CN115763591A - Vanadium diselenide-based photoelectric detector and preparation method thereof - Google Patents
Vanadium diselenide-based photoelectric detector and preparation method thereof Download PDFInfo
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Abstract
The application discloses a vanadium diselenide-based photoelectric detector and a preparation method thereof, wherein the preparation method comprises the following steps: (1) Transferring the single-crystal vanadium diselenide onto the silicon dioxide layer to form a vanadium diselenide layer; (2) Carrying out high-temperature annealing on the vanadium diselenide layer to obtain a 2H-phase vanadium diselenide layer; (3) Forming a first metal electrode and a second metal electrode on the silicon dioxide layer by a photoetching process and an electron beam evaporation method; (4) And (3) transferring the first metal electrode and the second metal electrode to the silicon oxide wafer processed in the step (2) by a dry transfer method. According to the method, a mechanical stripping process is selected to prepare a thin layer of 1T-phase vanadium diselenide layer, a 2H-phase vanadium diselenide layer is obtained through high-temperature annealing in an oxygen-free environment, and then a metal electrode is transferred on the annealed vanadium diselenide layer, so that the high-response-rate photodetector in an infrared band is obtained.
Description
Technical Field
The invention relates to the field of infrared photodetectors, in particular to a vanadium diselenide-based photodetector and a preparation method thereof.
Background
Since graphene was found, two-dimensional materials such as black phosphorus and transition metal dihalo-compounds composed of van der waals bonds have been widely studied because of their remarkable electrical and optical properties. The development of these nanomaterials opens a door for new photodetectors in terms of miniaturization and flattening of device systems.
The availability of infrared photodetectors as a device for converting an optical signal in a system into an electrical signal depends on the responsivity of the device to the infrared band. How to improve the responsivity of the optical detector in the infrared band is a problem to be solved at present.
Disclosure of Invention
Aiming at the problems, the invention provides a vanadium diselenide-based photoelectric detector and a preparation method thereof.
The technical scheme adopted by the invention is as follows:
a preparation method of a vanadium diselenide-based photoelectric detector comprises the following steps:
(1) Providing a silicon oxide wafer, wherein the silicon oxide wafer is provided with a silicon-based substrate and a silicon dioxide layer positioned above the silicon-based substrate, and transferring single-crystal vanadium diselenide onto the silicon dioxide layer by a mechanical stripping method to form a vanadium diselenide layer;
(2) Carrying out high-temperature annealing on the silicon oxide wafer with the vanadium diselenide layer in inert gas to obtain a 2H-phase vanadium diselenide layer;
(3) Providing a silicon oxide wafer, wherein the silicon oxide wafer is provided with a silicon-based substrate and a silicon dioxide layer positioned above the silicon-based substrate, and a first metal electrode and a second metal electrode are formed on the silicon dioxide layer through a photoetching process and an electron beam evaporation method;
(4) Transferring the first metal electrode and the second metal electrode to the silicon oxide wafer obtained by processing in the step (2) through a dry transfer method, so that the first metal electrode is positioned above the silicon dioxide layer and the 2H-phase vanadium diselenide layer, the second metal electrode is positioned above the silicon dioxide layer and the 2H-phase vanadium diselenide layer, and the first metal electrode and the second metal electrode are respectively positioned at two sides of the 2H-phase vanadium diselenide layer.
Due to coordination of transition metal atoms in different waysMeanwhile, the transition metal dihalo-compound retains different structural phases, mainly 1T phase and 2H phase, accompanied by coexistence of charge density wave and superconductivity. Vanadium diselenide (VSe) 2 ) Is a typical transition metal dihalo-compound, due to V 4+ -V 4+ Exhibits metallic properties by strong electron coupling. 1T-VSe 2 Has a 10 6 S m -1 Very high conductivity. VSe 2 Presents some unique features: it is usually present in the crystalline form of 1T (octahedral unit cell with symmetry group D3), which exhibits the characteristics of a metal, rather than the 2H form (triangular prismatic unit cell with symmetry D6H 4). At a temperature of 300K, 1T-VSe 2 The phase change is 2H phase, the semiconductor material is p-type direct forbidden band transition semiconductor material, and the optical energy gap is about 2.35eV, which is beneficial to forming photoelectric detection.
According to the method, after a thin layer of vanadium diselenide with a phase 1T is prepared and obtained through a mechanical stripping process, a vanadium diselenide layer with a phase 2H is obtained through high-temperature annealing in an oxygen-free environment, and then a metal electrode is transferred on the annealed vanadium diselenide layer, so that the high-response-rate photodetector in an infrared band is obtained. The infrared photoelectric detector made by the application can reach ohmic contact, and the responsivity R is up to 75AW under the wave band of 1550nm -1 The detectivity reaches 10 10 。
In an embodiment of the invention, the thickness of the vanadium diselenide layer is 20nm to 60nm.
In one embodiment of the present invention, the step (2) is performed by performing high temperature annealing in a tube furnace, and the specific steps of the high temperature annealing are as follows: heating at 350-380 deg.c for 2 hr.
When the silicon dioxide chip is actually used, the silicon dioxide chip with the vanadium diselenide layer is placed on a quartz boat and then sent into a tube furnace, gas in the tube furnace is firstly exhausted by a vacuum pump, then argon is introduced, then the annealing temperature is set to be 370 ℃, and the annealing time is set to be 2 hours.
In one embodiment of the present invention, the specific operation manner of step (1) is as follows:
adhering the single-crystal vanadium diselenide by using an adhesive tape to obtain a vanadium diselenide single-crystal adhesive tape;
cutting to obtain a small-sized PDMS film, and adhering the PDMS film to a thicker region of the vanadium diselenide single crystal adhesive tape to obtain a PDMS vanadium diselenide composite film;
covering one side of vanadium diselenide of the PDMS vanadium diselenide composite film on a silicon dioxide layer of an oxide silicon chip;
and after the pressing is carried out for a set time, removing the PDMS film by utilizing the difference of the adhesiveness of the vanadium diselenide to the silicon dioxide layer and the PDMS film, and forming the vanadium diselenide layer on the silicon dioxide layer.
Compared with the method for stripping the vanadium diselenide single crystal adhesive tape on the silicon oxide wafer, the vanadium diselenide layer obtained by the stripping method is larger and more uniform, and the residual adhesive is less.
In an embodiment of the present invention, in the step (1), a cleaning operation of the silicon oxide wafer is further included, where the cleaning operation is: and ultrasonic cleaning is sequentially carried out by deionized water, acetone and alcohol to remove residual dust or organic reagents on the silicon wafer, and then UV cleaning is carried out for 15min by an ultraviolet ozone machine.
The adhesion of the silica layer can be increased by cleaning to facilitate the separation of the PDMS film. In actual application, after cleaning is completed, the glass can be dried by nitrogen.
In one embodiment of the present invention, in the step (3), the first metal electrode and the second metal electrode are prepared by a photolithography process and an electron beam evaporation method.
In an embodiment of the present invention, in the step (4), a specific operation manner of transferring the first metal electrode and the second metal electrode onto the silicon oxide wafer processed in the step (2) is as follows:
dripping a PVA aqueous solution onto the PDMS film, scraping the redundant PVA aqueous solution by using a glass slide, and heating on a heating table to obtain a composite film combining the PDMS film and the PVA;
attaching one surface of PVA (polyvinyl alcohol) of the composite film to the first metal electrode and the second metal electrode of the silicon oxide wafer in the step (3) on the transfer platform, adjusting the temperature of the transfer platform to 90 ℃, and enabling the composite film to strip the first metal electrode and the second metal electrode from the silicon oxide wafer;
aligning the first metal electrode and the second metal electrode with the vanadium diselenide layer obtained in the step (2) by using a three-dimensional transfer platform, pressing the first metal electrode and the second metal electrode on the vanadium diselenide layer, and separating the PDMS film after keeping the set time, wherein the PVA, the first metal electrode and the second metal electrode are positioned on the vanadium diselenide layer;
the PVA was dissolved by dimethyl sulfoxide soaking.
In actual application, the scraping direction of the glass slide is upward, the set time can be 4min, and the soaking time can be 20-25 min.
The application also discloses a vanadium diselenide-based photodetector, including:
the silicon oxide wafer is provided with a silicon-based substrate and a silicon dioxide layer positioned above the silicon-based substrate;
a vanadium diselenide layer in a 2H phase located above the silicon dioxide layer;
a first metal electrode located above the silicon dioxide layer and the 2H-phase vanadium diselenide layer;
and the second metal electrode is positioned above the silicon dioxide layer and the 2H-phase vanadium diselenide layer and is respectively positioned at two sides of the 2H-phase vanadium diselenide layer together with the first metal electrode.
In an embodiment of the invention, the thickness of the vanadium diselenide layer is 20nm to 60nm.
The invention has the beneficial effects that: according to the method, a mechanical stripping process is selected to prepare a thin layer of 1T-phase vanadium diselenide layer, a 2H-phase vanadium diselenide layer is obtained through high-temperature annealing in an oxygen-free environment, and then a metal electrode is transferred on the annealed vanadium diselenide layer, so that the high-response-rate photodetector in an infrared band is obtained.
Drawings
FIG. 1 is a schematic diagram of a vanadium diselenide-based photodetector of the present application;
FIG. 2 is a graph of voltage versus current for photodetectors of the present application at different wavelengths of light;
FIG. 3 is a graph of the response of the photodetector of the present application over time at different wavelengths of light;
FIG. 4 is a photo-current diagram of a photodetector at different wavelengths according to the present application;
FIG. 5 is a graph of the detection rate of the photodetector of the present application at different wavelengths;
FIG. 6 is a graph of responsivity of a photodetector at different wavelengths according to the present application.
The figures are numbered:
1. a silicon-based substrate; 2. a silicon dioxide layer; 3. a vanadium diselenide layer; 4. a first metal electrode; 5. a second metal electrode.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. It is to be understood that the embodiments described are only a few embodiments of the present application and not all embodiments. The components of the embodiments of the present application, generally described and illustrated in the figures herein, can be arranged and designed in a wide variety of different configurations.
In the description of the present application, it should be noted that the terms "inside", "outside", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings or orientations or positional relationships that the products of the application usually place when using, and are only used for convenience in describing the present application and simplifying the description, but do not indicate or imply that the devices or elements that are referred to must have a specific orientation, be constructed in a specific orientation, and operate, and thus, should not be construed as limiting the present application. Furthermore, the terms "first," "second," and the like are used merely to distinguish one description from another, and are not to be construed as indicating or implying relative importance.
In the description of the present application, it is also to be noted that, unless otherwise explicitly specified or limited, the terms "disposed" and "connected" are to be interpreted broadly, e.g., as being either fixedly connected, detachably connected, or integrally connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present application can be understood in a specific case by those of ordinary skill in the art.
The present invention will be described in detail below with reference to the accompanying drawings.
As shown in fig. 1, a method for preparing a vanadium diselenide-based photodetector includes the following steps:
(1) Providing a silicon oxide wafer, wherein the silicon oxide wafer is provided with a silicon-based substrate 1 and a silicon dioxide layer 2 positioned above the silicon-based substrate, and transferring single-crystal vanadium diselenide onto the silicon dioxide layer 2 by a mechanical stripping method to form a vanadium diselenide layer 3;
(2) Carrying out high-temperature annealing on the silicon oxide wafer with the vanadium diselenide layer 3 in inert gas to obtain a 2H-phase vanadium diselenide layer 3;
(3) Providing a silicon oxide wafer, wherein the silicon oxide wafer is provided with a silicon-based substrate and a silicon dioxide layer positioned above the silicon-based substrate, and a first metal electrode 4 and a second metal electrode 5 are formed on the silicon dioxide layer through a photoetching process and an electron beam evaporation method;
(4) And (3) transferring the first metal electrode 4 and the second metal electrode 5 onto the silicon oxide wafer obtained by processing in the step (2) through a dry transfer method, so that the first metal electrode 4 is positioned above the silicon dioxide layer 2 and the 2H-phase vanadium diselenide layer 3, the second metal electrode 5 is positioned above the silicon dioxide layer 2 and the 2H-phase vanadium diselenide layer 3, and the first metal electrode and the second metal electrode are respectively positioned at two sides of the 2H-phase vanadium diselenide layer.
Due to the different coordination modes of the transition metal atoms, the transition metal dihalo-compound retains different structural phases, mainly 1T phase and 2H phase, accompanied by coexistence of charge density wave and superconductivity. Vanadium diselenide (VSe) 2 ) Is a typical transition metal dihalo-compound, due to V 4+ -V 4+ Exhibits metallic properties by strong electron coupling. 1T-VSe 2 Has a 10 6 S m -1 Very high conductivity. VSe 2 Presents some unique features: it is usually present in the crystalline form of 1T (octahedral unit cell with symmetry group D3), which exhibits the characteristics of a metal, rather than the 2H form (triangular prismatic unit cell with symmetry D6H 4). 1T-VSe at a temperature of 300K 2 Form a stable hexagonal phase, i.e. the phase changes to 2H phase, pThe optical energy gap of the semiconductor material with direct forbidden band transition is about 2.35eV, which is beneficial to forming photoelectric detection.
According to the method, a mechanical stripping process is selected to prepare a thin layer of 1T-phase vanadium diselenide layer, a 2H-phase vanadium diselenide layer is obtained through high-temperature annealing in an oxygen-free environment, and then a metal electrode is transferred on the annealed vanadium diselenide layer, so that the high-response-rate photodetector in an infrared band is obtained. The infrared photoelectric detector made by the application can reach ohmic contact, and the responsivity R is up to 75AW under the wave band 1550nm -1 The detectivity reaches 10 10 。
In this embodiment, the thickness of the vanadium diselenide layer is 20nm to 60nm.
In this embodiment, the silicon oxide wafer having the vanadium diselenide layer was placed on a quartz boat and then fed into a tube furnace, the gas in the tube furnace was first exhausted () by a vacuum pump, then argon gas was introduced, and then the annealing temperature was set at 370 ℃, and the annealing time was set at 2 hours.
In this embodiment, the specific operation manner of step (1) is as follows:
adhering the single-crystal vanadium diselenide by using an adhesive tape to obtain a vanadium diselenide single-crystal adhesive tape;
cutting to obtain a small-sized PDMS film, and adhering the PDMS film to a thicker region of the vanadium diselenide single-crystal adhesive tape to obtain a PDMS vanadium diselenide composite film;
covering one side of vanadium diselenide of the PDMS vanadium diselenide composite film on a silicon dioxide layer of an oxide silicon chip;
and after the pressing is carried out for a set time, removing the PDMS film by utilizing the difference of the adhesiveness of the vanadium diselenide to the silicon dioxide layer and the PDMS film, and forming the vanadium diselenide layer on the silicon dioxide layer.
Compared with the method for stripping the vanadium diselenide single crystal adhesive tape on the silicon oxide wafer, the vanadium diselenide layer obtained by the stripping method is larger and more uniform, and the residual adhesive is less.
In this embodiment, the step (1) further includes a cleaning operation of the silicon oxide wafer, where the cleaning operation is: and ultrasonic cleaning is sequentially carried out by deionized water, acetone and alcohol to remove residual dust or organic reagents on the silicon wafer, and then UV cleaning is carried out for 15min by an ultraviolet ozone machine.
The adhesion of the silica layer can be increased by cleaning to facilitate the separation of the PDMS film. In actual application, after cleaning is completed, the glass can be dried by nitrogen.
In this embodiment, in step (3), the first metal electrode and the second metal electrode are prepared by photolithography and electron beam evaporation. In practical application, the metal electrode may be made of Au, and the thicknesses of the first metal electrode 4 and the first metal electrode 5 are 30 to 50nm. The specific operation of the step (3) is as follows:
and (3) photoetching process: spin-coating a silicon dioxide layer of an oxidized silicon wafer with a photoresist (photoresist) at 4000rpm for 60s, and baking at 100 ℃ for 4min to ensure that the photoresist on the oxidized silicon wafer is formed into a uniform and flat film; then drawing an electrode pattern with the channel width of 8 mu m in a photoetching machine, setting a program, exposing by using ultraviolet light (405 nm), and irradiating a specific pattern; and finally, developing in a developing solution to expose the photoetching pattern, wherein the ratio of the developing solution to tetramethyl ammonium hydroxide/deionized water is =7:1, and the developing time is 16-25 s.
The electron beam evaporation method comprises the following steps: placing the device and metal Au to be plated with gold into a vacuum cavity, pumping out the cavity gas to form a vacuum environment, pre-melting the metal Au for ten minutes, opening a speed/film thickness monitor area, then beginning to evaporate metal onto the device, wherein the thickness is 40nm, soaking the substrate deposited with the gold in an acetone solution for 15-20 min after the gold plating is finished, and stripping the photoresist to generate a first metal electrode and a second metal electrode.
In this embodiment, in the step (4), the specific operation manner of transferring the first metal electrode and the second metal electrode to the silicon oxide wafer processed in the step (2) is as follows:
dripping a PVA aqueous solution onto the PDMS film, scraping the redundant PVA aqueous solution by using a glass slide, and heating on a heating table to obtain a composite film combining the PDMS film and the PVA;
attaching one PVA surface of the composite membrane to the first metal electrode and the second metal electrode of the silicon oxide wafer in the step (3) on the transfer platform, adjusting the temperature of the transfer platform to 90 ℃, and enabling the composite membrane to strip the first metal electrode and the second metal electrode from the silicon oxide wafer;
aligning the first metal electrode and the second metal electrode with the vanadium diselenide layer obtained in the step (2) by using a three-dimensional transfer platform, pressing the first metal electrode and the second metal electrode on the vanadium diselenide layer, and separating the PDMS film after keeping the set time, wherein the PVA, the first metal electrode and the second metal electrode are positioned on the vanadium diselenide layer;
PVA was dissolved by dimethyl sulfoxide soaking.
In actual application, the scraping direction of the glass slide is upward, the set time can be 4min, and the soaking time can be 20-25 min.
As shown in fig. 2, vanadium diselenide forms a good ohmic contact with the metal electrode, and after light is applied, the current is greater than that in the dark, indicating a response to light. As shown in fig. 3, it can be seen that the photodetector prepared by the present invention responds well to the infrared 1550 band. As shown in fig. 4, the photocurrent increased with increasing light intensity, indicating that the device was well-formed and responsive to light. As shown in FIGS. 5 and 6, the detectivity and responsivity do not change significantly with the change of light intensity as seen from the detectivity and responsivity graphs, indicating that the sensitivity of the device is consistent for different optical powers, and the responsivity of the photodetector is 75AW under the irradiation of the laser with the wavelength band of 1550nm, which can be read from the graphs -1 (ii) a Detection rate of 10 10 Jones shows that the detection sensitivity of the infrared detector in the infrared band is high, and a new idea is developed for the application fields of military radars, infrared cameras and the like.
The above description is only for the preferred embodiment of the present invention and is not intended to limit the scope of the present invention, and all equivalent structural changes made by using the contents of the present specification and the drawings can be directly or indirectly applied to other related technical fields and are included in the scope of the present invention.
Claims (9)
1. A preparation method of a vanadium diselenide-based photoelectric detector is characterized by comprising the following steps:
(1) Providing a silicon oxide wafer, wherein the silicon oxide wafer is provided with a silicon-based substrate and a silicon dioxide layer positioned above the silicon-based substrate, and transferring single-crystal vanadium diselenide onto the silicon dioxide layer by a mechanical stripping method to form a vanadium diselenide layer;
(2) Carrying out high-temperature annealing on the silicon oxide wafer with the vanadium diselenide layer in inert gas to obtain a 2H-phase vanadium diselenide layer;
(3) Providing a silicon oxide wafer, wherein the silicon oxide wafer is provided with a silicon-based substrate and a silicon dioxide layer positioned above the silicon-based substrate, and a first metal electrode and a second metal electrode are formed on the silicon dioxide layer through a photoetching process and an electron beam evaporation method;
(4) Transferring the first metal electrode and the second metal electrode to the silicon oxide wafer obtained by processing in the step (2) through a dry transfer method, so that the first metal electrode is positioned above the silicon dioxide layer and the 2H-phase vanadium diselenide layer, the second metal electrode is positioned above the silicon dioxide layer and the 2H-phase vanadium diselenide layer, and the first metal electrode and the second metal electrode are respectively positioned at two sides of the 2H-phase vanadium diselenide layer.
2. The method of claim 1, wherein the vanadium diselenide layer has a thickness of 20nm to 60nm.
3. The method for preparing a vanadium diselenide-based photodetector as claimed in claim 1, wherein the step (2) is performed by high temperature annealing through a tube furnace, and the high temperature annealing comprises the following specific steps: heating at 350-380 deg.c for 2 hr.
4. The method for preparing a vanadium diselenide-based photodetector according to claim 1, wherein the specific operation manner of the step (1) is as follows:
adhering the single-crystal vanadium diselenide by using an adhesive tape to obtain a vanadium diselenide single-crystal adhesive tape;
cutting to obtain a small-sized PDMS film, and adhering the PDMS film to a thicker region of the vanadium diselenide single-crystal adhesive tape to obtain a PDMS vanadium diselenide composite film;
covering one side of vanadium diselenide of the PDMS vanadium diselenide composite film on a silicon dioxide layer of an oxide silicon chip;
and after the pressing is carried out for a set time, removing the PDMS film by utilizing the difference of the adhesiveness of the vanadium diselenide to the silicon dioxide layer and the PDMS film, and forming the vanadium diselenide layer on the silicon dioxide layer.
5. The method for preparing a vanadium diselenide-based photodetector as claimed in claim 4, wherein the step (1) further comprises a cleaning operation of the silicon oxide wafer, wherein the cleaning operation is that: and ultrasonic cleaning is sequentially carried out by deionized water, acetone and alcohol to remove residual dust or organic reagents on the silicon wafer, and then UV cleaning is carried out for 15min by an ultraviolet ozone machine.
6. The method for preparing a vanadium diselenide-based photodetector according to claim 1, wherein in the step (3), the first metal electrode and the second metal electrode are prepared by a photolithography process and an electron beam evaporation method.
7. The method for preparing a vanadium diselenide-based photodetector according to claim 1, wherein in the step (4), the specific operation manner of transferring the first metal electrode and the second metal electrode to the silicon oxide wafer processed in the step (2) is as follows:
dripping a PVA aqueous solution onto the PDMS film, scraping the redundant PVA aqueous solution by using a glass slide, and heating on a heating table to obtain a composite film combining the PDMS film and the PVA;
attaching one surface of PVA (polyvinyl alcohol) of the composite film to the first metal electrode and the second metal electrode of the silicon oxide wafer in the step (3) on the transfer platform, adjusting the temperature of the transfer platform to 90 ℃, and enabling the composite film to strip the first metal electrode and the second metal electrode from the silicon oxide wafer;
aligning the first metal electrode and the second metal electrode with the vanadium diselenide layer obtained in the step (2) by using a three-dimensional transfer platform, pressing the first metal electrode and the second metal electrode on the vanadium diselenide layer, and separating the PDMS film after keeping the set time, wherein the PVA, the first metal electrode and the second metal electrode are positioned on the vanadium diselenide layer;
the PVA was dissolved by dimethyl sulfoxide soaking.
8. A vanadium diselenide-based photodetector, comprising:
the silicon oxide wafer is provided with a silicon-based substrate and a silicon dioxide layer positioned above the silicon-based substrate;
a 2H-phase vanadium diselenide layer located over the silicon dioxide layer;
a first metal electrode located above the silicon dioxide layer and the 2H-phase vanadium diselenide layer;
and the second metal electrode is positioned above the silicon dioxide layer and the 2H-phase vanadium diselenide layer and is respectively positioned at two sides of the 2H-phase vanadium diselenide layer together with the first metal electrode.
9. The vanadium diselenide-based photodetector of claim 8, wherein the vanadium diselenide layer has a thickness of 20nm to 60nm.
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