CN114214604A - Large-area nanotube film and preparation method thereof - Google Patents
Large-area nanotube film and preparation method thereof Download PDFInfo
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- CN114214604A CN114214604A CN202111470364.2A CN202111470364A CN114214604A CN 114214604 A CN114214604 A CN 114214604A CN 202111470364 A CN202111470364 A CN 202111470364A CN 114214604 A CN114214604 A CN 114214604A
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- 239000002071 nanotube Substances 0.000 title claims abstract description 73
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 41
- 239000000758 substrate Substances 0.000 claims abstract description 39
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 33
- 239000011888 foil Substances 0.000 claims abstract description 32
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000010937 tungsten Substances 0.000 claims abstract description 32
- 239000000843 powder Substances 0.000 claims abstract description 18
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000010453 quartz Substances 0.000 claims abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 10
- 229910052798 chalcogen Inorganic materials 0.000 claims abstract description 6
- 150000001787 chalcogens Chemical class 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 125000004354 sulfur functional group Chemical group 0.000 claims abstract description 5
- 229910052717 sulfur Inorganic materials 0.000 claims description 7
- 150000004770 chalcogenides Chemical class 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- VVRQVWSVLMGPRN-UHFFFAOYSA-N oxotungsten Chemical compound [W]=O VVRQVWSVLMGPRN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052711 selenium Inorganic materials 0.000 claims description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 3
- 239000011593 sulfur Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 229910003090 WSe2 Inorganic materials 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 241000282414 Homo sapiens Species 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000010411 electrocatalyst Substances 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- GJWAPAVRQYYSTK-UHFFFAOYSA-N [(dimethyl-$l^{3}-silanyl)amino]-dimethylsilicon Chemical compound C[Si](C)N[Si](C)C GJWAPAVRQYYSTK-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/305—Sulfides, selenides, or tellurides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
Abstract
The invention provides a large-area nanotube film and a preparation method thereof, wherein the film is a small-layer WY with an open top and filled with W oxide2An aligned nanotube film, wherein Y is a chalcogen; the nanotube film is prepared by the following method: placing tungsten foil, a substrate and sulfur group elementary substance powder into a quartz tube of a chemical vapor deposition system and vacuumizing, wherein the chemical vapor deposition system is provided with an infrared heating lamp, heating the tungsten foil to 850-900 ℃ by using the infrared heating lamp and keeping the temperature for 10-20min, and obtaining the few-layer WY with the top opening filled with W oxide through a one-step method by controlling the process of vacuumizing firstly and then naturally cooling after the reaction is finished2An aligned nanotube film. The invention adoptsPreparation of WY by infrared heating chemical vapor deposition2Compared with the traditional horizontal double-temperature zone/multi-temperature zone CVD, the oriented nanotube film has the advantages of simple operation, low cost, raw material saving, strong process controllability and the like.
Description
Technical Field
The invention relates to the technical field of preparation of one-dimensional nanotubes, in particular to a large-area nanotube film and a preparation method thereof.
Background
Non-renewable fossil fuels such as coal and petroleum make great contribution to the development of the human society, but also bring about increasingly serious problems of environmental pollution, energy crisis and the like. The exploration and research of renewable clean energy sources to replace the fossil energy sources widely applied at present are necessary ways to maintain the sustainable development of human beings. The hydrogen production by water electrolysis converts electric energy into chemical energy to be stored in hydrogen, and plays an important role in the future research of environment-friendly novel clean energy.
The preparation of a high-activity and stable electrocatalyst is a key problem for realizing high-yield and high-efficiency hydrogen production. For the water electrolysis hydrogen production technology, Pt, Ir, Ru oxides and the like show excellent catalytic effect, however, the catalysts are all based on noble metals and oxides thereof, and the low natural reserves and high cost thereof hinder the development pace of large-scale industrial application to a certain extent.
The transition metal sulfide TMDS nano material shows excellent catalytic effect in the field of hydrogen evolution by electrolyzing water, wherein high-activity edge sites have important contribution to hydrogen evolution. Therefore, the invention provides the preparation method of the TMDs nano material which comprises the edge sites, is simple and controllable to operate, has high yield and excellent catalytic effect, and has important significance.
Disclosure of Invention
The invention aims to provide a large-area nanotube film and a preparation method thereof, and aims to solve the problems that the existing electrocatalyst is high in cost, complex in preparation and difficult to apply on a large scale.
The technical scheme of the invention is as follows: a large-area nanotube film, the nanotube film is WY2An aligned nanotube film, wherein Y is a chalcogen; the nanotube film is prepared by the following method:
placing tungsten foil, substrate and sulfur group elementary substance powder into a quartz tube of a chemical vapor deposition system and vacuumizing, wherein the chemical vapor deposition system is provided with an infrared heating lamp, heating the tungsten foil to 850-900 ℃ by using the infrared heating lamp and keeping the temperature for 10-20min, and naturally cooling (keeping a vacuum state) after the reaction is finished to obtain the WY2An aligned nanotube film.
The WY2In the aligned nanotube film, Y is S or Se.
The WY2The oriented nanotube film is formed by opening at the top end and filling WY with tungsten oxide2A nanotube.
The substrate is a Si sheet or a W sheet, the shape of the substrate is square or round, and the size of the substrate is slightly smaller than that of the tungsten foil.
The tungsten foil is arranged above the substrate, and the sulfur family elementary substance powder is arranged at a position with a distance of 20-30 mm below the substrate.
The vacuum degree of the quartz tube is 5-10 Torr; the diameter of the light spot of the infrared heating lamp is adjustable; when the heating temperature of the tungsten foil is 850-900 ℃, the substrate temperature is 600-650 ℃, and the temperature of the chalcogenide elemental powder is 250-300 ℃.
A method for preparing large-area nanotube film, the nanotube film is WY2An aligned nanotube film, wherein Y is a chalcogen; the nanotube film is prepared by the following method:
placing tungsten foil, substrate and sulfur group elementary substance powder into a quartz tube of a chemical vapor deposition system and vacuumizing, wherein the chemical vapor deposition system is provided with an infrared heating lamp, heating the tungsten foil to 850-900 ℃ by using the infrared heating lamp and keeping the temperature for 10-20min, and naturally cooling (keeping a vacuum state) after the reaction is finished to obtain the WY2An aligned nanotube film.
The WY2In the oriented nanotube film, Y is S or Se; the WY2The oriented nanotube film is formed by opening at the top end and filling WY with tungsten oxide2A nanotube.
The substrate is a Si sheet or a W sheet, the shape of the substrate is square or round, and the size of the substrate is slightly smaller than that of the tungsten foil; the tungsten foil is arranged above the substrate, and the sulfur family elementary substance powder is arranged at a position with a distance of 20-30 mm below the substrate.
The vacuum degree of the quartz tube is 5-10 Torr; the diameter of the light spot of the infrared heating lamp is adjustable; when the heating temperature of the tungsten foil is 850-900 ℃, the substrate temperature is 600-650 ℃, and the temperature of the chalcogenide elemental powder is 250-300 ℃.
The invention adopts an infrared heating chemical vapor deposition method to prepare WY2Compared with the traditional horizontal double-temperature zone/multi-temperature zone CVD, the oriented nanotube film has the advantages of simple operation, low cost, raw material saving, strong process controllability and the like; also prepared by the invention2Aligned nanotube filmThe membrane is made of WO x Filled one-dimensional WX2The film has the advantages of few layers of oriented nanotube films, nanotube diameter of 50-100 nm, unsealed structure at the top end, good structural uniformity, simple operation and large-area controllable preparation.
Drawings
FIG. 1 shows the preparation of large area WSe prepared in example 1 on different substrates2Nanotube film.
FIG. 2 is the WSe prepared in example 12X-ray diffraction pattern of nanotubes.
FIG. 3 is a WSe prepared in example 12SEM image of nanotubes.
FIG. 4 is a WSe prepared in example 12TEM images of nanotubes.
FIG. 5 shows WS prepared in example 32X-ray diffraction pattern of nanotubes.
FIG. 6 shows WS prepared in example 32SEM image of nanotubes.
FIG. 7 shows WS prepared in example 32TEM images of nanotubes.
Detailed Description
The present invention is further illustrated by the following examples in which the procedures and methods not described in detail are conventional and well known in the art, and the starting materials or reagents used in the examples are commercially available, unless otherwise specified, and are commercially available.
Example 1
WSe2The preparation method of the oriented nanotube film comprises the following specific steps:
mixing tungsten foil and different substrates (2 x2 cm from left to right in sequence in FIG. 1)2 W substrate, 2X2 cm2Si substrate and 2 inch Si wafer substrate), elemental Se powder was placed in a quartz tube of an infrared heated chemical vapor deposition system and evacuated to 10 Torr.
Heating tungsten foil to 900 deg.C with infrared heating lamp (the spot diameter of the infrared heating lamp is 25 mm, and the spot size can be adjusted by heating lamp power), keeping at constant temperature for 15min, and naturally cooling to obtain W18O49Filled one-dimensional WSe2An aligned nanotube film. For the obtained one-dimensional WSe2The results of the oriented nanotube film characterization are shown in fig. 2-4 (similar spectra for different substrates).
Example 2
WSe2The preparation method of the oriented nanotube film comprises the following specific steps:
putting the tungsten foil, the substrate W sheet and the elementary substance Se powder into a quartz tube of an infrared heating chemical vapor deposition system, and vacuumizing to 5 Torr.
Heating tungsten foil to 850 deg.C with infrared heating lamp, maintaining at constant temperature for 20min, and naturally cooling to obtain W18O49Filled one-dimensional WSe2An aligned nanotube film. For the obtained one-dimensional WSe2Oriented nanotube films were characterized and had properties similar to those of the material obtained in example 1.
Example 3
WS (WS)2The preparation method of the oriented nanotube film comprises the following specific steps:
putting the tungsten foil, the substrate W sheet and the elemental S powder into a quartz tube of an infrared heating chemical vapor deposition system, and vacuumizing to 8 Torr.
Heating tungsten foil to 850 deg.C with infrared heating lamp, maintaining at constant temperature for 20min, and naturally cooling to obtain W18O49Filled one-dimensional WS2A nanotube film. For the obtained one-dimensional WS2The results of the characterization of the aligned nanotube film are shown in fig. 5 to 7.
Example 4
WS (WS)2The preparation method of the oriented nanotube film comprises the following specific steps:
putting the tungsten foil, the substrate W sheet and the elemental S powder into a quartz tube of an infrared heating chemical vapor deposition system, and vacuumizing to 8 Torr.
Heating tungsten foil to 880 deg.C with infrared heating lamp, maintaining at constant temperature for 15min, and naturally cooling to obtain W18O49Filled one-dimensional WS2A nanotube film. For the obtained one-dimensional WS2Oriented nanotube films were characterized and had properties similar to those of the material obtained in example 3.
Example 5
WS (WS)2The preparation method of the oriented nanotube film comprises the following specific steps:
putting the tungsten foil, the substrate W sheet and the elemental S powder into a quartz tube of an infrared heating chemical vapor deposition system, and vacuumizing to 8 Torr.
Heating tungsten foil to 900 deg.C with infrared heating lamp, maintaining at constant temperature for 10min, and naturally cooling to obtain W18O49Filled one-dimensional WS2A nanotube film. For the obtained one-dimensional WS2Oriented nanotube films were characterized and had properties similar to those of the material obtained in example 3.
Claims (10)
1. A large-area nanotube film, characterized in that the nanotube film is WY2An aligned nanotube film, wherein Y is a chalcogen; the nanotube film is prepared by the following method:
placing tungsten foil, substrate and sulfur group elementary substance powder into a quartz tube of a chemical vapor deposition system and vacuumizing, wherein the chemical vapor deposition system is provided with an infrared heating lamp, heating the tungsten foil to 850-900 ℃ by using the infrared heating lamp and keeping the temperature for 10-20min, and naturally cooling after the reaction is finished to obtain the WY2An aligned nanotube film.
2. The large area nanotube film of claim 1, wherein WY is2In the aligned nanotube film, Y is S or Se.
3. The large area nanotube film of claim 1, wherein WY is2The oriented nanotube film is formed by opening at the top end and filling WY with tungsten oxide2A nanotube.
4. The large area nanotube film of claim 1, wherein the substrate is a Si or W sheet, the substrate is square or circular in shape, and the substrate size is slightly smaller than the size of the tungsten foil.
5. The large area nanotube film of claim 1, wherein the tungsten foil is disposed over a substrate and the chalcogen powder is disposed below the substrate at a distance of 20-30 mm.
6. The large area nanotube film of claim 1, wherein the quartz tube vacuum is 5-10 Torr; the diameter of the light spot of the infrared heating lamp is adjustable; when the heating temperature of the tungsten foil is 850-900 ℃, the substrate temperature is 600-650 ℃, and the temperature of the chalcogenide elemental powder is 250-300 ℃.
7. The preparation method of the large-area nanotube film is characterized in that the nanotube film is WY2An aligned nanotube film, wherein Y is a chalcogen; the nanotube film is prepared by the following method:
placing tungsten foil, substrate and sulfur group elementary substance powder into a quartz tube of a chemical vapor deposition system and vacuumizing, wherein the chemical vapor deposition system is provided with an infrared heating lamp, heating the tungsten foil to 850-900 ℃ by using the infrared heating lamp and keeping the temperature for 10-20min, and naturally cooling after the reaction is finished to obtain the WY2An aligned nanotube film.
8. The method of claim 7, wherein WY is2In the oriented nanotube film, Y is S or Se; the WY2The oriented nanotube film is formed by opening at the top end and filling WY with tungsten oxide2A nanotube.
9. The preparation method according to claim 7, wherein the substrate is a Si sheet or a W sheet, the substrate is square or round, and the size of the substrate is slightly smaller than that of the tungsten foil; the tungsten foil is arranged above the substrate, and the sulfur family elementary substance powder is arranged at a position with a distance of 20-30 mm below the substrate.
10. The production method according to claim 7, wherein the degree of vacuum of the quartz tube is 5 to 10 Torr; the diameter of the light spot of the infrared heating lamp is adjustable; when the heating temperature of the tungsten foil is 850-900 ℃, the substrate temperature is 600-650 ℃, and the temperature of the chalcogenide elemental powder is 250-300 ℃.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5958358A (en) * | 1992-07-08 | 1999-09-28 | Yeda Research And Development Co., Ltd. | Oriented polycrystalline thin films of transition metal chalcogenides |
| US20170341935A1 (en) * | 2015-05-13 | 2017-11-30 | Shaanxi University Of Science & Technology | Porous hollow shell wo3/ws2 nanomaterial and method of preparing same |
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- 2021-12-03 CN CN202111470364.2A patent/CN114214604A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5958358A (en) * | 1992-07-08 | 1999-09-28 | Yeda Research And Development Co., Ltd. | Oriented polycrystalline thin films of transition metal chalcogenides |
| US20170341935A1 (en) * | 2015-05-13 | 2017-11-30 | Shaanxi University Of Science & Technology | Porous hollow shell wo3/ws2 nanomaterial and method of preparing same |
Non-Patent Citations (1)
| Title |
|---|
| 王天琦等: "WSe2纳米薄膜的制备及光电性能", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》, pages 020 - 36 * |
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