CN112938978A - Preparation method of vanadium carbide nanosheet - Google Patents
Preparation method of vanadium carbide nanosheet Download PDFInfo
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- CN112938978A CN112938978A CN202110235518.3A CN202110235518A CN112938978A CN 112938978 A CN112938978 A CN 112938978A CN 202110235518 A CN202110235518 A CN 202110235518A CN 112938978 A CN112938978 A CN 112938978A
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- INZDTEICWPZYJM-UHFFFAOYSA-N 1-(chloromethyl)-4-[4-(chloromethyl)phenyl]benzene Chemical compound C1=CC(CCl)=CC=C1C1=CC=C(CCl)C=C1 INZDTEICWPZYJM-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000002135 nanosheet Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 36
- 239000000463 material Substances 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000498 ball milling Methods 0.000 claims abstract description 14
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 12
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims abstract description 12
- 238000005530 etching Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000007790 solid phase Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000009830 intercalation Methods 0.000 claims abstract description 6
- 230000002687 intercalation Effects 0.000 claims abstract description 6
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 230000007935 neutral effect Effects 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000007873 sieving Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 229910052582 BN Inorganic materials 0.000 claims description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000004744 fabric Substances 0.000 claims description 2
- 239000012254 powdered material Substances 0.000 claims 1
- 239000007772 electrode material Substances 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000003990 capacitor Substances 0.000 description 4
- 239000000084 colloidal system Substances 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000001272 pressureless sintering Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000003828 vacuum filtration Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910000371 mercury(I) sulfate Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—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
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention relates to a preparation method of vanadium carbide nanosheets, which comprises the following steps of: al powder: weighing raw material powder according to the molar ratio of (1.0-1.2) to 1, mixing, and performing ball milling under an argon atmosphere to obtain solid phase powder; and then putting the solid phase powder into a self-propagating reaction kettle, carrying out self-propagating reaction in an argon atmosphere, crushing a reaction product, ball-milling in the argon atmosphere, sieving the obtained powder material, adding the powder material with the particle size of 300-plus-500 meshes into a hydrofluoric acid solution, etching while stirring, taking out after the end, washing with water to be neutral to obtain multilayer vanadium carbide, finally adding a tetramethylammonium hydroxide solution with the mass concentration of 25% for intercalation, and carrying out centrifugal collection to obtain the vanadium carbide nanosheet. The method has the advantages of low energy consumption, safety, environmental protection, simple and time-saving operation and low cost, and the prepared vanadium carbide nanosheet has stable performance and high purity, can be used as a supercapacitor electrode material, and has good capacitance performance.
Description
Technical Field
The invention belongs to the technical field of electrode materials, and particularly relates to a preparation method of vanadium carbide nanosheets.
Background
Vanadium carbide nanosheet (V)2C) Is a novel two-dimensional metal transition carbide and has good application prospect in many aspects, such as energy storage and conversion, catalysis, sensing, electromagnetism, optics, water purification and the like.
Vanadium carbide nanosheets are typically prepared by selectively etching the precursor material V2Al in AlC, and a precursor material V2The preparation method of AlC can influence the preparation effect of the vanadium carbide nanosheet to a great extent. At present, the precursor material V2The preparation method of AlC comprises the following steps: self-propagating high-temperature synthesis, pressureless sintering, hot-pressing sintering and other methods, wherein the pressureless sintering needs to be carried out under the condition of high temperature, the heating process is slow, the energy consumption is high, and the cost is high; the hot-pressing sintering has the defects of complex process and equipment, strict production control requirement, high requirement on mold materials, high energy consumption, lower production efficiency and high production cost, and the prepared crystal grains are small and compact in structure, so that the subsequent preparation of vanadium carbide and niobium nanosheets is not facilitated; the self-propagating high-temperature synthesis is a technology for synthesizing materials by utilizing self-heating and self-conducting effects of high chemical reaction heat between reactants, once the reactants are ignited, the reactants can automatically propagate to an unreacted area until the reaction is complete, the operation is simple, the materials can be synthesized under low pressure, the propagation of combustion waves of the reaction is extremely fast, the chemical energy generated by the combustion reaction is utilized to synthesize the materials, generally, energy supplement is not needed, the combustion time is short, the heating and cooling temperature gradient in the combustion process is large, high-concentration defects and unbalanced structures are easy to form, complex phases and metastable phases are easy to obtain, and the composite materials can be simply and directly obtained, but the precursor material V2AlC synthesized by adopting the self-propagating high temperature in the prior art is unstable in performance and not high in purity.
According to the invention, by improving the preparation method of the precursor material V2AlC, the Al layer in the V2AlC synthesized by self-propagating high temperature is easier to etch, so that the high-purity vanadium carbide nanosheet is stably synthesized, and the supercapacitor assembled by using the vanadium carbide nanosheet as an electrode material has good capacitance performance.
Disclosure of Invention
The invention aims to provide a method for preparing vanadium carbide nanosheets, which has the advantages of low energy consumption, safety, environmental protection, simplicity and time in operation, low cost and the like. The prepared vanadium carbide nanosheet is stable in performance and high in purity, and has good capacitance performance when being assembled into a super capacitor.
Technical scheme
A method for preparing vanadium carbide nanosheets, comprising the steps of:
(1) according to the formula V: al powder: weighing raw material powder according to the molar ratio of (1.0-1.2) to 1, mixing, and ball-milling under argon atmosphere to obtain solid phase powder;
(2) putting the solid phase powder into a self-propagating reaction kettle, carrying out self-propagating reaction in an argon atmosphere, crushing a reaction product, and carrying out ball milling in the argon atmosphere to obtain a powder material;
(3) sieving the powder material, adding the powder material with the particle size of 300-500 meshes into a hydrofluoric acid solution, etching while stirring, taking out after etching, and washing with deionized water to be neutral to obtain multilayer vanadium carbide;
(4) adding 25% tetramethylammonium hydroxide solution into the obtained multilayer vanadium carbide for intercalation, and after the intercalation is finished, centrifugally collecting to obtain vanadium carbide nanosheets.
Further, in the step (1), the ball milling speed is 200-.
Further, in the step (2), the solid-phase powder is put into a graphite box and then put into a self-propagating reaction kettle for self-propagating reaction.
Further, in the step (2), the ignition pressure of the self-propagating reaction is 0.2-0.6MPa, the ignition time is 2-6s, and the reaction kettle can be taken out after being cooled to the room temperature.
Further, in the step (3), the mass concentration of the hydrofluoric acid solution is 49%.
Further, in the step (3), 2g of the powder material was added to 40mL of the hydrofluoric acid solution.
Further, in the step (3), the rotation speed of the stirring is 300-.
Further, in the step (3), the etching temperature is 35 ℃ and the etching time is 48 hours.
The invention has the beneficial effects that: the invention provides a method for preparing vanadium carbide nanosheets, which is low in energy consumption, safe, environment-friendly, simple and time-saving in operation and low in cost, and the prepared vanadium carbide nanosheets are stable in performance and high in purity, can be used as electrode materials of super capacitors, and have good capacitance performance when assembled into the super capacitors.
Drawings
FIG. 1 is V2XRD diffraction pattern of AlC powder;
FIG. 2 is V2SEM spectra of AlC powder;
FIG. 3 is an XRD diffraction pattern of vanadium carbide nanosheets prepared in example 1;
FIG. 4 is an SEM image of vanadium carbide nanosheets prepared in example 1;
fig. 5 is a CV curve of a supercapacitor assembled with vanadium carbide nanosheets prepared in example 1.
Detailed Description
The technical solution of the present invention is further explained with reference to the accompanying drawings and specific embodiments.
Example 1
A method for preparing vanadium carbide nanosheets, comprising the steps of:
(1) according to the formula V: al powder: weighing 100 g of raw material powder according to the molar ratio of 2:1.2:1, mixing, and ball-milling in an argon atmosphere (ball-material ratio is 6: 1, ball-milling speed is 300r/min, ball-milling time is 4h) to obtain solid-phase powder;
(2) putting solid-phase powder into a graphite box with carbon cloth arranged in the inner layer and boron nitride coated on the surface, rolling tungsten wires into filaments, putting the filaments into the middle of the powder, putting the graphite box into a self-propagating reaction kettle, carrying out self-propagating reaction in argon atmosphere, controlling the argon pressure at 0.3MPa, igniting at high temperature for 2-6s, and cooling the reaction kettle to room temperatureTaking out after warming, crushing the reaction product, and ball-milling under argon atmosphere (ball-to-material ratio is 6: 1, ball-milling speed is 300r/min, ball-milling time is 1h) to obtain V2AlC powder material;
(3) sequentially sieving the powder material through sieves of 100 meshes, 200 meshes, 300 meshes, 400 meshes and 500 meshes to separate out powder with uniform particle size, adding 2g of the powder material of 300 meshes into 40mL of hydrofluoric acid solution with the mass concentration of 49%, stirring for 48h at 35 ℃ and 600r/min, taking out after etching, washing with deionized water to be neutral, and obtaining multilayer vanadium carbide;
(4) adding 16mL of 25 mass percent tetramethylammonium hydroxide solution into the obtained multilayer vanadium carbide for intercalation, adding a stirrer for stirring at room temperature for 4h, shaking by hand for 8min, taking out the mixture, adding deionized water to 45mL, and centrifuging (2000r/min, 10 min), wherein the TMAOH content in the first mixture is strong alkalinity and V is high2The content of C is less, so that the first solution with the color of brown yellow is directly poured into a waste liquid barrel, deionized water is slowly added into the tube wall and stands for 10min to remove tetramethyl ammonium hydroxide as much as possible, then deionized water is added into the tube wall to 45ml, the above steps are repeated for 5-10min, centrifugation is carried out (2000r/min and 10 min) is carried out to collect upper-layer colloid, the collected vanadium carbide nanosheet colloid is introduced into argon gas to remove dissolved oxygen in the colloid, and then a vacuum filtration bottle is used for vacuum filtration to obtain V with the effective mass of 10-20mg2The film C is used for assembling the super capacitor, and the rest colloid is put into a refrigerator for cold storage.
FIG. 1 shows V obtained in example 12The XRD diffraction pattern of AlC powder shows that the invention synthesizes high-purity V through self-propagating2AlC; FIG. 2 shows V obtained in example 12SEM atlas of AlC powder can show that V is prepared2AlC has a shale-like structure typical of MAX phase materials; FIG. 3 is an XRD diffraction pattern of the vanadium carbide nanosheets prepared in example 1, and it can be seen that V is synthesized by self-propagating2The high-purity V can be prepared from AlC precursor material2C; FIG. 4 is an SEM spectrum of the vanadium carbide nanosheet prepared in example 1, and it can be seen that high purity V is prepared2C has a single or few layer structure.
V adopting non-structural design2C nanosheet is subjected to suction filtration to form a film and used as an electrode material of a supercapacitor FIG. 5 is a capacity voltage curve of the supercapacitor assembled by adopting the vanadium carbide nanosheets prepared in example 1, and during testing, an electrolyte is a 1mol/L sulfuric acid solution, and a reference electrode is Hg/Hg2SO4It can be seen that the specific capacity reaches 266F/g at a scan rate of 2mV/s, indicating good capacitive performance.
Claims (8)
1. A preparation method of vanadium carbide nanosheets is characterized by comprising the following steps:
(1) according to the formula V: al powder: weighing raw material powder according to the molar ratio of (1.0-1.2) to 1, mixing, and ball-milling under argon atmosphere to obtain solid phase powder;
(2) putting the solid phase powder into a self-propagating reaction kettle, carrying out self-propagating reaction in an argon atmosphere, crushing a reaction product, and carrying out ball milling in the argon atmosphere to obtain a powder material;
(3) sieving the powder material, adding the powder material with the particle size of 300-500 meshes into a hydrofluoric acid solution, etching while stirring, taking out after etching, and washing with deionized water to be neutral to obtain multilayer vanadium carbide;
(4) adding 25% tetramethylammonium hydroxide solution into the obtained multilayer vanadium carbide for intercalation, and after the intercalation is finished, centrifugally collecting to obtain vanadium carbide nanosheets.
2. The preparation method of vanadium carbide nanosheets as claimed in claim 1, wherein in step (1), the ball milling rate is 200-.
3. The preparation method of vanadium carbide nanosheets as claimed in claim 1, wherein in step (2), the solid-phase powder is placed in a graphite box with a carbon cloth placed in the inner layer and boron nitride coated on the surface, and then placed in a self-propagating reaction kettle for self-propagating reaction.
4. The preparation method of vanadium carbide nanosheets according to claim 1, wherein in step (2), the self-propagating reaction ignition pressure is 0.2 to 0.6MPa and the ignition time is 2 to 6 s.
5. The method for producing vanadium carbide nanosheets according to claim 1, wherein in step (3), the hydrofluoric acid solution has a mass concentration of 49%.
6. The method for preparing vanadium carbide nanosheets of claim 1, wherein in step (3), 2g of the powdered material is added per 40mL of the hydrofluoric acid solution.
7. The method for preparing vanadium carbide nanosheets of claim 1, wherein in step (3), the rotational speed of the stirring is 300-.
8. The method for preparing vanadium carbide nanosheets according to any one of claims 1 to 7, wherein in step (3), the etching temperature is 35 ℃ and the etching time is 48 hours.
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| CN113336553A (en) * | 2021-06-29 | 2021-09-03 | 河南工业大学 | V2AlC bulk material synthesized by microwave sintering and preparation method and application thereof |
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| CN113830769A (en) * | 2021-09-22 | 2021-12-24 | 同济大学 | Non-linear nano hybrid material based on vanadium carbide and molybdenum disulfide and preparation method thereof |
| CN114572986A (en) * | 2022-04-14 | 2022-06-03 | 盐城工学院 | Two-dimensional VyCr2-yCSxPreparation method of nanosheet |
| CN114804106A (en) * | 2022-05-18 | 2022-07-29 | 中国科学技术大学 | Vanadium titanium carbide MXene material and preparation method and application thereof |
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| CN113830769A (en) * | 2021-09-22 | 2021-12-24 | 同济大学 | Non-linear nano hybrid material based on vanadium carbide and molybdenum disulfide and preparation method thereof |
| CN113830769B (en) * | 2021-09-22 | 2023-07-04 | 同济大学 | Nonlinear nanometer hybrid material based on vanadium carbide and molybdenum disulfide and preparation method thereof |
| CN114572986A (en) * | 2022-04-14 | 2022-06-03 | 盐城工学院 | Two-dimensional VyCr2-yCSxPreparation method of nanosheet |
| CN114804106A (en) * | 2022-05-18 | 2022-07-29 | 中国科学技术大学 | Vanadium titanium carbide MXene material and preparation method and application thereof |
| CN114804106B (en) * | 2022-05-18 | 2024-03-01 | 中国科学技术大学 | Vanadium titanium carbide MXene material, and preparation method and application thereof |
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