CN110112233B - Photoelectric detection structure and device based on silver nanowire-graphene/gallium oxide nano-column and preparation method - Google Patents
Photoelectric detection structure and device based on silver nanowire-graphene/gallium oxide nano-column and preparation method Download PDFInfo
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Abstract
The invention discloses a photoelectric detection structure based on silver nanowires-graphene/gallium oxide nano columns, a corresponding preparation method and a photoelectric detector. The structure includes: the nano-silver film comprises a substrate, a gallium oxide nano-column formed on the substrate and a silver nanowire-graphene composite film formed on the gallium oxide nano-column. The method comprises the steps of generating a gallium oxide nano column on a substrate, transferring the gallium oxide nano column to form a graphene film, and attaching a silver nanowire to the graphene film. The invention has the advantages of simple preparation process, low cost, easy large-scale production and the like. The photoelectric detector has the characteristics of self power supply and good spectrum selectivity, and has the characteristics of high responsivity, high sensitivity and the like for solar blind ultraviolet light.
Description
Technical Field
The invention belongs to the technical field of photoelectric detection, and particularly relates to a photoelectric detection structure based on silver nanowires-graphene/gallium oxide nano-columns, a device and a preparation method. The invention can be applied to solar blind deep ultraviolet detectors.
Background
In recent years, the forbidden band width E of silicon carbide, gallium nitride, aluminum nitride, zinc selenide, zinc oxide, gallium oxide and the like has appearedgCompared with the first two generations of semiconductor materials, the third generation semiconductor material with the grain size larger than 2.3eV has the advantages of large band gap, high breakdown electric field intensity, high saturated electron drift velocity, high thermal conductivity, small dielectric constant, strong radiation resistance and good chemical stability, and is very suitable for developing a radiation-resistant, high-frequency, high-power and high-density integrated semiconductor device. Gallium oxide (Ga)2O3) The band gap of the semiconductor material is 4.2-5.3eV (different crystal structures and optical anisotropy show different band gaps), and the semiconductor material is a direct band gap III-VI wide band gap semiconductor materialThe material has excellent chemical and thermal stability, and is a good third-generation semiconductor material.
Based on Ga2O3The solar blind ultraviolet detector has been reported, the research content is wide, the material morphology comprises nanometer, single crystal and thin film, the device structure comprises metal-semiconductor-metal (MSM) structure, Schottky junction, heterojunction, Avalanche Photodiode (APD) and the like, and some important research results are obtained. alpha-Ga2O3Belongs to Trigonal system (Trigonal), space group is R-3c, and lattice constant is
α＝β＝90°，γ＝120°。α-Ga2O3Possesses an ultra-large band gap of about 4.9eV, and is very suitable for manufacturing solar blind ultraviolet detectors.
Graphene is a crystal of a single atomic layer formed by tightly packing carbon atoms, and has attracted wide attention of scientists with novel structure and performance after being successfully prepared and reported for the first time in 2004 by the university of Manchester in England, and the unique two-dimensional plane structure of graphene endows the graphene with excellent mechanical, thermal, electrical and optical properties. The graphene has great potential as a transparent electrode due to good transmittance and conductivity, the absorption spectrum of the graphene has good transmittance in other wave bands except for an obvious absorption peak at 270nm, and the graphene can meet the requirement of the transparent electrode on optical coupling due to high light transmittance in a large wave band.
The graphene thin film which is discovered recently shows performances which are comparable to those of ITO in the aspects of conductivity, light transmittance and flatness. And the graphene film has the advantages of good chemical stability and low cost. Another advantage is that graphene has a high work function, making ohmic contact with p-type GaN possible. Some important advances have also been made in the large-scale preparation of graphene, where chemically reduced graphite oxide can be stably dispersed in aqueous solutions by electrostatic interaction. The direct CVD method for synthesizing single-layer and several-layer graphene transparent conductive films has also been successful. These advances provide the possibility for applications in graphene LCD, OLED, solar cells, and photodetectors.
Although the carrier mobility of graphene is high, the carrier concentration of graphene is not high, so that the conductivity of graphene still needs to be further improved, and although the surface resistance of graphene can be effectively reduced by a doping method, the stability of doped graphene is damaged. On the other hand, the graphene is inevitably damaged in the transfer process, and the electronic transmission performance of the graphene is greatly influenced by the damaged area.
Disclosure of Invention
Technical problem to be solved
Aiming at the problems in the field, the invention aims to solve the problems that the conductivity of the existing graphene still needs to be further improved and Ga2O3The photoelectric detector has the problem of reduced photoelectric detection rate due to the use of opaque metal as a positive electrode.
(II) technical scheme
In order to solve the above technical problems, in one aspect, the present invention provides a silver nanowire-graphene/gallium oxide nanorod-based photodetection structure, including: a substrate; a gallium oxide nanopillar formed on the substrate; and the silver nanowire-graphene composite film is formed on the gallium oxide nano column.
According to the preferred embodiment of the present invention, the gallium oxide nanocolumn is alpha-phase Ga2O3An array of nanopillars.
According to a preferred embodiment of the invention, the substrate is a transparent substrate.
The invention provides a preparation method of a photoelectric detection structure based on silver nanowire-graphene/gallium oxide nano-columns, which comprises the following steps: generating gallium oxide nano-pillars on a substrate; transferring the gallium oxide nano column to form a graphene film; and attaching silver nanowires on the graphene film.
According to a preferred embodiment of the present invention, the step of growing gallium oxide nanopillars on a substrate comprises: growing a GaOOH nano-pillar array on a substrate; annealing the GaOOH nano-pillar array to generate alpha-Ga2O3An array of nanopillars.
According to a preferred embodiment of the present invention, the step of transferring the graphene film on the gallium oxide nanocolumns comprises: and growing graphene by a chemical vapor deposition method and transferring the graphene to the upper part of the nano-pillar by a wet method to form the graphene film.
According to a preferred embodiment of the present invention, the step of attaching silver nanowires on the graphene thin film comprises: and (3) dripping the silver nanowire solution on the surface of the graphene through a dripping method.
According to a preferred embodiment of the invention, the substrate is a transparent substrate.
A third aspect of the invention provides a photodetector comprising a photodetecting structure as described above.
According to a preferred embodiment of the invention, the detection wavelength lies in the ultraviolet wavelength range.
(III) advantageous effects
The invention has the advantages of simple preparation process, low cost, easy large-scale production and the like. The ultraviolet detector based on the structure has the characteristic of good spectral selectivity, and has the characteristics of high responsivity, high sensitivity and the like for solar blind ultraviolet light.
Drawings
Fig. 1 is a schematic structural view of a solar blind ultraviolet photodetector including a silver nanowire-graphene/gallium oxide nanopillar photodetection structure according to the present invention.
Fig. 2 is a scanning electron microscope image of the silver nanowire-graphene thin film prepared by the method of the present invention.
Fig. 3 is an I-t curve measured by an embodiment of a solar blind ultraviolet photodetector of a photoelectric detection structure including silver nanowire-graphene/gallium oxide nano-pillars, which is manufactured by the method of the present invention, under irradiation of 254nm and 365nm laser.
Fig. 4 is an I-t curve measured by an embodiment of a solar blind ultraviolet photodetector of a photodetection structure including silver nanowire-graphene/gallium oxide nanopillars manufactured by the method of the present invention under irradiation of 254nm laser with different powers.
Detailed Description
The inventor of the present invention has noticed that the silver nanowire-graphene composite structure can effectively overcome the defect of graphene in conductivity, and at the same time, the silver nanowire spans the damaged region of graphene, and can solve the problem of reduced electron transport performance of graphene due to damage. In addition, the silver nanowire-graphene transparent electrode can solve the problems that the traditional metal electrode blocks the incidence of ultraviolet rays, the effective detection area is reduced, and the responsivity and the external quantum effect of the ultraviolet detector pair are affected.
Therefore, the invention provides a photoelectric detection structure, which is characterized in that a gallium oxide nano column is formed on a substrate, and then a silver nanowire-graphene composite film is formed on the gallium oxide nano column. The specific method for forming the silver nanowire-graphene composite film comprises the following steps: and transferring the gallium oxide nano-columns to form a graphene film, and attaching silver nanowires on the graphene film.
Here, the "gallium oxide nanopillar" refers to α -Ga2O3Nanopillar and beta-Ga2O3And (4) nano columns. The gallium oxide nano-column adopted in the invention is preferably alpha-Ga2O3The nano-column is proved to have poor high-temperature resistance of the transparent conductive substrate, the transparent conductive substrate is easy to soften at 700 ℃, the resistance under high temperature becomes very large, and the alpha-Ga prepared by annealing at lower temperature2O3The nano-pillars do not affect the conductivity of the substrate. Said alpha-Ga2O3The cross section of the nano column is quadrilateral or approximate quadrilateral, and through experimental tests, the height of the nano column is preferably 1-2 mu m, and the diagonal length of the cross section is preferably 80-500 nm.
Fig. 1 is a schematic structural view of a solar blind ultraviolet photodetector having a photodetection structure including silver nanowire-graphene/gallium oxide nanopillars according to the present invention, in which a quadrangular prism-shaped gallium oxide nanopillar 2 is formed on a substrate 1, a silver nanowire-graphene composite film 3 is formed thereon, and an electrode 4 is formed on the composite film 3.
The graphene layer is a single-layer or multi-layer graphene film covered on the alpha-Ga2O3Upper end of nano-column, with alpha-Ga2O3The nano-pillars are in close contact. The silver is nanoThe thread was dispersed in an ethanol solution at a concentration of 5 mg/ml. And dripping the Ag nanowire solution on the surface of the graphene by a dripping method, and dripping 20-80 mu L of the Ag nanowire solution.
The substrate in the present invention is preferably a transparent substrate, for example, fluorine-doped SnO2Transparent conductive FTO substrate, indium-doped SnO2A transparent conductive ITO electrode and an aluminum-doped ZnO transparent conductive AZO electrode. The thickness of the substrate is preferably 300-400 nm, and the light transmittance is 85-95%.
The step of growing gallium oxide nanopillars on the substrate is preferably to grow GaOOH nanopillar arrays on the substrate by a hydrothermal method and prepare alpha-Ga by using an annealing method and a high-temperature annealing method2O3An array of nanopillars.
The step of forming a graphene thin film on the gallium oxide nano-pillars is preferably to grow graphene by a chemical vapor deposition method and transfer the graphene to the upper side of the nano-pillars by a wet method to form the graphene thin film. The step of attaching the silver nanowires to the graphene film is preferably to drop a silver nanowire solution on the surface of the graphene film by a drop coating method.
The photoelectric detector provided by the invention comprises the photoelectric detection structure. The detection wavelength is in the ultraviolet wavelength range.
In order that the objects, technical solutions and advantages of the present invention will become more apparent, the present invention will be further described in detail with reference to the accompanying drawings in conjunction with the following specific embodiments. In the examples described below, the substrate used is FTO conductive glass, i.e., SnO doped with fluorine2Transparent conductive glass (SnO)2: F) the thickness was about 350nm, the resistance was 14 ohms, and the light transmittance was 90%.
Example 1:
(1) pretreating an FTO conductive glass substrate: ultrasonic cleaning with acetone, anhydrous alcohol and deionized water for 10min, and drying in oven.
(2) Preparation of alpha-Ga by hydrothermal method and annealing method2O3Nano-pillar array: leaning FTO conductive glass on the inner wall of a stainless steel high-pressure reaction kettle, and adding 5-10 mL of 0.5g/30mL Ga (NO)3)3Growing solution (80% over the substrate), screwing down the reaction kettle, placing in an oven, adding at 150 deg.CAnd heating for 6-12 hours to obtain the GaOOH nano-pillar array growing along the (110) crystal face. After the reaction is completed, the FTO substrate is taken out, washed clean by deionized water and dried at 50 ℃. Then the hydroxyl gallium oxide nano-column array is annealed for 4 hours at 500 ℃ to prepare alpha-Ga2O3An array of nanopillars.
(3) Growing on the surface of copper foil with the thickness of 25um by a chemical vapor deposition method to obtain continuous graphene, spin-coating PMMA with the concentration of 100mg/ml on the surface of the graphene by a spin coater, and baking for 5min at 170 ℃ on a constant temperature table after the spin coating; after baking, the side which is not coated with PMMA is placed into a plasma cleaning machine for treatment for 1min, graphene on the copper foil on the back side is removed, and then PMMA/graphene/copper foil is placed into FeCl with the concentration of 5mol/L3Etching copper foil in the solution for 30min, transferring to deionized water, soaking for 10min, and transferring to new 5mol/L FeCl3Etching the residual copper foil in the solution for 2h to remove floccules on the copper foil, transferring the completely etched copper foil to deionized water to clean the residual FeCl3Etching solution, transferring to dilute hydrochloric acid to further clean FeCl remained on the surface of the etching solution3Etching liquid and other impurities, finally transferring the graphene film into deionized water to clean residual hydrochloric acid on the surface of the graphene film, and after cleaning is finished, beating the graphene film for 15min by using a plasma cleaning machine to obtain SiO2Obtaining a sample PMMA/graphene/SiO by taking PMMA/graphene with Si2/Si；
(4) Mixing PMMA/graphene/alpha-Ga2O3After the nano-column/FTO sample is air-dried for 8 hours, completely baking the sample on a constant temperature table, and then putting the sample into a dichloromethane solution at 40 ℃ to remove PMMA glue;
(5) the silver nanowires are dispersed in an ethanol solution, and the concentration of the solution is 5 mg/ml. The silver nanowire solution is dripped on the surface of the graphene by a dripping method, and 20 mu L of the silver nanowire solution is dripped. The silver nanowire has a length of 50 μm and a diameter of 150 nm. And (3) dripping the silver nanowire dispersion liquid on the surface of the graphene by a dripping method, and then baking the graphene on a constant temperature table at the temperature of 100-140 ℃ for 10-15 min.
(6) And depositing a Ti/Au point electrode on the surface of the graphene film by utilizing a mask and a radio frequency magnetron sputtering technology to serve as a measuring electrode. Sputtering ofThe conditions were as follows: back bottom vacuum of 1X 10-4Pa, the substrate temperature is room temperature, the working atmosphere is Ar gas, the working pressure is 0.8Pa, the sputtering power is 40W, the sputtering time of the Ti layer is 30s, and the sputtering time of the Au layer is 70 s.
The solar blind ultraviolet detector manufactured by the embodiment and comprising the structure has the following performance characteristics:
fig. 2 is a scanning electron microscope image of the silver nanowire-graphene composite electrode fabricated in the above example.
Fig. 3 is an I-t curve measured by an embodiment of a solar blind ultraviolet photodetector of a photoelectric detection structure including silver nanowire-graphene/gallium oxide nano-pillars, which is manufactured by the method of the present invention, under irradiation of 254nm and 365nm laser. It can be seen that the detector prepared by the method of the invention has obvious response to 254nm laser and almost no response to 365nm laser.
Fig. 4 is an I-t curve measured by an embodiment of a solar blind ultraviolet photodetector of a photodetection structure including silver nanowire-graphene/gallium oxide nanopillars manufactured by the method of the present invention under irradiation of 254nm laser with different powers. It can be seen that: alpha-Ga under the illumination of 254nm wavelength light with different powers2O3The nanopillar array detector showed a clear response and the responsivity increased with increasing power of the 254nm laser.
Example 2
The dropping amount of the silver nanowire in example 1 was changed, and 40 μ L of the silver nanowire was dropped on the graphene to prepare silver nanowire-graphene- α -Ga2O3A nanopillar array solar blind ultraviolet detector. The I-t curve was measured at a voltage of 0 volts and it was found that the current instantaneously changed when the uv lamp was switched on and off, indicating that the detector had high sensitivity under 254nm uv irradiation in the solar dead zone.
Example 3
The dropping amount of the silver nanowire in example 1 was changed, and 40 μ L of the silver nanowire was dropped on the graphene to prepare silver nanowire-graphene- α -Ga2O3A nanopillar array solar blind ultraviolet detector. The I-t curve was measured at a voltage of 0 volts and it was found that the current instantaneously changed when the UV lamp was turned on and off, indicating that the detector was operating atThe solar blind area has high sensitivity under the irradiation of 254nm ultraviolet light.
Example 4
The steps (1), (2), (3) and (4) are the same as those in the embodiment 1, and after the step (4) is finished, a piece of completely etched and cleaned graphene is fished by the obtained graphene/nano column/FTO sample. Mixing PMMA/double-layer graphene/alpha-Ga2O3After the nano-column/FTO sample is air-dried for 8 hours, completely baking the sample on a constant temperature table, and then putting the sample into a dichloromethane solution at 40 ℃ to remove PMMA glue; obtaining a sample of double-layer graphene/alpha-Ga2O3nano-pillars/FTO;
the obtained double-layer graphene/alpha-Ga2O3The nano-pillar/FTO structure is similar to example 1. Based on double-layer graphene/alpha-Ga2O3The voltage is applied to two ends of an electrode of the solar blind type ultraviolet detector of the nano-column/FTO to measure the photoelectric performance, an I-t curve is measured under the voltage of 0 volt, and the current changes instantly when the ultraviolet lamp is controlled to be switched on and switched off, which shows that the detector has high sensitivity under the irradiation of 254nm ultraviolet light in the solar blind area. The test results were all similar to example 1.
According to the embodiment, the silver nanowires and the graphene are compounded, the silver wires play a role in connecting high-crystal-boundary particles, replace high-crystal-boundary parts with poor conductivity and damaged parts generated in the graphene transfer process, and become a new carrier transmission path, so that the carrier efficiency can be greatly improved.
alpha-Ga prepared by the invention2O3The nano-pillar array has the advantages of controllable appearance, uniform size, simple preparation process, low cost, easy large-scale production and the like. The ultraviolet detector based on the structure has the characteristics of self power supply and good spectrum selectivity, and has the characteristics of high responsivity, high sensitivity and the like for solar blind ultraviolet light.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. A photoelectric detection structure based on silver nanowire-graphene/gallium oxide nano-pillars is characterized by comprising:
a transparent substrate; wherein the transparent substrate is SnO doped with fluorine2Transparent conductive FTO substrate, indium-doped SnO2A transparent conductive ITO electrode or an aluminum-doped ZnO transparent conductive AZO electrode;
the gallium oxide nano column is formed on the transparent substrate; wherein the gallium oxide nano-column is alpha-phase Ga2O3The array, and the step of generating the gallium oxide nano-pillars on the transparent substrate comprises: growing a GaOOH nano-pillar array on a substrate by a hydrothermal method; annealing the GaOOH nano-pillar array at 500 ℃ to generate alpha-Ga2O3A nanopillar array;
the silver nanowire-graphene composite film is formed on the gallium oxide nano column, and the forming steps comprise: growing graphene by a chemical vapor deposition method, transferring the graphene to the upper part of the gallium oxide nano column by a wet method to form a graphene film, and attaching a silver nanowire to the graphene film; wherein the silver nanowire has a length of 50 μm and a diameter of 150 nm.
2. A preparation method of a photoelectric detection structure based on silver nanowires-graphene/gallium oxide nano columns is characterized by comprising the following steps:
generating a GaOOH nano-pillar array on a transparent substrate by a hydrothermal method; annealing the GaOOH nano-pillar array at 500 ℃ to generate alpha-Ga2O3A nanopillar array; wherein the transparent substrate is SnO doped with fluorine2Transparent conductive FTO substrate, indium-doped SnO2A transparent conductive ITO electrode or an aluminum-doped ZnO transparent conductive AZO electrode;
growing graphene by chemical vapor deposition and transferring it to the alpha-Ga by wet process2O3Forming a graphene film above the nano-pillar array;
attaching silver nanowires to the graphene film; wherein the silver nanowire has a length of 50 μm and a diameter of 150 nm.
3. The method of claim 2, wherein the step of attaching silver nanowires on the graphene thin film comprises: and (3) dripping the silver nanowire solution on the surface of the graphene through a dripping method.
4. A uv photodetector comprising the photodetecting structure according to claim 1.
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