CN110467358A - A kind of rhenium disulfide nanometer sheet and its preparation method and application for evolving hydrogen reaction - Google Patents
A kind of rhenium disulfide nanometer sheet and its preparation method and application for evolving hydrogen reaction Download PDFInfo
- Publication number
- CN110467358A CN110467358A CN201910616451.0A CN201910616451A CN110467358A CN 110467358 A CN110467358 A CN 110467358A CN 201910616451 A CN201910616451 A CN 201910616451A CN 110467358 A CN110467358 A CN 110467358A
- Authority
- CN
- China
- Prior art keywords
- nanometer sheet
- rhenium disulfide
- hydrogen reaction
- evolving hydrogen
- disulfide nanometer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
- C03C17/3429—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating
- C03C17/3464—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating comprising a chalcogenide
- C03C17/347—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating comprising a chalcogenide comprising a sulfide or oxysulfide
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/24—Doped oxides
- C03C2217/241—Doped oxides with halides
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/28—Other inorganic materials
- C03C2217/287—Chalcogenides
- C03C2217/288—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/71—Photocatalytic coatings
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/15—Deposition methods from the vapour phase
- C03C2218/152—Deposition methods from the vapour phase by cvd
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Combustion & Propulsion (AREA)
- Inorganic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The invention belongs to technical field of nano material, disclose a kind of rhenium disulfide nanometer sheet and its preparation method and application for evolving hydrogen reaction.The rhenium disulfide nanometer sheet is using Re-Te eutectic and sulphur powder as raw material, FTO electro-conductive glass is substrate, using chemical vapour deposition technique, under an inert atmosphere, Re-Te eutectic is built among quartz ampoule, is placed in flat-temperature zone I and is warming up to 450~500 DEG C of heat preservations, sulphur powder is placed in the carrier gas upstream end of same quartz ampoule, it is placed in flat-temperature zone II and is warming up to 120~170 DEG C of heat preservations, make Re steam and sulphur steam reaction in Re-Te eutectic, anisotropic growth is made on FTO substrate.ReS of the invention2Nanometer sheet setting is arranged on FTO substrate, ReS2There is a large amount of electro-chemical activity position substrate in conjunction with FTO at nanometer sheet edge, can be used as the electrode of evolving hydrogen reaction, is expected to be applied to catalyzing manufacturing of hydrogen field.
Description
Technical field
The invention belongs to technical field of nano material, receive more particularly, to a kind of rhenium disulfide for evolving hydrogen reaction
Rice piece and its preparation method and application.
Background technique
In recent years, people start to notice Transition-metal dichalcogenide (TMDC) two-dimensional material, these materials are by two dimension
Molecular layer is stacked by faint Interaction between layers, and interlayer is interacted by weak Van der Waals force, is easy shape
At the very thin laminated structure of thickness.TMDC two-dimensional material also has high carrier mobility, and chemical stability is good, photosensitivity and
The features such as mechanical flexibility.In addition, it has also been found that TMDC material has the application potential in catalyst field, such as electrochemical catalysis
Hydrogen manufacturing, photocatalysis hydrogen production etc..Two-dimentional ReS2As a member of TMDC material family, there are wide direct band gap, and special 1T phase
Structure reduces interlayer coupling, keeps band gap very unobvious with the variation of the number of plies, and no matter ReS2How much is the number of plies, is all straight
Tape splicing gap semiconductor, this and other TMDC two-dimensional material properties are distinguished by number of plies modulation, and two dimension ReS2It is special also to show
In-plane anisotropy.As general TMDC material, ReS2There is electro-chemical activity position at the edge of laminated structure, because
This, two-dimentional ReS2It is expected to apply to electrochemical catalysis field.But the two dimension that current chemical vapour deposition technique (CVD) prepares
ReS2Nanometer sheet is parallel to substrate more, and only the marginal position on nanometer sheet periphery can be exposed, and intensively erect arrangement
ReS2Nanometer sheet can expose a large amount of marginal position.ReS is erect although also having been reported that2The preparation of nanometer sheet, but it is used
Substrate and non-conductive, transparent (such as SiO2Substrate), limit its application in terms of photoelectrocatalysis liberation of hydrogen.Therefore, it is necessary to develop
A kind of new process carrys out the ReS of the preparation setting arrangement on the substrate of conductive, transparent2Nanometer sheet.
Summary of the invention
In order to solve above-mentioned the shortcomings of the prior art and disadvantage, primary and foremost purpose of the present invention is that providing one kind can be used for
The rhenium disulfide nanometer sheet of evolving hydrogen reaction.
Another object of the present invention is to provide the preparation methods of the above-mentioned rhenium disulfide nanometer sheet that can be used for evolving hydrogen reaction.
A further object of the present invention is to provide the applications of the above-mentioned rhenium disulfide nanometer sheet that can be used for evolving hydrogen reaction.
The purpose of the present invention is realized by following technical proposals:
A kind of rhenium disulfide nanometer sheet for evolving hydrogen reaction, the rhenium disulfide nanometer sheet are with Re-Te eutectic
It is raw material with sulphur powder, FTO electro-conductive glass is that under protective atmosphere, Re-Te congruent melting is closed using chemical vapour deposition technique for substrate
Gold is built among quartz ampoule, is placed in flat-temperature zone I and is warming up to 450~500 DEG C of heat preservations, sulphur powder is placed in the load of same quartz ampoule
Gas upstream end is placed in flat-temperature zone II and is warming up to 120~170 DEG C of heat preservations, keeps Re steam in Re-Te eutectic and sulphur steam anti-
It answers, anisotropic growth is made on FTO substrate, and the rhenium disulfide nanometer sheet setting is arranged on FTO substrate.
Preferably, the protective atmosphere is argon gas, nitrogen or helium.
Preferably, the rate that the flat-temperature zone I heats up is 10~20 DEG C/min, and the rate that the flat-temperature zone II heats up is 30
~40 DEG C/min.
Preferably, the time of the heat preservation of the flat-temperature zone I and II is 30~45min.
11. the rhenium disulfide nanometer sheet according to claim 1 for evolving hydrogen reaction, which is characterized in that the Re-
The mass ratio of Re:Te is 1:(1~4 in Te eutectic).
Preferably, the molar ratio of the Re-Te eutectic and sulphur is 1:(2.1~3).
The preparation method of the rhenium disulfide nanometer sheet for evolving hydrogen reaction, comprises the following specific steps that:
S1. it weighs Re and Te to be fitted into corundum boat and uniformly mix, is placed in quartz ampoule, is seated in the center of CVD furnace
FTO electro-conductive glass face down is placed on corundum boat by I middle section of flat-temperature zone；
S2. sulphur powder is packed into quartz boat, is placed on the upstream end of CVD furnace quartz ampoule, be seated in the flat-temperature zone II of CVD furnace；
S3. protective atmosphere is passed through sufficiently to substitute the air in CVD boiler tube, then adjusts carrier gas flux；CVD furnace center is permanent
Warm area I is warming up to 450~500 DEG C of heat preservations, and flat-temperature zone II is begun to warm up when flat-temperature zone I reaches 400 DEG C, is warming up to 120~170
DEG C heat preservation, the rhenium disulfide nanometer sheet for evolving hydrogen reaction is made in subsequent cooled to room temperature.
Preferably, the area of FTO Conducting Glass described in step S1 is (1.5~2) cm × 2cm.
Preferably, the time of heat preservation described in step S3 is 30~45min.
Application in the rhenium disulfide nanometer sheet catalyzing manufacturing of hydrogen field for evolving hydrogen reaction.
The principle of the present invention: Re-Te eutectic reduces the fusing point of Re, can melt at 450 DEG C, evaporate Re
Steam, sulphur is warming up to 150 DEG C of fusings by the control of another flat-temperature zone and evaporates S steam, in the transport process of inert carrier gas
Two kinds of reaction sources meet reaction, and growth is deposited on FTO glass.It is rough due to FTO glass surface, it provides not only perhaps
More nucleation sites, and for the ReS with anisotropic low symmetrical 1T structure2, very easy hair on a rough surface
Life face outgrowth finally obtains intensive setting arrangement ReS2Nanometer sheet, these nanometer sheets can expose a large amount of margin location
It sets.
Compared with prior art, the invention has the following advantages:
1. provided by the present invention for the ReS of evolving hydrogen reaction2Nanometer sheet is to erect to be arranged in substrate surface, can be exposed
Out largely with the marginal position of catalytic activity.
2. the ReS that the present invention obtains2Nanometer sheet is directly grown on FTO transparent conductive glass, can be directly as liberation of hydrogen
The electrode of reaction, convenient for being used in photoelectrocatalysis field.
Detailed description of the invention
Fig. 1 is experimental provision used in rhenium disulfide nanometer sheet of the preparation for evolving hydrogen reaction in embodiment 1.
Fig. 2 is the electron scanning micrograph of the rhenium disulfide nanometer sheet for evolving hydrogen reaction prepared in embodiment 1.
Fig. 3 is the Raman spectrogram of the rhenium disulfide nanometer sheet for evolving hydrogen reaction prepared in embodiment 1.
Fig. 4 is the X ray diffracting spectrum of the rhenium disulfide nanometer sheet for evolving hydrogen reaction prepared in embodiment 1.
Fig. 5 is to have the FTO electro-conductive glass of rhenium disulfide nanometer sheet to be used as photochemical catalyst electrode growth in embodiment 1, in light
The current versus time curve measured under pulse irradiation.
Fig. 6 is to measure when having the FTO electro-conductive glass of rhenium disulfide nanometer sheet to be used as photochemical catalyst electrode growth in embodiment 1
Linear sweep voltammetry curve.
Fig. 7 is that the electronic scanner microscope of the rhenium disulfide nanometer sheet that can be used for evolving hydrogen reaction prepared in embodiment 2 shines
Piece.
Fig. 8 is the Raman spectrogram of the rhenium disulfide nanometer sheet that can be used for evolving hydrogen reaction prepared in embodiment 2.
Fig. 9 is that the electronic scanner microscope of the rhenium disulfide nanometer sheet that can be used for evolving hydrogen reaction prepared in embodiment 3 shines
Piece.
Figure 10 is the Raman spectrogram of the rhenium disulfide nanometer sheet that can be used for evolving hydrogen reaction prepared in embodiment 3.
Specific embodiment
The contents of the present invention are further illustrated combined with specific embodiments below, but should not be construed as limiting the invention.
Unless otherwise specified, the conventional means that technological means used in embodiment is well known to those skilled in the art.Except non-specifically
Illustrate, reagent that the present invention uses, method and apparatus is the art conventional reagents, method and apparatus.
The embodiment of the present invention is used as carrier gas using argon gas (Guangzhou English Lay, 99.999%)；Using Re powder (Aladdin,
99.99%), Te powder (Aladdin, 99.99%), sublimed sulfur (Chengdu Bo Ruite chemical technology Co., Ltd, 99.95%) are made
For reactant.Select FTO electro-conductive glass as growth substrates.Chemical vapor deposition (CVD) system used is Henan Nuo Badi
The NBD-01200-50IT high temperature process furnances of material Science and Technology Ltd. production.Using scanning electron microscope (SEM, S-
3400N, Hitachi) morphology analysis is carried out to sample；Using micro- Confocal laser-scanning microscopy instrument (FinderVista, the Chinese of standing upright
Light) and X-ray diffractometer (*/D8ADVANCE, German Bruker) to sample carry out material phase analysis, the optical maser wavelength of Raman spectrum
Laser light source for 532nm, optical power 10W, time of integration 3s, X-ray diffractometer uses copper target, wavelength 0.15418nm.
Experimental provision of the invention is as shown in Figure 1, using chemical gas-phase deposition system, including quartz ampoule, quartz boat and just
Yu Zhou.
Embodiment 1
1. preparation:
(1) Te for weighing the Re and 200mg of 50mg is packed into corundum boat and uniformly mixes, and is placed in warm area I.
(2) weigh 0.6g sulphur powder be packed into quartz boat, be placed on CVD furnace upstream end sulphur powder position installation heating tape with
Temperature control individually is carried out to sulphur, temperature controlled zone is warm area II.
(3) the FTO electro-conductive glass face down cleaned up is placed on corundum boat.
(4) 200sccm high-purity argon gas 4h is passed through sufficiently to substitute the air in CVD boiler tube, and then adjusting carrier gas flux is
50sccm。
(5) CVD furnace temperature area I is warming up to 475 DEG C with the rate of 15 DEG C/min, and constant temperature 45min, sulphur is with heating tape temperature control, In
Warm area I is begun to warm up when reaching 475 DEG C, is warming up to 150 DEG C with the rate of 30 DEG C/min, constant temperature 45min is then naturally cooled to
Room temperature, reaction terminate, and anisotropic growth, which is made, on FTO substrate erects arrangement rhenium disulfide nanometer sheet.
2. performance test: Fig. 2 is the electronics of the rhenium disulfide nanometer sheet that can be used for evolving hydrogen reaction prepared in the present embodiment
Flying-spot microscope photo.As can be known from Fig. 2, there is a large amount of nanometer sheet to erect arrangement, densely grow on substrate.Fig. 3 is this
The Raman spectrogram of the rhenium disulfide nanometer sheet that can be used for evolving hydrogen reaction of embodiment preparation, can obviously observe ReS2Spy
Peak is levied, illustrates the ReS for generating highly crystalline2.Fig. 4 is that the rhenium disulfide that can be used for evolving hydrogen reaction prepared in embodiment 1 is received
The X ray diffracting spectrum of rice piece, peak position correspond to ReS2(001), (100), (101), (- 1-11), (02-1), (121) crystal face.
Fig. 5 is to have the FTO electro-conductive glass of rhenium disulfide nanometer sheet to be used as photochemical catalyst electrode growth in embodiment 1, in optical pulse irradiation
Under the current versus time curve that measures.Fig. 6 is to have the FTO electro-conductive glass of rhenium disulfide nanometer sheet to be used as light growth in embodiment 1
The linear sweep voltammetry curve measured when catalysis electrode.Wherein reference electrode is silver silver chloride electrode, and auxiliary electrode is platinized platinum electricity
Pole, working electrode are the FTO electro-conductive glass manufactured in the present embodiment with rhenium disulfide nanometer sheet, and electrolyte is 0.5M's
Na2SO4Solution.Fig. 5,6 show ReS obtained2Nanometer sheet has certain photocatalysis performance.Test result shows the present embodiment
It obtains and is grown on the crystalline quality of FTO electro-conductive glass and preferably erects the ReS of arrangement2Nanometer sheet, and can be used for photocatalysis system
Hydrogen.
Embodiment 2
1. preparation:
(1) Te for weighing the Re and 200mg of 50mg is packed into corundum boat and uniformly mixes, and is placed in warm area I.
(2) weigh 0.6g sulphur powder be packed into quartz boat, be placed on CVD furnace upstream end sulphur powder position installation heating tape with
Temperature control individually is carried out to sulphur, temperature controlled zone is warm area II.
(3) the FTO electro-conductive glass face down cleaned up is placed on corundum boat.
(4) 200sccm high-purity argon gas 4h is passed through sufficiently to substitute the air in CVD boiler tube, and then adjusting carrier gas flux is
50sccm。
(5) CVD furnace temperature area I is warming up to 500 DEG C with the rate of 10 DEG C/min, and constant temperature 30min, sulphur is with heating tape temperature control, In
Warm area I is begun to warm up when reaching 500 DEG C, is warming up to 170 DEG C with the rate of 30 DEG C/min, constant temperature 30min is then naturally cooled to
Room temperature, reaction terminate, and anisotropic growth, which is made, on FTO substrate erects arrangement rhenium disulfide nanometer sheet.
2. performance test: Fig. 7 is the electronics of the rhenium disulfide nanometer sheet that can be used for evolving hydrogen reaction prepared in the present embodiment
Flying-spot microscope photo.As can be known from Fig. 7, there is a large amount of nanometer sheet to erect arrangement, densely grow on substrate.Fig. 8 is this
The Raman spectrogram of the rhenium disulfide nanometer sheet that can be used for evolving hydrogen reaction of embodiment preparation, can obviously observe ReS2Spy
Peak is levied, illustrates the ReS for generating highly crystalline2。
Embodiment 3
1. preparation:
(1) Te for weighing the Re and 200mg of 50mg is packed into corundum boat and uniformly mixes, and is placed in warm area I.
(2) weigh 0.6g sulphur powder be packed into quartz boat, be placed on CVD furnace upstream end sulphur powder position installation heating tape with
Temperature control individually is carried out to sulphur, temperature controlled zone is warm area II.
(3) the FTO electro-conductive glass face down cleaned up is placed on corundum boat.
(4) 200sccm high-purity argon gas 4h is passed through sufficiently to substitute the air in CVD boiler tube, and then adjusting carrier gas flux is
50sccm。
(5) CVD furnace temperature area I is warming up to 450 DEG C with the rate of 20 DEG C/min, and constant temperature 45min, sulphur is with heating tape temperature control, In
Warm area I is begun to warm up when reaching 450 DEG C, is warming up to 120 DEG C with the rate of 40 DEG C/min, constant temperature 45min is then naturally cooled to
Room temperature, reaction terminate, and anisotropic growth, which is made, on FTO substrate erects arrangement rhenium disulfide nanometer sheet.
2. performance test: Fig. 9 is the electronics of the rhenium disulfide nanometer sheet that can be used for evolving hydrogen reaction prepared in the present embodiment
Flying-spot microscope photo.As can be known from Fig. 7, nanometer sheet setting is arranged in FTO substrate surface, compared to embodiment 1,2, this reality
The nanometer sheet density for applying example growth is slightly lower.Figure 10 is the rhenium disulfide nanometer sheet manufactured in the present embodiment that can be used for evolving hydrogen reaction
Raman spectrogram can obviously observe ReS2Characteristic peak, illustrate the ReS for having similarly generated highly crystalline2。
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by change, modification, substitution, combination and simplify,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of rhenium disulfide nanometer sheet for evolving hydrogen reaction, which is characterized in that the rhenium disulfide nanometer sheet is with Re-Te
Eutectic and sulphur powder are raw material, and FTO electro-conductive glass is substrate, using chemical vapour deposition technique, under protective atmosphere, by Re-
Te eutectic is built among quartz ampoule, is placed in flat-temperature zone I and is warming up to 450~500 DEG C of heat preservations, sulphur powder is placed in same stone
The carrier gas upstream end of English pipe is placed in flat-temperature zone II and is warming up to 120~170 DEG C of heat preservations, make Re steam in Re-Te eutectic and
Sulphur steam reaction, anisotropic growth is made on FTO substrate, and the rhenium disulfide nanometer sheet setting is arranged on FTO substrate.
2. the rhenium disulfide nanometer sheet according to claim 1 for evolving hydrogen reaction, which is characterized in that the protective atmosphere
For argon gas, nitrogen or helium.
3. the rhenium disulfide nanometer sheet according to claim 1 for evolving hydrogen reaction, which is characterized in that the flat-temperature zone I
The rate of heating is 10~20 DEG C/min, and the rate that the flat-temperature zone II heats up is 30~40 DEG C/min.
4. the rhenium disulfide nanometer sheet according to claim 1 for evolving hydrogen reaction, which is characterized in that the flat-temperature zone I
Time with II heat preservation is 30~45min.
5. the rhenium disulfide nanometer sheet according to claim 1 for evolving hydrogen reaction, which is characterized in that the Re-Te is total
The mass ratio of Re:Te is 1:(1~4 in fusion gold).
6. the rhenium disulfide nanometer sheet according to claim 1 for evolving hydrogen reaction, which is characterized in that the Re-Te is total
The molar ratio of fusion gold and sulphur is 1:(2.1~3).
7. the preparation method of the rhenium disulfide nanometer sheet according to claim 1-6 for evolving hydrogen reaction, special
Sign is, comprises the following specific steps that:
S1. it weighs Re and Te to be fitted into corundum boat and uniformly mix, is placed in quartz ampoule, is seated in the center constant temperature of CVD furnace
FTO electro-conductive glass face down is placed on corundum boat by I middle section of area；
S2. sulphur powder is packed into quartz boat, is placed on the upstream end of CVD furnace quartz ampoule, be seated in the flat-temperature zone II of CVD furnace；
S3. protective atmosphere is passed through sufficiently to substitute the air in CVD boiler tube, then adjusts carrier gas flux；CVD furnace center flat-temperature zone
I is warming up to 450~500 DEG C of heat preservations, and flat-temperature zone II is begun to warm up when flat-temperature zone I reaches 400 DEG C, is warming up to 120~170 DEG C of guarantors
The rhenium disulfide nanometer sheet for evolving hydrogen reaction is made in temperature, subsequent cooled to room temperature.
8. the preparation method of the rhenium disulfide nanometer sheet according to claim 7 for evolving hydrogen reaction, which is characterized in that step
The area of FTO Conducting Glass described in rapid S1 is (1.5~2) cm × 2cm.
9. the preparation method of the rhenium disulfide nanometer sheet according to claim 7 for evolving hydrogen reaction, which is characterized in that step
The time of heat preservation described in rapid S3 is 30~45min.
10. answering in the rhenium disulfide nanometer sheet catalyzing manufacturing of hydrogen field described in any one of claims 1-6 for evolving hydrogen reaction
With.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910616451.0A CN110467358A (en) | 2019-07-09 | 2019-07-09 | A kind of rhenium disulfide nanometer sheet and its preparation method and application for evolving hydrogen reaction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910616451.0A CN110467358A (en) | 2019-07-09 | 2019-07-09 | A kind of rhenium disulfide nanometer sheet and its preparation method and application for evolving hydrogen reaction |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110467358A true CN110467358A (en) | 2019-11-19 |
Family
ID=68507185
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910616451.0A Pending CN110467358A (en) | 2019-07-09 | 2019-07-09 | A kind of rhenium disulfide nanometer sheet and its preparation method and application for evolving hydrogen reaction |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110467358A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114715948A (en) * | 2022-06-10 | 2022-07-08 | 中国人民解放军国防科技大学 | Method for preparing single-layer rhenium disulfide by chemical vapor deposition |
| CN115627497A (en) * | 2022-12-21 | 2023-01-20 | 广东工业大学 | Preparation method and application of NiFeSe/NF catalyst |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105236762A (en) * | 2015-09-17 | 2016-01-13 | 电子科技大学 | Chemical vapor deposition preparation method for vertically-arranged hafnium disulfide nano-sheet |
| CN105821383A (en) * | 2016-06-07 | 2016-08-03 | 电子科技大学 | Method for preparing rhenium disulfide film |
| CN105839072A (en) * | 2016-04-19 | 2016-08-10 | 陕西师范大学 | Method for preparing rhenium disulfide thin film through chemical vapor deposition |
| CN107024516A (en) * | 2017-02-24 | 2017-08-08 | 西安交通大学 | A kind of rhenium disulfide nano-chip arrays film adsorbed sensor and preparation method |
| 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 |
| CN109023295A (en) * | 2018-07-16 | 2018-12-18 | 广东工业大学 | A kind of rhenium disulfide film of large-area two-dimensional and its preparation method and application |
-
2019
- 2019-07-09 CN CN201910616451.0A patent/CN110467358A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105236762A (en) * | 2015-09-17 | 2016-01-13 | 电子科技大学 | Chemical vapor deposition preparation method for vertically-arranged hafnium disulfide nano-sheet |
| CN105839072A (en) * | 2016-04-19 | 2016-08-10 | 陕西师范大学 | Method for preparing rhenium disulfide thin film through chemical vapor deposition |
| CN105821383A (en) * | 2016-06-07 | 2016-08-03 | 电子科技大学 | Method for preparing rhenium disulfide film |
| CN107024516A (en) * | 2017-02-24 | 2017-08-08 | 西安交通大学 | A kind of rhenium disulfide nano-chip arrays film adsorbed sensor and preparation method |
| 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 |
| CN109023295A (en) * | 2018-07-16 | 2018-12-18 | 广东工业大学 | A kind of rhenium disulfide film of large-area two-dimensional and its preparation method and application |
Non-Patent Citations (2)
| Title |
|---|
| CUI ET AL.: "《Tellurium-Assisted Epitaxial Growth of Large-Area, Highly Crystalline ReS2 Atomic Layers on Mica Substrate》", 《ADVANCED MATERIALS》 * |
| 鲁逸人: "《镉系纳米材料的气相合成、结构和性能研究》", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114715948A (en) * | 2022-06-10 | 2022-07-08 | 中国人民解放军国防科技大学 | Method for preparing single-layer rhenium disulfide by chemical vapor deposition |
| CN115627497A (en) * | 2022-12-21 | 2023-01-20 | 广东工业大学 | Preparation method and application of NiFeSe/NF catalyst |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Li et al. | Large-area highly-oriented SiC nanowire arrays: synthesis, Raman, and photoluminescence properties | |
| Uosaki et al. | Preparation of a highly ordered Au (111) phase on a polycrystalline gold substrate by vacuum deposition and its characterization by XRD, GISXRD, STM/AFM, and electrochemical measurements | |
| CN110467358A (en) | A kind of rhenium disulfide nanometer sheet and its preparation method and application for evolving hydrogen reaction | |
| Pal et al. | Switching of ferroelectric liquid crystal doped with cetyltrimethylammonium bromide-assisted CdS nanostructures | |
| JP2013166692A (en) | Method for producing substrate with conductive diamond film formed thereon | |
| KR20090065472A (en) | Deposition apparatus and deposition method | |
| Wang et al. | Ultra-long high quality catalyst-free WO3 nanowires for fabricating high-performance visible photodetectors | |
| Salman et al. | Nanocrystalline ZnO film grown on porous silicon layer by radio frequency sputtering system | |
| CN109023295A (en) | A kind of rhenium disulfide film of large-area two-dimensional and its preparation method and application | |
| Wang et al. | Ultrafast nucleation and growth of high-quality monolayer MoSe2 crystals via vapor-liquid-solid mechanism | |
| Kang et al. | Large scale growth of vertically standing MoS2 flakes on 2D nanosheet using organic promoter | |
| CN109437124A (en) | A method of synthesis single layer Transition-metal dichalcogenide | |
| Shet et al. | Effects of substrate temperature and RF power on the formation of aligned nanorods in ZnO thin films | |
| JP7036448B2 (en) | Graphene containing heteroatoms | |
| Xu et al. | Self-assembled catalyst growth and optical properties of single-crystalline ZnGa2O4 nanowires | |
| CN113186590B (en) | Preparation method of centimeter-level molybdenum trioxide single crystal | |
| Guo et al. | Growth and mechanism of MoS2 nanoflowers with ultrathin nanosheets | |
| EP0371145B1 (en) | Process for vapor-phase synthesis of diamond | |
| Shang et al. | Growth behavior of β-Ga2O3 nanowires synthesized by chemical vapor deposition | |
| Wan et al. | Synthesis and characterization of high voltage electrodeposited phosphorus doped DLC films | |
| Fritzsche et al. | Atmospheric pressure metal organic chemical vapor deposition of thin germanium films | |
| Zhang et al. | Catalyst-assisted heteroepitaxial strategy for highly ordered β-Ga2O3 nanoarrays and their optical property investigation | |
| Hao et al. | Dy3+ Doped All‐Inorganic Perovskite Nanocrystals Glass toward High‐Performance and High‐Stability Silicon Photodetectors | |
| Khandpekar et al. | Growth, structural, optical and electrical behavior of glycine potassium nitrate (GPN) crystal with non-linear optical response | |
| JP3640716B2 (en) | Inorganic material in which CdS ultrafine crystals are present, method for producing the same, and photoelectrochemical device using the same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20191119 |