber-shaped vanadium oxide powder by using oil bath pan |
| CN109052472A (en) * | 2018-08-13 | 2018-12-21 | 郑州比克电池有限公司 | A kind of layer structure V6O13Positive electrode and preparation method thereof |
| CN110306236A (en) * | 2019-07-12 | 2019-10-08 | 暨南大学 | Large scale V6O13Single-chip and preparation method thereof |
| CN110422879A (en) * | 2019-08-21 | 2019-11-08 | 电子科技大学 | A kind of high latent heat of phase change vanadium oxide powder and preparation method thereof |
| CN112604706A (en) * | 2021-01-15 | 2021-04-06 | 荆楚理工学院 | Preparation method and application of nitrogen-containing super-crosslinked polymer-derived Co @ CN catalyst |
-
2021
- 2021-04-09 CN CN202110382706.9A patent/CN113264555A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090117464A1 (en) * | 2007-11-07 | 2009-05-07 | Korea Institute Of Science And Technology | Fabrication method for electrode active material and lithium battery comprising electrode active material fabricated therefrom |
| CN203525722U (en) * | 2013-09-13 | 2014-04-09 | 蚌埠市天星树脂有限责任公司 | Auto-rotation reaction kettle |
| CN104617264A (en) * | 2015-01-08 | 2015-05-13 | 南京航空航天大学 | Synthetic method of high-performance one-dimensional nanostructure vanadium oxide lithium ion battery electrode material |
| CN105540666A (en) * | 2015-12-21 | 2016-05-04 | 桂林理工大学 | Method for preparing nanofiber-shaped vanadium oxide powder by using oil bath pan |
| CN109052472A (en) * | 2018-08-13 | 2018-12-21 | 郑州比克电池有限公司 | A kind of layer structure V6O13Positive electrode and preparation method thereof |
| CN110306236A (en) * | 2019-07-12 | 2019-10-08 | 暨南大学 | Large scale V6O13Single-chip and preparation method thereof |
| CN110422879A (en) * | 2019-08-21 | 2019-11-08 | 电子科技大学 | A kind of high latent heat of phase change vanadium oxide powder and preparation method thereof |
| CN112604706A (en) * | 2021-01-15 | 2021-04-06 | 荆楚理工学院 | Preparation method and application of nitrogen-containing super-crosslinked polymer-derived Co @ CN catalyst |
Non-Patent Citations (2)
| Title |
|---|
| ZHENDONG WAN ET AL.: "Synthesis and Electrochemical Properties of Fibrous V6O13 for Li-ion Batteries", 《2018 IOP CONF. SER.: MATER. SCI. ENG.》 * |
| ZHENGGUANG ZOU ET AL.: "V6O13Nanosheets Synthesized From Ethanol-Aqueous Solutions asHigh Energy Cathode Material for Lithium-Ion Batteries", 《ELECTROCHIMICA ACTA》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113929140A (en) * | 2021-09-15 | 2022-01-14 | 扬州大学 | Transition metal doped V6O13Nanobelt material and preparation method and application thereof |
| CN113929140B (en) * | 2021-09-15 | 2023-05-26 | 扬州大学 | V doped with transition metal 6 O 13 Nano belt material and preparation method and application thereof |
| CN114804204A (en) * | 2022-06-07 | 2022-07-29 | 烟台大学 | Preparation of V by solvothermal-carbon reduction method 6 O 13 Method for preparing nano ball material |
| CN114804204B (en) * | 2022-06-07 | 2023-11-28 | 烟台大学 | V is prepared by solvothermal-carbon reduction method 6 O 13 Method for preparing nanometer flower ball material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100530780C (en) | Composite lithium titanate electrode material and preparation method thereof | |
| CN111799468B (en) | Lithium ion battery anode material jointly modified by ionic conductor and heterostructure, preparation method and application | |
| EP3565038A1 (en) | Method for preparing graphene/ternary material composite for use in lithium ion batteries and product thereof | |
| Zhao et al. | Rapid hydrothermal and post-calcination synthesis of well-shaped LiNi0. 5Mn1. 5O4 cathode materials for lithium ion batteries | |
| CN108821348B (en) | Cobalt sulfide nanosheet material and preparation method thereof | |
| CN106207158B (en) | The preparation method of rich lithium manganate cathode material for lithium | |
| CN108448109A (en) | A kind of stratiform lithium-rich manganese-based anode material and preparation method thereof | |
| Zhao et al. | A simple and facile one-step strategy to synthesize orthorhombic LiMnO2 nano-particles with excellent electrochemical performance | |
| CN104577072A (en) | Preparation method of graphene-oxide-based MoO2 high-performance electrode material of lithium/sodium ion battery | |
| CN113264555A (en) | Two-dimensional V6O13Preparation method and application of nanosheet | |
| Zhang et al. | Research status of spinel LiMn2O4 cathode materials for lithium ion batteries | |
| CN114864896A (en) | In-situ carbon-coated nano lithium iron phosphate cathode material and preparation method thereof | |
| CN110862109B (en) | Method for preparing ternary cathode material of lithium ion battery by hydrothermal auxiliary coprecipitation strategy | |
| CN109052474B (en) | Preparation method and application of large-particle sodium chromite material | |
| CN114436345A (en) | Ternary cathode material of lithium ion battery and preparation method thereof | |
| CN108232186A (en) | A kind of preparation method of single crystal grain and its application in the secondary battery | |
| Wang et al. | Nano-sized over-lithiated oxide by a mechano-chemical activation-assisted microwave technique as cathode material for lithium ion batteries and its electrochemical performance | |
| CN116119739A (en) | Ion doped manganese-based sodium ion positive electrode material and preparation method and application thereof | |
| CN110190277A (en) | A kind of anode material for lithium-ion batteries LiMnO2@C and preparation method thereof | |
| Lu et al. | Research progress of cathode materials for lithium-ion batteries | |
| CN114956210A (en) | Single crystal lithium ion battery anode material with different layered structures and preparation method and application thereof | |
| CN101521275B (en) | Method for preparing nickel lithium silicate as positive pole material of secondary lithium-ion battery | |
| CN114759179A (en) | Method for synthesizing anode material sodium iron phosphate for sodium ion battery | |
| CN114906882A (en) | Preparation method and application of niobium-based bimetal oxide negative electrode material | |
| CN104037410A (en) | Preparation method of lithium ion battery positive pole material LiFePO4/C |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210817 |
|
| RJ01 | Rejection of invention patent application after publication |