CN116377594B - Passivation method based on InN nano-column on p-GaAs substrate, passivation final product composite structure and application thereof - Google Patents
Passivation method based on InN nano-column on p-GaAs substrate, passivation final product composite structure and application thereof Download PDFInfo
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- 229910001218 Gallium arsenide Inorganic materials 0.000 title claims abstract description 95
- 238000002161 passivation Methods 0.000 title claims abstract description 90
- 238000000034 method Methods 0.000 title claims abstract description 72
- 239000000758 substrate Substances 0.000 title claims abstract description 72
- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 239000012467 final product Substances 0.000 title claims abstract description 17
- 239000002061 nanopillar Substances 0.000 claims abstract description 52
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 15
- 239000002074 nanoribbon Substances 0.000 claims abstract description 6
- 230000008569 process Effects 0.000 claims description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 17
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 6
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 5
- 230000002378 acidificating effect Effects 0.000 claims description 5
- 238000005868 electrolysis reaction Methods 0.000 claims description 5
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 4
- 239000008055 phosphate buffer solution Substances 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 abstract description 24
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 24
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 15
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 239000000969 carrier Substances 0.000 abstract description 3
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000000231 atomic layer deposition Methods 0.000 description 4
- 239000006104 solid solution Substances 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 3
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- 230000002708 enhancing effect Effects 0.000 description 2
- 230000001965 increasing effect Effects 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical group [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 239000002127 nanobelt Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
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- DJHGAFSJWGLOIV-UHFFFAOYSA-K Arsenate3- Chemical compound [O-][As]([O-])([O-])=O DJHGAFSJWGLOIV-UHFFFAOYSA-K 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 229910000673 Indium arsenide Inorganic materials 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229940000489 arsenate Drugs 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- 230000001627 detrimental effect Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- 229910052737 gold Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- RPQDHPTXJYYUPQ-UHFFFAOYSA-N indium arsenide Chemical compound [In]#[As] RPQDHPTXJYYUPQ-UHFFFAOYSA-N 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
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- 230000006641 stabilisation Effects 0.000 description 1
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- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/50—Processes
- C25B1/55—Photoelectrolysis
-
- 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
- C25B11/054—Electrodes comprising electrocatalysts supported on a carrier
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- 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
- C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
- C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
-
- 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
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/32—Anodisation of semiconducting materials
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C30B29/403—AIII-nitrides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a passivation method based on InN nano-pillars on a p-GaAs substrate, a passivation final product composite structure and application thereof. The passivation end product composite structure comprises a p-GaAs substrate and an In (As) N nanoribbon grown on the p-GaAs substrate. The electrochemical anode passivation method for the InN nano-column on the p-GaAs substrate can effectively and simply passivate In atomic clusters In the InN nano-column; meanwhile, the p-GaAs/In (As) N heterostructure formed by the passivation end product composite structure meets the hydrogen evolution potential, increases the internal Fermi potential barrier, enhances the separation and transfer efficiency of photogenerated carriers, and can obviously improve the photoelectric conversion efficiency. The p-GaAs/In (As) N heterojunction has larger specific surface area, has stronger absorption to sunlight and is suitable for photoelectrically decomposing water to produce hydrogen.
Description
Technical Field
The invention relates to the field of GaAs and InN nano materials, in particular to a passivation method based on InN nano columns on a p-GaAs substrate, a passivation final product composite structure and application thereof.
Background
Photoelectrochemical (PEC) water splitting hydrogen production is capable of efficiently converting and storing solar energy as clean, renewable hydrogen energy. In recent years, the III-V compound nano-pillar has wide application prospect in the field of PEC water decomposition, and has stronger light absorption capacity and light response compared with narrow bandgap semiconductors such as wide bandgap semiconductors GaN, alN, gaAs, inN and the like. Wherein the conduction band bottom position (CBM: 4.00eV vs. Vac) of p-GaAs is very suitable for a PEC hydrogen evolution photoelectrode, and can just form a type II p-n heterojunction with InN. However, due to the problems of surface state accumulation, photo-generated carrier accumulation and the like, the PEC decomposition water performance of the photoelectrode has a large bottleneck, the current hydrogen production efficiency is not high, and a certain distance exists from the industrialized production.
Passivation is an effective means for surface state accumulation. Currently, there are several methods commonly used to improve PEC water splitting properties by passivation:
the prior literature discloses a method of taking (NH 4 ) 2 S and MoS 2 Iso-sulfide combined passivation III-V semiconductor GaAs/InGaP 2 In the application examples (Lim, h., young, j.l., geisz, j.f.et al, high performance III-V photoelectrodes for solar water splitting via synergistically tailored structure and stopper, nat Commun 10,3388 (2019)), the method reduces overpotential and increases photocurrent, slows down photo-generated carrier loss caused by surface dangling bonds to some extent, but the passivation layer sulfide introduced by the method has poor stability in air, and long-time high-efficiency PEC photoelectrolysis can be realized by means of combined passivation of a plurality of sulfide solutions with high concentration.
The prior literature discloses a method for adopting thin layers of Pt and TiO 2 I.e. thin noble metals and inert oxides combined passivation of group III-V semiconductor GaAs/InGaP 2 Is described (Varadhan, P., fu, HC., kao, YC. Et al. An efficient and stable photoelectrochemical system with% solid-to-hydrogen conversion efficiency via InGaP/GaAs double junction. Nat Commun 10,5282 (2019)). The method is implemented by conventional passivation meansAmong the advantages that can be achieved, the durability of the thin noble metal and inert oxide on the surface makes the device exhibit more excellent stability over time (180 h); however, due to the poor conductivity of the inert oxide, a slightly thicker inert oxide can seriously impair the performance of the photovoltaic device, while Atomic Layer Deposition (ALD) techniques are often required to achieve deposition of a thin inert oxide, requiring very high equipment and time costs, which is detrimental to large scale applications of the techniques.
Disclosure of Invention
In order to overcome the bottlenecks of high cost, insignificant passivation effect and the like of the traditional passivation technology at present, the invention aims to provide a passivation method based on InN nano-pillars on a p-GaAs substrate, a passivation end product composite structure and application thereof. The passivation method has simple process and low cost; meanwhile, the passivation product can realize solid solution doping, greatly strengthen the hydrogen evolution performance of the photoelectrode, and provide a novel thought for the preparation of other semiconductor composite catalytic materials.
The invention adopts an electrochemical anode treatment method to passivate InN nano-pillars growing on a p-GaAs substrate, wherein the p-GaAs substrate is heavily p-doped gallium arsenide, and the doping concentration reaches 5.1 multiplied by 10 19 cm -3 ～5.8×10 19 cm -3 . Through the novel passivation method, in atom clusters In the InN nano-column are rapidly eliminated, and the formed passivation product In (As) N nano-belt can effectively improve the photolytic water hydrogen evolution performance.
The invention provides a passivation method based on InN nano-pillars on a p-GaAs substrate, which comprises the following steps:
(1) Growing InN nano-pillars on the p-GaAs substrate by adopting a molecular beam epitaxial growth process;
(2) Applying anode voltage to the InN nano-column on the p-GaAs in weak acid aqueous solution to perform electrochemical anode treatment to obtain a passivation final product composite structure; the electrochemical anode treatment process is that electrolysis is carried out from 0-1.4V vs. AgCl in each round, and the number of treatment rounds is 50-300 rounds.
The invention uses electrochemical anode treatment method to passivate InN nano column on p-GaAs, passivates surface state, and is considered to solve high levelThe cost and passivation effect are not obvious, and the method is convenient, quick and long-acting. At a certain anode voltage, the indium atom clusters In the InN nano-pillar are oxidized into In 3+ The method comprises the steps of carrying out a first treatment on the surface of the At the same time, the As element of the p-GaAs substrate can escape and In under the electrochemical action 3+ And combining to realize passivation effect. Further, the passivation product produced can be regarded As In (As) N formed by doping InAs In solid solution form, greatly strengthening the internal fermi barrier. Because the internal fermi barrier is an important factor for restricting the driving force of the II-type heterojunction, the passivation product can effectively enhance the hydrogen evolution capability of the device, and In (As) N formed by solid solution doping enables As atoms to have a more stable chemical environment, so that the device is not easy to be disabled by air oxidation, and has stronger stability. Therefore, the passivation method for treating InN nano-pillars on p-GaAs by electrochemical anode treatment and the photoelectrocatalysis hydrogen production of p-GaAs/In (As) N of a passivation end product composite structure have important application prospects In photoelectrolysis water.
It is further preferable that the p-GaAs substrate in step (1) is subjected to a cleaning treatment, firstly organic contaminants on the surface of the substrate are removed by using an organic solvent, then the p-GaAs substrate is treated by using hydrochloric acid to treat the surface oxide layer, and finally the surface oxide layer is dried by using high-purity dry nitrogen gas; the organic solvent is used for removing organic pollutants on the surface of the p-GaAs substrate, which is sequentially spin-washed in acetone and absolute ethyl alcohol, and then rinsed with water; the concentration of the hydrochloric acid is 5-20wt%.
Further preferably, the p-GaAs substrate in step (1) is heavily p-doped gallium arsenide with a doping concentration of up to 5.1X10 19 cm -3 ～5.8×10 19 cm -3 。
Further preferably, the general standard for heavy doping is >1E18 cm-3.
Further preferably, the specific conditions of the molecular beam epitaxy growth process in step (1) are: the growth temperature is 350-450 ℃.
Further preferably, the specific conditions of the molecular beam epitaxy growth process in step (1) are: equivalent pressure of In beam is 1.58×10 -7 ～5.17×10 -7 Torr。
Further preferably, the specific conditions of the molecular beam epitaxy growth process in step (1) are: the rotating speed of the p-GaAs substrate is 5-10 r/min.
Further preferably, the specific conditions of the molecular beam epitaxy growth process in step (1) are: the flow rate of the nitrogen is 1-5 sccm.
Further preferably, the specific conditions of the molecular beam epitaxy growth process in step (1) are: the power of the plasma source is 200-400W.
Further preferably, the specific conditions of the molecular beam epitaxy growth process in step (1) are: the growth time is 1-3 h.
Further preferably, the weak acid aqueous solution in step (1) has a pH of 4 to 7.
Further preferably, the weak acid aqueous solution in step (1) has a pH of 5 to 7.
Further preferably, the weakly acidic aqueous solution in step (1) is selected from a sulfate solution or a phosphate buffer solution which is not electrochemically reducible.
The invention provides a passivation end product composite structure prepared by the passivation method, which comprises a p-GaAs substrate and an In (As) N nano-belt growing on the p-GaAs substrate.
Further preferably, the width of the In (As) N nanoribbons In the passivated end product composite structure ranges from nano-scale to micro-scale, being loosely porous nanoribbons.
The invention also provides application of the passivation final product composite structure prepared by the passivation method in photoelectrocatalysis hydrogen production.
Further preferably, the passivation final product composite structure prepared by the passivation method is applied to the electrolysis of water to produce hydrogen.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) The invention aims at the defects of the materials to realize high-efficiency self-passivation and change waste into valuable, and provides a novel idea for preparing other semiconductor composite catalytic materials. The intolerance defect of the narrow forbidden band semiconductor to electrochemical corrosion is effectively utilized, the metal clusters introduced by the growth process limitation of the III nitride nano material in the growth process are effectively consumed, and a good passivation effect is achieved.
(2) The scheme of the invention is more efficient and economical. The passivation mode adopted by the invention is a self-passivation mode under electrochemical anodic treatment, is safer and more thorough than the traditional sulfide passivation mode, and fig. 4 is an I-V curve during electrochemical anodic treatment, so that the current in the passivation process is large, and the passivation effect is excellent; compared with the novel ALD deposition mode, the method has low time cost, and meanwhile, the equipment cost (5.5-6.5 ten thousand yuan) of the required electrochemical workstation is far lower than that of ALD equipment (150 ten thousand yuan).
(3) The passivation final product composite structure produced by the invention can effectively improve the hydrogen production performance of the device by photolysis of water. Conventional passivation methods, such as sulfidation, are performed by passivating dangling bonds at the surface, and the substantial sulfidation that may occur to the host material during sulfidation may result in loss of the host material, and the resulting accessory sulfides may even impair hydrogen production performance of the device. In the present invention, the solid solution alloy into which the metal clusters are converted is also effective in enhancing the internal fermi barrier of the type ii heterojunction. Fig. 5 shows the energy band conditions before and after electrochemical anodic treatment simulated by theoretical calculation, and it can be found that after electrochemical anodic treatment, the fermi barrier in the heterojunction system is greatly enhanced, the photo-generated carriers of the system are easier to separate and transfer, and the photoelectric conversion efficiency is remarkably improved.
(4) The electrochemical anode passivation method for the InN nano-column on the p-GaAs substrate can effectively and simply passivate In atomic clusters In the InN nano-column; meanwhile, the p-GaAs/In (As) N heterostructure formed by the passivation end product composite structure meets the hydrogen evolution potential, increases the internal Fermi potential barrier, enhances the separation and transfer efficiency of photogenerated carriers, and can obviously improve the photoelectric conversion efficiency. The p-GaAs/In (As) N heterojunction disclosed by the invention has a larger specific surface area, has stronger absorption to sunlight and is suitable for photoelectrolysis of water to produce hydrogen.
For a better understanding and implementation, the present invention is described in detail below with reference to the drawings.
Drawings
FIG. 1 is a schematic illustration of a process flow for passivating InN nanopillars on p-GaAs.
Fig. 2 is a graph of the results of AIMD calculation simulation of the passivation process.
Fig. 3 is a Raman graph of a passivation-assisted experiment.
FIG. 4 is an I-V curve for electrochemical anodization, i.e., passivation.
Fig. 5 is a graph of the energy band situation before and after electrochemical anodization simulated by theoretical calculation.
Fig. 6 is a TEM topography of InN nanopillars grown on p-GaAs in example 1.
Fig. 7 is a photo-dark current density-bias plot of the passivation end product composite structures of example 1, example 2, and of InN nanopillars on p-GaAs of comparative example 1.
Fig. 8 is a graph of photocurrent density versus time for the passivation end product composite structure of example 1 and the InN nano-pillars on p-GaAs of comparative example 1.
Fig. 9 is a graph of photocurrent density versus time for the 7200s test of the passivation end product composite structure of example 1 after 900s of photocurrent density versus time test.
Detailed Description
Terms of orientation such as up, down, left, right, front, rear, front, back, top, bottom, etc. mentioned or possible mentioned in this specification are defined with respect to their construction, and they are relative concepts. Therefore, the position and the use state of the device may be changed accordingly. These and other directional terms should not be construed as limiting terms.
The implementations described in the following exemplary examples are not representative of all implementations consistent with the present disclosure. Rather, they are merely examples of implementations consistent with aspects of the present disclosure.
The terminology used in the present disclosure is for the purpose of describing particular embodiments only and is not intended to be limiting of the disclosure. As used in this disclosure, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It should also be understood that the term "and/or" as used herein refers to and encompasses any or all possible combinations of one or more of the associated listed items.
FIG. 1 is a schematic illustration of a process flow for passivating InN nanopillars on p-GaAs.
Fig. 2 is a graph of the results of AIMD calculation simulation of the passivation process. As can be seen from fig. 2, the In atoms on the GaAs supercell gradually combine with the As evolved In the GaAs substrate under the action of the electric field to form In-As bonds.
Fig. 3 is a Raman graph of a passivation-assisted experiment. As can be seen from fig. 3, a layer of metallic indium on GaAs substrate deposited by MBE (molecular beam epitaxy) method after electrochemical anode treatment, the Raman plot also clearly shows that a significant In-As peak is formed. Notably, no characteristic peak of high valence arsenate was exhibited.
Example 1
A passivation method based on InN nano-pillars on a p-GaAs substrate and application of the passivation method to photoelectrocatalysis hydrogen production of a passivation end product composite structure thereof comprise the following steps:
(1) Selection of a substrate: a p-GaAs substrate is used.
(2) And (3) cleaning the substrate: firstly, sequentially cleaning a substrate by using acetone and absolute ethyl alcohol, and then removing an oxide layer on the p-GaAs substrate by using 20wt% hydrochloric acid; finally, drying by high-purity dry nitrogen with the purity of 5N;
(3) Growth of InN nano-pillars on p-GaAs substrate: adopting a molecular beam epitaxial growth process, controlling the temperature of the substrate obtained In the step (2) to be 450 ℃, the rotating speed of the substrate to be 10r/min, and the equivalent pressure of In beam to be 5.17 multiplied by 10 -7 And (3) growing InN nano-pillars on the p-GaAs substrate obtained in the step (2) with the nitrogen flow of 2sccm, the plasma source power of 400W and the growth time of 2h, wherein the height of the nano-pillars exceeds 400nm, and the diameter of the nano-pillars is 50nm.
(4) And (3) placing the InN nano-pillar epitaxial wafer on the p-GaAs substrate into a sulfate solution with pH=5, starting electrolysis from 0-1.4V vs. AgCl, and performing electrochemical anode treatment, wherein the number of treatment rounds is 200. And after the electrochemical anode treatment is finished, the passivation is finished, and a passivation final product composite structure is obtained.
FIG. 4 is a graph of I-V curves during electrochemical anodization, i.e., passivation, and as can be seen from FIG. 4, the InN nanopillars on p-GaAs have not been electrochemically activated during the first round of electrochemical anodization; and the current of the electrochemical anodic treatment can exceed 100mA when reaching the tenth round, and the current exceeds 250mA when the twentieth round of electrochemical anodic treatment is performed. Therefore, under electrochemical anode treatment, the InN nano-pillars on the p-GaAs undergo a severe chemical reaction; however, it was not seen during the experiment that the InN nanopillars on p-GaAs produced significant gas, so this chemical reaction was not an anodic oxygen generating reaction, but an oxidation reaction of the In atoms.
Fig. 5 is a graph of the energy band situation before and after electrochemical anodization simulated by theoretical calculation. As can be seen from fig. 5, after electrochemical anodic treatment, the fermi level of InN is converted into In (As) N is greatly raised, and since the fermi level of p-GaAs is heavily pinned to the valence band, the fermi level of InN is lower, and thus the fermi barrier between In (As) N and p-GaAs is greatly enhanced, further enhancing the internal driving force between type ii heterojunctions.
Fig. 6 is a TEM topography of InN nanopillars grown on p-GaAs in example 1. As can be seen from fig. 6, the height of the nano-pillars exceeds 400nm and the diameter is 50nm, but the non-uniform whole of the nano-pillars up and down takes the shape of teeth with the lower part being small and the upper part being large, and the interface between the nano-pillars and the substrate has a plurality of particle agglomeration, which points to that a plurality of In atom clusters are not yet incorporated into the nano-pillars In the growing process. These In clusters can introduce a large number of surface states to the surface of the nano-pillars, which strongly impair the photoelectrolytic water-producing hydrogen performance.
Example 2
A passivation method based on InN nano-pillars on a p-GaAs substrate and application of the passivation method to photoelectrocatalysis hydrogen production of a passivation end product composite structure thereof comprise the following steps:
(1) Selection of a substrate: a p-GaAs substrate is used.
(2) And (3) cleaning the substrate: firstly, sequentially cleaning a substrate by using acetone and absolute ethyl alcohol, and then removing an oxide layer on the p-GaAs substrate by using 20wt% hydrochloric acid; finally, drying by high-purity dry nitrogen with the purity of 5N;
(3) Growth of InN nano-pillars on p-GaAs substrate: adopting a molecular beam epitaxial growth process, controlling the temperature of the substrate obtained In the step (2) to be 450 ℃, the rotating speed of the substrate to be 10r/min, and the equivalent pressure of In beam to be 5.17 multiplied by 10 -7 And (3) growing InN nano-pillars on the p-GaAs substrate obtained in the step (2) with the nitrogen flow of 2sccm, the plasma source power of 400W and the growth time of 2h, wherein the height of the nano-pillars exceeds 400nm, and the diameter of the nano-pillars is 50nm.
(4) And (3) placing the InN nano-pillar epitaxial wafer on the p-GaAs substrate into a sulfate solution with pH=5, starting electrolysis from 0-1.4V vs. AgCl, and performing electrochemical anode treatment, wherein the number of treatment rounds is 100. And after the electrochemical anode treatment is finished, the passivation is finished, and a passivation final product composite structure is obtained.
Comparative example 1
An application of electro-optic catalysis of InN nano-pillars grown on a p-GaAs substrate without passivation for hydrogen production, comprising the steps of:
(1) Selection of a substrate: a p-GaAs substrate is adopted;
(2) And (3) cleaning the substrate: firstly, sequentially cleaning a substrate by using acetone and absolute ethyl alcohol, and then removing an oxide layer on the p-GaAs substrate by using 20wt% hydrochloric acid; finally, drying by high-purity dry nitrogen;
(3) Growth of InN nano-pillars on p-GaAs substrate: adopting a molecular beam epitaxial growth process, controlling the temperature of the substrate obtained In the step (2) to be 450 ℃, the rotating speed of the substrate to be 10r/min, and the equivalent pressure of In beam to be 5.17 multiplied by 10 -7 4, growing InN nano-pillars on the p-GaAs substrate obtained in the step 2, wherein the height of the nano-pillars exceeds 400nm, and the diameter is about 50nm, and the Torr is that the nitrogen flow is 2sccm, the power of a plasma source is 400W, and the growth time is 2 h; obtaining the InN nano-pillar on the p-GaAs.
The InN nano-column on the passivation final product composite structure prepared in the example 1-2 and the final product p-GaAs prepared in the comparative example 1 is applied to photoelectrolysis of water to produce hydrogen, and the product is required to be manufactured into a photoelectrode, and the specific steps are as follows:
(i) Forming ohmic contact with the back of the p-GaAs by using electron beam evaporation to deposit metal layers Ti and Au;
(ii) Then, connecting the metal wires with the metal layer, and sealing the metal layer by liquid tin soldering;
(iii) Protecting the entire metal back with insulating epoxy;
(iv) The electrochemical workstation is used for photoelectrochemical testing, and the photoelectrochemical testing is specifically as follows:
(1) a phosphate solution with ph=9.4 was used as the electrolyte;
(2) the prepared photoelectrode is used as a cathode, an Ag/AgCl electrode is used as a reference electrode, and a Pt sheet is used as an anode;
(3) xe lamp with 300W power (light intensity 100 mW/cm) 2 ) As a light source.
The test results in a light dark current density versus bias curve, see fig. 7. The passivation final product composite structure prepared In example 1, i.e., p-GaAs/In (As) N photoelectrode, had a photocurrent density of-21.24 mA/cm when biased at-1.00V vs. RHE 2 Dark current density of-1.32 mA/cm 2 The net photocurrent density was 19.92mA/cm 2 The optical gain reaches 1609.10 percent.
The test results in a light dark current density versus bias curve, see fig. 7. The passivation final product composite structure prepared In example 2, i.e., p-GaAs/In (As) N photoelectrode, had a photocurrent density of-21.32 mA/cm when biased at-1.00V vs. RHE 2 Dark current density of-4.17 mA/cm 2 The net photocurrent density was 17.15mA/cm 2 The optical gain reaches 511.27 percent.
The test results in a light dark current density versus bias curve, see fig. 7. The InN nano-pillars on p-GaAs prepared in comparative example 1, i.e., the p-GaAs/InN photoelectrode, had a photocurrent density of-6.28 mA/cm when biased at-1.00V vs. RHE 2 Dark current density of-7.28 mA/cm 2 There was no optical gain, but rather optical quenching, much lower than the effect of example 1.
The test results in a photocurrent density versus time curve, see fig. 8. The passivation final product composite structure prepared In example 1, namely the p-GaAs/In (As) N photoelectrode, when biased at-1.00V vs. RHE, has photocurrent density decreasing first and then increasing under 900s of illumination, and the current decreasing In the short time is caused by the fact that the state of the photoelectrode is not stable yet; the photocurrent density was increased by 36.60% when 900s was reached compared to the lowest photocurrent density point.
The test results in a photocurrent density versus time curve, see fig. 8. The InN nano-pillars on the p-GaAs prepared in comparative example 1, namely the p-GaAs/InN photoelectrodes, continuously decrease the photocurrent density under 900s of illumination when biased at-1.00V vs. RHE. The optical current density was reduced by 48.07% when 900s was reached, compared to the point where the optical current density was stable at the beginning.
The test results in a photocurrent density versus time curve, see fig. 9. The passivation final product composite structure prepared In example 1, namely the p-GaAs/In (As) N photoelectrode can continuously and stably produce hydrogen under the illumination of 7200s after 900s of photocurrent density-time test is carried out under the bias voltage of minus 1.00V vs. When the current reaches the minimum value of the photocurrent density, the current only loses 7.04% compared with the initial photocurrent density stabilization point; the subsequent photocurrent density again began to increase, with a current increase of 12.50% when 7200s was reached.
The above examples and comparative examples show that starting from 0-1.4 v vs. agcl, electrochemical anodic treatment is performed, the passivation scheme with the number of treatment rounds of 200 rounds is better, and the resulting passivation end product composite structure has good and stable effect in application to photoelectrolysis of water to hydrogen production.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention.
Claims (11)
1. The passivation method based on the InN nano-pillar on the p-GaAs substrate is characterized by comprising the following steps:
(1) Growing InN nano-pillars on the p-GaAs substrate by adopting a molecular beam epitaxial growth process;
(2) Applying anode voltage to the InN nano-column on the p-GaAs in an acidic aqueous solution to perform electrochemical anode treatment to obtain a passivation final product composite structure; the acidic aqueous solution is selected from sulfate solution or phosphate buffer solution which does not have electrochemical reducibility; the pH value of the acidic aqueous solution is 4-7; the electrochemical anode treatment process comprises the steps of carrying out electrolysis from 0-1.4V vs. AgCl in each round, wherein the number of treatment rounds is 50-300 rounds; the passivation end product composite structure includes a p-GaAs substrate and an In (As) N nanoribbon grown on the p-GaAs substrate.
2. The method for passivating InN nano-pillars on a p-GaAs substrate according to claim 1, wherein the p-GaAs substrate in step (1) is heavily p-doped gallium arsenide with a doping concentration of 5.1X10 19 cm -3 ～5.8×10 19 cm -3 。
3. The passivation method based on InN nano-pillars on a p-GaAs substrate according to claim 1, wherein the specific conditions of the molecular beam epitaxial growth process in step (1) are as follows: the growth temperature is 350-450 ℃.
4. The passivation method based on InN nano-pillars on a p-GaAs substrate according to claim 1, wherein the specific conditions of the molecular beam epitaxial growth process in step (1) are as follows: equivalent pressure of In beam is 1.58×10 -7 ～5.17×10 -7 Torr。
5. The passivation method based on InN nano-pillars on a p-GaAs substrate according to claim 1, wherein the specific conditions of the molecular beam epitaxial growth process in step (1) are as follows: the rotating speed of the p-GaAs substrate is 5-10 r/min.
6. The passivation method based on InN nano-pillars on a p-GaAs substrate according to claim 1, wherein the specific conditions of the molecular beam epitaxial growth process in step (1) are as follows: the flow rate of the nitrogen is 1-5 sccm.
7. The passivation method based on InN nano-pillars on a p-GaAs substrate according to claim 1, wherein the specific conditions of the molecular beam epitaxial growth process in step (1) are as follows: the power of the plasma source is 200-400W.
8. The passivation method based on InN nano-pillars on a p-GaAs substrate according to claim 1, wherein the specific conditions of the molecular beam epitaxial growth process in step (1) are as follows: the growth time is 1-3 h.
9. The method of passivation of InN nanopillars on p-GaAs substrates according to claim 1, wherein the pH of the acidic aqueous solution of step (2) is 5-7.
10. The method of claim 1, wherein the number of processing cycles in step (2) is 200.
11. A passivation method based on InN nano-pillars on a p-GaAs substrate according to any of claims 1-10, characterized In that the width of the In (As) N nanoribbons In the passivation end product composite structure is from nano-scale to micro-scale, loosely porous nanoribbons.
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| CN109132997A (en) * | 2018-09-29 | 2019-01-04 | 华南理工大学 | (In) the GaN nano-pillar and the preparation method and application thereof being grown on Ti substrate |
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| CN111074344A (en) * | 2019-12-10 | 2020-04-28 | 华南理工大学 | (In) GaN nano-column grown on GaAs substrate and preparation method and application thereof |
| CN113270314A (en) * | 2021-05-13 | 2021-08-17 | 中国科学院半导体研究所 | III group nitride with conical nano structure and preparation method thereof |
| CN114657641A (en) * | 2022-02-22 | 2022-06-24 | 华南理工大学 | Annealed Si-based InN nano-column heterojunction and preparation method and application thereof |
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| CN110747506A (en) * | 2019-10-22 | 2020-02-04 | 华南理工大学 | Transition metal doped InxGa1-xN nano column and preparation method and application thereof |
| CN111074344A (en) * | 2019-12-10 | 2020-04-28 | 华南理工大学 | (In) GaN nano-column grown on GaAs substrate and preparation method and application thereof |
| CN113270314A (en) * | 2021-05-13 | 2021-08-17 | 中国科学院半导体研究所 | III group nitride with conical nano structure and preparation method thereof |
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