CN114657641A - Annealed Si-based InN nano-column heterojunction and preparation method and application thereof - Google Patents
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Abstract
The invention discloses an annealed Si-based InN nano-column heterojunction and a preparation method and application thereof. The preparation method comprisesThe method comprises the following steps: (1) growing an InN nano column on a Si substrate by adopting a molecular beam epitaxial growth process; (2) annealing the InN nano column obtained in the step (1) to obtain a Si-based InN nano column heterojunction; the annealing atmosphere is N2A sulfur atmosphere, an oxygen atmosphere, or a selenium atmosphere under protection. The InN nanorod heterojunction comprises a substrate and InN nanorods grown on the substrate, wherein the InN nanorods are annealed in different atmospheres to form the heterojunction. The Si-based InN nano-column heterojunction photoelectrode is prepared by a method with low cost and simple process. The heterojunction photoelectrode can be used for photoelectrocatalysis water decomposition hydrogen production, greatly improves the hydrogen production efficiency, and provides an effective strategy for large-scale hydrogen energy preparation by utilizing solar energy.
Description
Technical Field
The invention relates to the field of InN nano-columns, in particular to an annealed Si-based InN nano-column heterojunction and a preparation method and application thereof.
Background
Photoelectrochemical water splitting to produce hydrogen has shown great potential in addressing global energy crisis and environmental issues. The InN nano-column has a small band gap (0.65eV), and is suitable for the energy band position of water oxidation, so that the InN nano-column becomes an option of a photo-anode. In addition, the InN nano-column has an energy band position suitable for water redox reaction and a high surface area to volume ratio, so that the InN nano-column is expected to be used for efficient photoelectrochemical water decomposition. However, the problems of fast recombination of bulk and surface charges and slow oxidation kinetics of InN nanocolumns lead to the need for additional bias to facilitate charge transfer. Today, building semiconductor heterostructures to tune the energy band of the heterojunction is considered to be one of the most efficient methods to facilitate the separation of bulk and surface charges. Particularly, coupling semiconductors having excellent water oxidation or reduction ability to form a heterostructure can activate electrons and holes of two semiconductors, and can show unique advantages in water decomposition. Therefore, in order to realize efficient photoelectrochemical water splitting, the construction of a heterojunction based on InN nanopillars is crucial.
Chemical vapor deposition is a material preparation method with low cost and simple process, but no literature discloses that InN nano-columns are arranged in different atmospheres (N)2Sulfur atmosphere, oxygen atmosphere and selenium atmosphere under protection) to prepare the InN nano-column heterojunction, thereby realizing the high-efficiency photoelectrochemical water splitting photoelectrode based on the InN nano-column.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide an annealed Si-based InN nano-column heterojunction, a preparation method thereof and application thereof in photoelectrochemical water decomposition hydrogen production.
The purpose of the invention is realized by the following technical scheme.
A preparation method of an annealing treated Si-based InN nanorod heterojunction comprises the following steps:
(1) growing an InN nano column on a Si substrate by adopting a molecular beam epitaxial growth process;
(2) annealing the InN nano column obtained in the step (1) to obtain a Si-based InN nano column heterojunction; the annealing atmosphere is N2A sulfur atmosphere, an oxygen atmosphere, or a selenium atmosphere under protection.
Preferably, the annealing is carried out at 400-500 ℃ for 5-30 min.
Preferably, the annealing is annealing at 500 ℃ for 5 min.
Preferably, the density of the InN nano-columns is 150-200 mu m-2。
Preferably, the height of the InN nano-column is 150-500 nm, and the diameter of the InN nano-column is 60-100 nm.
Preferably, the growing of InN nano-pillars on a Si substrate includes the steps of:
adopting a molecular beam epitaxial growth process, controlling the temperature of the Si substrate to be 380-450 ℃, the rotating speed of the Si substrate to be 10r/min, and the equivalent pressure of the In beam to be 1 multiplied by 10-7～2.5×10-7The nitrogen flow is 1-3 sccm, the nitrogen plasma source power is 200-400W, the growth time is 1-5 h, and InN nano-columns grow on the Si substrate.
Preferably, the Si substrate is an n-type Si substrate, and the conductivity is <0.005 Ω.
The Si-based InN nano-column heterojunction prepared by the preparation method comprises a substrate and InN nano-columns grown on the substrate, wherein the InN nano-columns are annealed in different atmospheres to form the heterojunction. .
The Si-based InN nano-column heterojunction is applied to preparation of a photoelectrode.
Preferably, the preparation of the photoelectrode comprises the following steps:
and depositing a metal layer and the Si back of the Si-based InN nano-column heterojunction by electron beam evaporation to form ohmic contact, connecting the metal layer by a metal wire, and protecting the whole metal back by insulating epoxy resin.
Preferably, the metal layer is Ti/Au alloy, and the thickness is 20nm/80 nm.
The photoelectrode is applied to a photoelectrolysis hydrogen production system.
Preferably, the pH value of the electrolyte of the system is 0-14.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) when the Si-based InN nano-column heterojunction photoelectrode subjected to annealing treatment is applied to hydrogen production by photoelectrolysis of water, the nano-column structure reduces the migration distance from a photon-generated carrier to a semiconductor/electrolyte interface, reduces the recombination probability of the photon-generated carrier, and is more beneficial to allowing photon-generated electrons and holes to respectively participate in hydrogen evolution and oxygen evolution reactions.
(2) When the Si-based InN nano-column heterojunction photoelectrode subjected to annealing treatment is applied to hydrogen production by photoelectrolysis of water, the heterojunction promotes separation of bulk charges and surface charges, activates electrons and holes of two semiconductors, and can effectively improve the water photolysis efficiency.
(3) The preparation method is simple in preparation process, does not need to be carried out in harsh environments such as vacuum and high temperature, and greatly saves the preparation cost.
Drawings
Fig. 1 is a SEM top view of a Si-based InN nanocolumn heterojunction annealed in a sulfur atmosphere in example 1.
Fig. 2 is an SEM cross-sectional view of the Si-based InN nanorod heterojunction annealed in a sulfur atmosphere in example 1.
Fig. 3 is a linear scanning curve diagram of the Si-based InN nanorod heterojunction photoelectrode annealed in a sulfur atmosphere in example 1.
Fig. 4 is a linear scan plot of the Si-based InN nanorod heterojunction photoelectrode annealed in an oxygen atmosphere in example 2.
Fig. 5 is a linear scan plot of Si-based InN nanorod heterojunction photoelectrode annealed in selenium atmosphere in example 3.
Fig. 6 is a linear scan graph of the Si-based InN nanorod heterojunction photoelectrode annealed in a selenium atmosphere in example 4.
Fig. 7 is a linear scan graph of the Si-based InN nanorod photoelectrode of comparative example 1.
Fig. 8 is a linear scan graph of a Si-based InN nanorod heterojunction photoelectrode annealed in a sulfur atmosphere in comparative example 2.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
A preparation method of an annealed Si-based InN nanorod heterojunction comprises the following steps:
(1) selecting a substrate: an n-type Si substrate (conductivity <0.005 Ω) was used.
(2) And (3) growing the InN nano-columns: adopting a molecular beam epitaxial growth process, controlling the substrate temperature In the step (1) to be 400 ℃, the substrate rotating speed to be 10r/min and the In beam equivalent pressure to be 1.43 multiplied by 10-7Torr, nitrogen flow rate was 2sccm, plasma source power was 400W, and growth time was 2 hours.
(3) The preparation method of the InN nano-column heterojunction comprises the following steps: adopting chemical vapor deposition process to make the prepared InN nano column be in N2Annealing at 500 ℃ for 5min In a sulfur atmosphere under protection to obtain InN/In2S3A nanopillar heterojunction.
As shown in fig. 1, SEM top view of the Si-based InN nanorod heterojunction annealed in a sulfur atmosphere in this example.
As shown in fig. 2, the SEM cross-sectional view of the Si-based InN nanorod heterojunction annealed in a sulfur atmosphere in this example.
The Si-based InN nanorod heterojunction annealed in the sulfur atmosphere of the present example was used for photoelectrolysis of water: the prepared Si-based InN/In2S3The method for manufacturing the photoelectrode by the nano-pillar heterojunction comprises the following specific steps: forming ohm by using electron beam evaporation to deposit metal layer and Si backThe metal layer is then connected with metal wires and the entire metal back is protected with an insulating epoxy. Finally, an electrochemical workstation was used for the photoelectrochemical tests, as follows: 0.5mol/L Na was used2SO4Solution as electrolyte, prepared photoelectrode as anode, Ag/AgCl as reference electrode, Pt wire as cathode, and 300W Xe lamp (light intensity 100 mW/cm)2) As a light source, a photocurrent density-bias curve was tested. InN/In prepared by the process2S3The linear scanning curve of the nanorod heterojunction photoelectrode is shown in FIG. 3, and when the photoelectrode is biased at 1.23V vs. RHE, the photocurrent density is 2.44mA/cm2。
Example 2
A preparation method of an annealed Si-based InN nanorod heterojunction comprises the following steps:
(1) selecting a substrate: an n-type Si substrate (conductivity <0.005 Ω) was used.
(2) And (3) growing the InN nano-columns: adopting a molecular beam epitaxial growth process, controlling the substrate temperature In the step (1) to be 400 ℃, the substrate rotating speed to be 10r/min and the In beam equivalent pressure to be 1.43 multiplied by 10-7Torr, nitrogen flow rate was 2sccm, plasma source power was 400W, and growth time was 2 hours.
(3) The preparation method of the InN nano-column heterojunction comprises the following steps: adopting chemical vapor deposition process to make the prepared InN nano column be in N2Annealing at 500 deg.C for 5min under protection of oxygen to obtain InN/In2O3A nanopillar heterojunction.
The Si-based InN nanorod heterojunction annealed in the sulfur atmosphere of the present example was used for photoelectrolysis of water: the prepared Si-based InN/In2O3The method for manufacturing the photoelectrode by the nano-pillar heterojunction comprises the following specific steps: and forming ohmic contact between the metal layer and the Si back surface by electron beam evaporation deposition, connecting the metal layer by a metal wire, and protecting the whole metal back surface by insulating epoxy resin. Finally, an electrochemical workstation was used for the photoelectrochemical tests, as follows: 0.5mol/L Na was used2SO4The solution is used as electrolyte, the prepared photoelectrode is used as anode, Ag/AgCl is used as reference electrode, and Pt wire is used as reference electrodeAs a cathode, and a 300W Xe lamp (light intensity-100 mW/cm)2) As a light source, a photocurrent density-bias curve was obtained by testing. InN/In prepared by the process2O3The linear scanning curve of the nanorod heterojunction photoelectrode is shown in FIG. 4, and when the photoelectrode is biased at 1.23V vs. RHE, the photocurrent density is 0.33mA/cm2。
Example 3
A preparation method of an annealed Si-based InN nanorod heterojunction comprises the following steps:
(1) selecting a substrate: an n-type Si substrate (conductivity <0.005 Ω) was used.
(2) And (3) growing the InN nano-columns: adopting a molecular beam epitaxial growth process, controlling the substrate temperature In the step (1) to be 400 ℃, the substrate rotating speed to be 10r/min and the In beam equivalent pressure to be 1.43 multiplied by 10-7Torr, nitrogen flow rate was 2sccm, plasma source power was 400W, and growth time was 2 hours.
(3) The preparation method of the InN nanorod heterojunction comprises the following steps: the prepared InN nano column is arranged on N by adopting a chemical vapor deposition process2Annealing at 500 deg.C for 5min under the protection of selenium atmosphere to obtain InN/In2Se3A nanopillar heterojunction.
The Si-based InN nanorod heterojunction annealed in the sulfur atmosphere of the present example was used for photoelectrolysis of water: the prepared Si-based InN/In2Se3The method for manufacturing the nano-pillar heterojunction into the photoelectrode comprises the following specific steps: ohmic contact is formed with the Si backside by depositing a metal layer by electron beam evaporation, and then a metal wire is connected to the metal layer and the entire metal backside is protected with an insulating epoxy. Finally, an electrochemical workstation was used for the photoelectrochemical tests, as follows: 0.5mol/L Na was used2SO4Solution as electrolyte, prepared photoelectrode as anode, Ag/AgCl as reference electrode, Pt wire as cathode, and 300W Xe lamp (light intensity 100 mW/cm)2) As a light source, a photocurrent density-bias curve was obtained by testing. InN/In prepared by the process2Se3The linear scanning curve of the nanorod heterojunction photoelectrode is shown in FIG. 5, and the photocurrent density of the photoelectrode is 0.79mA/cm under the bias of 1.23V vs. RHE2。
Example 4
A preparation method of an annealed Si-based InN nanorod heterojunction comprises the following steps:
(1) selecting a substrate: an n-type Si substrate (conductivity <0.005 Ω) was used.
(2) And (3) growing the InN nano-columns: adopting a molecular beam epitaxial growth process, controlling the substrate temperature In the step (1) to be 400 ℃, the substrate rotating speed to be 10r/min and the In beam equivalent pressure to be 1.43 multiplied by 10-7The nitrogen flow was 2sccm, the plasma source power was 400W, and the growth time was 2 hours.
(3) The preparation method of the InN nano-column heterojunction comprises the following steps: adopting chemical vapor deposition process to make the prepared InN nano column be in N2Annealing at 400 ℃ for 30min In a sulfur atmosphere under protection to obtain InN/In2S3A nanopillar heterojunction.
The Si-based InN nanorod heterojunction annealed in the sulfur atmosphere of the present example was used for photoelectrolysis of water: the prepared Si-based InN/In2S3The method for manufacturing the photoelectrode by the nano-pillar heterojunction comprises the following specific steps: ohmic contact is formed with the Si backside by depositing a metal layer by electron beam evaporation, and then a metal wire is connected to the metal layer and the entire metal backside is protected with an insulating epoxy. Finally, an electrochemical workstation was used for the photoelectrochemical tests, as follows: 0.5mol/L Na was used2SO4Solution as electrolyte, prepared photoelectrode as anode, Ag/AgCl as reference electrode, Pt wire as cathode, and 300W Xe lamp (light intensity 100 mW/cm)2) As a light source, a photocurrent density-bias curve was obtained by testing. InN/In prepared by the process2S3The linear scanning curve graph of the nanorod heterojunction photoelectrode is shown in FIG. 6, and when the photoelectrode is biased at 1.23V vs. RHE, the photocurrent density is 0.84mA/cm2。
Comparative example 1
The preparation method of the Si-based InN nano column comprises the following steps:
(1) selecting a substrate: an n-type Si substrate (conductivity <0.005 Ω) was used.
(2) And (3) growing the InN nano-columns: miningUsing molecular beam epitaxial growth process, controlling the substrate temperature In step (1) at 400 deg.C, the substrate rotation speed at 10r/min, and the In beam equivalent pressure at 1.43 × 10-7Torr, nitrogen flow rate was 2sccm, plasma source power was 400W, and growth time was 2 hours.
The Si-based InN nanocolumn of this comparative example was used for photo-electrolysis of water: the prepared Si-based InN nano-column is manufactured into a photoelectrode, and the specific steps are as follows: and forming ohmic contact between the metal layer and the Si back surface by electron beam evaporation deposition, connecting the metal layer by a metal wire, and protecting the whole metal back surface by insulating epoxy resin. Finally, an electrochemical workstation was used for the photoelectrochemical tests, as follows: 0.5mol/L Na was used2SO4Solution as electrolyte, prepared photoelectrode as anode, Ag/AgCl as reference electrode, Pt wire as cathode, and 300W Xe lamp (light intensity 100 mW/cm)2) As a light source, a photocurrent density-bias curve was obtained by testing. The linear scanning curve chart of the InN nano-column photoelectrode prepared by the process is shown in figure 7, and the photoelectrode has the photocurrent density of 0.05mA/cm under the bias voltage of 1.23V vs2。
Comparative example 2
A preparation method of an annealed Si-based InN nanorod heterojunction comprises the following steps:
(1) selecting a substrate: an n-type Si substrate (conductivity <0.005 Ω) was used.
(2) And (3) growing the InN nano-columns: adopting a molecular beam epitaxial growth process, controlling the substrate temperature In the step (1) to be 400 ℃, the substrate rotating speed to be 10r/min and the In beam equivalent pressure to be 1.43 multiplied by 10-7Torr, nitrogen flow rate was 2sccm, plasma source power was 400W, and growth time was 2 hours.
(3) The preparation method of the InN nano-column heterojunction comprises the following steps: adopting chemical vapor deposition process to make the prepared InN nano column be in N2Annealing at 600 ℃ for 10min In a sulfur atmosphere under protection to obtain InN/In2S3A nanopillar heterojunction.
The Si-based InN nanorod heterojunction annealed in the sulfur atmosphere of the present example was used for photoelectrolysis of water: the prepared Si-based InN/In2S3Fabrication of nanopillar heterojunctionThe light forming electrode comprises the following specific steps: and forming ohmic contact between the metal layer and the Si back surface by electron beam evaporation deposition, connecting the metal layer by a metal wire, and protecting the whole metal back surface by insulating epoxy resin. Finally, an electrochemical workstation was used for the photoelectrochemical tests, as follows: 0.5mol/L Na was used2SO4Solution as electrolyte, prepared photoelectrode as anode, Ag/AgCl as reference electrode, Pt wire as cathode, and 300W Xe lamp (light intensity 100 mW/cm)2) As a light source, a photocurrent density-bias curve was obtained by testing. InN/In prepared by the process2S3The linear scanning curve graph of the nanorod heterojunction photoelectrode is shown in FIG. 8, and when the photoelectrode is biased at 1.23V vs. RHE, the photocurrent density is 0.05mA/cm2。
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A preparation method of an annealed Si-based InN nanorod heterojunction is characterized by comprising the following steps:
(1) growing an InN nano column on a Si substrate by adopting a molecular beam epitaxial growth process;
(2) annealing the InN nano column obtained in the step (1) to obtain a Si-based InN nano column heterojunction; the annealing atmosphere is N2A sulfur atmosphere, an oxygen atmosphere, or a selenium atmosphere under protection.
2. The method of claim 1, wherein the annealing is performed at 400 to 500 ℃ for 5 to 30 min.
3. The method of claim 2, wherein the annealing is annealing at 500 ℃ for 5 min.
4. The method according to any one of claims 1 to 3, wherein the density of the InN nano-pillars is 150 to 200 μm-2。
5. The method according to any one of claims 1 to 3, wherein the InN nanocolumn has a height of 150 to 500nm and a diameter of 60 to 100 nm.
6. The method of any one of claims 1-3, wherein the growing InN nanopillars on a Si substrate comprises the steps of:
adopting a molecular beam epitaxial growth process, controlling the temperature of the Si substrate to be 380-450 ℃, the rotating speed of the Si substrate to be 10r/min, and the equivalent pressure of the In beam to be 1 multiplied by 10-7～2.5×10-7And (3) Torr, the nitrogen flow is 1-3 sccm, the nitrogen plasma source power is 200-400W, the growth time is 1-5 h, and the InN nano-column grows on the Si substrate.
7. The production method according to any one of claims 1 to 3, wherein the Si substrate is an n-type Si substrate and has an electric conductivity of <0.005 Ω.
8. A Si-based InN nanocolumn heterojunction produced by the production method as set forth in any one of claims 1 to 7.
9. The use of a Si-based InN nanorod heterojunction as claimed in claim 8 in the fabrication of photoelectrodes.
10. Use according to claim 9, characterized in that the preparation of the photoelectrode comprises the following steps:
forming ohmic contact between a metal layer and the Si back of the Si-based InN nano-column heterojunction by electron beam evaporation deposition, connecting a metal wire with the metal layer, and protecting the whole metal back by using insulating epoxy resin; the metal layer is Ti/Au alloy.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114875493A (en) * | 2022-04-29 | 2022-08-09 | 华南理工大学 | InN-VIA group heterojunction on Si substrate and preparation method and application thereof |
| CN116377594A (en) * | 2023-04-04 | 2023-07-04 | 华南理工大学 | Passivation method based on InN nano-column on p-GaAs substrate, passivation final product composite structure and application thereof |
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| CN116377594B (en) * | 2023-04-04 | 2023-09-01 | 华南理工大学 | Passivation method based on InN nano-column on p-GaAs substrate, passivation final product composite structure and application thereof |
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