CN108428934B - Microsphere AlV3O9Method for serving as positive electrode of aluminum ion battery - Google Patents
Microsphere AlV3O9Method for serving as positive electrode of aluminum ion battery Download PDFInfo
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 56
- 239000004005 microsphere Substances 0.000 title claims abstract description 35
- -1 aluminum ion Chemical class 0.000 claims abstract description 49
- 229910016864 AlV3O9 Inorganic materials 0.000 claims abstract description 18
- 239000007772 electrode material Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 13
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000011888 foil Substances 0.000 claims abstract description 8
- 239000010405 anode material Substances 0.000 claims abstract description 6
- 239000003792 electrolyte Substances 0.000 claims abstract description 6
- NJMWOUFKYKNWDW-UHFFFAOYSA-N 1-ethyl-3-methylimidazolium Chemical compound CCN1C=C[N+](C)=C1 NJMWOUFKYKNWDW-UHFFFAOYSA-N 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 12
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 11
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 11
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 11
- 238000012360 testing method Methods 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 6
- 238000010335 hydrothermal treatment Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 claims description 4
- 229940009861 aluminum chloride hexahydrate Drugs 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 4
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 239000011829 room temperature ionic liquid solvent Substances 0.000 claims description 3
- 238000002474 experimental method Methods 0.000 claims description 2
- 230000002349 favourable effect Effects 0.000 claims 1
- 229910052750 molybdenum Inorganic materials 0.000 claims 1
- 239000011733 molybdenum Substances 0.000 claims 1
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 abstract description 5
- 238000011161 development Methods 0.000 abstract description 5
- 238000000840 electrochemical analysis Methods 0.000 abstract description 4
- FQERWQCDIIMLHB-UHFFFAOYSA-N 1-ethyl-3-methyl-1,2-dihydroimidazol-1-ium;chloride Chemical compound [Cl-].CC[NH+]1CN(C)C=C1 FQERWQCDIIMLHB-UHFFFAOYSA-N 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 239000002131 composite material Substances 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- HIMLGVIQSDVUJQ-UHFFFAOYSA-N aluminum vanadium Chemical compound [Al].[V] HIMLGVIQSDVUJQ-UHFFFAOYSA-N 0.000 description 11
- 239000007774 positive electrode material Substances 0.000 description 8
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 5
- 239000002243 precursor Substances 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229940063656 aluminum chloride Drugs 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000010485 coping Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- H01M10/058—Construction or manufacture
-
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
Microsphere AlV3O9As a method for preparing the positive electrode of the aluminum ion battery, the microsphere AlV is prepared by a hydrothermal method3O9The microstructure and the morphology of the microsphere are verified by an off-site scanning electron microscope, and the prepared microsphere AlV3O9As the anode material of the aluminum ion battery, high-purity aluminum foil as the cathode, and anhydrous aluminum chloride (AlCl)3) And 1-ethyl-3-methylimidazole chloride ([ EMIm)]Cl) was prepared in a molar mass of 1.3:1 as an electrolyte for an aluminum ion cell as a yellowish transparent ionic room temperature liquid. The battery formed by the composite material has excellent electrochemical performance in an electrochemical test, the first discharge specific capacity is 321.7mA h/g and the charge specific capacity is 294mA h/g under the current density of 100 mA/g. AlV3O9The 3-dimensional microspheres consist of a nano-layered structure and are beneficial to Al3+Embedding and extracting the electrode material. Microsphere AlV3O9The application in the aluminum ion battery lays a foundation for the development of other electrode materials in the aluminum ion battery.
Description
Technical Field
The invention relates to a hydrothermal method for preparing AlV3O9The microsphere is used as a positive electrode material of the aluminum ion battery and applied to the aluminum ion battery. The invention belongs to an electrode material for electrochemical energy storage and conversion in the field of new energy, and can be used in the field of new energy.
Background
Renewable energy is an important component of energy supply systems. At present, the development and utilization scale of global renewable energy is continuously enlarged, the application cost is rapidly reduced, and the development of renewable energy becomes the core content of energy transformation promotion and important way for coping with climate change in many countries, and is also an important measure for promoting energy production and consumption revolution and energy transformation in China. An efficient and sustainable energy storage mode is urgently needed in modern society. The large-scale use of renewable energy sources is not achieved mainly due to the continuity of the way they are produced, and they are also not storable (statistically, less than one percent of renewable energy sources can be stored at present). Therefore, the development of efficient, low-cost and environmentally friendly electrochemical storage systems is a must path for sustainable renewable energy. The continuous consumption of fossil fuels, the dramatic emission of greenhouse gases, and the steep rise in PM2.5 have attracted widespread attention over the past decades. Therefore, people are seeking and developing renewable green new energy sources, such as wind energy, solar energy and the like. Due to the non-uniformity of the distribution of these renewable energy sources over time and space, they are often required to be used with efficient energy storage devices.
At present, in the field of efficient new energy, lithium ion batteries have been widely used in life, and have been developed rapidly due to the increasing development demand of power automobiles, but the content of metal lithium in earth crust is quite limited, and the energy density of carbides thereof in lithium ion batteries is greatly limited, which hardly meets the increasing research on the energy density of power batteries, thus severely limiting the further application thereof in power batteries.
Therefore, other metal ion batteries are receiving wide attention of scientists, including metal ion batteries of Na, Mg, Zn, K, Al and the like, but the storage amount of metal aluminum in the earth crust is the most abundant, which greatly reduces the cost of the aluminum ion battery to a certain extent, and the volume energy density is quite high, which lays a theoretical foundation for improving the energy density of the aluminum ion battery. It is well known that the key role of improving the energy density of the battery is the positive electrode material, so the research on the positive electrode material of the aluminum ion battery is wide at present, but the AlV provided by the invention3O9Microspheres have not been studied in aluminum ion batteries.
Disclosure of Invention
The invention aims to prepare AlV by using a hydrothermal treatment method3O9The microspheres are applied to the aluminum ion battery by utilizing the three-dimensional space structure of the microspheres, and a novel method is provided for improving the energy density of the aluminum ion battery. Wherein the ions inserted and extracted in the charge and discharge process are Al3+Is not AlCl4 -This realizes the redox reaction of three electrons in the aluminum ion battery, which provides the possibility for the aluminum ion battery to be commercialized in the future.
Micro-meterBall AlV3O9The method for serving as the anode of the aluminum ion battery is characterized by comprising the following steps of preparing the electrode, assembling the battery and testing:
(1) microsphere AlV3O9Preparing materials: ammonium metavanadate (molecular weight 116.98) was first dissolved in 40mL of deionized water (DI) at a temperature of 80 degrees and to this solution was added dropwise a hydrochloric acid solution with magnetic stirring. Aluminum chloride hexahydrate (molecular weight 241.43) was then added to the above solution, stirred well for 10 minutes and then placed in a 50mL autoclave for hydrothermal treatment. The solution cooled to room temperature was then washed three times by centrifugation with water and ethanol, respectively, after which the resulting precipitate was placed in a vacuum oven for 12h at 80 ℃. Finally, calcining the microspheres in a muffle furnace to obtain microspheres AlV3O9A material.
(2) Preparing an electrode material: cutting a molybdenum sheet and a high-purity aluminum foil into sheets with the specification of 1cm multiplied by 2cm, respectively ultrasonically washing the sheets for 3 times by using deionized water and absolute alcohol, then drying the sheets in a vacuum drying oven at 60 ℃, finally preparing a sol solution of the material prepared in the step (1) and Polytetrafluoroethylene (PTFE) in NMP (N-methyl pyrrolidone) to be coated on the molybdenum sheet, and drying the sol solution in the drying oven to obtain AlV (aluminum vanadium)3O9The electrode material is used as the anode material of the aluminum ion battery.
(3) Assembling the aluminum ion battery: firstly, anhydrous aluminum chloride (AlCl)3) And 1-ethyl-3-methylimidazole chloride ([ EMIm)]Cl) is prepared in a glove box according to the molar mass of 1.3:1, both are poured into a three-neck flask, and the mixture is uniformly stirred for 30 minutes to obtain a light yellow transparent room-temperature ionic liquid as an electrolyte of the aluminum ion battery. And (3) finally, taking the electrode material prepared in the step (2) and the aluminum foil as the anode and the cathode of the aluminum ion battery respectively, and preparing the aluminum ion battery in a glove box (the water oxygen content is less than 0.1%).
Further, in step (1), the amounts of ammonium metavanadate and aluminum chloride hexahydrate were 105.3mg (0.9mmol) and 434.6mg (1.8mmol), respectively.
Further, in step (1), a hydrochloric acid solution is added dropwise to the solution so that the final pH is stabilized at 2 to 4.
Further, in the step (1), the conditions of hydrothermal treatment in the reaction kettle are as follows: the temperature is 120-180 ℃ and the time is 3-8h.
Further, in the step (1), the treatment conditions are calcined in a muffle furnace: the temperature is 300-600 ℃, and the time is 2-4 h.
Further, in the step (2), PTFE is used as a binder of the aluminum ion battery, and the PTFE and AlV are mixed3O9The mass ratio of the materials is 2:8.
Further, in the step (2), the drying conditions of the prepared electrode material in the vacuum drying oven are as follows: the temperature is 80-120 ℃ and the time is 6-12h, so as to dry the NMP organic solvent and avoid the oxidation of the electrode material.
In step (3), the assembly of the aluminum ion battery is prepared in a glove box in order to avoid the reaction of the electrolyte and moisture in the air, etc., and this also contributes to the repeatable operation of the experiment.
The electrochemical test conditions of the assembled battery are as follows: the current density is 100mA/g, the voltage range is 0.1V-0.9V, and the test conditions of the current density and the voltage range in different charging and discharging curves are as follows: the current densities were 100mA/g, 200mA/g and 300mA/g, respectively.
The invention prepares AlV by hydrothermal treatment3O9The microsphere is used as the anode material of the aluminum ion battery, the microscopic morphology and the structure of the microsphere are verified by an off-field Scanning Electron Microscope (SEM), the electrochemical performance of the microsphere is obtained by constant current charge-discharge tests, and the excellent electrochemical performance of the microsphere lays a foundation for the commercialization of the aluminum ion battery.
Drawings
FIG. 1 shows the AlV microspheres as the positive electrode material of the aluminum-ion battery prepared by the invention3O9Off-field Scanning Electron Microscopy (SEM) images of the precursors.
FIG. 2 shows the AlV microspheres as the positive electrode material of the aluminum-ion battery prepared by the invention3O9Off-field Scanning Electron Microscopy (SEM) images of (a).
FIG. 3 shows the AlV microspheres as the positive electrode material of the aluminum-ion battery prepared by the invention3O9First charge and discharge graph (current density of 100 mA/g).
FIG. 4 shows the AlV microspheres as the positive electrode material of the aluminum-ion battery prepared by the invention3O9Differential plot of capacity at a current density of 100 mA/g.
FIG. 5 shows the AlV microspheres as the positive electrode material of the aluminum-ion battery prepared by the invention3O9Graphs of charge and discharge at different current densities (100mA/g, 200mA/g and 300 mA/g).
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and examples. The technical solutions of the present invention are clearly and completely described, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention
Examples one,
Step one, microsphere AlV3O9Preparing materials:
1. 105.3mg (0.9mmol) of ammonium metavanadate (NH)4VO3) Dissolved in 40mL of deionized water at a temperature of 80 c, to which a hydrochloric acid solution was added dropwise with vigorous magnetic stirring to stabilize the final PH at 3.
2. 434.6mg (1.8mmol) of AlCl36H2O and 500mg PVP were added to the above solution under magnetic stirring, and after 10 minutes stirring a yellow suspension was obtained.
3. The precursor solution was added to a 50mL reaction kettle and heat treated at 160 degrees for 6 hours. Washing the obtained dark green precipitate with deionized water and anhydrous ethanol for three times, and drying in vacuum oven at 80 deg.C for 6 hr to obtain AlV3O9The precursor of (1). The scanning electron micrograph is shown in figure 1.
4. Heating the obtained precursor to 450 ℃ at the speed of 2 ℃/min in a muffle furnace, then carrying out heat preservation and calcination for 2 hours to finally obtain highly-crystallized AlV3O9. The scanning electron micrograph is shown in FIG. 2.
Step two, preparing an electrode material: mixing molybdenum sheet and high-purity aluminumCutting the foil into sheets with the specification of 1cm multiplied by 2cm, respectively ultrasonically washing the sheets for 3 times by using deionized water and absolute ethyl alcohol, then drying the sheets in a vacuum drying oven at 60 ℃, and finally, mixing the material prepared in the step (1) and Polytetrafluoroethylene (PTFE) according to the mass ratio of 8: 2, preparing a sol solution in NMP, coating the sol solution on a molybdenum sheet, and drying the molybdenum sheet in a drying oven at 120 ℃ for 8 hours to obtain AlV3O9The electrode material is used as the anode material of the aluminum ion battery.
Step three, assembling the aluminum ion battery: firstly, AlCl is added3And [ EMIm]And preparing Cl in a glove box according to the molar mass of 1.3:1, pouring the Cl and the Cl into a three-neck flask, and uniformly stirring for 30 minutes to obtain a light yellow transparent room-temperature ionic liquid serving as an electrolyte of the aluminum ion battery. And (3) finally, taking the electrode material prepared in the step (2) and the aluminum foil as the anode and the cathode of the aluminum ion battery respectively, and preparing the aluminum ion battery in a glove box (the water oxygen content is less than 0.1%).
Step four, assembling the electrochemical test conditions of the battery, wherein the test conditions of the first charge-discharge curve are as follows: the current density is 100mA/g, the voltage range is 0.1V-0.9V, and the test conditions of the current density and the voltage range in different charging and discharging curves are as follows: the current density is 100mA/g, 200mA/g and 300mA/g respectively, and the voltage range is 0.1V-0.9V. The test results are shown in fig. 3, 4 and 5, respectively.
Examples two,
The steps are the same as the first step of the embodiment;
step two, preparing an electrode material: cutting a molybdenum sheet and a high-purity aluminum foil into sheets with the specification of 1cm multiplied by 2cm, respectively ultrasonically washing the sheets for 3 times by using deionized water and absolute alcohol, then drying the sheets in a vacuum drying oven at 60 ℃, and finally, mixing the material prepared in the step (1) and Polytetrafluoroethylene (PTFE) according to the mass ratio of 9: 1 preparing a sol solution in NMP to coat on a molybdenum sheet, and drying the molybdenum sheet in a drying oven at 120 ℃ for 8h to obtain AlV3O9The electrode material is used as the anode material of the aluminum ion battery.
Step three is the same as the step three of the example;
step four, the same as the step four of the first embodiment;
examples III,
The steps are the same as the first step of the embodiment;
step two is the same as the step two of the embodiment;
step three is the same as the step three of the example;
step four, assembling the electrochemical test conditions of the battery, wherein the test conditions of the first charge-discharge curve are as follows: the current density is 100mA/g, the voltage range is 0.2V-1.0V, and the test conditions of the current density and the voltage range in different charging and discharging curves are as follows: the current density is 100mA/g, 200mA/g and 300mA/g respectively, and the voltage range is 0.2V-1.0V.
The above embodiments are only intended to illustrate the technical solution of the present invention and not to limit the same, and it should be understood by those of ordinary skill in the art that the specific embodiments of the present invention can be modified or substituted with equivalents with reference to the above embodiments, and any modifications or equivalents without departing from the spirit and scope of the present invention are within the scope of the claims to be appended.
Claims (7)
1. Microsphere AlV3O9The method for serving as the anode of the aluminum ion battery is characterized by comprising the following steps of preparing the electrode, assembling the battery and testing:
(1) microsphere AlV3O9Preparing materials: firstly, dissolving ammonium metavanadate with the molecular weight of 116.98 in 40mL of deionized water at the temperature of 80 ℃, and dropwise adding a hydrochloric acid solution into the solution under magnetic stirring; then adding aluminum chloride hexahydrate with the molecular weight of 241.43 into the solution, fully stirring for 10 minutes, placing the solution into a 50mL reaction kettle for hydrothermal treatment, then centrifugally washing the solution cooled to room temperature with water and ethanol for three times respectively, and then placing the obtained precipitate into a vacuum drying oven for treatment for 12 hours at the temperature of 80 ℃; finally, calcining the microspheres in a muffle furnace to obtain microspheres AlV3O9A material;
(2) preparing an electrode material: cutting a molybdenum sheet and a high-purity aluminum foil into sheets with the specification of 1cm multiplied by 2cm, respectively ultrasonically washing the sheets for 3 times by using deionized water and absolute alcohol, then drying the sheets in a vacuum drying oven at 60 ℃, finally preparing the material prepared in the step (1) and Polytetrafluoroethylene (PTFE) into a sol solution in NMP to be coated on the molybdenum sheet, and putting the sol solution on the molybdenum sheetDrying in a drying oven to obtain AlV3O9The electrode material is used as the anode material of the aluminum ion battery;
(3) assembling the aluminum ion battery: firstly, AlCl is added3And [ EMIm]Preparing Cl in a glove box according to the molar mass of 1.3:1, pouring the Cl and the Cl into a three-neck flask, and uniformly stirring for 30 minutes to obtain a light yellow transparent room-temperature ionic liquid serving as an electrolyte of the aluminum ion battery; finally, the electrode material and the aluminum foil prepared in the step (2) are respectively used as the anode and the cathode of the aluminum ion battery, and the aluminum ion battery is prepared in a glove box with the water oxygen content of less than 0.1%;
in the step (1), the hydrothermal treatment conditions in the reaction kettle are as follows: the temperature is 120-180 ℃ and the time is 3-8 h;
in the step (1), the calcination treatment conditions in a muffle furnace are as follows: the temperature is 300-600 ℃, and the time is 2-4 h.
2. Microspheres AlV according to claim 13O9The method for preparing the positive electrode of the aluminum ion battery is characterized in that in the step (1), the amounts of ammonium metavanadate and aluminum chloride hexahydrate are respectively 105.3mg and 434.6 mg.
3. Microspheres AlV according to claim 13O9The method as the positive electrode of the aluminum ion battery is characterized in that in the step (1), a hydrochloric acid solution is dropwise added to the solution so that the final pH is stabilized at 2-4.
4. Microspheres AlV according to claim 13O9The method as the positive electrode of the aluminum ion battery is characterized in that in the step (2), PTFE is used as a binder of the aluminum ion battery, and the binder and AlV3O9The mass ratio of the materials is 2:8.
5. Microspheres AlV according to claim 13O9The method for preparing the anode of the aluminum ion battery is characterized in that in the step (2), the drying conditions of the prepared electrode material in a vacuum drying oven are as follows: the temperature is 80-120 ℃ and the time is 6-12 h.
6. Microspheres AlV according to claim 13O9The method as the positive electrode of the aluminum ion battery is characterized in that in the step (3), the assembly of the aluminum ion battery is prepared in a glove box to avoid the reaction of the electrolyte and the moisture in the air, and the method is also favorable for the repeatable operation of the experiment.
7. Microspheres AlV according to claim 13O9The method for serving as the anode of the aluminum ion battery is characterized in that the test conditions of the first charge-discharge curve are as follows: the current density is 100mA/g, and the voltage range is 0.1V-0.9V; the test conditions of the material on different charging and discharging curves are as follows: the current densities were 100mA/g, 200mA/g and 300mA/g, respectively.
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| WO2007055172A1 (en) * | 2005-11-10 | 2007-05-18 | Matsushita Electric Industrial Co., Ltd. | Nonaqueous electrolyte solution and secondary battery containing same |
| KR101344455B1 (en) * | 2011-10-13 | 2013-12-26 | 주식회사 지엘비이 | Spinel lithium manganese oxide as cathode material for lithium secondary battery and a method for producing the same |
| CN104701541A (en) * | 2015-01-06 | 2015-06-10 | 北京科技大学 | Lithium-ion battery with WS2 serving as positive electrode and preparation method of lithium-ion battery |
| CN106601501A (en) * | 2017-03-07 | 2017-04-26 | 扬州大学 | Preparation method of three-dimensional band-shaped structure AlV3O9 electrode material for supercapacitor |
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2018
- 2018-04-11 CN CN201810322459.1A patent/CN108428934B/en not_active Expired - Fee Related
Non-Patent Citations (1)
| Title |
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| 3D hierarchicalAlV3O9 microspheres:First synthesis,excellentlithiumioncathode properties,andinvestigationof electrochemicalmechanism;Gongzheng Yang etc.;《ELSEVIER》;20150509;正文第281-292页 * |
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