CN110143616A - A kind of preparation method of the rhenium disulfide nanometer sheet of vertical-growth - Google Patents
A kind of preparation method of the rhenium disulfide nanometer sheet of vertical-growth Download PDFInfo
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- CN110143616A CN110143616A CN201910364778.3A CN201910364778A CN110143616A CN 110143616 A CN110143616 A CN 110143616A CN 201910364778 A CN201910364778 A CN 201910364778A CN 110143616 A CN110143616 A CN 110143616A
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- USWJSZNKYVUTIE-UHFFFAOYSA-N bis(sulfanylidene)rhenium Chemical compound S=[Re]=S USWJSZNKYVUTIE-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title claims abstract description 42
- 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
- 239000000758 substrate Substances 0.000 claims abstract description 29
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 23
- 239000010703 silicon Substances 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000005864 Sulphur Substances 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 10
- YSZJKUDBYALHQE-UHFFFAOYSA-N rhenium trioxide Chemical compound O=[Re](=O)=O YSZJKUDBYALHQE-UHFFFAOYSA-N 0.000 claims abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 210000004907 gland Anatomy 0.000 claims abstract description 8
- 239000011261 inert gas Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 239000010431 corundum Substances 0.000 claims description 7
- 229910052593 corundum Inorganic materials 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 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
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 230000008021 deposition Effects 0.000 claims description 4
- 238000002203 pretreatment 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
- 238000000034 method Methods 0.000 abstract description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 239000001257 hydrogen Substances 0.000 abstract description 4
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 4
- 238000002474 experimental method Methods 0.000 abstract description 3
- 230000005518 electrochemistry Effects 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 229910052702 rhenium Inorganic materials 0.000 description 10
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 description 10
- 238000010792 warming Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 230000000694 effects Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000005137 deposition process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000004506 ultrasonic cleaning 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
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 150000003623 transition metal compounds Chemical class 0.000 description 1
Classifications
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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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G47/00—Compounds of rhenium
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The invention discloses a kind of preparation methods of the rhenium disulfide nanometer sheet of vertical-growth, it is placed in again after rhenium trioxide is placed on silicon wafer A in reaction boat, carbon cloth substrate is laid in above reaction boat, then by silicon wafer B gland in carbon cloth substrate, while also in the both ends indwelling blow vent of reaction boat；Sulphur powder is placed in reaction vessel, reaction boat and reaction vessel are placed in quartz glass tube, quartz glass tube is placed in vacuum tube furnace, then in the case where inert gas atmosphere encloses, electron tubes type in-furnace temperature is risen to 650-850 DEG C, 20-40min is kept the temperature to get the rhenium disulfide nanometer sheet of vertical-growth is arrived.Preparation method simple process provided by the invention, prepared three-dimensional rhenium disulfide nanometer sheet, which produces hydrogen catalyst as electrochemistry, has preferable electro catalytic activity, and stability is good.Simultaneously because growth substrates are cheap, experiment condition controllability is good, is easy to introduce in actual industrial production, therefore has broad application prospects in Green Chemistry industry.
Description
Technical field
The present invention relates to electrochemical catalysis to produce hydrogen catalyst preparation technical field, and in particular to a kind of two sulphur of vertical-growth
Change the preparation method of rhenium nanometer sheet.
Background technique
In recent years, emerging two-dimension nano materials have been shown to have the great potential as important electrochemical catalyst.
This kind of ultra-thin nano material nature difference compared with its block is very big, and the diffusion path of ultrathin nanometer piece is short, can effectively promote
Into electric charge transfer.Two-dimensional material can become exploration excitation relatively easily using a variety of strategy preparations and regulation microstructure
The ideal object of catalytic activity and electronics transfer.Wherein rhenium disulfide is due to its low structural symmetry and other two sulphur of transition metal
Compound is different in performance, has anisotropy optically and electrically, especially two sulphur of three-dimensional structure vertical-growth
Change rhenium nanometer sheet, for the rhenium disulfide nanometer sheet of two-dimensional structure, active site can expose to the maximum extent, from
And keeping its electron transfer efficiency higher, catalytic activity is more preferable.
The preparation method of three-dimensional structure rhenium disulfide nanometer sheet is mainly vapour deposition process at present, vapour deposition process compared to
Other technologies technique is simpler, more controllable, is widely used in recent years.But vapour deposition process is utilized to synthesize
The three-dimensional structure rhenium disulfide nanometer sheet of larger area is there are still defect, in the rhenium disulfide nanometer sheet of the three-dimensional structure such as obtained
Rhenium disulfide nanometer sheet and the deposition rate that a certain amount of two-dimensional structure can be mixed with are more low.
More in-depth study is carried out in order to produce hydrogen catalysis effect to rhenium disulfide, and pushes its practicalization, is needed
Find the high preparation method of a kind of simple process, three-dimensional structure rhenium disulfide nanometer sheet yield.
Summary of the invention
The purpose of the invention is to overcome the problems of the prior art, a kind of rhenium disulfide nanometer of vertical-growth is provided
The preparation method of piece.
The present invention provides a kind of preparation methods of the rhenium disulfide nanometer sheet of vertical-growth, comprising the following steps:
It is placed in after rhenium trioxide is placed on silicon wafer A in reaction boat, carbon cloth substrate is laid in above reaction boat again then,
Again by silicon wafer B gland in carbon cloth substrate, while also in the equal indwelling blow vent in both ends of reaction boat；
Sulphur powder is placed in reaction vessel, boat and reaction vessel is reacted and is placed in quartz glass tube, then by quartz glass
Pipe is placed in vacuum tube furnace, then in the case where inert gas atmosphere encloses, electron tubes type in-furnace temperature is risen to 650-850 DEG C, is protected
Warm 20-40min, i.e., deposition obtains the rhenium disulfide nanometer sheet of vertical-growth in carbon cloth substrate；
Wherein, the rhenium trioxide and the mass ratio of sulphur powder are 0.4-2:100.
Preferably, silicon wafer A and carbon cloth substrate are passing through pretreatment using preceding.
Preferably, the pre-treatment step of silicon wafer A is as follows:
Silicon wafer A is cleaned by ultrasonic in dehydrated alcohol, isopropanol and acetone respectively, pretreatment silicon wafer is obtained after dry.
Preferably, the pre-treatment step of carbon cloth substrate is as follows: by carbon cloth substrate respectively in dehydrated alcohol and deionized water
Ultrasonic cleaning obtains pretreatment carbon cloth substrate after dry.
Preferably, the inert gas is argon gas.
Preferably, in vacuum tube furnace heating rate be 30-50 DEG C/min, inert gas flow 50-100sccm, very
Blank pipe formula furnace gas pressure is 1 × 10-2-10Pa。
Preferably, the reaction boat is corundum boat, and the reaction vessel is quartzy tile.
Preferably, the rhenium disulfide nanometer sheet prepared is three-dimensional petal-like structures, size 5-20nm.
Compared with prior art, the beneficial effects of the present invention are:
(1) present invention makes presoma generate enrichment in conversion zone by the method for silicon wafer gland carbon cloth substrate, to make
React more abundant, reaction efficiency improves, and finds in an experiment, the base prepared using the method for silicon wafer gland carbon cloth substrate
It is all the rhenium disulfide nanometer sheet of three-dimensional structure in sheet, the yield of three-dimensional structure rhenium disulfide nanometer sheet is bigger, and structure is more
Densification, and the rhenium disulfide nanometer sheet of compact texture has big specific surface area, active site quantity is able to a large amount of exposures.
(2) the rhenium disulfide nanometer chip size for the three-dimensional structure that method of the invention is prepared is small, quantity is more, thickness is thin,
And the diffusion path of the thin nanometer sheet of thickness is short, can effectively facilitate electric charge transfer.
(3) the rhenium disulfide nanometer sheet preparation process of vertical-growth provided by the invention is simple, is used as three-dimensional material
Electrochemistry, which produces hydrogen catalyst, has preferable electro catalytic activity, and stability is good, is easy to introduce in actual industrial production, therefore green
It has broad application prospects in colour chemistry industry.
Detailed description of the invention
Fig. 1 is the XRD diagram of the rhenium disulfide nanometer sheet for the vertical-growth that the embodiment of the present invention 7 is prepared；
Fig. 2 is the SEM figure for the rhenium disulfide nanometer sheet that the embodiment of the present invention 7 and comparative example 1 are prepared, wherein scheming (a) is
The SEM of the rhenium disulfide nanometer sheet for the vertical-growth that embodiment 7 is prepared schemes, and figure (b) is the rhenium disulfide that comparative example 1 is prepared
The SEM of nanometer sheet schemes；
Fig. 3 is the H2-producing capacity figure of the rhenium disulfide nanometer sheet for the vertical-growth that the embodiment of the present invention 7 is prepared, wherein
10mA/cm2Overpotential under current density is 468V.
Specific embodiment
In order to enable those skilled in the art to more fully understand, technical solution of the present invention is practiced, below with reference to specific
The invention will be further described for embodiment and attached drawing, but illustrated embodiment is not as a limitation of the invention.
Experimental method described in following each embodiments is conventional method unless otherwise specified；The reagent and material, such as
Without specified otherwise, can be commercially available on the market.
Embodiment 1
A kind of preparation method of the rhenium disulfide nanometer sheet of vertical-growth, comprising the following steps:
Step 1, the pretreatment of silicon wafer A: will the silicon wafer A having a size of 1cm × 1.8cm respectively dehydrated alcohol, isopropanol and
It is cleaned by ultrasonic 10min in acetone, pretreatment silicon wafer is obtained after drying；
The pretreatment of carbon cloth substrate: will be having a size of 1.8cm × 4.5cm carbon cloth substrate respectively in dehydrated alcohol and deionized water
Middle ultrasonic cleaning 10min, 5min obtain pretreatment carbon cloth substrate after then drying in 60 DEG C of baking ovens；
Step 2,2mg rhenium trioxide is weighed, is placed in corundum boat again after being laid on pretreatment silicon wafer, it then will pretreatment
Carbon cloth substrate is laid in above corundum boat, then by silicon wafer B gland in pretreatment carbon cloth substrate, while also at the both ends of reaction boat
Equal indwelling blow vent；
It weighs 500mg sulphur powder to be deposited in quartzy tile, corundum boat and quartzy tile is then placed in quartz glass tube
It is interior, then corundum boat and quartzy tile are put into quartz glass tube, it is 1 × 10 that quartz glass tube, which is placed in vacuum degree,-2Pa's
In tube furnace, under conditions of argon flow is 50sccm, tube furnace is set to be warming up to 650 DEG C with 30 DEG C/min heating rate, life
After long 40min, room temperature is naturally cooled to, i.e., deposition obtains the curing of three-dimensional petal-like structures vertical-growth in carbon cloth substrate
Rhenium nanometer sheet, the average-size of the rhenium disulfide nanometer sheet are 15nm；The rhenium disulfide nanometer sheet of obtained vertical-growth is set
In sample box kept dry, prevent from reacting with oxygen.
Embodiment 2
A kind of preparation method of the rhenium disulfide nanometer sheet of vertical-growth, the preparation method is the same as that of Example 1, the difference is that
Tube furnace is warming up to 700 DEG C with the heating rate of 30 DEG C/min in embodiment 2, obtains two sulphur of vertical-growth after growing 20min
Change rhenium nanometer sheet, the average-size of the rhenium disulfide nanometer sheet is 20nm.
Embodiment 3
A kind of preparation method of the rhenium disulfide nanometer sheet of vertical-growth, the preparation method is the same as that of Example 1, the difference is that
Vacuum degree is 1Pa in tube furnace in embodiment 3, and argon flow 80sccm, tube furnace is with the heating rate heating of 30 DEG C/min
To 700 DEG C, the rhenium disulfide nanometer sheet of vertical-growth is obtained after growing 30min, the average-size of the rhenium disulfide nanometer sheet is
5nm。
Embodiment 4
A kind of preparation method of the rhenium disulfide nanometer sheet of vertical-growth, the preparation method is the same as that of Example 1, the difference is that
Vacuum degree is 10Pa in tube furnace in embodiment 4, and argon flow 100sccm, tube furnace is with the heating rate liter of 40 DEG C/min
Temperature obtains the rhenium disulfide nanometer sheet of vertical-growth, the average-size of the rhenium disulfide nanometer sheet after growing 40min to 700 DEG C
For 10nm.
Embodiment 5
A kind of preparation method of the rhenium disulfide nanometer sheet of vertical-growth, the preparation method is the same as that of Example 1, the difference is that
Tube furnace is warming up to 750 DEG C with the heating rate of 40 DEG C/min in embodiment 5, obtains two sulphur of vertical-growth after growing 20min
Change rhenium nanometer sheet, the average-size of the rhenium disulfide nanometer sheet is 8nm.
Embodiment 6
A kind of preparation method of the rhenium disulfide nanometer sheet of vertical-growth, the preparation method is the same as that of Example 1, the difference is that
Tube furnace is warming up to 800 DEG C with the heating rate of 50 DEG C/min in embodiment 6, obtains two sulphur of vertical-growth after growing 40min
Change rhenium nanometer sheet, the average-size of the rhenium disulfide nanometer sheet is 10nm.
Embodiment 7
A kind of preparation method of the rhenium disulfide nanometer sheet of vertical-growth, the preparation method is the same as that of Example 1, the difference is that
Vacuum degree is 1Pa in tube furnace in embodiment 7, and the dosage of rhenium trioxide is 3mg, and sulphur powder dosage is 500mg, and tube furnace is with 50
DEG C/heating rate of min is warming up to 700 DEG C, the rhenium disulfide nanometer sheet of vertical-growth, the curing are obtained after growing 30min
The average-size of rhenium nanometer sheet is 5nm.
Embodiment 8
A kind of preparation method of the rhenium disulfide nanometer sheet of vertical-growth, the preparation method is the same as that of Example 1, the difference is that
Vacuum degree is 1Pa in tube furnace in embodiment 8, and the dosage of rhenium trioxide is 5mg, and sulphur powder dosage is 500mg, and tube furnace is with 40
DEG C/heating rate of min is warming up to 700 DEG C, the rhenium disulfide nanometer sheet of vertical-growth, the curing are obtained after growing 30min
The average-size of rhenium nanometer sheet is 8nm.
Embodiment 9
A kind of preparation method of the rhenium disulfide nanometer sheet of vertical-growth, the preparation method is the same as that of Example 1, the difference is that
Vacuum degree is 10Pa in tube furnace in embodiment 9, and the dosage of rhenium trioxide is 7mg, and sulphur powder dosage is 500mg, and tube furnace is with 30
DEG C/heating rate of min is warming up to 700 DEG C, the rhenium disulfide nanometer sheet of vertical-growth, the curing are obtained after growing 30min
The average-size of rhenium nanometer sheet is 15nm.
Embodiment 10
A kind of preparation method of the rhenium disulfide nanometer sheet of vertical-growth, the preparation method is the same as that of Example 1, the difference is that
Vacuum degree is 10Pa in tube furnace in embodiment 10, and the dosage of rhenium trioxide is 10mg, and sulphur powder dosage is 500mg, tube furnace with
The heating rate of 40 DEG C/min is warming up to 700 DEG C, obtains the rhenium disulfide nanometer sheet of vertical-growth after growing 30min, two sulphur
The average-size for changing rhenium nanometer sheet is 10nm.
Comparative example 1
A kind of preparation method of rhenium disulfide nanometer sheet, the preparation method is the same as that of Example 1, the difference is that in comparative example 1
There is no gland silicon wafer in the pretreatment carbon cloth substrate being laid with above corundum boat.
The effect of the rhenium disulfide nanometer sheet for the vertical-growth that embodiment 1-10 is prepared is essentially identical, therefore only to implementation
The performance of the rhenium disulfide nanometer sheet for the vertical-growth that example 7 and comparative example 1 are prepared is detected, to illustrate effect of the invention
Fruit is specifically shown in Fig. 1-3.Wherein, Fig. 1 is the XRD of the rhenium disulfide nanometer sheet for the vertical-growth that the embodiment of the present invention 7 is prepared
Figure, as shown in Figure 1, the peak position of the rhenium disulfide nanometer sheet for the vertical-growth that embodiment 7 is prepared is consistent with standard card, in addition to
Outside the peak of carbon cloth substrate, without other miscellaneous peaks, this illustrates the rhenium disulfide nanometer sheet purity is high of preparation, without other impurities.
Fig. 2 is the SEM figure for the rhenium disulfide nanometer sheet that the embodiment of the present invention 7 and comparative example 1 are prepared, and figure (a) is to implement
The SEM of the rhenium disulfide nanometer sheet for the vertical-growth that example 7 is prepared schemes, and figure (b) is the rhenium disulfide nanometer that comparative example 1 is prepared
The SEM of piece schemes, and is petal-shaped, without plane two from figure (a) as can be seen that rhenium disulfide nanometer sheet sheet vertical growth is obvious
The presence of shape, size 5-20nm are tieed up, specific surface area increases very much；From figure (b) as can be seen that three-dimensional structure is petal-like
Rhenium disulfide nanometer sheet and the rhenium disulfide nanometer sheet of two-dimensional structure mix growth, and the two without clear superiority, illustrates this hair
The bright method by silicon wafer gland carbon cloth substrate facilitates the growth of three-dimensional structure rhenium disulfide nanometer sheet.
Fig. 3 is the H2-producing capacity figure for the rhenium disulfide nanometer sheet that the present invention implements 7 vertical-growths prepared, wherein
10mA/cm2Overpotential under current density is 468V, and carbon cloth substrate is in 10mA/cm2There is no overpotential, when rhenium disulfide nanometer
In carbon cloth substrate, overpotential is obviously reduced piece vertical-growth, and performance significantly improves.
The present invention describes preferred embodiment and its effect.It is created once a person skilled in the art knows basic
Property concept, then additional changes and modifications may be made to these embodiments.So it includes excellent that the following claims are intended to be interpreted as
It selects embodiment and falls into all change and modification of the scope of the invention.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (8)
1. a kind of preparation method of the rhenium disulfide nanometer sheet of vertical-growth, which comprises the following steps:
It is placed in after rhenium trioxide is placed on silicon wafer A in reaction boat, carbon cloth substrate is laid in above reaction boat again then, then will
Silicon wafer B gland in carbon cloth substrate, while also reaction boat the equal indwelling blow vent in both ends；
Sulphur powder is placed in reaction vessel, boat is reacted and reaction vessel is placed in quartz glass tube, then quartz glass tube is set
In in vacuum tube furnace, then in the case where inert gas atmosphere encloses, electron tubes type in-furnace temperature is risen to 650-850 DEG C, keeps the temperature 20-
40min, i.e., deposition obtains the rhenium disulfide nanometer sheet of vertical-growth in carbon cloth substrate；
Wherein, the rhenium trioxide and the mass ratio of sulphur powder are 0.4-2:100.
2. the preparation method of the rhenium disulfide nanometer sheet of vertical-growth according to claim 1, which is characterized in that silicon wafer A
Passing through pretreatment using preceding with carbon cloth substrate.
3. the preparation method of the rhenium disulfide nanometer sheet of vertical-growth according to claim 2, which is characterized in that silicon wafer A
Pre-treatment step it is as follows:
Silicon wafer A is cleaned by ultrasonic in dehydrated alcohol, isopropanol and acetone respectively, pretreatment silicon wafer is obtained after dry.
4. the preparation method of the rhenium disulfide nanometer sheet of vertical-growth according to claim 2, which is characterized in that carbon cloth base
The pre-treatment step at bottom is as follows: carbon cloth substrate being cleaned by ultrasonic in dehydrated alcohol and deionized water respectively, is obtained after dry pre-
Handle carbon cloth substrate.
5. the preparation method of the rhenium disulfide nanometer sheet of vertical-growth according to claim 1, which is characterized in that described lazy
Property gas be argon gas.
6. the preparation method of the rhenium disulfide nanometer sheet of vertical-growth according to claim 5, which is characterized in that vacuum tube
Heating rate is 30-50 DEG C/min, inert gas flow 50-100sccm in formula furnace, and gas pressure intensity is 1 in vacuum tube furnace
×10-2-10Pa。
7. the preparation method of the rhenium disulfide nanometer sheet of vertical-growth according to claim 1, which is characterized in that described anti-
Ying Zhouwei corundum boat, the reaction vessel are quartzy tile.
8. the preparation method of the rhenium disulfide nanometer sheet of vertical-growth according to claim 1, which is characterized in that prepare
Rhenium disulfide nanometer sheet be three-dimensional petal-like structures, size 5-20nm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110372040A (en) * | 2019-08-22 | 2019-10-25 | 哈尔滨工业大学 | A method of rhenium disulfide nanometer sheet is prepared using liquid phase removing transfer |
| CN111509230A (en) * | 2020-04-26 | 2020-08-07 | 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 |
| CN111945132A (en) * | 2020-08-28 | 2020-11-17 | 陕西科技大学 | Vertically-grown niobium disulfide nanosheet and preparation method and application thereof |
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| CN111945132A (en) * | 2020-08-28 | 2020-11-17 | 陕西科技大学 | Vertically-grown niobium disulfide nanosheet and preparation method and application thereof |
| 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 |
| CN116495789A (en) * | 2023-04-24 | 2023-07-28 | 闽都创新实验室 | Preparation method and application of ultrathin rhenium sulfide nanosheets |
| CN116495789B (en) * | 2023-04-24 | 2024-04-30 | 闽都创新实验室 | Preparation method and application of ultrathin rhenium sulfide nanosheets |
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