CN112708905A - Z-type InGaN/Cu2O nano-column heterojunction and preparation method and application thereof - Google Patents
Z-type InGaN/Cu2O nano-column heterojunction and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a Z-shaped InGaN/Cu2A preparation method and application of an O nano-pillar heterojunction. Z-type InGaN/Cu2The O nano-pillar heterojunction comprises a substrate, InGaN nano-pillars grown on the substrate and Cu deposited on the InGaN nano-pillars2And O. The invention adopts a method with low cost and simple process to prepare the InGaN nanorod heterojunction with Z-shaped energy band arrangement. The heterojunction manufactured photoelectrode can be used for unbiased photoelectrocatalysis water decomposition hydrogen production, external energy input is not needed, hydrogen production cost is greatly improved, and the heterojunction manufactured photoelectrode has great significance for large-scale hydrogen energy production.
Description
Technical Field
The invention relates to the field of InGaN nano-column photoelectrocatalysis, in particular to Z-type InGaN/Cu2O nano-pillar heterojunction and preparation method thereofAnd applications thereof.
Background
The development of unbiased photoelectrochemical water splitting to produce hydrogen shows great potential in addressing global energy crisis and environmental issues. The InGaN nano-pillars have adjustable band gaps (0.65 eV-3.4 eV), and the light absorption can be adjusted by changing the indium composition, so that the InGaN nano-pillars are ideal for photoelectrodes. In addition, the InGaN nanopillar has an energy band position suitable for the water redox reaction, a longer charge diffusion distance, a high surface area to volume ratio and an excellent theoretical solar energy-to-hydrogen (STH) efficiency (27%), so that the InGaN nanopillar is very beneficial to photoelectrochemical full water decomposition. However, problems with rapid recombination of bulk and surface charges and slow oxidation kinetics of InGaN nano-pillars result in 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. In particular, coupling semiconductors with excellent water oxidation or reduction capabilities to form a Z-type heterostructure can activate both the electrons and holes of the two semiconductors, showing their unique advantage in water splitting. Therefore, in order to realize unbiased photoelectrochemical water decomposition, the construction of the Z-type InGaN nanorod heterojunction is very important.
Cu2O is a direct band gap semiconductor electrode material (
2.0eV) with visible light response and a positive conduction band potential, it is one of the most attractive photocathode materials and is expected to be a promising candidate for matching InGaN nano-pillars. At present, Cu2O has been successfully supported on Ga2O3，WO3And BiVO4And the like on various metal oxides to construct a type II heterostructure photoanode. Although effective charge separation of bulk photoelectrodes is achieved, type II heterojunction photoelectrodes have limited utility in unbiased photocatalysts. Thus, through the InGaN nanopillars and Cu2The O design of the Z-shaped heterojunction photoelectrode has great significance for unbiased photoelectrolysis.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention firstly aims to provide Z-type InGaN/Cu2An O nano-pillar heterojunction;
the invention also aims to provide a method for preparing the Z-type InGaN/Cu2A method of O nano-pillar heterojunction;
the present invention further provides the above-mentioned Z-type InGaN/Cu2The application of the O nano-column heterojunction in the non-bias photoelectrocatalysis water decomposition hydrogen production greatly improves the production cost of hydrogen energy.
The purpose of the invention is realized by the following technical scheme.
Z-type InGaN/Cu2An O-nanorod heterojunction comprises a substrate, InGaN nanorods grown on the substrate, and Cu deposited on the InGaN nanorods2O。
Preferably, the substrate is an n-type Si substrate; more preferably, the n-type Si substrate has a conductivity <0.005 Ω.
Preferably, the In atoms In the InGaN nano-columns account for 7% -10% of the metal atoms (In, Ga).
Preferably, the height of the InGaN nano column is 200-500 nm, and the diameter of the InGaN nano column is 65-100 nm.
Preferably, the density of the InGaN nano-pillars is 150-200 mu m-2。
Preferably, the Cu2O is grown on the InGaN nano-column, and the preparation method adopts an electrochemical deposition method.
The preparation method of the InGaN nano-pillar comprises the following steps:
the molecular beam epitaxial growth process is adopted, the substrate temperature is controlled to be 900-950 ℃, the substrate rotating speed is 5-10 r/min, and the equivalent pressure of the Ga beam is 1 multiplied by 10-7～2.5×10-7Torr, equivalent pressure of In beam is 2.0X 10-8～5×10-8The nitrogen flow is 2-5 sccm, the plasma source power is 200-400W, and the growth time is 1-3 h to prepare the InGaN nanocolumn.
The Z-shaped InGaN/Cu2The preparation method of the O nano-pillar heterojunction comprises the following steps：
Adopting an electrochemical deposition method, taking a copper sulfate solution and a copper acetate solution as electrolyte, respectively taking an InGaN nano-column, a Pt wire and Ag/AgCl as a working electrode, a counter electrode and a reference electrode, performing electrodeposition for 5-30 min under the bias of-0.8-0.4V vs. Ag/AgCl, and carrying out electrodeposition on Cu2Depositing O on the InGaN nano-column to obtain Z-type InGaN/Cu2And an O nano-pillar heterojunction.
Preferably, the concentration of the copper sulfate is 30-50 mM, and more preferably 40 mM; the concentration of copper acetate is 70 to 90mM, more preferably 80 mM.
Preferably, the InGaN nano-column is used for electrodepositing Cu2And before O, sequentially carrying out ultrasonic cleaning by using ethanol, acetone and water.
Preferably, the obtained Z-type InGaN/Cu2Annealing the O nano-pillar heterojunction for 0.5-5 h at 550-700 ℃ under a protective atmosphere; more preferably, the annealing is carried out at 600 ℃ for 1 h.
Preferably, the Cu2The grain diameter of O is 50 nm-100 nm.
The Z-type InGaN/Cu2The application of the O nano-column heterojunction in unbiased photoelectrocatalysis water decomposition hydrogen production.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) 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.
(2) The Z-type InGaN/Cu of the present invention2The O nano-column heterojunction has high electron transport dynamics and can realize the hydrogen production by the photoelectrolysis without bias voltage.
Drawings
FIG. 1 shows the Z-type InGaN/Cu in example 12SEM top view of O nanopillar heterojunction.
FIG. 2 shows the Z-type InGaN/Cu in example 12SEM cross-sectional view of O-nanorod heterojunctions.
FIG. 3 shows the Z-type InGaN/Cu in example 12Linear scan graph of O nanopillar heterojunction.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Example 1
Z-type InGaN/Cu2The preparation method of the O nano-pillar 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 InGaN nano-pillars: adopting molecular beam epitaxial growth process, controlling substrate temperature at 930 deg.C, substrate rotation speed at 10r/min, and Ga beam equivalent pressure at 2 × 10-7Torr, In beam equivalent pressure 3X 10-8And (3) preparing the InGaN nano-column by the aid of the Torr, nitrogen flow of 2sccm, plasma source power of 400W and growth time of 3 hours, wherein In atoms of the prepared InGaN nano-column account for 10%.
(3) Z-type InGaN/Cu2The preparation method of the O nano-pillar heterojunction comprises the following steps: and ultrasonically cleaning the prepared InGaN nano-column for 10min by ethanol, acetone and water in sequence. Then, performing electrodeposition for 5min under the bias of-0.4V vs. Ag/AgCl by adopting an electrochemical deposition method and using 40mM copper sulfate and 80mM copper acetate electrolyte and using InGaN nano-columns, Pt wires and Ag/AgCl as a working electrode, a counter electrode and a reference electrode respectively; most preferably the obtained InGaN/Cu2O is at 600 DEG and N2Annealing for 1h under the atmosphere to obtain heterojunction, and the prepared Cu2The grain diameter of O is 50 nm.
As shown in FIG. 1, the Z-type InGaN/Cu of this example2Scanning electron microscope top view of the O-nanopillar heterojunction.
As shown in FIG. 2, the Z-type InGaN/Cu of this example2Scanning electron microscope cross-sectional view of O nano-pillar heterojunction
The Z-type InGaN/Cu of this example2The O nano-column heterojunction is used for photo-electrolysis of water: the prepared Z-type InGaN/Cu2The method for manufacturing the photoelectrode by the O nano column 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 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 Z-shaped InGaN/Cu prepared by the process2The linear scanning curve diagram of the O nano-pillar heterojunction is shown in figure 3, when the photoelectrode is biased at 1.2V vs. RHE, the photocurrent density is 6.8mA/cm2。
Example 2
Z-type InGaN/Cu2The preparation method of the O nano-pillar heterojunction comprises the following steps:
(2) selecting a substrate: an n-type Si substrate (conductivity <0.005 Ω) was used.
(2) And (3) growing the InGaN nano-pillars: adopting molecular beam epitaxial growth process, controlling substrate temperature at 930 deg.C, substrate rotation speed at 10r/min, and Ga beam equivalent pressure at 2 × 10-7Torr, In beam equivalent pressure 3X 10-8And (3) preparing the InGaN nano-column by the aid of the Torr, nitrogen flow of 2sccm, plasma source power of 400W and growth time of 3 hours, wherein In atoms of the prepared InGaN nano-column account for 10%.
(3) Z-type InGaN/Cu2The preparation method of the O nano-pillar heterojunction comprises the following steps: and ultrasonically cleaning the prepared InGaN nano-column for 10min by ethanol, acetone and water in sequence. Then, carrying out electrodeposition for 30min under the bias of-0.4V vs. Ag/AgCl by adopting an electrochemical deposition method and using 40mM copper sulfate and 80mM copper acetate electrolyte and using InGaN nano-columns, Pt wires and Ag/AgCl as a working electrode, a counter electrode and a reference electrode respectively; most preferably the obtained InGaN/Cu2O is at 600 DEG and N2Annealing for 1h under the atmosphere to obtain heterojunction, and the prepared Cu2The grain diameter of O is 100 nm.
The Z-type InGaN/Cu of this example2The O nano-column heterojunction is used for photo-electrolysis of water: the prepared Z-type InGaN/Cu2The method for manufacturing the photoelectrode by the O nano column 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, a photoelectrochemical test was performed using an electrochemical workstation, in particularThe following were used: 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 Z-shaped InGaN/Cu prepared by the process2When the O nano-pillar heterojunction photoelectrode is biased at 1.2V vs. RHE, the photocurrent density is 5.2mA/cm2。
Example 3
Z-type InGaN/Cu2The preparation method of the O nano-pillar heterojunction comprises the following steps:
(3) selecting a substrate: an n-type Si substrate (conductivity <0.005 Ω) was used.
(2) And (3) growing the InGaN nano-pillars: adopting molecular beam epitaxial growth process, controlling substrate temperature at 930 deg.C, substrate rotation speed at 10r/min, and Ga beam equivalent pressure at 2 × 10-7Torr, In beam equivalent pressure 3X 10-8And (3) preparing the InGaN nano-column by the aid of the Torr, nitrogen flow of 2sccm, plasma source power of 400W and growth time of 3 hours, wherein In atoms of the prepared InGaN nano-column account for 10%.
(3) Z-type InGaN/Cu2The preparation method of the O nano-pillar heterojunction comprises the following steps: and ultrasonically cleaning the prepared InGaN nano-column for 10min by ethanol, acetone and water in sequence. Then, carrying out electrodeposition for 15min under the bias of-0.4V vs. Ag/AgCl by adopting an electrochemical deposition method and using 40mM copper sulfate and 80mM copper acetate electrolyte and using InGaN nano-columns, Pt wires and Ag/AgCl as a working electrode, a counter electrode and a reference electrode respectively; most preferably the obtained InGaN/Cu2O is at 600 DEG and N2Annealing for 1h under the atmosphere to obtain heterojunction, and the prepared Cu2The grain diameter of O is 80 nm.
The Z-type InGaN/Cu of this example2The O nano-column heterojunction is used for photo-electrolysis of water: the prepared Z-type InGaN/Cu2The method for manufacturing the photoelectrode by the O nano column 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, electrochemical stations are used for photoelectrochemical tests, such asThe following: 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. Z-type InGaN/Cu2When the O nano-pillar heterojunction photoelectrode is biased at 1.2V vs. RHE, the photocurrent density is 7.2mA/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. Z-type InGaN/Cu2The O nano-pillar heterojunction is characterized by comprising a substrate, InGaN nano-pillars grown on the substrate and Cu deposited on the InGaN nano-pillars2O。
2. A Z-type InGaN/Cu as claimed in claim 12The O nano-pillar heterojunction is characterized in that the substrate is an n-type Si substrate.
3. A Z-type InGaN/Cu as claimed in claim 12The O nano-pillar heterojunction is characterized In that the In atom In the InGaN nano-pillar accounts for 7% -10% of the metal atoms In and Ga.
4. A Z-type InGaN/Cu as claimed in claim 12The O nanorod heterojunction is characterized in that the height of the InGaN nanorod is 200-500 nm, and the diameter of the InGaN nanorod is 65-100 nm.
5. A Z-type InGaN/Cu as claimed in claim 12The O nano-pillar heterojunction is characterized in that the density of the InGaN nano-pillar is 150-200 mu m-2。
6. A Z-type InGaN/Cu as claimed in claim 12The O nanorod heterojunction is characterized in that the preparation method of the InGaN nanorod comprises the following steps:
the molecular beam epitaxial growth process is adopted, the substrate temperature is controlled to be 900-950 ℃, the substrate rotating speed is 5-10 r/min, and the equivalent pressure of the Ga beam is 1 multiplied by 10-7～2.5×10-7Torr, equivalent pressure of In beam is 2.0X 10-8～5×10-8The nitrogen flow is 2-5 sccm, the plasma source power is 200-400W, and the growth time is 1-3 h to prepare the InGaN nanocolumn.
7. Preparation of the Z-type InGaN/Cu as described in any of claims 1 to 62A method of O nanopillar heterojunction, comprising the steps of:
adopting an electrochemical deposition method, taking a copper sulfate solution and a copper acetate solution as electrolyte, respectively taking an InGaN nano-column, a Pt wire and Ag/AgCl as a working electrode, a counter electrode and a reference electrode, performing electrodeposition for 5-30 min under the bias of-0.8-0.4V vs. Ag/AgCl, and carrying out electrodeposition on Cu2Depositing O on the InGaN nano-column to obtain Z-type InGaN/Cu2And an O nano-pillar heterojunction.
8. The method of claim 7, wherein:
the concentration of the copper sulfate is 30-50 mM, and the concentration of the copper acetate is 70-90 mM;
the Cu2The grain diameter of O is 50 nm-100 nm.
9. The method of claim 7, wherein:
the obtained Z-type InGaN/Cu2Annealing the O nano-pillar heterojunction for 0.5-5 h at 550-700 ℃ under a protective atmosphere.
10. A Z-type InGaN/Cu as claimed in any of claims 1 to 62The O nano-column heterojunction is applied to unbiased photoelectrocatalysis water decomposition hydrogen production.
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