CN112071652B - Three-dimensional hedgehog-shaped ZnO/SnO2Heterostructure, preparation method thereof and application thereof in ultraviolet detector - Google Patents
Three-dimensional hedgehog-shaped ZnO/SnO2Heterostructure, preparation method thereof and application thereof in ultraviolet detector Download PDFInfo
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Abstract
The invention discloses three-dimensional hedgehog shaped ZnO/SnO2Heterostructure, preparation method and application thereof, wherein the heterostructure is composed of ZnO nanorod and SnO2Octahedral blocks, SnO2Octahedron on the substrate, ZnO nano-rod on SnO2The whole surface of the octahedral block is in a hedgehog structure. The invention uses the solution synthesis method to grow large-area hedgehog-shaped ZnO/SnO on the substrate2And the heterostructure is further used as a working electrode, Pt is used as a counter electrode, the two electrodes are connected through a heat sealing film, and iodine electrolyte or deionized water is injected into the middle of the device to obtain the ultraviolet detector with good self-energy supply characteristic, and the heterostructure is applied to the field of ultraviolet detection. The method is simple to operate, low in cost, suitable for large-scale production and high in practical value.
Description
Technical Field
The invention belongs to the technical field of semiconductor detection materials and preparation thereof, and relates to hedgehog-shaped ZnO/SnO2Heterostructure, preparation method and application in ultraviolet detector.
Background
The ultraviolet detector is widely applied to the national defense military and civil fields such as missile early warning, communication, environment monitoring and the like, and the traditional ultraviolet detector has large volume, needs an external power supply and has higher manufacturing and maintenance cost, so that the practical application of the ultraviolet detector is limited to a certain extent. Therefore, the semiconductor self-powered ultraviolet detector which can realize quick response and tiny signal detection to ultraviolet light under the condition of no external voltage and has low cost and easy preparation becomes the current research hotspot.
SnO2As a wide band gap (3.6 eV) semiconductor metal oxide, it is considered to be one of the most promising photodetection materials due to its advantages such as high electron mobility, large exciton confinement energy (130 meV), and good chemical stability. However, the rapid recombination of photogenerated carriers reduces the SnO-based2Performance and sensitivity of the ultraviolet detector. In order to improve SnO2Ultraviolet detecting property of, andother semiconductor materials are an effective method of building heterostructures. ZnO is II-VI family direct band gap semiconductor material, the forbidden band width is 3.37 eV at room temperature, the exciton binding energy is 60 meV, and the material is SnO2A typical type II band structure can be formed. Thus, ZnO is considered to be a metal in combination with SnO2Coupled to improve its ultraviolet detection properties.
Recently, three-dimensional nano materials with special shapes formed by one-dimensional and two-dimensional structure units are concerned, and have potential application prospects in the field of photoelectric detection due to the fact that the three-dimensional nano materials not only have the characteristics of one-dimensional and two-dimensional structures, but also have unique excellent performances. At present, three-dimensional ZnO/SnO is reported2The preparation method of the heterostructure mainly comprises methods of chemical vapor deposition, thermal evaporation, electrodeposition and the like, but the methods are complex to operate, high in cost and not beneficial to application and popularization, mainly focuses on the fields of photocatalysis, gas-sensitive sensing and the like, and is not applied to an ultraviolet detector. Therefore, a method with simple process and low cost for preparing three-dimensional ZnO/SnO is found2The heterostructure ultraviolet detector has important significance. Currently, special hedgehog shaped ZnO/SnO is prepared by solution method2No methods have been reported for heterostructures and application in uv detectors.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides three-dimensional hedgehog shaped ZnO/SnO2A heterostructure, a method of making the same and applications thereof. The invention uses the solution synthesis method to grow large-area hedgehog-shaped ZnO/SnO on the substrate2And the heterostructure is further used as a working electrode, Pt is used as a counter electrode, the two electrodes are connected through a heat sealing film, and iodine electrolyte or deionized water is injected into the middle of the device, so that the ultraviolet detector with good self-energy supply characteristic is obtained and is applied to the field of ultraviolet detection. The method is simple to operate, low in cost, suitable for large-scale production and high in practical value.
The purpose of the invention is realized by the following technical scheme:
three-dimensional hedgehog-shaped ZnO/SnO2Heterostructure of ZnO nanorodsAnd SnO2Octahedral block, ZnO nano-rod grown on SnO2The whole surface of the octahedral block is in a hedgehog structure.
The three-dimensional hedgehog shaped ZnO/SnO2A method of fabricating a heterostructure comprising the steps of:
step one, sequentially carrying out ultrasonic cleaning on a substrate in acetone, ethanol and deionized water for 10-30 minutes, then sputtering a ZnO film with the thickness of 200 nm-3 mu m on a conductive surface of the substrate, and annealing for 1-3 hours at 300-500 ℃ in air;
step two, vertically placing the substrate sputtered with the ZnO film into a beaker containing stannous fluoride solution with the concentration of 0.03-0.07 mol/L for reaction for 1-4 hours at room temperature, naturally airing, annealing for 1-3 hours at the temperature of 400-600 ℃ in the air, and taking out the substrate after the annealing furnace is cooled;
step three, growing SnO2Sputtering a ZnO seed layer with the thickness of 5-30 nm on the substrate, and then putting the substrate into a vacuum annealing furnace to anneal for 1-3 hours at the temperature of 300-500 ℃ in the air;
step four, vertically placing the substrate in the step three into a reaction kettle containing a mixed solution of zinc acetate and hexamethylenetetramine with the concentration of 0.01-0.03 mol/L, preserving the heat for 1-6 hours at the temperature of 80-120 ℃, taking out the substrate after cooling to the room temperature, dripping deionized water on the surface of the substrate, and naturally drying the substrate to obtain hedgehog ZnO/SnO2A nanostructured material.
The three-dimensional hedgehog shaped ZnO/SnO2The heterostructure can be used in an ultraviolet detector grown with hedgehog shaped ZnO/SnO2The substrate of the heterostructure is a working electrode, the working electrode and a counter electrode are connected through a heat sealing film, iodine electrolyte or deionized water is injected between the two electrodes to serve as electrolyte, and the specific manufacturing method is as follows:
step one, sequentially carrying out ultrasonic cleaning on a substrate in acetone, ethanol and deionized water for 10-30 minutes, then sputtering a ZnO film with the thickness of 200 nm-3 mu m on a conductive surface of the substrate, and annealing for 1-3 hours at 300-500 ℃ in air;
step two, vertically placing the substrate sputtered with the ZnO film into a beaker containing stannous fluoride solution with the concentration of 0.03-0.07 mol/L for reaction for 1-4 hours at room temperature, naturally airing, annealing for 1-3 hours at the temperature of 400-600 ℃ in the air, and taking out the substrate after the annealing furnace is cooled;
step three, growing SnO2Sputtering a ZnO seed layer with the thickness of 5-30 nm on the substrate, and then putting the substrate into a vacuum annealing furnace to anneal for 1-3 hours at the temperature of 300-500 ℃ in the air;
step four, vertically placing the substrate in the step three into a reaction kettle containing a mixed solution of zinc acetate and hexamethylenetetramine with the concentration of 0.01-0.03 mol/L, preserving the heat for 1-6 hours at the temperature of 80-120 ℃, taking out the substrate after cooling to the room temperature, dripping deionized water on the surface of the substrate, and naturally drying the substrate to obtain the hedgehog-shaped ZnO/SnO2A substrate of a heterostructure;
step five, growing hedgehog shaped ZnO/SnO2The substrate and the counter electrode are connected through a heat sealing film at 100-200 ℃, and iodine electrolyte or deionized water is injected into the middle.
The ultraviolet detector has the visible light blind characteristic, can detect ultraviolet light without applying external bias and has the self-driving characteristic.
In the present invention, the substrate on which the sample is grown may be one of ITO and FTO.
In the invention, the counter electrode is one of a Pt electrode, ITO and FTO.
In the invention, the sputtering conditions of the ZnO film and the ZnO seed layer are as follows: the oxygen-argon ratio is 18:42 sccm, the working pressure is 1.2-1.7 Pa, and the sputtering power is 80-120W.
In the invention, the ZnO film in the first step can be a ZnO nanorod array, and the specific steps are as follows: the method comprises the steps of sequentially carrying out ultrasonic cleaning on a substrate in acetone, ethanol and deionized water for 10-30 minutes, preparing a ZnO seed layer with the thickness of 5-30 nm on the substrate by using magnetron sputtering, vertically placing the substrate into a reaction kettle containing a mixed solution of zinc acetate and hexamethylenetetramine with the concentration of 0.01-0.03 mol/L, preserving the temperature for 1-6 hours at 80-120 ℃, taking out the substrate after cooling to the room temperature, dripping and washing the surface with deionized water, and naturally drying.
In the invention, annealing treatment is carried out after the fourth step: prepared hedgehog shaped ZnO/SnO2The heterostructure is annealed at 400-500 ℃ in air, argon or nitrogen atmosphere, and after annealing, the crystal quality of a sample is improved, and the ultraviolet detection performance of the device is enhanced.
In the invention, the modification of the Ag nanoparticles can be carried out after the fourth step: adding hedgehog shaped ZnO/SnO2Putting the heterostructure into 0.01-0.05 mol/L silver nitrate solution, irradiating by ultraviolet light, and applying on the hedgehog ZnO/SnO2Depositing Ag nano particles on the surface.
Compared with the prior art, the invention has the following advantages:
the invention synthesizes hedgehog shaped ZnO/SnO with special three-dimensional appearance and good performance on a substrate by using a solution method2Heterostructure, and can be controlled by controlling the length, diameter, density and SnO of ZnO nanorod2The high-performance self-powered ultraviolet detector is obtained by the octahedron size, sample annealing, precious metal modification and other modes, can quickly respond to ultraviolet light with specific wavelength, has high current density and good stability, has large development potential, and is suitable for large-scale production and application.
Drawings
FIG. 1 is SnO grown on an ITO substrate2Low power SEM images of octahedral blocks;
FIG. 2 is hedgehog shaped ZnO/SnO2Low and high power SEM images of the heterostructure;
FIG. 3 is hedgehog shaped ZnO/SnO2XRD pattern of the heterostructure;
FIG. 4 is hedgehog shaped ZnO/SnO2A spectral response diagram of the heterostructure UV detector device;
FIG. 5 is hedgehog shaped ZnO/SnO2And (3) a photocurrent density curve of the heterostructure ultraviolet detection device.
Detailed Description
The technical solutions of the present invention are further described below with reference to the following examples, but the present invention is not limited thereto, and any modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Example 1:
this example provides a hedgehog shaped ZnO/SnO2A method of fabricating a heterostructure, the method comprising the steps of:
step one, the ITO substrate is sequentially subjected to ultrasonic cleaning in acetone, ethanol and deionized water for 20 minutes respectively.
Depositing a ZnO film with the thickness of 2 mu m on the ITO substrate in a radio frequency sputtering mode under the conditions that the oxygen-argon ratio is 18:42 sccm, the working pressure is 1.5 Pa and the sputtering power is 100W; putting the tube into a vacuum tube annealing furnace for annealing for 2 hours at 450 ℃; putting the annealed ZnO film with the conductive surface facing upwards at room temperature at the bottom of a beaker filled with 0.05 mol/L stannous fluoride solution, reacting for 2 hours, taking out the substrate, naturally airing, and annealing at 600 ℃ for 2 hours in the air to obtain a product SnO2Octahedron.
As shown in FIG. 1, the SEM characterization result shows that SnO2Nanoparticles in the form of octahedral blocks with an average size of about 800 nm.
Step three, in the radio frequency sputtering mode, under the conditions that the oxygen-argon ratio is 18:42 sccm, the working pressure is 1.5 Pa and the sputtering power is 100W, in SnO2Sputtering a ZnO seed layer with the thickness of 10 nm on the surface of the octahedron; annealing at 450 deg.C for 2 hr, vertically placing into a reaction kettle containing 0.01 mol/L mixed solution of zinc acetate and hexamethylenetetramine, sealing, placing the reaction kettle into a drying oven, reacting at 95 deg.C for 2 hr, naturally cooling to room temperature, taking out, washing sample surface with deionized water, and naturally drying to obtain hedgehog-shaped ZnO/SnO2A heterostructure.
ZnO/SnO shown from FIG. 2a2The low power SEM image of the heterostructure shows that ZnO/SnO2The whole body is in a hedgehog structure. ZnO/SnO as shown in FIG. 2b2SnO can be observed in high-power SEM images of heterostructures2A large number of ZnO nano-rods grow on the surface of the octahedron, and the length of the ZnO nano-rods is about 400-500 nm.
From the hedgehog shaped ZnO/SnO shown in FIG. 32The XRD pattern of the heterostructure can be observed except for the experimentHedgehog shaped ZnO/SnO outside diffraction peak of the used substrate2The heterostructure has SnO2 (110) And (211) crystal plane, and also has the characteristic peaks of ZnO (100), (002), (101), (102), (110) and (103) crystal planes, which indicates ZnO/SnO2The sample is made of tetragonal SnO2Octahedral block and hexagonal crystal ZnO nano rod.
Example 2:
this example provides a hedgehog shaped ZnO/SnO2The method for manufacturing the heterostructure ultraviolet detector comprises the following steps:
the hedgehog shaped ZnO/SnO synthesized in example 12The heterostructure is used as a working electrode, the Pt electrode is used as a counter electrode, and hedgehog shaped ZnO/SnO is grown2The ITO and Pt counter electrodes are connected together through a heat sealing film by hot pressing at 140 ℃ for 14 seconds, and iodine electrolyte solution is injected into the device to prepare the hedgehog shaped ZnO/SnO2Heterostructure ultraviolet detector.
For the prepared hedgehog shaped ZnO/SnO2The spectral response of the heterostructure device was tested and the results are shown in figure 4. As can be seen from FIG. 4, hedgehog shaped ZnO/SnO2The heterostructure ultraviolet detector has no response to visible light, ultraviolet light with the wavelength of 300-390 nm shows strong photocurrent response, and the heterostructure ultraviolet detector also has no response to light before 300 nm, so that the heterostructure ultraviolet detector can be used for ultraviolet light detection with specific wavelength.
Connecting the device with an electrochemical workstation under the condition of no voltage, and using 365 nm light as a simulated ultraviolet light source to prepare the hedgehog-shaped ZnO/SnO2The heterostructure ultraviolet detector was subjected to ultraviolet detection performance test, and the results are shown in fig. 5. As is clear from FIG. 5, when the ultraviolet light was irradiated, the photocurrent density rapidly increased to 0.94 mA cm-2When the ultraviolet light is turned off, the photocurrent density rapidly decreases and decays to an initial state, indicating that the device is sensitive to ultraviolet light. ZnO/SnO after 10 cycle test cycles2The photocurrents of the ultraviolet detectors show the same change rule, and the maximum photocurrent density value is kept stable and almost not attenuated. Zn prepared by the methodO/SnO2The ultraviolet detector has the advantages of high response speed, good stability and self-powered property.
Example 3:
this example differs from example 1 in that: the hedgehog shaped ZnO/SnO of example 12And (3) annealing the heterostructure (at 400 ℃, keeping the temperature for 2 hours in air, nitrogen or argon), and after annealing the sample, improving the crystal quality of the sample, thereby being beneficial to improving the ultraviolet detection performance of the device.
Example 4:
this example differs from example 1 in that: the hedgehog shaped ZnO/SnO in example 12Putting the heterostructure into 0.03 mol/L silver nitrate solution, irradiating for 5 minutes by using ultraviolet light, and putting the heterostructure into the hedgehog-shaped ZnO/SnO2Modifying the surface with Ag nano particles to obtain hedgehog shaped Ag @ ZnO/SnO2The nano composite material inhibits ZnO/SnO2The rapid recombination of the heterojunction photo-generated electron-hole pairs further improves the ultraviolet detection performance of the device.
Claims (9)
1. Three-dimensional hedgehog-shaped ZnO/SnO applied to ultraviolet detector2A method for preparing a heterostructure, characterized in that it comprises the following steps:
step one, sequentially carrying out ultrasonic cleaning on a substrate in acetone, ethanol and deionized water for 10-30 minutes, then sputtering a ZnO film with the thickness of 200 nm-3 mu m on a conductive surface of the substrate, and annealing for 1-3 hours at 300-500 ℃ in air;
step two, vertically placing the substrate sputtered with the ZnO film into a beaker containing stannous fluoride solution with the concentration of 0.03-0.07 mol/L for reaction for 1-4 hours at room temperature, naturally airing, annealing for 1-3 hours at the temperature of 400-600 ℃ in the air, and taking out the substrate after the annealing furnace is cooled;
step three, growing SnO2Sputtering a ZnO seed layer with the thickness of 5-30 nm on the substrate, and then putting the substrate into a vacuum annealing furnace to anneal for 1-3 hours at the temperature of 300-500 ℃ in the air;
step four, vertically placing the substrate in the step three into a chamber containing zinc acetate and hexa-zinc with the concentration of 0.01-0.03 mol/LKeeping the temperature of a reaction kettle of the methenamine mixed solution at 80-120 ℃ for 1-6 hours, taking out the substrate after cooling to room temperature, dripping deionized water on the surface of the substrate, and naturally drying the substrate to obtain hedgehog-shaped ZnO/SnO applied to an ultraviolet detector2A nanostructured material.
2. The three-dimensional hedgehog shaped ZnO/SnO applied in ultraviolet detector according to claim 12The preparation method of the heterostructure is characterized in that the substrate is one of ITO and FTO.
3. The three-dimensional hedgehog shaped ZnO/SnO applied in ultraviolet detector according to claim 12The preparation method of the heterostructure is characterized in that the sputtering conditions of the ZnO film and the ZnO seed layer are as follows: the oxygen-argon ratio is 18:42 sccm, the working pressure is 1.2-1.7 Pa, and the sputtering power is 80-120W.
4. The three-dimensional hedgehog shaped ZnO/SnO applied in ultraviolet detector according to claim 12The preparation method of the heterostructure is characterized in that annealing treatment is carried out after the fourth step: prepared hedgehog shaped ZnO/SnO2And annealing the heterostructure at 400-500 ℃ in air, argon or nitrogen atmosphere.
5. The three-dimensional hedgehog shaped ZnO/SnO applied in ultraviolet detector according to claim 12The preparation method of the heterostructure is characterized in that the modification of the Ag nano particles is carried out after the fourth step: adding hedgehog shaped ZnO/SnO2Putting the heterostructure into 0.01-0.05 mol/L silver nitrate solution, irradiating by ultraviolet light, and applying on the hedgehog ZnO/SnO2Depositing Ag nano particles on the surface.
6. The three-dimensional hedgehog shaped ZnO/SnO applied in ultraviolet detector according to claim 12The preparation method of the heterostructure is characterized in that the first step is replaced by the following steps: sequentially carrying out ultrasonic cleaning on the substrate in acetone, ethanol and deionized water for 10-30 minutes, and carrying out magnetron sputtering on the substratePreparing a ZnO seed layer of 5-30 nm, vertically placing the substrate into a reaction kettle containing a mixed solution of zinc acetate and hexamethylenetetramine with the concentration of 0.01-0.03 mol/L, preserving the heat at 80-120 ℃ for 1-6 hours, taking out the substrate after cooling to room temperature, dripping deionized water on the surface of the substrate, and naturally drying the substrate.
7. A three-dimensional hedgehog shaped ZnO/SnO prepared by the method of any one of claims 1-62A heterostructure.
8. The three-dimensional hedgehog shaped ZnO/SnO of claim 72Use of a heterostructure for an ultraviolet detector grown with hedgehog shaped ZnO/SnO2The substrate of the heterostructure is a working electrode, the working electrode and a counter electrode are connected through a heat sealing film, and iodine electrolyte or deionized water is injected between the two electrodes to serve as electrolyte.
9. The three-dimensional hedgehog shaped ZnO/SnO of claim 82Use of a heterostructure in an ultraviolet detector, characterized in that the counter electrode is one of a Pt electrode, ITO and FTO.
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