CN114572986B - Two-dimensional V y Cr 2-y CS x Preparation method of nano-sheet - Google Patents
Two-dimensional V y Cr 2-y CS x Preparation method of nano-sheet Download PDFInfo
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000011651 chromium Substances 0.000 claims abstract description 77
- 239000000463 material Substances 0.000 claims abstract description 31
- 150000003839 salts Chemical class 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000137 annealing Methods 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000007873 sieving Methods 0.000 claims abstract description 11
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 239000011261 inert gas Substances 0.000 claims abstract description 10
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 9
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 230000007935 neutral effect Effects 0.000 claims abstract description 8
- 238000010298 pulverizing process Methods 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 4
- 238000005554 pickling Methods 0.000 claims abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 239000011812 mixed powder Substances 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 9
- 229910052721 tungsten Inorganic materials 0.000 claims description 9
- 239000010937 tungsten Substances 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 229910052717 sulfur Inorganic materials 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000007788 liquid Substances 0.000 claims 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 8
- 238000012983 electrochemical energy storage Methods 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 abstract description 3
- 239000000376 reactant Substances 0.000 abstract description 2
- 239000011734 sodium Substances 0.000 description 14
- 239000010936 titanium Substances 0.000 description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 125000000524 functional group Chemical group 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 6
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 5
- 239000007772 electrode material Substances 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 239000002064 nanoplatelet Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- 229910021589 Copper(I) bromide Inorganic materials 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- JDZCKJOXGCMJGS-UHFFFAOYSA-N [Li].[S] Chemical compound [Li].[S] JDZCKJOXGCMJGS-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- VVNXEADCOVSAER-UHFFFAOYSA-N lithium sodium Chemical compound [Li].[Na] VVNXEADCOVSAER-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- 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
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- Y02E60/13—Energy storage using capacitors
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Abstract
The invention relates to a two-dimensional V y Cr 2‑y CS x Preparation method of nanosheets according to chemical formula V y Cr 2‑y The metering ratio in AlC is that the vanadium powder, the chromium powder, the aluminum powder and the carbon powder are evenly mixed, and thenAdding into a self-propagating reaction tank, adding 5-15 cm tungsten wire, and igniting under inert gas to obtain V y Cr 2‑y Pulverizing AlCMX block material, sieving with 300-400 mesh sieve to obtain V y Cr 2‑y AlCMX powder, znS and Na 2 S/K 2 And mixing the mixed salt, annealing under the protection of inert gas, and finally pickling and washing with water until the mixture is neutral. The method is simple, does not relate to high-risk reactants such as hydrofluoric acid and the like, has mild reaction conditions, adopts a mixed salt solvent which can be recycled, meets the requirements of sustainable development and environmental protection, and prepares the two-dimensional V y Cr 2‑y CS x The nano-sheet has good electrochemical energy storage performance.
Description
Technical Field
The invention relates to a two-dimensional V y Cr 2-y CS x A preparation method of a nano-sheet belongs to the technical field of low-dimensional nano-materials.
Background
MXenes is a generic term for a new two-dimensional transition metal carbide or carbonitride. In 2011, the Gogotsi and Barsoum subject group at university of American German Lei Saier selectively etched Ti with hydrofluoric acid 3 AlC 2 The A layer in MAX phase obtains a novel two-dimensional Ti 3 C 2 A nano-sheet. In the process of etching the A layer, the two-dimensional Ti is synchronously etched 3 C 2 The surface of the nanoplatelets is introduced with a large number of functional groups, therefore, its structural formula is generally written as Ti 3 C 2 T x (t= F, OH or O). MAX is M n+1 AX n Abbreviations for phases (n=1, 2or 3), where M is an early transition metal element, a is a third or fourth main group element, and X is C or N. Due to the diversity of sources of MAX phase materials, some columns are similar to Ti 3 C 2 T x Materials of a nature and structure, e.g. V 2 CT x 、Nb 2 CT x 、Mo 2 TiC 2 T x Etc. are collectively referred to as MXenes. MXees materials having good mechanical, electrochemical and optical properties, e.g. Ti 3 C 2 T x The elastic modulus of the polymer is up to 500GPa, the conductivity exceeds 10000S/cm, and the surface rich functional groups endow the polymer with extremely high hydrophilicity, catalytic activity and the like. Therefore, MXnes has good application potential in the fields of super capacitors, lithium-sodium ion batteries, catalysts, water treatment and the like.
In general, the MXenes material is etched by using hydrofluoric acid (in-situ hydrofluoric acid), and the functional group on the surface is F, OH or O. Recent studies indicate that the functional groups on the surface of MXenes have important effects on their catalytic properties and energy storage properties. Thus, modulating the surface functionality of mxnes by rational means is of great interest. For example, cuCl has been used in the prior art 2 、CuBr 2 、CuI 2 Preparation of perhalogen functional MXenes such as Ti with an etchant 3 C 2 Cl x 、Ti 3 C 2 Br x 、Ti 3 C 2 I x . the-OH, -O functional groups introduced by the conventional liquid phase etching method can be avoided by introducing the perhalogen functional groups, so that the affinity between the MXees material and metal cations can be endowed, and the performance of the metal ion battery is improved; it has also been shown that the introduction of holothiolic functions into MXees materials imparts novel properties to the materials, such as improved lithium sulfur battery performance, and that the current preparation of MXees containing sulfur functions is focused primarily on titanium-based MXees such as Ti 3 C 2 T x . With titanium-based MXenes such as Ti 3 C 2 T x Compared with the prior art, the vanadium-based MXenes have better lithium-philic property and electrochemical energy storage property, and the development of the vanadium-based MXenes is expected to have better property, and no V for preparing a holothiolic functional group exists at present y Cr 2-y CS x Is reported in (3). In addition, the traditional method for vulcanizing MXenes mainly adopts a high-temperature annealing method to enable sulfur powder, thiourea and the like to react with the sulfur powder to replace F, OH or O. The method is not only tedious, but also extremely easy to cause the damage of the two-dimensional material structure in the annealing process.
Disclosure of Invention
The present invention aims to solve the above-mentioned disadvantages of the prior art and provides a two-dimensional V y Cr 2-y CS x The nano-sheet preparation method has good electrochemical energy storage performance.
Technical proposal
The invention synthesizes the V with high defect by adopting a self-propagating high temperature synthesis (SHS) method y Cr 2-y MAX of AlC, then one-step etching V by molten salt method y Cr 2-y AlC to obtain two-dimensional V of holothioic functional group y Cr 2-y CS x The specific scheme is as follows:
two-dimensional V y Cr 2-y CS x The preparation method of the nano-sheet comprises the following steps:
(1) According to chemical formula V y Cr 2-y Taking the metering ratio of AlC, uniformly mixing vanadium powder, chromium powder, aluminum powder and carbon powder, and then adding the mixture into a self-propagating reaction tank; said formula V y Cr 2-y AlC, 0<y≤2；
(2) Adding tungsten filament into self-propagating reactor, igniting under inert gas protection, reacting to obtain V y Cr 2-y AlC MAX block material;
(3) Will V y Cr 2-y Pulverizing AlC MAX block material, sieving to obtain V y Cr 2-y AlC MAX powder;
(4) Will V y Cr 2-y AlC MAX powder, znS and Na 2 S/K 2 S, uniformly mixing the mixed salt to obtain mixed powder;
(5) Annealing the mixed powder in the step (4) under the protection of inert gas, and then pickling and washing with water to be neutral to obtain two-dimensional V y Cr 2-y CS x A nano-sheet.
Further, in step (1), the compound of formula V y Cr 2-y In AlC, y is more than or equal to 1 and less than or equal to 2.
Further, in the step (2), the length of the tungsten filament is 5-15 cm, and the inert gas is nitrogen or argon.
Further, in the step (3), the sieving is 300-400 mesh sieving.
Further, in step (4), V y Cr 2-y The mass ratio of AlC MAX powder to ZnS is 1 (3-9).
Further, in step (4), the ZnS and Na 2 S/K 2 The mass ratio of the S mixed salt is 1:6, and the Na is as follows 2 S/K 2 In S mixed salt, na 2 S and K 2 The mass ratio of S is 1:1.
Further, in the step (5), the annealing treatment temperature is 700-950 ℃ and the annealing time is 3-10h.
In the step (5), the inert gas is nitrogen or argon, and the acid solution used for acid washing is 1mol/L hydrochloric acid solution or sulfuric acid solution.
The invention has the beneficial effects that:
the invention firstly uses vanadium powder, chromium powder, aluminum powder and carbon powder as raw materials to prepare V with high defect y Cr 2-y AlC MAX, then adopt Na 2 S/K 2 S mixed salt is used as a solvent, znS is used as an etchant to prepare the two-dimensional V of the holothiofunctional group y Cr 2-y CS x A nano-sheet. The method is simple, does not involve high-risk reactants such as hydrofluoric acid and the like, has mild reaction conditions, can be recycled by adopting the mixed salt solvent, meets the requirements of continuous development and environmental protection, and can obtain the V of the full-sulfur functional group y Cr 2-y CS x It has good electrochemical energy storage performance.
Drawings
FIG. 1 is a two-dimensional V obtained in example 1 2 CS x Scanning electron microscope image of the nanoplatelets.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
Two-dimensional V 2 CS x The preparation method of the nano-sheet comprises the following steps:
(1) Mixing 51 g of vanadium powder, 32.4 g of aluminum powder and 12 g of carbon powder uniformly, and adding the mixture into a self-propagating reaction tank;
(2) Adding 15 cm tungsten filament, igniting under argon protection, reacting to obtain V 2 AlC MAX block material;
(3) Will V 2 Pulverizing AlC MAX block material, sieving with 300-400 mesh sieve to obtain V 2 AlC MAX powder;
(4) Will V 2 AlC MAX powder, znS and Na 2 S/K 2 The S mixed salt was prepared in a 1:9:54 ratio (Na 2 S/K 2 In S mixed salt, na 2 S and K 2 The mass ratio of S is 1:1), and the mixed powder is obtained;
(5) Annealing the mixed powder in the step (4) for 10 hours at 950 ℃ under the protection of argon, washing with 1mol/L sulfuric acid solution, and washing with water to be neutral to obtain two-dimensional V 2 CS x The yield of the nano sheet material is 15%.
Two-dimensional V prepared in example 1 2 CS x The scanning electron microscope of the nano-sheet is shown in figure 1.
Will be two-dimensional V 2 CS x Suction filtering to form film, and directly using V 2 CS x The film is a working electrode, YP50 active carbon is a counter electrode, a saturated calomel electrode is a reference electrode, and 1mol/L H is used 2 SO 4 As an electrolyte, two-dimensional V was measured at a current density of 1A/g 2 CS x The specific capacity of the nano-sheet electrode material is up to 392F/g.
Example 2
Two-dimensional V 1 Cr 1 CS x The preparation method of the nano-sheet comprises the following steps:
(1) Uniformly mixing 25.5 g of vanadium powder, 26 g of chromium powder, 21.6 g of aluminum powder and 12 g of carbon powder, and adding the mixture into a self-propagating reaction tank;
(2) Adding tungsten filament with length of 5 cm, igniting under nitrogen protection, reacting to obtain V 1 Cr 1 AlC MAX block material;
(3) Will V 1 Cr 1 Pulverizing AlC MAX block material, sieving with 300-400 mesh sieve to obtain V 1 Cr 1 AlC MAX powder;
(4) Will V y Cr 2-y AlC MAX powder, znS and Na 2 S/K 2 The S mixed salt was prepared in a 1:3:3 (Na 2 S/K 2 In S mixed salt, na 2 S and K 2 The mass ratio of S is 1:1), and the mixed powder is obtained;
(5) Annealing the mixed powder in the step (4) for 3 hours at 700 ℃ under the protection of nitrogen, washing with 1mol/L hydrochloric acid solution, and washing with water to be neutral to obtain two-dimensional V 1 Cr 1 CS x The yield of the nano sheet material is 25%.
Will be two-dimensional V 1 Cr 1 CS x Suction filtering to form film, and directly using V 1 Cr 1 CS x The film is a working electrode, YP50 active carbon is a counter electrode, a saturated calomel electrode is a reference electrode, and 1mol/L H is used 2 SO 4 As an electrolyte, two-dimensional V was measured at a current density of 1A/g 1 Cr 1 CS x The specific capacity of the nano-sheet electrode material is up to 351F/g.
Example 3
Two-dimensional V 1.5 Cr 0.5 CS x The preparation method of the nano-sheet comprises the following steps:
(1) Uniformly mixing 38.25 g of vanadium powder, 13 g of chromium powder, 27 g of aluminum powder and 12 g of carbon powder, and adding the mixture into a self-propagating reaction tank;
(2) Adding 10 cm tungsten filament, igniting under nitrogen protection, reacting to obtain V 1.5 Cr 0.5 AlC MAX block material;
(3) Will V 1.5 Cr 0.5 Pulverizing AlC MAX block material, sieving with 300-400 mesh sieve to obtain V 1.5 Cr 0.5 AlC MAX powder;
(4) Will V 1.5 Cr 0.5 AlC MAX powder, znS and Na 2 S/K 2 The S mixed salt was prepared in a 1:6:18 ratio (Na as described 2 S/K 2 In S mixed salt, na 2 S and K 2 S in a mass ratio of 1:1)Evenly mixing the materials in a mass ratio to obtain mixed powder;
(5) Annealing the mixed powder in the step (4) for 6 hours at 800 ℃ under the protection of argon, washing with 1mol/L hydrochloric acid solution, and washing with water to be neutral to obtain two-dimensional V 1.5 Cr 0.5 CS x The yield of the nano sheet material is 72%.
Will be two-dimensional V 1.5 Cr 0.5 CS x Suction filtering to form film, and directly using V 1.5 Cr 0.5 CS x The film is a working electrode, YP50 active carbon is a counter electrode, a saturated calomel electrode is a reference electrode, and 1mol/L H is used 2 SO 4 As an electrolyte, two-dimensional V was measured at a current density of 1A/g 1.5 Cr 0.5 CS x The specific capacity of the nano-sheet electrode material is up to 435F/g.
Example 4
Two-dimensional V 1.8 Cr 0.2 CS x The preparation method of the nano-sheet comprises the following steps:
(1) Uniformly mixing 45.9 g of vanadium powder, 5.2 g of chromium powder, 32.4 g of aluminum powder and 12 g of carbon powder, and adding the mixture into a self-propagating reaction tank;
(2) Adding 10 cm tungsten filament, igniting under nitrogen protection, reacting to obtain V 1.8 Cr 0.2 AlC MAX block material;
(3) Will V 1.8 Cr 0.2 Pulverizing AlC MAX block material, sieving with 300-400 mesh sieve to obtain V 1.8 Cr 0.2 AlC MAX powder;
(4) Will V 1.8 Cr 0.2 AlC MAX powder, znS and Na 2 S/K 2 The S mixed salt was prepared in a 1:6:36 ratio (Na 2 S/K 2 In S mixed salt, na 2 S and K 2 The mass ratio of S is 1:1), and the mixed powder is obtained;
(5) Annealing the mixed powder in the step (4) for 10 hours at 800 ℃ under the protection of argon, washing with 1mol/L hydrochloric acid solution, and washing with water to be neutral to obtain two-dimensional V 1.8 Cr 0.2 CS x The yield of the nanosheet material was 57%.
Will be two-dimensional V 1.8 Cr 0.2 CS x Suction filtering to form film, and directly using V 1.8 Cr 0.2 CS x The film is a working electrode, YP50 active carbon is a counter electrode, a saturated calomel electrode is a reference electrode, and 1mol/L H is used 2 SO 4 As an electrolyte, two-dimensional V was measured at a current density of 1A/g 1.8 Cr 0.2 CS x The specific capacity of the nano-sheet electrode material is up to 335F/g.
Example 5
Two-dimensional V 1.2 Cr 0.6 CS x The preparation method of the nano-sheet comprises the following steps:
(1) Uniformly mixing 30.6 g of vanadium powder, 15.6 g of chromium powder, 30.0 g of aluminum powder and 12 g of carbon powder, and adding the mixture into a self-propagating reaction tank;
(2) Adding 10 cm tungsten filament, igniting under nitrogen protection, reacting to obtain V 1.2 Cr 0.6 AlC MAX block material;
(3) Will V 1.2 Cr 0.6 Pulverizing AlC MAX block material, sieving with 300-400 mesh sieve to obtain V 1.2 Cr 0.6 AlC MAX powder;
(4) Will V 1.2 Cr 0.6 AlC MAX powder, znS and Na 2 S/K 2 The S mixed salt was prepared in a 1:6:54 ratio (Na 2 S/K 2 In S mixed salt, na 2 S and K 2 The mass ratio of S is 1:1), and the mixed powder is obtained;
(5) Annealing the mixed powder in the step (4) for 8 hours at 800 ℃ under the protection of argon, washing with 1mol/L sulfuric acid solution, and washing with water to be neutral to obtain two-dimensional V 1.2 Cr 0.6 CS x The yield of the nanosheet material was 63%.
Will be two-dimensional V 1.2 Cr 0.6 CS x Suction filtering to form film, and directly using V 1.2 Cr 0.6 CS x The film is a working electrode, YP50 active carbon is a counter electrode, a saturated calomel electrode is a reference electrode, and 1mol/L H is used 2 SO 4 As an electrolyte, two-dimensional V was measured at a current density of 1A/g 1.2 Cr 0.6 CS x Nanosheet electricityThe specific capacity of the polar material is as high as 375F/g.
In summary, a V of the present invention y Cr 2-y CS x The nano sheet is a fluoride-free two-dimensional material prepared based on a molten salt method, has good energy storage performance, and can be used as an electrode material of a super capacitor. The preparation can meet the requirements of continuous development and environmental protection, and has wide sources and low price.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the invention is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Claims (6)
1. Two-dimensional V y Cr 2-y CS x The preparation method of the nano-sheet is characterized by comprising the following steps:
(1) According to chemical formula V y Cr 2-y Taking the metering ratio of AlC, uniformly mixing vanadium powder, chromium powder, aluminum powder and carbon powder, and then adding the mixture into a self-propagating reaction tank; said formula V y Cr 2-y AlC, 0<y≤2；
(2) Adding tungsten filament into self-propagating reactor, igniting under inert gas protection, reacting to obtain V y Cr 2-y AlC MAX block material;
(3) Will V y Cr 2-y Pulverizing AlC MAX block material, sieving to obtain V y Cr 2-y AlC MAX powder;
(4) Will V y Cr 2-y AlC MAX powder, znS and Na 2 S/K 2 S, uniformly mixing the mixed salt to obtain mixed powder;
(5) Annealing the mixed powder in the step (4) under the protection of inert gas, and then pickling and washingTo neutral to obtain two-dimensional V y Cr 2-y CS x A nanosheet;
in the step (2), the length of the tungsten filament is 5-15 cm, and the inert gas is nitrogen or argon;
in the step (5), the annealing treatment temperature is 700-950 ℃ and the annealing time is 3-10h.
2. The two-dimensional V of claim 1 y Cr 2-y CS x A method for producing nanosheets, characterized in that in step (1), the chemical formula V y Cr 2-y In AlC, y is more than or equal to 1 and less than or equal to 2.
3. The two-dimensional V of claim 1 y Cr 2-y CS x The preparation method of the nano-sheet is characterized in that in the step (3), the sieving is performed through a 300-400 mesh sieve.
4. The two-dimensional V of claim 1 y Cr 2-y CS x A method for preparing nanosheets is characterized in that in the step (4), V y Cr 2- y The mass ratio of AlC MAX powder to ZnS is 1 (3-9).
5. The two-dimensional V of claim 1 y Cr 2-y CS x A method for producing nanosheets, characterized in that in step (4), znS and Na are mentioned 2 S/K 2 The mass ratio of the S mixed salt is 1:6, and the Na is as follows 2 S/K 2 In S mixed salt, na 2 S and K 2 The mass ratio of S is 1:1.
6. The two-dimensional V as claimed in any one of claims 1 to 5 y Cr 2-y CS x The preparation method of the nano-sheet is characterized in that in the step (5), the inert gas is nitrogen or argon, and the acid liquid used for acid washing is 1mol/L saltAn acid solution or a sulfuric acid solution.
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