CN110143616B - Preparation method of vertically-grown rhenium disulfide nanosheet - Google Patents
Preparation method of vertically-grown rhenium disulfide nanosheet Download PDFInfo
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- USWJSZNKYVUTIE-UHFFFAOYSA-N bis(sulfanylidene)rhenium Chemical compound S=[Re]=S USWJSZNKYVUTIE-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 239000002135 nanosheet Substances 0.000 title claims abstract description 83
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000758 substrate Substances 0.000 claims abstract description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 29
- 239000004744 fabric Substances 0.000 claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 24
- 239000010703 silicon Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- YSZJKUDBYALHQE-UHFFFAOYSA-N rhenium trioxide Chemical compound O=[Re](=O)=O YSZJKUDBYALHQE-UHFFFAOYSA-N 0.000 claims abstract description 12
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 239000011261 inert gas Substances 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 6
- 238000003825 pressing Methods 0.000 claims abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 239000010431 corundum Substances 0.000 claims description 7
- 229910052593 corundum Inorganic materials 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000010453 quartz Substances 0.000 claims description 5
- 238000000151 deposition Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 2
- 239000002055 nanoplate Substances 0.000 claims 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 7
- 239000001257 hydrogen Substances 0.000 abstract description 7
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 7
- 239000003054 catalyst Substances 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 7
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 238000007740 vapor deposition Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000004075 alteration Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000027756 respiratory electron transport chain Effects 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- -1 transition metal disulfides Chemical class 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
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- B01J35/39—
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G47/00—Compounds of rhenium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
Abstract
The invention discloses a preparation method of vertically-grown rhenium disulfide nanosheets, which comprises the steps of placing rhenium trioxide on a silicon wafer A and then placing the silicon wafer A into a reaction boat, paving a carbon cloth substrate above the reaction boat, pressing a silicon wafer B onto the carbon cloth substrate, and reserving air vents at two ends of the reaction boat; and (3) placing sulfur powder into a reaction container, placing the reaction boat and the reaction container into a quartz glass tube, placing the quartz glass tube into a vacuum tube furnace, raising the temperature in the vacuum tube furnace to 650 plus materials 850 ℃ in the atmosphere of inert gas, and preserving the heat for 20-40min to obtain the vertically-grown rhenium disulfide nanosheet. The preparation method provided by the invention is simple in process, and the prepared three-dimensional rhenium disulfide nanosheet has good electrocatalytic activity and good stability when being used as an electrochemical hydrogen production catalyst. Meanwhile, the growth substrate is cheap, the experimental conditions are good in controllability, and the method is easy to introduce into actual industrial production, so that the method has a wide application prospect in the green chemical industry.
Description
Technical Field
The invention relates to the technical field of preparation of electrochemical catalytic hydrogen production catalysts, in particular to a preparation method of vertically-grown rhenium disulfide nanosheets.
Background
In recent years, emerging two-dimensional nanomaterials have demonstrated great potential to become important electrochemical catalysts. Compared with the bulk of the ultrathin nano material, the ultrathin nano material has great property difference, and the diffusion path of the ultrathin nano sheet is short, so that the charge transfer can be effectively promoted. The two-dimensional material can be easily prepared and the microstructure can be regulated by adopting various strategies, and becomes an ideal object for exploring and exciting catalytic activity and electron transfer. The rhenium disulfide is different from other transition metal disulfides in performance due to the low structural symmetry, has optical and electrical anisotropy, and particularly has the active sites exposed to the maximum extent compared with rhenium disulfide nanosheets with two-dimensional structures, so that the rhenium disulfide nanosheets are higher in electron transfer efficiency and better in catalytic activity.
At present, the preparation method of the rhenium disulfide nanosheet with the three-dimensional structure is mainly a vapor deposition method, and compared with other technologies, the vapor deposition method is simpler and more controllable in process and is widely applied in recent years. However, the method for synthesizing the rhenium disulfide nanosheet with the large-area three-dimensional structure by using the vapor deposition method still has the defects that the obtained rhenium disulfide nanosheet with the three-dimensional structure is mixed with a certain amount of rhenium disulfide nanosheet with the two-dimensional structure, the deposition rate is low, and the like.
In order to carry out more intensive research on the hydrogen production catalysis effect of rhenium disulfide and promote the practical process of the hydrogen production catalysis effect, a preparation method which is simple in process and high in yield of rhenium disulfide nanosheets with three-dimensional structures needs to be found urgently.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a preparation method of a vertically-grown rhenium disulfide nanosheet.
The invention provides a preparation method of a vertically-grown rhenium disulfide nanosheet, which comprises the following steps:
putting rhenium trioxide on the silicon wafer A and then putting the silicon wafer A into a reaction boat, then paving a carbon cloth substrate above the reaction boat, pressing the silicon wafer B on the carbon cloth substrate, and simultaneously reserving vent holes at two ends of the reaction boat;
putting sulfur powder into a reaction container, putting a reaction boat and the reaction container into a quartz glass tube, putting the quartz glass tube into a vacuum tube furnace, raising the temperature in the vacuum tube furnace to 650 plus materials and 850 ℃ in an inert gas atmosphere, and preserving the temperature for 20-40min, namely depositing on a carbon cloth substrate to obtain vertically-grown rhenium disulfide nanosheets;
wherein the mass ratio of the rhenium trioxide to the sulfur powder is 0.4-2: 100.
Preferably, both the silicon wafer a and the carbon cloth substrate are pretreated before use.
Preferably, the pretreatment steps of the silicon wafer A are as follows:
and ultrasonically cleaning the silicon wafer A in absolute ethyl alcohol, isopropanol and acetone respectively, and drying to obtain the pretreated silicon wafer.
Preferably, the pretreatment step of the carbon cloth substrate is as follows: and ultrasonically cleaning the carbon cloth substrate in absolute ethyl alcohol and deionized water respectively, and drying to obtain the pretreated carbon cloth substrate.
Preferably, the inert gas is argon.
Preferably, the heating rate in the vacuum tube furnace is 30-50 ℃/min, the flow rate of the inert gas is 50-100sccm, and the gas pressure in the vacuum tube furnace is 1 multiplied by 10-2-10Pa。
Preferably, the reaction boat is a corundum boat, and the reaction vessel is a quartz tile.
Preferably, the prepared rhenium disulfide nanosheet is of a three-dimensional petal-shaped structure, and the size is 5-20 nm.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the invention, the precursor is enriched in the reaction region by a method of covering the carbon cloth substrate with the silicon wafer, so that the reaction is more sufficient, the reaction efficiency is improved, and experiments show that the rhenium disulfide nanosheets with three-dimensional structures are basically prepared by the method of covering the carbon cloth substrate with the silicon wafer, the production amount of the rhenium disulfide nanosheets with three-dimensional structures is larger, the structures are more compact, the rhenium disulfide nanosheets with compact structures have large specific surface areas, and the number of active sites is greatly exposed.
(2) The three-dimensional rhenium disulfide nanosheet prepared by the method is small in size, large in quantity and thin in thickness, and the thin nanosheet is short in diffusion path and can effectively promote charge transfer.
(3) The vertically-grown rhenium disulfide nanosheet provided by the invention is simple in preparation process, has good electrocatalytic activity when being used as a three-dimensional material as an electrochemical hydrogen production catalyst, is good in stability, and is easy to introduce into actual industrial production, so that the rhenium disulfide nanosheet has a wide application prospect in the green chemical industry.
Drawings
Fig. 1 is an XRD pattern of vertically-grown rhenium disulfide nanosheets prepared in example 7 of the present invention;
fig. 2 is SEM images of rhenium disulfide nanosheets prepared in example 7 of the present invention and comparative example 1, wherein (a) is an SEM image of vertically-grown rhenium disulfide nanosheets prepared in example 7, and (b) is an SEM image of rhenium disulfide nanosheets prepared in comparative example 1;
FIG. 3 is a hydrogen production performance diagram of vertically grown rhenium disulfide nanosheets prepared in example 7 of the present invention, wherein 10mA/cm2The overpotential at current density was 468V.
Detailed Description
In order to make the technical solutions of the present invention better understood and implemented by those skilled in the art, the present invention is further described below with reference to the following specific embodiments and the accompanying drawings, but the embodiments are not meant to limit the present invention.
The experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1
A preparation method of vertically-grown rhenium disulfide nanosheets comprises the following steps:
step 1, pretreating a silicon wafer A: ultrasonically cleaning a silicon wafer A with the size of 1cm multiplied by 1.8cm in absolute ethyl alcohol, isopropanol and acetone for 10min respectively, and drying to obtain a pretreated silicon wafer;
pretreatment of the carbon cloth substrate: ultrasonically cleaning a carbon cloth substrate with the size of 1.8cm multiplied by 4.5cm in absolute ethyl alcohol and deionized water for 10min and 5min respectively, and then drying in a drying oven at the temperature of 60 ℃ to obtain a pretreated carbon cloth substrate;
step 2, weighing 2mg of rhenium trioxide, paving the rhenium trioxide on a pretreated silicon wafer, then placing the rhenium trioxide in a corundum boat, paving a pretreated carbon cloth substrate above the corundum boat, pressing a silicon wafer B on the pretreated carbon cloth substrate, and simultaneously keeping vent holes at two ends of the reaction boat;
weighing 500mg of sulfur powder and stacking the sulfur powder in quartz tiles, then placing the corundum boat and the quartz tiles in a quartz glass tube, and then placing the corundum boatPutting quartz tiles into a quartz glass tube, and placing the quartz glass tube in a vacuum degree of 1 × 10-2In a Pa tubular furnace, under the condition that the argon flow is 50sccm, heating the tubular furnace to 650 ℃ at the heating rate of 30 ℃/min, growing for 40min, and naturally cooling to room temperature, namely depositing on a carbon cloth substrate to obtain a three-dimensional petal-shaped structure vertically-grown rhenium disulfide nanosheet, wherein the average size of the rhenium disulfide nanosheet is 15 nm; and placing the obtained vertically-grown rhenium disulfide nanosheet in a sample box for drying and storage to prevent reaction with oxygen.
Example 2
The preparation method of the vertically-grown rhenium disulfide nanosheet is the same as that in example 1, except that in example 2, the temperature of a tubular furnace is increased to 700 ℃ at the temperature rise rate of 30 ℃/min, and the vertically-grown rhenium disulfide nanosheet is obtained after the rhenium disulfide nanosheet grows for 20min, wherein the average size of the rhenium disulfide nanosheet is 20 nm.
Example 3
The preparation method of the vertically-grown rhenium disulfide nanosheet is the same as that in example 1, except that in example 3, the vacuum degree in a tubular furnace is 1Pa, the argon flow is 80sccm, the temperature of the tubular furnace is increased to 700 ℃ at the temperature increasing rate of 30 ℃/min, and the vertically-grown rhenium disulfide nanosheet is obtained after growth for 30min, wherein the average size of the rhenium disulfide nanosheet is 5 nm.
Example 4
The preparation method of the vertically-grown rhenium disulfide nanosheet is the same as that in example 1, except that in example 4, the vacuum degree in a tubular furnace is 10Pa, the argon flow is 100sccm, the temperature of the tubular furnace is increased to 700 ℃ at the temperature increasing rate of 40 ℃/min, and the vertically-grown rhenium disulfide nanosheet is obtained after growth for 40min, wherein the average size of the rhenium disulfide nanosheet is 10 nm.
Example 5
The preparation method of the vertically-grown rhenium disulfide nanosheet is the same as that in example 1, except that in example 5, the temperature of a tubular furnace is increased to 750 ℃ at the heating rate of 40 ℃/min, and the vertically-grown rhenium disulfide nanosheet is obtained after growth for 20min, wherein the average size of the rhenium disulfide nanosheet is 8 nm.
Example 6
The preparation method of the vertically-grown rhenium disulfide nanosheet is the same as that in example 1, except that in example 6, the temperature of a tubular furnace is increased to 800 ℃ at a heating rate of 50 ℃/min, and the vertically-grown rhenium disulfide nanosheet is obtained after growth for 40min, wherein the average size of the rhenium disulfide nanosheet is 10 nm.
Example 7
The preparation method of the vertically-grown rhenium disulfide nanosheet is the same as that in example 1, except that in example 7, the vacuum degree in a tubular furnace is 1Pa, the dosage of rhenium trioxide is 3mg, the dosage of sulfur powder is 500mg, the temperature of the tubular furnace is increased to 700 ℃ at the heating rate of 50 ℃/min, and the vertically-grown rhenium disulfide nanosheet is obtained after growth for 30min, wherein the average size of the rhenium disulfide nanosheet is 5 nm.
Example 8
The preparation method of the vertically-grown rhenium disulfide nanosheet is the same as that in example 1, except that in example 8, the vacuum degree in a tubular furnace is 1Pa, the dosage of rhenium trioxide is 5mg, the dosage of sulfur powder is 500mg, the temperature of the tubular furnace is increased to 700 ℃ at the temperature increase rate of 40 ℃/min, and the vertically-grown rhenium disulfide nanosheet is obtained after growth for 30min, wherein the average size of the rhenium disulfide nanosheet is 8 nm.
Example 9
The preparation method of the vertically-grown rhenium disulfide nanosheet is the same as that in example 1, except that in example 9, the vacuum degree in a tubular furnace is 10Pa, the dosage of rhenium trioxide is 7mg, the dosage of sulfur powder is 500mg, the temperature of the tubular furnace is increased to 700 ℃ at the temperature increase rate of 30 ℃/min, and the vertically-grown rhenium disulfide nanosheet is obtained after growth for 30min, wherein the average size of the rhenium disulfide nanosheet is 15 nm.
Example 10
The preparation method of the vertically-grown rhenium disulfide nanosheet is the same as that in example 1, except that in example 10, the vacuum degree in a tubular furnace is 10Pa, the dosage of rhenium trioxide is 10mg, the dosage of sulfur powder is 500mg, the temperature of the tubular furnace is increased to 700 ℃ at the temperature increase rate of 40 ℃/min, and the vertically-grown rhenium disulfide nanosheet is obtained after growth for 30min, wherein the average size of the rhenium disulfide nanosheet is 10 nm.
Comparative example 1
A preparation method of a rhenium disulfide nanosheet, which is the same as that in example 1, except that in comparative example 1, no capping silicon wafer is arranged on a pretreated carbon cloth substrate laid above a corundum boat.
The effect of the vertically grown rhenium disulfide nanosheets prepared in examples 1-10 is substantially the same, and therefore only the performance of the vertically grown rhenium disulfide nanosheets prepared in example 7 and comparative example 1 is tested to illustrate the effect of the present invention, see fig. 1-3 in particular. Fig. 1 is an XRD pattern of a vertically-grown rhenium disulfide nanosheet prepared in embodiment 7 of the present invention, and as shown in fig. 1, the peak position of the vertically-grown rhenium disulfide nanosheet prepared in embodiment 7 is consistent with that of a standard card, except for the peak of the carbon cloth substrate, there are no other miscellaneous peaks, which indicates that the prepared rhenium disulfide nanosheet has high purity and no other impurities.
Fig. 2 is SEM images of rhenium disulfide nanosheets prepared in example 7 and comparative example 1 of the present invention, wherein (a) is an SEM image of vertically-grown rhenium disulfide nanosheets prepared in example 7, and (b) is an SEM image of rhenium disulfide nanosheets prepared in comparative example 1, and as can be seen from (a), the rhenium disulfide nanosheets are obviously grown upright in a sheet shape, are petal-shaped, have no planar two-dimensional shape, have a size of 5-20nm, and have a greatly increased specific surface area; as can be seen from the figure (b), the three-dimensional petal-shaped rhenium disulfide nanosheets and the two-dimensional rhenium disulfide nanosheets grow in a mixed mode, and both have no obvious advantages, so that the method for pressing the carbon cloth substrate with the silicon wafer is beneficial to the growth of the three-dimensional rhenium disulfide nanosheets.
FIG. 3 is a hydrogen production performance diagram of vertically grown rhenium disulfide nanosheets prepared in example 7 of the present invention, wherein 10mA/cm2The overpotential under the current density is 468V, and the carbon cloth substrate is 10mA/cm2And no overpotential exists, when the rhenium disulfide nanosheet vertically grows on the carbon cloth substrate, the overpotential is obviously reduced, and the performance is obviously improved.
The present invention describes preferred embodiments and effects thereof. Additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. A preparation method of vertically-grown rhenium disulfide nanosheets is characterized by comprising the following steps:
putting rhenium trioxide on the silicon wafer A and then putting the silicon wafer A into a reaction boat, then paving a carbon cloth substrate above the reaction boat, pressing the silicon wafer B on the carbon cloth substrate, and simultaneously reserving vent holes at two ends of the reaction boat;
putting sulfur powder into a reaction container, putting a reaction boat and the reaction container into a quartz glass tube, putting the quartz glass tube into a vacuum tube furnace, raising the temperature in the vacuum tube furnace to 650 plus materials and 850 ℃ in an inert gas atmosphere, and preserving the temperature for 20-40min, namely depositing on a carbon cloth substrate to obtain vertically-grown rhenium disulfide nanosheets;
the heating rate in the vacuum tube furnace is 30-50 ℃/min, the flow rate of the inert gas is 50-100sccm, and the gas pressure in the vacuum tube furnace is 1 multiplied by 10-2-10Pa；
Wherein the mass ratio of the rhenium trioxide to the sulfur powder is 0.4-2: 100; the rhenium disulfide nanosheet is of a three-dimensional petal-shaped structure, and the size is 5-20 nm.
2. The method of preparing vertically grown rhenium disulfide nanoplates as in claim 1, wherein both wafer a and the carbon cloth substrate are pretreated prior to use.
3. The method for preparing vertically-grown rhenium disulfide nanosheets as recited in claim 2, wherein the pre-treating step of wafer a is as follows:
and ultrasonically cleaning the silicon wafer A in absolute ethyl alcohol, isopropanol and acetone respectively, and drying to obtain the pretreated silicon wafer.
4. The method for preparing vertically grown rhenium disulfide nanosheets of claim 2, wherein the pretreatment of the carbon cloth substrate comprises the steps of: and ultrasonically cleaning the carbon cloth substrate in absolute ethyl alcohol and deionized water respectively, and drying to obtain the pretreated carbon cloth substrate.
5. The method of making vertically grown rhenium disulfide nanoplates as in claim 1, wherein the inert gas is argon.
6. The method of preparing vertically grown rhenium disulfide nanosheets of claim 1, wherein the reaction boat is a corundum boat and the reaction vessel is a quartz tile.
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| CN111509230B (en) * | 2020-04-26 | 2022-03-11 | 武汉纺织大学 | Tin disulfide composite flexible carbon cloth electrode material and preparation method thereof |
| CN111792675A (en) * | 2020-06-23 | 2020-10-20 | 肇庆市华师大光电产业研究院 | Preparation method and application of rhenium disulfide nanosheet |
| CN111945132B (en) * | 2020-08-28 | 2023-01-06 | 陕西科技大学 | Vertically-grown niobium disulfide nanosheet and preparation method and application thereof |
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| CN108689432A (en) * | 2018-06-07 | 2018-10-23 | 肇庆市华师大光电产业研究院 | A method of growing rhenium disulfide nanometer sheet in the silicon base of non-oxidation layer |
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