CN115744989A - alpha-MoO 3 Nanobelt, preparation method and energy storage application of nanobelt in proton battery - Google Patents
alpha-MoO 3 Nanobelt, preparation method and energy storage application of nanobelt in proton battery Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 238000004146 energy storage Methods 0.000 title abstract description 4
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
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- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 15
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- 238000000034 method Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 9
- 239000013543 active substance Substances 0.000 claims description 9
- 239000010936 titanium Substances 0.000 claims description 9
- 229910052719 titanium Inorganic materials 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
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- DFGKGUXTPFWHIX-UHFFFAOYSA-N 6-[2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]acetyl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)C1=CC2=C(NC(O2)=O)C=C1 DFGKGUXTPFWHIX-UHFFFAOYSA-N 0.000 description 2
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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
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Abstract
The invention relates to an alpha-MoO 3 A nanobelt, a preparation method and an energy storage application thereof in a proton battery belong to the technical field of proton batteries. The preparation method comprises the following steps: adding MoO 3 Uniformly dispersing the nano particles serving as a precursor in deionized water, and carrying out hydrothermal reaction on the dispersion liquid; then cooling, washing and drying the hydrothermal product to obtain the alpha-MoO 3 A nanoribbon. The invention has the advantages of cheap and easily obtained raw materials, mild reaction conditions, short reaction time, low cost, low toxicity, simplicity and feasibility, and no template or surface activityThe sex agent uses water as a reaction solvent. alpha-MoO of the invention 3 The nanobelt can be applied to a proton battery, and achieves excellent rate capability, high energy density and long cycle stability.
Description
Technical Field
The invention belongs to the technical field of proton batteries, and particularly relates to alpha-MoO 3 Nanobelts, a preparation method and an energy storage application thereof in proton batteries.
Background
In order to solve the problem of energy shortage at present and meet the requirement of human on energy, the development of an electrochemical energy storage system with high energy density, high power density and long cycle life has important significance. The high performance of electrochemical energy storage devices is highly dependent on their electrode materials, which in turn depend on the choice of carriers. Therefore, the search for new electrode materials and suitable carriers with advanced electrochemical properties is the key to the development of electrochemical energy storage systems with high energy density, high power density and long cycle life. Ideal carriers require lower relative atomic mass, stronger electronic gain and electronic loss capability, and higher electron transfer ratio. Proton (H) + ) Considered as an ideal carrier, proton cells are receiving wide attention due to their small proton radius, high ion mobility and low cost. Albeit with alkali metal ions (e.g. Li) + 、Na + And K + ) Has been shown to be an effective carrier in rechargeable cells, but in aqueous cells alkali metal ions combine with water to form hydrated metal ions of larger size ((ii))
) It is more difficult in the process of intercalation/deintercalation in the electrode material. In particular at high current densities, the reaction kinetics become sluggish, leading to lower power densities. In addition, since a large amount of metal charge tends to cause cracking or powdering of the electrode material, the cycle stability is still not ideal. Protons of minimum ionic radius and high ionic conductivity as carriers (hydronium ion: H) 3 O + About, an
) Will have advantages over other metal ions, but the acidic electrolyte is liable to damage the structure of the electrode material, resulting in poor cycle performance. So despite their uniqueness, proton batteries have had a rather limited search for electrode materials that store protons in acidic electrolytes. Therefore, the search for an electrode material for a proton battery having excellent performance is advantageous for chargingThe excellent electrochemical performance of the proton battery is brought into play and the practical application of the proton battery is developed.
MoO 3 As a faraday electrode material widely used in alkali metal batteries, it is considered to be suitable for a proton battery electrode and exhibits an ultra-fast proton storage property. However, moO 3 The intrinsic electronic conductivity of the material is low, the electrochemical active sites are limited, the reaction specific surface area is insufficient, the reaction kinetics are slow, the electrochemical performance of the material in proton storage is seriously influenced, and the specific capacity of the material is lower and the capacity attenuation is faster. To improve MoO 3 Different strategies have been proposed, such as compounding with other metallic materials, but are not suitable for use in acidic electrolytes due to dissolution problems; the method of compounding with carbon material needs several preparation steps and thus increases the preparation cost. Thus, a novel MoO having high conductivity and structural stability in an acid electrolyte is prepared through a simple process 3 The electrode material provides a good experimental basis for guiding the development of the electrode material of the proton battery and realizing the practical application of the proton battery.
Disclosure of Invention
In view of the above problems or needs for improvement in the conventional aqueous proton battery, it is an object of the present invention to provide a simple α -MoO 3 Preparation method of nanobelt by mixing MoO 3 The nano particles are subjected to hydrothermal reaction to obtain alpha-MoO 3 The nanobelt solves the problems of easy dissolution of an electrode material, poor cycle stability and the like in the conventional aqueous proton battery, further improves the electrochemical performance of the aqueous proton battery, and realizes excellent rate performance, high energy density and long cycle stability.
According to a first aspect of the invention, there is provided an α -MoO 3 Preparation method of nanobelt by mixing MoO 3 Nano particles are uniformly dispersed in deionized water as a precursor, and the MoO 3 The size of the nano particles is 100nm-200nm; carrying out hydrothermal reaction on the dispersion liquid, wherein the temperature of the hydrothermal reaction is 120-160 ℃, and the time is 1-24 h; then cooling, washing and drying the hydrothermal product to obtain the alpha-MoO 3 A nanoribbon.
Preferably, said MoO in step (1) 3 The nanoparticles are two-phase mixed nanoparticles of a monoclinic phase and an orthorhombic phase.
According to another aspect of the invention, the alpha-MoO prepared by the method is provided 3 A nanoribbon comprising oxygen vacancies.
Preferably, the length of the nanobelt is 2 to 5 μm.
Preferably, the width of the nanoribbon is 200nm to 600nm.
According to another aspect of the present invention, there is provided the α -MoO of any one of the items 3 The application of the nanobelt as an electrode material of an aqueous proton battery.
Preferably, the application is specifically: reacting alpha-MoO 3 Uniformly mixing the nanobelt serving as an active substance with carbon black and polyvinylidene fluoride to obtain a mixture, dripping N-methylpyrrolidone into the mixture, dripping the mixture on a titanium sheet, and drying to obtain alpha-MoO 3 An aqueous proton battery electrode sheet as an electrode material.
Generally, compared with the prior art, the above technical solution conceived by the present invention mainly has the following technical advantages:
(1) alpha-MoO prepared by the method of the invention 3 Electrode at a current density of 1 Ag -1 The specific capacitance is as high as 285.3mAh g -1 . When the current density is increased by 50 times, the initial capacity of the electrode can still be retained by 75%. After 23000 cycles, the alpha-MoO prepared by the method of the invention 3 The electrode can still maintain the original capacity, nano-belt shape and crystal structure.
(2) alpha-MoO prepared by the method of the invention 3 The preparation method of the nanobelt only needs to be carried out on MoO 3 The nano particles can be subjected to one-step hydrothermal reaction, so that the appearance can be changed into a nano belt, the agglomeration problem is reduced, the diffusion path of hydronium ions is shortened, the specific surface area of the electrode material is increased, the volume expansion of the electrode material in the circulation process is relieved, and the electrochemical performance is favorably improved.
(3) alpha-MoO prepared by the method of the invention 3 Nanoribbons due to their nanoribbonsThe shape has rich oxygen vacancies, larger interlayer spacing, better conductivity and ion diffusivity, and can improve the electrochemical performance of the water system proton battery.
(4) alpha-MoO prepared by the method of the invention 3 The preparation method of the nanobelt has the advantages of cheap and easily obtained raw materials, mild reaction conditions, short reaction time, low cost, low toxicity, simplicity, feasibility, no template or surfactant and water as a reaction solvent.
Drawings
FIG. 1 is the original MoO of example 1 3 Nanoparticles and alpha-MoO prepared by hydrothermal method 3 X-ray diffraction pattern of the nanobelts.
FIG. 2 is the α -MoO produced in example 1 3 Scanning electron microscopy images of nanoribbons.
FIG. 3 is the α -MoO produced in example 1 3 Transmission electron microscopy images of nanobelts.
FIG. 4 is the α -MoO generated in example 1 3 The nanobelts are taken as cyclic voltammetry graphs of the proton battery electrode under different voltage sweep rates.
FIG. 5 is the α -MoO produced in example 1 3 The nanobelt is taken as a constant current charge-discharge curve diagram of the proton battery electrode under different current densities.
FIG. 6 is the α -MoO generated in example 1 3 The nanobelt is used as a test chart for the cycling stability of the electrode of the proton battery.
FIG. 7 is the α -MoO generated in example 2 3 Scanning electron microscopy of nanoribbons.
FIG. 8 is the α -MoO generated in example 2 3 The nanobelt is taken as a constant current charge-discharge curve diagram of the proton battery electrode under different current densities.
FIG. 9 is the α -MoO generated in example 3 3 Scanning electron microscopy images of nanoribbons.
FIG. 10 is the α -MoO generated in example 3 3 The nanobelt is taken as a constant current charge-discharge curve diagram of the proton battery electrode under different current densities.
FIG. 11 is a hydrothermal preparation of α -MoO of example 4 3 X-ray diffraction pattern of the nanobelts.
FIG. 12 shows example 4Formed alpha-MoO 3 Scanning electron microscopy of nanoribbons.
FIG. 13 is a hydrothermal preparation of α -MoO of example 5 3 X-ray diffraction pattern of nanoribbons.
FIG. 14 is the α -MoO generated in example 5 3 Scanning electron microscopy of nanoribbons.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the respective embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The invention relates to alpha-MoO 3 The preparation method of the nanoribbon aqueous proton battery electrode comprises the following steps:
(1) Adding MoO 3 Dispersing nanoparticles (commercially available and purchased from Bohuas nanotechnology (Ningbo) Co., ltd.) serving as a precursor in deionized water, transferring the dispersion to an inner container of a reaction kettle, sealing, and then putting the reaction kettle into an air-blowing drying oven to react for 1-24 h at 120-160 ℃;
(2) Cooling, washing and drying the hydrothermal product to obtain alpha-MoO 3 A nanoribbon;
(3) Mixing alpha-MoO 3 The nanobelt serving as an active substance is mixed with carbon black and polyvinylidene fluoride according to the mass ratio of 8:1:1 in N-methyl pyrrolidone, uniformly mixing, dripping the obtained mixture on a titanium sheet, and then placing the titanium sheet in a forced air drying oven to dry for 2 to 12 hours at the temperature of between 60 and 100 ℃ to obtain alpha-MoO 3 An electrode sheet.
In some embodiments, the precursor MoO in step 1) 3 The nanoparticles are two-phase mixed nanoparticles of a monoclinic phase and an orthorhombic phase, and have a size of 100-200nm.
In some embodiments, the precursor α -MoO in step 1) 3 The mass of the nano particles is 144mg, the volume of the deionized water is 30ml 3 Dissolving the nano particles in deionized water and stirringStirring for 30min.
In some embodiments, the product obtained after the hydrothermal reaction in the step 2) is filtered by suction with deionized water and absolute ethyl alcohol for 5 to 7 times, and then is dried in a forced air drying oven at 40 ℃ for 2 hours.
In some embodiments, step 3) will be alpha-MoO 3 Mixing the powders of the nanobelt, the carbon black and the polyvinylidene fluoride, and grinding for 20-30 min.
In some embodiments, step 3) adds N-methylpyrrolidone dropwise to the alpha-MoO 3 The nanobelts, carbon black and polyvinylidene fluoride mixed powder, continuously ground, and then the slurry was transferred to a vial and stirred for 30min.
In some embodiments, the α -MoO 3 The mass of the nanobelt as an active substance, the mixture of carbon black and polyvinylidene fluoride was 25mg, and the dropping amount of N-methylpyrrolidone in step 3) was 500 μ L.
In some examples, α -MoO 3 Electrode sheet with 1.0M H 2 SO 4 Electrochemical tests were performed for the electrolyte.
Example 1
Simple alpha-MoO 3 The preparation method of the nanobelt mainly comprises the following steps of:
adding MoO 3 Dissolving nanoparticles as a precursor in deionized water: weighing a two-phase mixed MoO having a size of 100-200nm, a monoclinic phase and a orthorhombic phase 3 144mg of nanoparticle precursor was dissolved in 30ml of deionized water and magnetically stirred for 30min to form a mixed solution.
Carrying out hydrothermal reaction on the mixed solution: and transferring the mixed solution to the inner container of a reaction kettle, sealing, and then putting the reaction kettle into a forced air drying oven to react for 24 hours at 120 ℃.
Cooling and washing the hydrothermal product to obtain alpha-MoO 3 Nano-belt: after the reaction kettle is cooled, carrying out suction filtration for 5 times by using deionized water, and drying for 6 hours in a blast drying oven at 40 ℃ to obtain alpha-MoO 3 Nano-belt powder.
Preparation of alpha-MoO 3 Nano strip electrode sheet:
mixing alpha-MoO 3 Nano belt as active substance and carbon black and polyvinylidene fluorideAnd the mass ratio of the difluoroethylene is 8:1:1 in N-methyl pyrrolidone, wherein the alpha-MoO is uniformly mixed 3 The total mass of the nanoribbons, carbon black and polyvinylidene fluoride was 25mg and the N-methylpyrrolidone was 500. Mu.L. The obtained mixture is dripped on a titanium sheet and then is dried for 2 hours in a forced air drying oven at 60 ℃ to obtain alpha-MoO 3 An electrode plate.
alpha-MoO prepared by the embodiment of the invention is combined with the attached drawing 3 Nanobelt and prepared alpha-MoO 3 The proton battery performance test of the nano strip electrode slice shows that:
for the prepared alpha-MoO 3 Carrying out X-ray diffraction test, scanning electron microscope morphology test and transmission electron microscope morphology test on the nanobelts:
FIG. 1 shows the original MoO of this example 3 Nanoparticles and alpha-MoO prepared by hydrothermal method 3 X-ray diffraction patterns of the nanobelts, illustrating the alpha-MoO under the conditions 3 And (5) forming crystals.
FIG. 2 shows the hydrothermal preparation of α -MoO in this example 3 Scanning electron micrograph of nanobelt, illustrating alpha-MoO 3 Presenting the structure of a nanoribbon.
FIG. 3 shows the hydrothermal preparation of α -MoO in this example 3 Transmission Electron microscopy of nanoribbons, also demonstrating α -MoO 3 Presenting the structure of a nanoribbon.
For the prepared alpha-MoO 3 And (3) carrying out proton battery electrochemical performance test on the nanoribbon electrode plate:
FIG. 4 shows α -MoO generated in this example 3 The cyclic voltammogram of the nanoribbon as the proton battery electrode under different voltage sweep rates can be seen, and 3 pairs of peaks related to the redox reaction exist in a potential window of-0.5-0.3V, which indicates that the charge storage is a multi-step process.
FIG. 5 shows α -MoO generated in this example 3 The constant current charge and discharge curve of the nano-belt as the proton battery electrode under different current densities can be seen from the graph, when the current densities are 1.0, 2.0, 5.0, 10.0, 20.0, 50.0 and 100.0A g -1 The specific capacities were 285.3, 265.8, 252.4, 243.8, 235.8, 214.4 and 145.8mAh g-1, respectively.
FIG. 6 shows α -MoO generated in this example 3 The nanoribbon is used as a test chart of the cycling stability of the proton battery electrode, and the graph can show that the electrode can still keep 103.0 percent of the initial capacity after 23000 cycles, which indicates the excellent electrochemical cycling performance.
Example 2
Simple alpha-MoO 3 The preparation method of the nanobelt mainly comprises the following steps of:
adding MoO 3 Dissolving nanoparticles as a precursor in deionized water: weighing a two-phase mixed MoO of a monoclinic phase and a orthorhombic phase having a size of 100-200nm 3 144mg of nanoparticle precursor was dissolved in 30ml of deionized water and magnetically stirred for 30min to form a mixed solution.
Carrying out hydrothermal reaction on the mixed solution: and transferring the mixed solution to the inner container of a reaction kettle, sealing, and then putting the reaction kettle into a forced air drying oven to react for 6 hours at 120 ℃.
Cooling and washing the hydrothermal product to obtain alpha-MoO 3 Nano-belt: after the reaction kettle is cooled, carrying out suction filtration for 5 times by using deionized water, and placing the reaction kettle into a forced air drying oven for drying for 6 hours at the temperature of 40 ℃ to obtain alpha-MoO 3 And (4) nano-belt powder.
Preparation of alpha-MoO 3 Nano strip electrode sheet:
mixing alpha-MoO 3 The nanobelt serving as an active substance is mixed with carbon black and polyvinylidene fluoride according to the mass ratio of 8:1:1 in N-methyl pyrrolidone, wherein the alpha-MoO is uniformly mixed 3 The total mass of the nanoribbons, carbon black and polyvinylidene fluoride was 25mg and the N-methylpyrrolidone was 500. Mu.L. The obtained mixture is dripped on a titanium sheet and then is dried for 2 hours in a forced air drying oven at the temperature of 60 ℃ to obtain alpha-MoO 3 An electrode sheet.
alpha-MoO prepared by the embodiment of the invention is combined with the attached drawing 3 Nanobelt and prepared alpha-MoO 3 The proton battery performance test of the nano strip electrode slice shows that:
for the prepared alpha-MoO 3 And (3) carrying out a scanning electron microscope morphology test on the nanobelt:
FIG. 7 shows the hydrothermal method of this examplePrepared alpha-MoO 3 Scanning Electron microscopy of nanoribbons demonstrating α -MoO 3 Presenting the structure of a nanoribbon.
For the prepared alpha-MoO 3 And (3) carrying out proton battery electrochemical performance test on the nanoribbon electrode plate:
FIG. 8 shows the α -MoO generated in this example 3 The constant current charge and discharge curve of the nano-belt as the proton battery electrode under different current densities can be seen from the graph, when the current densities are 1.0, 2.0, 5.0, 10.0, 20.0, 50.0 and 100.0A g -1 The specific capacities are 182.41, 170.00, 159.17, 152.22, 146.67, 136.11 and 113.89mAh g -1 。
Example 3
Simple alpha-MoO 3 The preparation method of the nanobelt mainly comprises the following steps of:
adding MoO 3 Dissolving nanoparticles as a precursor in deionized water: weighing a two-phase mixed MoO of a monoclinic phase and a orthorhombic phase having a size of 100-200nm 3 144mg of nanoparticle precursor, which is dissolved in 30ml of deionized water, and magnetically stirred for 30min to form a mixed solution.
Carrying out hydrothermal reaction on the mixed solution: and transferring the mixed solution to the inner container of a reaction kettle, sealing, and then putting the reaction kettle into a forced air drying oven to react for 12 hours at 120 ℃.
Cooling and washing the hydrothermal product to obtain alpha-MoO 3 Nano-belt: after the reaction kettle is cooled, carrying out suction filtration for 5 times by using deionized water, and placing the reaction kettle into a forced air drying oven for drying for 6 hours at the temperature of 40 ℃ to obtain alpha-MoO 3 And (4) nano-belt powder.
Preparation of alpha-MoO 3 Nano strip electrode sheet:
reacting alpha-MoO 3 The nanobelt serving as an active substance is mixed with carbon black and polyvinylidene fluoride according to the mass ratio of 8:1:1 in N-methyl pyrrolidone, wherein the alpha-MoO is uniformly mixed 3 The total mass of the nanoribbons, carbon black and polyvinylidene fluoride was 25mg and that of N-methylpyrrolidone was 500. Mu.L. The obtained mixture is dripped on a titanium sheet and then is dried for 2 hours in a forced air drying oven at the temperature of 60 ℃ to obtain alpha-MoO 3 An electrode plate.
alpha-MoO prepared by the embodiment of the invention is combined with the attached drawing 3 Nanobelt and prepared alpha-MoO 3 The proton battery performance test of the nano strip electrode slice shows that:
for the prepared alpha-MoO 3 And (3) carrying out a scanning electron microscope morphology test on the nanobelt:
FIG. 9 is a hydrothermal preparation of α -MoO in accordance with this example 3 Scanning Electron microscopy of nanoribbons demonstrating α -MoO 3 Presenting the structure of a nanoribbon.
For the prepared alpha-MoO 3 And (3) carrying out proton battery electrochemical performance test on the nanoribbon electrode plate:
FIG. 10 shows α -MoO generated in this example 3 The constant current charge and discharge curve chart of the electrode of the proton battery under different current densities by using the nano-belt can be seen, and the current densities of the electrode of the proton battery are 1.0, 2.0, 5.0, 10.0, 20.0, 50.0 and 100.0A g -1 The specific capacities are 218.89, 205.50, 194.72, 188.06, 182.22, 170.83 and 136.11mAh g -1 。
Example 4
Simple alpha-MoO 3 The preparation method of the nanobelt mainly comprises the following steps of:
adding MoO 3 Dissolving the nano particles as a precursor in deionized water: weighing a two-phase mixed MoO of a monoclinic phase and a orthorhombic phase having a size of 100-200nm 3 144mg of nanoparticle precursor was dissolved in 30ml of deionized water and magnetically stirred for 30min to form a mixed solution.
Carrying out hydrothermal reaction on the mixed solution: and transferring the mixed solution to the inner container of a reaction kettle, sealing, and then putting the reaction kettle into a forced air drying oven to react for 1 hour at 120 ℃.
Cooling and washing the hydrothermal product to obtain alpha-MoO 3 Nano-belt: after the reaction kettle is cooled, carrying out suction filtration for 5 times by using deionized water, and drying for 6 hours in a blast drying oven at 40 ℃ to obtain alpha-MoO 3 Nano-belt powder.
Preparation of alpha-MoO 3 Nano strip electrode sheet:
mixing alpha-MoO 3 Nano belt as active substance and carbon black, polyvinylidene fluoride as base materialThe amount ratio is 8:1:1 in N-methyl pyrrolidone, wherein the alpha-MoO is uniformly mixed 3 The total mass of the nanoribbons, carbon black and polyvinylidene fluoride was 25mg and the N-methylpyrrolidone was 500. Mu.L. The obtained mixture is dripped on a titanium sheet and then is dried for 2 hours in a forced air drying oven at the temperature of 60 ℃ to obtain alpha-MoO 3 An electrode plate.
alpha-MoO prepared by the embodiment of the invention is combined with the attached drawing 3 Description of nanobelts:
for the prepared alpha-MoO 3 Carrying out X-ray diffraction test and scanning electron microscope morphology test on the nanobelt:
FIG. 11 shows the hydrothermal preparation of α -MoO in this example 3 X-ray diffraction test of the nanobelt shows that the alpha-MoO is in the condition 3 And (5) forming crystals.
FIG. 12 shows the hydrothermal preparation of α -MoO in this example 3 Scanning electron micrograph of nanobelt, illustrating alpha-MoO 3 Presenting the structure of a nanoribbon.
Example 5
Simple alpha-MoO 3 The preparation method of the nanobelt mainly comprises the following steps of:
adding MoO 3 Dissolving nanoparticles as a precursor in deionized water: weighing a two-phase mixed MoO of a monoclinic phase and a orthorhombic phase having a size of 100-200nm 3 144mg of nanoparticle precursor, which is dissolved in 30ml of deionized water, and magnetically stirred for 30min to form a mixed solution.
Carrying out hydrothermal reaction on the mixed solution: and transferring the mixed solution to an inner container of a reaction kettle, sealing, and then putting the reaction kettle into a forced air drying oven for reacting for 24 hours at 160 ℃.
Cooling and washing the hydrothermal product to obtain alpha-MoO 3 Nano-belt: after the reaction kettle is cooled, carrying out suction filtration for 5 times by using deionized water, and drying for 6 hours in a blast drying oven at 40 ℃ to obtain alpha-MoO 3 Nano-belt powder.
Preparation of alpha-MoO 3 Nano strip electrode sheet:
mixing alpha-MoO 3 The nanobelt serving as an active substance is mixed with carbon black and polyvinylidene fluoride according to the mass ratio of 8:1:1 in a ratio ofMixing N-methyl pyrrolidone to obtain alpha-MoO 3 The total mass of the nanoribbons, carbon black and polyvinylidene fluoride was 25mg and that of N-methylpyrrolidone was 500. Mu.L. The obtained mixture is dripped on a titanium sheet and then is dried for 2 hours in a forced air drying oven at the temperature of 60 ℃ to obtain alpha-MoO 3 An electrode sheet.
alpha-MoO prepared by the embodiment of the invention is combined with the attached drawing 3 Description of the nanobelts:
for the prepared alpha-MoO 3 Carrying out X-ray diffraction test and scanning electron microscope morphology test on the nanobelts:
FIG. 13 is a hydrothermal preparation of α -MoO in accordance with this example 3 X-ray diffraction testing of the nanobelts shows that the alpha-MoO is under the condition 3 And (5) forming crystals.
FIG. 14 shows the hydrothermal preparation of α -MoO in this example 3 Scanning electron micrograph of nanobelt, illustrating alpha-MoO 3 Presenting the structure of a nanoribbon.
It will be understood by those skilled in the art that the foregoing is only an exemplary embodiment of the present invention, and is not intended to limit the invention to the particular forms disclosed, since various modifications, substitutions and improvements within the spirit and scope of the invention are possible and within the scope of the appended claims.
Claims (7)
1. alpha-MoO 3 The preparation method of the nanobelt is characterized in that MoO is added 3 Nano particles are uniformly dispersed in deionized water as a precursor, and the MoO 3 The size of the nano particles is 100nm-200nm; carrying out hydrothermal reaction on the dispersion liquid, wherein the temperature of the hydrothermal reaction is 120-160 ℃, and the time is 1-24 h; then cooling, washing and drying the hydrothermal product to obtain the alpha-MoO 3 A nanoribbon.
2. The α -MoO of claim 1 3 The preparation method of the nanobelt is characterized in that the MoO in the step (1) 3 The nanoparticles are two-phase mixed nanoparticles of a monoclinic phase and an orthorhombic phase.
3. As claimed in claim 1 or2 the alpha-MoO prepared by the method 3 A nanoribbon characterized in that said nanoribbon contains oxygen vacancies.
4. The α -MoO of claim 3 3 The nanobelt is characterized in that the length of the nanobelt is 2 to 5 μm.
5. The α -MoO of claim 3 or 4 3 The nanoribbon is characterized in that the width of the nanoribbon is 200 nm-600 nm.
6. The α -MoO according to any of claims 3 to 5 3 The application of the nanobelt as an electrode material of a water-based proton battery.
7. The application according to claim 6, wherein the application is in particular: reacting alpha-MoO 3 Uniformly mixing the nanobelt serving as an active substance with carbon black and polyvinylidene fluoride to obtain a mixture, dripping N-methylpyrrolidone into the mixture, dripping the mixture on a titanium sheet, and drying to obtain alpha-MoO 3 An aqueous proton battery electrode sheet as an electrode material.
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| CN107021523A (en) * | 2017-01-19 | 2017-08-08 | 青岛科技大学 | A kind of orthorhombic phase α MoO3The preparation method and its photocatalytic applications of nanobelt |
| US20170349447A1 (en) * | 2016-05-23 | 2017-12-07 | University Of Connecticut | Mesoporous metal oxides, preparation and applications thereof |
| CN108539190A (en) * | 2018-03-30 | 2018-09-14 | 华南理工大学 | The molybdenum trioxide of a kind of oxygen-containing vacancy and using it as the water system aluminium ion battery of negative electrode active material and their preparation method |
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| US20170349447A1 (en) * | 2016-05-23 | 2017-12-07 | University Of Connecticut | Mesoporous metal oxides, preparation and applications thereof |
| CN107021523A (en) * | 2017-01-19 | 2017-08-08 | 青岛科技大学 | A kind of orthorhombic phase α MoO3The preparation method and its photocatalytic applications of nanobelt |
| CN108539190A (en) * | 2018-03-30 | 2018-09-14 | 华南理工大学 | The molybdenum trioxide of a kind of oxygen-containing vacancy and using it as the water system aluminium ion battery of negative electrode active material and their preparation method |
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