CN112382691A - Self-powered detector containing gallium nitride/gallium oxide nano-pillar array and preparation method - Google Patents
Self-powered detector containing gallium nitride/gallium oxide nano-pillar array and preparation method Download PDFInfo
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- CN112382691A CN112382691A CN202011107111.4A CN202011107111A CN112382691A CN 112382691 A CN112382691 A CN 112382691A CN 202011107111 A CN202011107111 A CN 202011107111A CN 112382691 A CN112382691 A CN 112382691A
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Abstract
The invention belongs to the technical field of photoelectric detectors, and particularly relates to a self-powered detector containing a gallium nitride/gallium oxide nano-pillar array and a preparation method thereof. The detector is structurally characterized by comprising electrodes, a flexible substrate, a p-type gallium nitride layer, a beta-gallium oxide nano-column array and electrodes which are sequentially arranged, wherein a filling layer wraps the side face of the beta-gallium oxide nano-column array and is used for filling the beta-gallium oxide nano-column array, and a graphene transparent electrode is further arranged between the beta-gallium oxide nano-column array and the electrodes. The heterojunction formed by the gallium nitride/gallium oxide nano-column array is used as a core of the device, the gallium oxide nano-array is prepared on the gallium nitride film, the interface between the gallium oxide and the gallium nitride has small lattice mismatch and low conduction band offset, the performance of a high photoelectric detector can be further improved, the detector can be driven to work without an external power supply, the use range of the detector is further expanded, and the device has potential application prospects in the field of solar blind ultraviolet detection.
Description
Technical Field
The invention belongs to the technical field of photoelectric detectors, and particularly relates to a self-powered detector containing a gallium nitride/gallium oxide nano-pillar array and a preparation method thereof.
Background
Because of its strong absorption ability, stratospheric ozone is called a solar blind zone because ultraviolet rays of 280nm or less from the sun cannot penetrate the atmosphere to reach the earth's surface. The solar blind photodetector is a photodetector operating in this area. Since interference from solar radiation can be avoided, very weak signals can be accurately detected under daylight illumination. Therefore, solar blind photodetectors have many potential applications, such as in the fields of missile alarming and tracking, high voltage arc discharge detection, ozone monitoring, and non-line-of-sight optical communications.
Since wide bandgap oxide semiconductor materials have the characteristics of large bandgap, solution processability, low cost, environmental protection, etc., many heterojunction structures based on wide bandgap semiconductors have been proven to be capable of realizing solar blind photodetectors. It is well known that practical applications of photodetectors require fast response speed, high signal-to-noise ratio, low power consumption and low manufacturing costs, and that most detectors are of the photoconductive type, with relatively slow response speed, and in addition, usually require an external power supply to separate the photo-generated electron-hole pairs, obtaining the desired responsivity, which not only greatly increases the size and power consumption of the device, but also greatly limits their range of use. Therefore, it is important to produce a high performance self-powered photodetector that can operate without an external power source.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide a self-powered solar blind photodetector with high sensitivity and fast response speed without consuming external power, and to provide a self-powered solar blind photodetector comprising a gan/gan nanorod array and a method for manufacturing the same.
The technical content of the invention is as follows:
the invention provides a self-powered detector containing a gallium nitride/gallium oxide nano-pillar array, which is a structure comprising a flexible substrate, a p-type gallium nitride layer, a beta-gallium oxide nano-pillar array, a filling layer and an electrode;
the detector is structurally characterized by comprising an electrode, a flexible substrate, a p-type gallium nitride layer, a beta-gallium oxide nano-column array and an electrode which are sequentially arranged, wherein a filling layer wraps the side surface of the beta-gallium oxide nano-column array and is used for filling the beta-gallium oxide nano-column array;
a graphene transparent electrode is further arranged between the beta-gallium oxide nano-column array and the electrode, and the thickness of the graphene transparent electrode is 150-200 nm;
the flexible substrate comprises one of transparent conductive flexible substrates such as polyethylene terephthalate (PET), a polyimide substrate, a polypropylene hexamethylene diester substrate and the like, the thickness of the flexible substrate is 70-80 mu m, and the transparent conductive flexible substrate has good optical transparency and low resistivity, so that the flexibility and the light absorption rate of the photoelectric detection device can be improved by using the transparent conductive substrate as the flexible transparent conductive substrate, and higher sensitivity is obtained;
the material of the filling layer (also called a dielectric layer) comprises PMMA;
the electrodes comprise Ti/Au electrodes with the thickness of 100-200 nm;
the growth structure of the p-type gallium nitride layer sequentially comprises a sapphire substrate, a GaN buffer layer, a heavily doped n-GaN layer and a p-type GaN layer, wherein the growth thicknesses of the GaN buffer layer, the heavily doped n-GaN layer and the p-type GaN are respectively 25-30nm, 2-3 mu m and 300-400 nm.
The beta-gallium oxide nanorod array is vertically adsorbed on the p-type gallium nitride layer by taking gallium metal as a gallium vapor source through a CVD (chemical vapor deposition) process, and the p-type gallium nitride and the beta-gallium oxide form a two-dimensional heterojunction with a vertical structure;
the diameter of the beta-gallium oxide nano column is 50-150nm, the length of the beta-gallium oxide nano column is 1-1.5 mu m, and the gallium oxide nano column array is used for replacing a traditional three-dimensional structure, so that the carrier mobility is improved, the light absorption coefficient is improved, and the photoelectric detector has higher sensitivity and higher response speed;
the invention also provides a preparation method of the self-powered detector containing the gallium nitride/gallium oxide nano-pillar array, which comprises the following steps:
1) cleaning the flexible substrate: sequentially soaking the substrate in acetone, ethanol and deionized water, performing ultrasonic treatment, taking out, washing with deionized water, and drying with dry N2Drying for later use;
2) preparing a p-type gallium nitride layer: growing a GaN layer on a sapphire substrate by adopting an MOCVD method, sequentially epitaxially growing a 25-30nmGaN buffer layer, a 2-3 mu m heavily doped n-GaN layer and a 300-400nm Mg-doped P-type GaN layer, and then corroding the heavily doped n-GaN layer by adopting an electrochemical corrosion method to obtain a P-type gallium nitride layer;
3) preparing a beta-gallium oxide nano-pillar array: forming a beta-gallium oxide nanorod array on the p-type gallium nitride layer by using metal gallium as a vapor source through a CVD (chemical vapor deposition) process, spin-coating a PMMA (polymethyl methacrylate) layer on the side surface of the beta-gallium oxide nanorod array, and curing PMMA;
4) preparing a graphene transparent electrode: growing graphene on a Cu substrate with a PMMA layer on the top by a CVD (chemical vapor deposition) process, etching the Cu substrate for separation, transferring the separated graphene to the beta-gallium oxide nano-column array obtained in the step 3), drying and cleaning to obtain a graphene transparent electrode;
5) etching the formed two-dimensional heterojunction of the p-type gallium nitride and the beta-gallium oxide nano-column array by an electrochemical stripping method to heavily dope n-GaN, and transferring the heterojunction onto the flexible substrate in the step 1) after removing the heterojunction;
6) and respectively depositing Ti/Au electrodes on the flexible substrate and the graphene transparent electrode, and mutually connecting to form a passage, thus obtaining the self-powered detector.
Step 3) the CVD preparation process of the beta-gallium oxide nanorod array comprises the steps of depositing Au on a p-type gallium nitride substrate, then placing the p-type gallium nitride substrate in a quartz tube, taking gallium metal as a gallium vapor source, and reacting to form the beta-gallium oxide nanorod, wherein the specific operation comprises the following steps:
first at 10-5In vacuum of a support, depositing Au on a p-type gallium nitride/sapphire substrate, and annealing at 600 ℃ for 1h to form gold nanoparticles;
using gallium metal with the purity of 99.999 percent as a gallium vapor source, placing 0.5g of Ga in a quartz boat, and clamping a p-type gallium nitride/sapphire substrate with an Au coating on the quartz boat;
placing a quartz boat in the center of a conventional horizontal tube furnace, setting the temperature in the tube at 900 ℃, the heating rate at 10 ℃/min, and keeping the constant argon (Ar) flow of 100-120 bubbles per minute in the quartz tube for 6 hours in the growth process;
and after the completion, naturally cooling the CVD system to obtain the beta-gallium oxide nano-pillar array.
And 4) after drying, cleaning the top PMMA layer by using acetone and deionized water.
The working principle of the self-powered solar blind photoelectric detector based on the gallium nitride/gallium oxide nano-pillar array heterojunction is as follows: the heterojunction is formed on the contact surface of the gallium nitride and the gallium oxide nano-pillar array, the compressive stress is applied to the gallium nitride by utilizing the photoelectric piezoelectric effect of the gallium nitride, negative piezoelectric charges are generated on an interface close to the gallium oxide, so that the energy band of the gallium nitride is improved, meanwhile, a built-in electric field is enhanced, light is decomposed more quickly, and the electron mobility is improved.
The invention has the beneficial effects that:
the self-powered detector based on the heterojunction of the gallium nitride/gallium oxide nano-pillar array takes the heterojunction formed by the gallium nitride/gallium oxide nano-pillar array as the core of a device, utilizes the piezoelectric photoelectric effect of gallium nitride to adjust the height of a potential barrier, and effectively controls the transmission of carriers, thereby manufacturing a self-powered solar-blind photoelectric detector, and having potential application prospect in the field of solar-blind ultraviolet detection;
in the preparation method of the self-powered detector, the gallium oxide nano array is prepared on the gallium nitride film, and the interface between the gallium oxide and the gallium nitride has small lattice mismatch and low conduction band offset, so that the performance of a high photoelectric detector can be further improved; the transparent conductive graphene electrode is adopted, and the graphene has high conductivity and optical transparency in the whole wavelength range, so that the graphene can be used as the transparent conductive electrode to improve the absorption coefficient of a photoelectric detector and obtain higher responsivity; adopt flexible transparent conductive substrate PET for the detector flexible is folding, not only can be applied to fields such as wearable ultraviolet detection of portable, and inside production presses electric potential when the detector is crooked moreover, makes and need not external power supply and orders about detector work, further enlarges the application range of detector.
Drawings
Fig. 1 is a schematic structural diagram of a self-powered detector based on a gan/gan nanopillar array according to the present invention, wherein the arrow indicates the c-axis direction of gan;
FIG. 2 is a schematic structural diagram of a p-type gallium nitride layer prepared according to the present invention;
FIG. 3 is a flow chart of the fabrication of a self-powered detector based on GaN/GaN nanorod arrays according to the present invention;
FIG. 4 is a schematic illustration of the preparation of a beta-gallium oxide nanoarray in a tube furnace according to the present invention;
FIG. 5 is a band diagram of GaN and GaN oxides according to the invention;
FIG. 6 is an energy band diagram of a GaN/GaN nanorod heterojunction of the present invention;
FIG. 7 is an energy band diagram and carrier transport of a GaN/GaN nanorod heterojunction under strain according to the present invention;
FIG. 8 is a semi-logarithmic graph of the I-V curve of a heterojunction solar-blind UV photodetector with GaN/GaN nanoarrays prepared by the present invention;
FIG. 9 is a graph of the I-V curves of a photodetector with a graphene electrode and a photodetector with a Ti/Au electrode according to the present invention in a semi-logarithmic manner.
Detailed Description
The present invention is described in further detail below by way of specific embodiments and accompanying illustrations, it being understood that these examples are intended only to illustrate the invention and not to limit the scope of the invention, which is defined by the claims appended hereto, as modified by those skilled in the art to which the invention pertains, after reading the present disclosure, and all equivalent forms thereof.
All the raw materials and reagents of the invention are conventional market raw materials and reagents unless otherwise specified.
Example 1
A self-powered solar blind photoelectric detector based on a gallium nitride/gallium oxide nano-pillar array heterojunction:
the schematic structural diagram of the photodetector is shown in fig. 1, and the photodetector comprises a PET flexible substrate 1, a p-type gallium nitride layer 2, a PMMA filling layer 3, a beta-gallium oxide nanorod array 4, a graphene transparent conductive electrode 5 and a Ti/Au electrode 6;
the growth structure schematic diagram of the P-type gallium nitride layer 2 is shown in fig. 2, and the P-type gallium nitride layer comprises a sapphire substrate 7, a GaN buffer layer 8, a heavily doped n-GaN layer 9 and a Mg-doped P-type GaN layer 2.
Example 2
A schematic flow chart of a process for preparing a self-powered solar-blind photodetector based on a gallium nitride/gallium oxide nanorod array heterojunction is shown in fig. 3:
1) cleaning the flexible substrate: sequentially soaking the PET substrate 1 in acetone, ethanol and deionized water, performing ultrasonic treatment for 10 minutes respectively, taking out, washing with deionized water, and finally washing with dry N2Drying for later use;
2) preparing a p-type gallium nitride layer: sequentially growing a 25-30nm GaN buffer layer 8, a 2-3 mu m heavily doped n-GaN layer 9 and a 300-400nm Mg doped P-GaN layer 2 on the C surface of the sapphire substrate 7 by using MOCVD equipment;
3) preparing a beta-gallium oxide nano-pillar array: forming a beta-gallium oxide nanorod array on the p-type gallium nitride layer 2 by using gallium metal as a vapor source through a CVD (chemical vapor deposition) process, as shown in FIG. 4, specifically comprising the following steps:
a. au is deposited on the p-type gallium nitride layer 2 obtained in step two, at 10-5Annealing for 1 hour at 600 ℃ in vacuum to form gold nanoparticles;
b. using Ga metal 17 (purity: 99.999%) as a Ga vapor source, 0.5g of Ga metal 17 was put into a quartz boat 16, and an Au-coated substrate was sandwiched on the boat, the whole system was loaded in the center of a quartz tube 13, and the quartz tube 13 was placed in tube furnaces 14, 15 at a temperature of 900 ℃ and a heating rate of 10 ℃ for min-1For 6 hours;
c. in the growth process, the flow controller 12 is used to keep the constant argon flow of 100-120 bubbles/min in the quartz tube 13, and after the treatment is finished, the CVD system is naturally cooled;
spin-coating a PMMA layer 3 on the beta-gallium oxide nano-pillar array 4, wherein the beta-gallium oxide nano-pillar array is wrapped in the PMMA layer by the PMMA layer, the end part of gallium oxide is exposed, and then the PMMA layer is cured;
4) preparing a graphene transparent electrode: growing graphene on a Cu substrate with a top PMMA layer by a CVD (chemical vapor deposition) process, etching the Cu substrate by beta-gallium oxide for separation, transferring the separated graphene to the beta-gallium oxide nano-column array obtained in the step 3), drying at 110 ℃ for 30 minutes, and cleaning the top PMMA layer by using acetone and deionized water to obtain a graphene transparent electrode;
5) the heavily doped n-GaN layer 9 is etched by electrochemical etching: pretreating the sapphire substrate by using a laser linear cutting mode, thinning the sapphire substrate 7 to be 100m thick, combining deionized water to prepare a selective etching solution (0.3mol/L oxalic acid solution), carrying out electrochemical etching by using a direct-current constant-voltage power supply, wherein bubbles are generated along with the generation of reaction in the electrochemical etching process, and if no bubbles are generated around n-GaN, the etching is finished;
transferring the gallium nitride/gallium oxide heterojunction structure separated from the heavily doped n-GaN layer 9 to a flexible substrate PET1 processed by S1;
6) Ti/Au electrodes 6 with the thickness of 100-200nm are respectively deposited on the PET flexible substrate 1 and the graphene transparent electrode 5 through a mask plate and are mutually connected to form a passage, and then the self-powered solar blind photodetector is obtained.
As shown in FIG. 5, which is an energy band diagram of GaN and gallium oxide prepared in the example, it can be seen that the band gap of p-type GaN is 3.4eV, and the band gap of gallium oxide is 4.9 eV. The conduction band spacing between gallium nitride and gallium oxide is 0.74eV, and the valence band spacing is 0.78 eV;
as shown in fig. 6, which is an energy band diagram of a heterojunction formed by contacting gallium nitride/gallium oxide nano-pillars prepared in the example, it can be seen from the diagram that diffusion and transfer of carriers occur between the gallium nitride/gallium oxide nano-pillars until thermal equilibrium is reached and fermi level is equal everywhere in the heterojunction. At this time, a positive space charge region is formed on one side of the N region of the interface, and the band bends downwardKoji; a negative space charge region is formed on one side of the interface P region, and the energy band is bent upwards; the junction barrier is formed at the interface, so that the dark current of the photoelectric detector can be effectively reduced, and as shown in fig. 8, the dark current of the photoelectric detector under zero bias is only 5.1 × 10-12A。
Fig. 7 shows a schematic diagram of an energy band diagram and carrier transmission when compressive stress is applied to the c-axis direction of p-type gallium nitride under unbiased illumination of the gallium nitride/gallium oxide nanorod heterojunction prepared in the example, and it can be seen from the diagram that negative piezoelectric charges are generated at an interface close to the gallium oxide, the energy band of the gallium nitride is increased, and meanwhile, a built-in electric field is enhanced, so that more light is absorbed and decomposed faster, and the response and carrier transfer rate of the photodetector are improved.
FIG. 8 shows the dark, 254nm illumination (200 μ W/cm) of the GaN/GaN nanoarray heterojunction solar-blind UV photodetector prepared in the example2) And 254nm illumination (200. mu.W/cm) at a compression set of 3.6%2) The semi-logarithmic graph of the I-V curve of (1). As can be seen, the illumination was at 254nm (200. mu.W/cm)2) At zero bias, the current goes from 5.1X 10 in dark-12A increases to only 7.3X 10-10The self-powered effect is not obvious;
but with 3.6% compressive stress on p-type gallium nitride, the zero bias extrusion current increased greatly to 2.9 x 10-7A. Compared with dark current, the light-emitting diode has an improved dark current by 5 orders of magnitude, and compared with the light only at 254nm (200 muW/cm)2) The current is increased by 3 orders of magnitude, and the piezoelectric photoelectric effect of the gallium nitride is proved to effectively adjust the height of a potential barrier and control the transmission of carriers, so that the solar blind photoelectric detector with zero power consumption is realized, and the solar blind photoelectric detector has considerable development prospect in the field of solar blind ultraviolet detection.
FIG. 9 shows the photo-detector using graphene electrode and the photo-detector using Ti/Au electrode prepared in example under 254nm illumination (200 μ W/cm)2) The following semi-logarithmic plot of the I-V curve, from which it can be seen that the excellent UV transparency of the graphene electrode provides enhanced UV photodetector light collection, and thus the beta-Ga with graphene top electrode2O3the/GaN ultraviolet photoelectric detector has higher photocurrent than the Au/Ti electrode.
Claims (10)
1. A self-powered detector containing a gallium nitride/gallium oxide nanorod array is characterized by comprising a flexible substrate, a p-type gallium nitride layer, a beta-gallium oxide nanorod array, a filling layer and an electrode.
2. The self-powered detector as claimed in claim 1, wherein the detector is structured by sequentially arranging an electrode, a flexible substrate, a p-type gallium nitride layer, a beta-gallium oxide nanorod array and an electrode, and the filling layer wraps the side surface of the beta-gallium oxide nanorod array.
3. The self-powered probe of claim 2, wherein the array of beta-gallium oxide nanopillars and the electrodes further comprise graphene transparent electrodes therebetween.
4. A self-powered probe as defined in claim 1 or 2 wherein the flexible substrate comprises one of a polyethylene terephthalate substrate, a polyimide substrate, a polypropylene adipate substrate.
5. A self-powered probe as claimed in claim 1 or 2, characterised in that the material of the filling layer comprises PMMA.
6. A self-powered probe as claimed in claim 1 or 2, wherein the gallium nitride layer is structured as a sapphire substrate, a GaN buffer layer, a heavily doped n-GaN layer and a p-type GaN, arranged in sequence.
7. A self-powered detector as claimed in claim 1 or 2, wherein the β -gan nanopillar array is a two-dimensional heterojunction with a vertical structure formed by p-gan and β -gan, wherein the p-gan layer is vertically adsorbed on the p-gan layer by CVD process using gallium metal as a gallium vapor source.
8. The preparation method of the self-powered detector of the GaN/GaN-containing nano-pillar array according to any of claims 1 to 7, comprising the following steps:
1) cleaning the flexible substrate;
2) preparing a p-type gallium nitride layer;
3) preparing a beta-gallium oxide nano-pillar array: forming a beta-gallium oxide nano-pillar array on the p-type gallium nitride layer through a CVD (chemical vapor deposition) process, spin-coating a PMMA (polymethyl methacrylate) layer on the side surface of the beta-gallium oxide nano-pillar array, and curing PMMA;
4) preparing a graphene transparent electrode: growing graphene on a Cu substrate with a PMMA layer at the top, etching the Cu substrate for separation, transferring the separated graphene to the beta-gallium oxide nano-column array obtained in the step 3), drying and cleaning to obtain a graphene transparent electrode;
5) transferring the formed two-dimensional heterojunction of the p-type gallium nitride and the beta-gallium oxide nano-pillar array to the flexible substrate in the step 1);
6) and respectively depositing Ti/Au electrodes on the flexible substrate and the graphene transparent electrode, and mutually connecting to form a passage, thus obtaining the self-powered detector.
9. The method for manufacturing a self-powered detector as claimed in claim 8, wherein the p-type gallium nitride layer in step 2) is manufactured by sequentially epitaxially growing a GaN buffer layer, a heavily doped n-GaN layer and p-type GaN on a sapphire substrate by MOCVD, and then etching the heavily doped n-GaN layer to obtain the total p-type gallium nitride layer.
10. The method for preparing a self-powered detector as claimed in claim 8, wherein the CVD process for preparing the beta-gallium oxide nanorod array in step 3) comprises depositing Au on a p-type gallium nitride layer, placing the p-type gallium nitride layer in a quartz tube, and reacting to form the beta-gallium oxide nanorod by using gallium metal as a gallium vapor source.
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