CN110629195A - Method for constructing semiconductor and metal sulfide heterogeneous electrode by chemical vapor deposition method - Google Patents
Method for constructing semiconductor and metal sulfide heterogeneous electrode by chemical vapor deposition method Download PDFInfo
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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
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- 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
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- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- C25B1/55—Photoelectrolysis
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- 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
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention relates to a method for constructing a semiconductor and metal sulfide heterogeneous electrode by a chemical vapor deposition method, which comprises the following steps: (1) cleaning a semiconductor as a substrate; (2) taking metal oxide powder and sulfur powder; (3) the semiconductor substrate was placed on a ceramic boat containing a metal oxide, and the ceramic boat was placed in the middle of a vacuum tube furnace, and then the ceramic boat containing sulfur powder was placed 15cm upstream from the middle of the vacuum tube furnace. (4) The pressure in the quartz tube of the vacuum tube furnace was evacuated to 7.5X 10 by a vacuum pump‑2Torr was used and the pressure was again increased to a normal pressure with a flow of 200sccm of high purity nitrogen gas, and this was repeated three times and the flow of high purity nitrogen gas was adjusted to 50sccm and maintain. (5) And editing a temperature control program of the vacuum tube furnace. (6) After the vapor deposition process is finished, after the vacuum tube furnace is naturally cooled to the room temperature, a heterogeneous composite sample of the semiconductor substrate supported metal vulcanized nanosheet array can be obtained. The preparation process has low cost and high efficiency.
Description
Technical Field
The invention relates to a method for constructing a semiconductor and metal sulfide heterogeneous electrode by a chemical vapor deposition method, belonging to the field of nano functional materials.
Background
Due to the large-scale use of fossil fuels, there are increasingly serious environmental problems and energy crisis, which have prompted people to search for new clean energy sources. Hydrogen is considered an ideal clean energy source that is expected to replace fossil fuels. The photoelectrochemical cell water splitting technology can effectively convert renewable solar energy into a clean hydrogen energy source. At present, many semiconductors (e.g. Si, TiO)2、ZnO、CuO、Fe2O3Etc.) exhibit the potential to collect photogenerated carriers and to stimulate hydrogen or oxygen evolution reactions, but most semiconductors suffer from insufficient surface catalytic activity. In recent years, two-dimensional transition metal sulfides are widely researched in the field of electrocatalytic hydrogen production due to the advantages of excellent active sites at the edges, stable chemical properties, abundant resources, low price and the like. In view of this, the surface of the semiconductor photoelectrode is loaded with transition metal sulfide as a cocatalyst, and the method is a universal scheme for effectively improving the photoelectrochemistry hydrogen production efficiency. At present, metal sulfide powder is usually prepared into sol in a laboratory, and a spin coating process is adopted to prepare a film on the surface of a substrate, and the method has two defects that (1) a large amount of contact junction potential barriers exist among a cocatalyst, a semiconductor and cocatalyst particles, so that the transmission of charge carriers is hindered; (2) after the cocatalyst is accumulated to form a film, the effective active area contacted with the electrolyte and the incident light wave front is inevitably reduced, and the number of active sites of the cocatalyst is reduced. In view of the above two analyses, a new synthesis scheme is explored, the combination mode of the cocatalyst and the semiconductor and the microstructure of the cocatalyst are improved, and the catalysis-assisting function of the transition metal sulfide on the semiconductor photoelectric electrode can be improved.
The few-layer transition metal sulfide nanosheets have excellent electro-catalytic hydrogen evolution activity, and the hydrogen production efficiency of semiconductor photoelectrodes can be effectively improved by integrating the few-layer transition metal sulfide nanosheets on the surface of a photosensitive semiconductor. We disclose a universal method for growing metal sulfide nanosheets directly on a semiconductor electrode, the grown nanosheets being vertically arranged to form a three-dimensional porous array structure, having the following typical structural advantages: (1) the directly grown metal sulfide nanosheets are in close contact with a semiconductor, so that interface transmission of photon-generated carriers is facilitated; (2) preferentially exposing the surface of the catalyst to contact with the electrolyte, so as to ensure the high-efficiency operation of the catalytic reaction; (3) the three-dimensional porous structure increases scattering and absorption of incident light, and facilitates electrolyte permeation and gas product overflow.
Disclosure of Invention
The invention aims to solve the existing problems and provides a method for constructing a semiconductor and metal sulfide heterogeneous electrode by a chemical vapor deposition method, wherein the chemical vapor deposition method is used for growing metal sulfide nanosheets to prepare the semiconductor and metal sulfide heterogeneous photoelectrode.
The invention aims to realize the method for constructing the semiconductor and metal sulfide heterogeneous electrode by the chemical vapor deposition method, which is characterized by comprising the following steps of:
(1) cleaning a semiconductor substrate, respectively cleaning the semiconductor substrate for 20min by using acetone, ethanol and deionized water, thoroughly removing organic residues and impurities on the surface, and drying the semiconductor substrate by using nitrogen for later use;
(2) according to the molar ratio of metal elements to sulfur elements of 1: 200 weighing metal oxide powder and sulfur powder, and respectively placing the metal oxide powder and the sulfur powder in two ceramic boats;
(3) placing the cleaned semiconductor substrate on the ceramic boat filled with the metal oxide powder in the step (2), placing the ceramic boat filled with the metal oxide powder in the middle of a vacuum tube furnace, and then placing the ceramic boat filled with the sulfur powder in the step (2) at a position 15cm away from the middle upstream of the vacuum tube furnace;
(4) pumping the pressure in the quartz tube of the vacuum tube furnace to 7.5X 10-2Torr by using a vacuum pump, refilling the quartz tube furnace to a normal pressure state by using high-purity nitrogen at the flow rate of 200sccm, and adjusting the flow rate of the high-purity nitrogen to 50sccm and keeping the flow rate;
(5) editing a temperature control program of the vacuum tube furnace, wherein the temperature rising speed is 10 ℃/min, the temperature rises to 750 ℃ and 850 ℃, and the temperature is kept for 15 min;
(6) in a vacuum tube furnace, metal atoms thermally evaporated from metal oxide powder and sulfur atom steam thermally evaporated from sulfur powder are crystallized on a semiconductor substrate, after the vapor deposition process is finished, and after the vacuum tube furnace is naturally cooled to room temperature, a heterogeneous composite sample of a semiconductor substrate supported metal sulfide nanosheet array can be obtained, namely a semiconductor and metal sulfide heterogeneous electrode is obtained and can be directly used as a photoelectrochemical decomposition water electrode.
In the step (1), the semiconductor substrate is a sheet semiconductor of 1.5cm × 2 cm.
In the step (2), the width of the ceramic boat is 2 cm.
In the step (4), the pressure in the quartz tube of the vacuum tube furnace is pumped to 7.5X 10-2Torr by using a vacuum pump, and the quartz tube is refilled to a normal pressure state by using high-purity nitrogen at the flow rate of 200 sccm; such steps were repeated 3 times.
The invention has the following features and advantages:
1. the preparation process has low cost, high efficiency and easy control, and is suitable for batch production.
2. And (3) placing the semiconductor substrate on a ceramic boat, so that the metal sulfide nanosheets can vertically grow to form a three-dimensional nanosheet array structure with unique advantages.
3. And (4) filling nitrogen for multiple times in the step (4) to fully remove oxygen in the tube furnace, so that the metal sulfide nanosheets with high purity and high crystallinity can be grown.
4. The method for preparing the metal sulfide nanosheet array is suitable for various semiconductor substrates, and is a universal scheme for constructing a semiconductor and a metal sulfide heterogeneous electrode.
The two-dimensional transition metal sulfide has excellent hydrogen evolution activity, and the loading of the transition metal sulfide cocatalyst on the surface of the semiconductor photoelectrode is a universal scheme for effectively improving the photoelectrochemistry hydrogen production efficiency. In view of the above, the invention utilizes the chemical vapor deposition method to load the metal sulfide nanosheets on the surface of the semiconductor, and the loaded nanosheets vertically stand on the surface of the substrate to form an array structure, so that not only are active sites preferentially exposed, but also incident light scattering paths can be increased, and the electrolyte permeation and gas product overflow are facilitated. The nanosheet array prepared by the chemical vapor deposition method is an ideal structure for constructing a photoelectrochemical electrode.
Drawings
FIG. 1 shows the Si and the ReS obtained2Digital photos of the heterogeneous electrodes.
FIG. 2 is TiO2ReS grown on nanofiber substrates2Scanning electron microscopy of the nanosheet array.
FIG. 3 shows MoS grown on the surface of Si substrate2Scanning electron microscopy of the nanosheet array.
Detailed Description
The following examples are intended to further illustrate the invention.
Example 1
ReS2The nano-sheets are treated by ReO in a vacuum tube furnace through a chemical vapor deposition method3And one-step synthesis of ReS on Si substrate by using S powder as raw material2Nanosheets.
The specific experimental steps are as follows: firstly, preparing a piece of Si with the thickness of 1.5cm multiplied by 2cm, ultrasonically cleaning the Si with acetone, ethanol and deionized water for 20min respectively, and then cleaning the Si with BOE (buffered oxide etching solution) for 30 s. Then, the cleaned Si is placed in a chamber filled with ReO3The ceramic boat of powder was placed in the middle of a vacuum tube furnace, and then 500mgS of powder was weighed into another ceramic boat, and the ceramic boat was placed at the upstream 15cm from the middle of the vacuum tube furnace. Then, the pressure in the vacuum tube furnace was increased to 7.5X 10 by a vacuum pump-2Torr was added, and the atmosphere was refilled with high-purity nitrogen gas, and this was repeated three times, and finally the nitrogen gas flow rate was kept at 50sccm, and nitrogen gas was continuously introduced. Next, the temperature in the furnace was raised to 750 ℃ at a temperature raising rate of 10 ℃/min and continued at 750 ℃ for 15min, after which the furnace was allowed to cool naturally. After the furnace is cooled to room temperature, a large amount of ReS2The nano-sheet is formed on the surface of Si, and can be directly used as a photocathode.
FIG. 1 is a digital photograph of the prepared photoelectrode, wherein ReS can be seen2A dense black film is formed on the surface of the Si.
Example 2
ReS2The nano-sheets are treated by ReO in a vacuum tube furnace through a chemical vapor deposition method3And S powder as raw material in TiO2And (3) synthesizing on the substrate in one step. The specific experimental steps are as follows: weighing ReO35mg of S powder and 500mg of S powder, which are respectively placed in two ceramic boats. Taking 50mg TiO2Nanofibers in ReO3On the powder. Then, will be charged with ReO3And TiO2The ceramic boat of (1) was placed in the middle of a vacuum tube furnace, and the ceramic boat containing S powder was placed upstream 15cm from the middle of the vacuum tube furnace. Then, the pressure in the vacuum tube furnace was increased to 7.5X 10 by a vacuum pump-2Torr was added, and the atmosphere was refilled with high-purity nitrogen gas, and this was repeated three times, and finally, nitrogen gas was continuously introduced while maintaining a flow rate of 50 sccm. Next, the temperature in the furnace was raised to 750 ℃ at a temperature raising rate of 10 ℃/min and maintained at 750 ℃ for 15min, after which the furnace was allowed to cool naturally. After the vacuum tube furnace is cooled to room temperature, TiO2Large amount of ReS grows on the surface2The nano-sheet can be directly used as a photoelectrode.
(a), (b) of FIG. 2 clearly shows ReS2With nano-sheets vertically distributed in TiO2The surface of the fiber.
Example 3
MoS2The nano-sheets are subjected to MoO in a vacuum tube furnace by a chemical vapor deposition method3And S powder is taken as a raw material to be synthesized on the Si substrate in one step. The specific experimental steps are as follows: firstly, preparing a piece of Si with the thickness of 1.5cm multiplied by 2cm, ultrasonically cleaning the Si with acetone, ethanol and deionized water for 20min respectively, and then cleaning the Si with BOE (buffered oxide etching solution) for 30 s. Weighing 5mgMoO3Putting into a ceramic boat. Then, the cleaned p-Si is put in a container filled with MoO3A ceramic boat of powder and placing the ceramic boat in the middle of a vacuum tube furnace. 500mg of sulfur powder was weighed into another ceramic boat, and the ceramic boat was placed 15cm upstream from the middle of the vacuum tube furnace. Then, the pressure in the vacuum tube furnace was increased to 7.5X 10 by a vacuum pump-2Torr, refilling the pressure to normal pressure with high-purity nitrogen, repeating the operation for three times, and finally keeping the nitrogen flowNitrogen was continuously introduced at a flow rate of 50 sccm. Next, the temperature in the furnace was raised to 800 ℃ at a temperature rise rate of 10 ℃/min and maintained at 800 ℃ for 15 min. After the reaction is finished, the furnace is allowed to cool naturally. After the vacuum tube furnace is cooled to room temperature, a large amount of MoS grows on the surface of Si2The nano-sheet can be directly used as a photoelectric cathode.
FIG. 3 (a), (b) clearly shows MoS2Microstructure, MoS2The nano sheet array is uniformly distributed on the surface of the Si.
The hydrogen production efficiency of semiconductor photoelectrolysis water is mainly limited by low surface catalytic activity, and transition metal sulfide is loaded on the surface of a photoelectrode as a hydrogen evolution reaction catalyst, so that the surface catalytic activity is improved, and the method is an effective scheme for improving the efficiency of the semiconductor photochemical electrode. Conventional spin coating methods do not promote atomic contact between the catalyst and the semiconductor and the resulting particle film reduces the catalytically active surface. According to the invention, the metal sulfide is directly grown on the surface of the semiconductor by adopting a chemical vapor deposition method, so that the close contact of an interface is ensured, the three-dimensional porous nanosheet array is formed, the contact between the surface of the catalyst and an electrolyte is preferentially exposed, the scattering and absorption of incident light can be increased, the permeation of the electrolyte and the overflow of a gas product are facilitated, and the three-dimensional porous nanosheet array is an ideal structure for constructing a photoelectrochemical electrode.
Claims (4)
1. A method for constructing a semiconductor and metal sulfide heterogeneous electrode by a chemical vapor deposition method is characterized by comprising the following processes:
(1) cleaning a semiconductor substrate, respectively cleaning the semiconductor substrate for 20min by using acetone, ethanol and deionized water, thoroughly removing organic residues and impurities on the surface, and drying the semiconductor substrate by using nitrogen for later use;
(2) according to the molar ratio of metal elements to sulfur elements of 1: 200 weighing metal oxide powder and sulfur powder, and respectively placing the metal oxide powder and the sulfur powder in two ceramic boats;
(3) placing the cleaned semiconductor substrate on the ceramic boat filled with the metal oxide powder in the step (2), placing the ceramic boat filled with the metal oxide powder in the middle of a vacuum tube furnace, and then placing the ceramic boat filled with the sulfur powder in the step (2) at a position 15cm away from the middle upstream of the vacuum tube furnace;
(4) pumping the pressure in the quartz tube of the vacuum tube furnace to 7.5X 10-2Torr by using a vacuum pump, refilling the quartz tube furnace to a normal pressure state by using high-purity nitrogen at the flow rate of 200sccm, and adjusting the flow rate of the high-purity nitrogen to 50sccm and keeping the flow rate;
(5) editing a temperature control program of the vacuum tube furnace, wherein the temperature rising speed is 10 ℃/min, the temperature rises to 750 ℃ and 850 ℃, and the temperature is kept for 15 min;
(6) in a vacuum tube furnace, metal atoms thermally evaporated from metal oxide powder and sulfur atom steam thermally evaporated from sulfur powder are crystallized on a semiconductor substrate, after the vapor deposition process is finished, and after the vacuum tube furnace is naturally cooled to room temperature, a heterogeneous composite sample of a semiconductor substrate supported metal sulfide nanosheet array can be obtained, namely a semiconductor and metal sulfide heterogeneous electrode is obtained and can be directly used as a photoelectrochemical decomposition water electrode.
2. The method of claim 1, wherein in step (1), the semiconductor substrate is a 1.5cm x 2cm semiconductor wafer.
3. The method of claim 1, wherein in step (2), the ceramic boat has a width of 2 cm.
4. The method of claim 1, wherein in the step (4), the pressure in the quartz tube of the vacuum tube furnace is pumped to 7.5 x 10 "2 Torr by a vacuum pump, and the quartz tube is refilled with high purity nitrogen gas at a flow rate of 200sccm to the atmospheric pressure state; such steps were repeated 3 times.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112030184A (en) * | 2020-07-27 | 2020-12-04 | 南京航空航天大学 | Amorphous molybdenum sulfide film modified silicon photoelectric cathode and preparation method thereof |
| CN113666341A (en) * | 2021-08-24 | 2021-11-19 | 昆明理工大学 | Preparation method of chalcogenide tubular material |
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| CN113666341A (en) * | 2021-08-24 | 2021-11-19 | 昆明理工大学 | Preparation method of chalcogenide tubular material |
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Application publication date: 20191231 |
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