CN115867055A - SiC-graphene core-shell nanowire array, preparation method thereof and application of SiC-graphene core-shell nanowire array in self-powered photoelectric detector - Google Patents
SiC-graphene core-shell nanowire array, preparation method thereof and application of SiC-graphene core-shell nanowire array in self-powered photoelectric detector Download PDFInfo
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Abstract
The invention belongs to the technical field of semiconductor nano material preparation, and particularly relates to a SiC-graphene core-shell nanowire array, a preparation method thereof and application thereof in a self-powered photoelectric detector, which comprises the following steps: and processing the SiC surface, then carrying out electrochemical corrosion treatment on the SiC surface to obtain a 4H-SiC nanowire array film, then preparing a SiC-graphene core-shell nanowire array, and preparing the self-powered photoelectric detector by adopting the SiC-graphene core-shell nanowire array. Preparing a 4H-SiC nanowire array through electrochemical corrosion, then preparing graphene on the outer layer surface of the SiC nanowire array in an epitaxial manner, and finally forming the SiC-graphene core-shell nanowire array; the preparation method provided by the invention not only effectively overcomes the defect that the SiC nanowire serving as a photoelectric detection sensitive unit cannot meet the requirement of high performance, but also can realize the preparation of the wide-spectrum photoelectric detector by regulating and controlling the number of layers of graphene.
Description
Technical Field
The invention belongs to the technical field of semiconductor nano material preparation, and particularly relates to a SiC-graphene core-shell nanowire array, a preparation method thereof and application thereof in a self-powered photoelectric detector.
Background
Since the last 90 s, the preparation of silicon carbide (SiC) and the related performance research have become the international research focus in the semiconductor field, and compared with the first generation semiconductor materials (Si, ge, etc.) and the second generation semiconductor materials (GaAs, gaP, inP, inAs, etc.), the silicon carbide has more excellent performance. The SiC has the excellent performances of wide forbidden band, high critical breakdown field strength, high electron mobility, high electron saturation drift velocity, low intrinsic carrier concentration, high thermal conductivity, good chemical stability, strong anti-irradiation capability and the like, is especially compatible with the current mature silicon integrated circuit process, and is an ideal material for manufacturing high-temperature resistant, high-pressure resistant, anti-irradiation and high-frequency high-power semiconductor devices. The SiC one-dimensional nano material has unique and excellent properties which cannot be compared with bulk materials, such as better optical and electrical properties, but because of the slower response speed of the silicon carbide material, the requirement of a high-performance photoelectric detector on the high response speed can not be met by only using the SiC nano wire as a sensitive unit of photoelectric detection.
Graphene attracts more and more attention since being discovered by Geim research groups in 2004, is a carbon material with a two-dimensional honeycomb structure formed by close packing of single-layer carbon atoms, has very excellent mechanical, thermal, optical, electrical and chemical properties such as ultrahigh carrier mobility, ultra-large specific surface area, perfect quantum tunneling effect, half-integer quantum Hall effect and the like due to the unique crystal and electronic energy band structure, and is expected to be widely applied to microelectronic devices, sensors, energy storage materials and the like. Therefore, if one or more layers of graphene are coated on the surface of the SiC nanowire array, the composite structure of the SiC nanowire array has unique performance advantages, and the SiC-graphene core-shell nanowire array is bound to become an important development direction of photoelectric detection materials. The SiC is a photoelectric detection material with excellent performance, and a semiconductor material with high performance and high response speed is expected to be obtained by virtue of the property that graphene has high-speed response capability to light after being compounded with graphene.
The high-performance photoelectric detector plays more and more important roles in the fields of environmental monitoring, implanted biological detectors, space detection and the like, and the conventional photoelectric detector in the market at present has low resolution on the illumination wave band, and most of the photoelectric detectors can work only by an external power supply. The self-powered photoelectric detector can convert optical signals into electric signals through a photoelectric excitation process based on a photovoltaic effect, can work without an external power supply, has flexibility and adaptability, and can be divided into a pn junction type, a Schottky junction type and a photoelectrochemical type according to interface characteristics. By means of the Schottky junction generated at the interface of the silicon carbide and the graphene, photoproduction electron-hole pairs can be effectively separated, and the driving force of photocurrent is generated, so that the self-powered photoelectric detector is obtained, and the development of the self-powered SiC-graphene core-shell nanowire array-based photoelectric detector with high performance is very important and scientific.
At present, the research and development of the graphene epitaxial coating SiC nanowire core-shell array structure and the self-powered photoelectric detection device thereof are reported in documents and related patents, and the existing preparation method mainly comprises the following steps: (1) The method is not easy to control the number of graphene layers on the outer layer and is easy to generate graphite or SiO 2 (ii) a (2) The SiC nano material and chlorine gas are reacted to generate graphene, but the chlorine gas is toxic, carbon tetrachloride generated by the reaction is corrosive, the environment is polluted, the flow of the gas and the temperature and pressure of an atmosphere furnace need to be controlled in the reaction atmosphere, and the reaction condition is harsh; (3) And the method directly uses SiC nano material to grow grapheneThe method graphene has many defects and is easy to fall off (patent: CN 104495850A). Based on the method, the preparation method of the SiC-graphene core-shell nanowire array is relatively simple in process and suitable for industrial batch production, and the defects of the existing preparation technology of the SiC-graphene core-shell nanowire array are overcome.
Disclosure of Invention
Aiming at the technical defects, the invention provides the SiC-graphene core-shell nanowire array, the preparation method thereof and the application thereof in the self-powered photoelectric detector, the invention prepares the 4H-SiC nanowire array through electrochemical corrosion, then prepares the graphene on the outer layer surface of the 4H-SiC nanowire array by adopting a chemical vapor deposition method for epitaxy, and finally forms the SiC-graphene core-shell nanowire array, and the chemical vapor deposition method is adopted to ensure that the graphene is not easy to fall off; the SiC-graphene core-shell nanowire array prepared by the invention not only effectively overcomes the defect that the SiC nanowire serving as a photoelectric detection sensitive unit cannot meet the requirement of high performance, but also can realize the preparation of a wide-spectrum photoelectric detector by regulating the number of layers of graphene when a chemical vapor deposition method is used, so that the prepared SiC-graphene core-shell nanowire array becomes one of effective ways for realizing the application of the graphene in the field of microelectronics.
In order to solve the technical problem, the invention adopts the following technical scheme:
the preparation method of the SiC-graphene core-shell nanowire array is characterized by comprising the following steps:
(1) Cleaning, drying, etching, protecting and balancing Si content of the SiC wafer to obtain a processed SiC wafer;
(2) Preparing a 4H-SiC nanowire array film: taking the SiC wafer treated in the step (1) as an anode, taking a graphite sheet as a cathode, and taking HF and C 2 H 5 OH、H 2 O 2 The formed etching solution is used as electrolyte, electrochemical corrosion treatment is carried out on the SiC wafer by an anodic oxidation method, and then stripping treatment is carried out to obtain the 4H-SiC nanowire array film;
(3) Preparing a SiC-graphene core-shell nanowire array: and (3) placing the 4H-SiC nanowire array film obtained in the step (2) into a vacuum radio frequency induction chemical vapor deposition furnace, introducing argon gas with the flow rate of 2L/min into the vacuum radio frequency induction chemical vapor deposition furnace, maintaining the pressure of 5mbar in a reaction cavity, maintaining the temperature of the system at 1300-1700 ℃, and reacting for 1-1.5H to obtain the SiC-graphene core-shell nanowire array, wherein the chemical vapor deposition method is adopted, the C of 4H-SiC is used as a carbon source, graphene is grown in situ on the surface of the 4H-SiC nanowire array film, so that the technical defect that the graphene is easy to fall off in the prior art is effectively overcome, and the chemical vapor deposition method is adopted to control the number of layers of the graphene.
Preferably, the cleaning treatment in the step (1) adopts an RCA standard cleaning method and adopts nitrogen for drying;
the etching treatment method in the step (1) comprises the following steps: and etching the SiC wafer by adopting high-purity hydrogen at 1300-1580 ℃ in a vacuum radio frequency induction chemical vapor deposition furnace until the surface of the SiC wafer has no scratch, thereby forming the surface with a regular step structure.
Preferably, the method for protecting treatment in step (1) is: at 900-1100 deg.C and 10 deg.C 2 -10 5 Introducing 2L/min of hydrogen under Pa, and maintaining for 10-20min.
Preferably, the method for balancing Si content in step (1) comprises: at 10 2 -10 5 Introducing silane at 800-900 deg.C under Pa in an amount of 0.5mL/min for 7-13min, and maintaining at 1000-1100 deg.C for 4-6min.
Preferably, HF and C in the step (2) 2 H 5 OH、H 2 O 2 In a volume ratio of 2.5-3.5:6: the conditions of the electrochemical corrosion treatment are as follows: and performing electrochemical corrosion treatment at room temperature for 15-25min.
Preferably, the method for maintaining the system temperature in step (3) is as follows: the temperature is increased to 1600-1700 ℃, then the temperature is naturally reduced to 1300-1400 ℃, and the alternating temperature rise and fall operation is repeated.
Preferably, in the step (2), an imaging process of the SiC wafer may be further performed to form a patterned SiC nanowire array on the surface of the SiC wafer, and the imaging process method includes: dispersing polystyrene microspheres in an ethanol solution to obtain a dispersion solution, spin-coating the dispersion solution on the SiC wafer to be treated in the step (1), plating a tin catalyst on the polystyrene microspheres by a thermal evaporation method, ultrasonically removing the polystyrene microspheres in absolute ethanol, placing the polystyrene microspheres in a hydrofluoric acid solution to remove the tin catalyst to obtain an imaged SiC wafer, wherein the polystyrene microspheres are used for forming imaging, and the tin catalyst accelerates the imaging of the surface of the SiC nanowire array to obtain an array pattern structure;
then HF and C 2 H 5 OH、H 2 O 2 The formed etching liquid is used as electrolyte, electrochemical corrosion treatment is carried out on the imaged SiC wafer through an anodic oxidation method, and then stripping treatment is carried out to obtain the 4H-SiC nanowire array film.
Preferably, in the step (2), polystyrene microspheres with the diameter of 100-2000nm are dispersed in an ethanol solution to obtain a dispersion liquid with the mass percent of 0.01-1 wt%;
the thermal evaporation method comprises the following steps: at a vacuum degree of 3.0X 10 -2 Metal tin is evaporated under pa, and the evaporation time is 1-1.5h;
the tin catalyst removing method comprises the following steps: soaking in 25% hydrofluoric acid solution for 10-15min.
The invention also protects the SiC-graphene core-shell nanowire array prepared by the preparation method.
The invention also protects the application of the SiC-graphene core-shell nanowire array in the preparation of the self-powered photoelectric detector, and the application method comprises the following steps:
(1) Cleaning and drying the SiC-graphene core-shell nanowire array;
(2) Filling the edge of the SiC-graphene core-shell nanowire array with polyimide for insulation, coating anisole with the weight percentage of 4wt% on the top of the SiC-graphene core-shell nanowire array in a circumferential direction in a rotating manner, and curing on a hot plate to obtain a top electrode;
depositing Ti/Au on the SiC surface of the SiC-graphene core-shell nanowire array to be used as a back electrode of the photoelectric detector;
and then removing anisole by hot acetone to prepare the self-powered photoelectric detector based on the SiC-graphene core-shell nanowire array.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention also carries out etching, protection and silicon content balancing treatment after cleaning the SiC wafer, and the reason is that: the SiC-graphene core-shell nanowire array is prepared by adopting a single crystal SiC substrate, because a plurality of scratches are remained on the surface of silicon carbide after the silicon carbide is treated by a Chemical Mechanical Polishing (CMP) process, the graphite prepared by directly growing the silicon carbide has poor appearance and quality, and the appearance and quality of a sample obtained by growing the silicon carbide on an even step are good, and hydrogen etching is a well-known feasible scheme capable of removing defects such as scratches on the surface of the sample; however, improper hydrogen etching can cause lattice defects on the surface of the SiC substrate and silicon compound deposition, which excessively reduces silicon enrichment on the surface of the SiC substrate, and usually uses SiO and SiH 4 And waiting for the gas to restore the SiC surface balance, namely performing treatment for balancing the silicon content.
2. The invention has the main advantages that: the microstructure and the array pattern structure of the SiC nano array can be well controlled by regulating and controlling the etching process parameters, the method has the advantages of simple process for preparing the SiC nano array, stable performance and low cost, and has good repeatability, the stripping method is simple, the stripped SiC nano array film is complete, the success rate is high, the prepared SiC nano array has the advantages of regular orientation, the same length and the same diameter of the nano wire, and the prepared nano wire array has large size (reaching 6 inches).
3. The method not only effectively overcomes the defect that the SiC nanowire serving as a photoelectric detection sensitive unit cannot meet the requirement on high performance, but also can realize the preparation of a wide-spectrum photoelectric detector by regulating the number of layers of the graphene, so that the prepared SiC-graphene core-shell nanowire array becomes one of the most effective ways for realizing the application of the graphene in the field of microelectronics. In addition, the SiC-graphene core-shell nanowire array is obtained by adopting an in-situ growth method, and has good stability and heat dissipation capacity, so that graphene is not easy to fall off, and a photoelectric device with excellent performance is expected to be obtained to meet the requirements of some high-performance application fields.
4. The SiC-graphene core-shell nanowire array film prepared by the invention can be applied to a self-powered photoelectric detector, and the photoelectric detector can work under the irradiation of external light with certain power without external bias voltage, so that the power consumption of a device is obviously reduced. Meanwhile, the prepared SiC-graphene core-shell nanowire array film improves the photoresponse capability and the light conversion rate of the device, so that the device can generate stronger photoresponse current.
Drawings
FIG. 1 is a block diagram of a self-powered photodetector made in accordance with the present invention;
FIG. 2 is an SEM cross-sectional view of a SiC-graphene core-shell nanowire array prepared in example 2 of the present invention;
FIG. 3 is an SEM image of graphene in the SiC-graphene core-shell nanowire array prepared in example 1 of the present invention;
fig. 4 is an IV curve diagram of a self-powered photodetector prepared using the SiC-graphene core-shell nanowire array of embodiment 1 of the present invention under a 365nm excitation light source;
fig. 5 is an IT curve graph of a self-powered photodetector prepared by using the SiC-graphene core-shell nanowire array of embodiment 1 of the present invention under 365nm excitation light source and 0V bias.
Detailed Description
The following detailed description of specific embodiments of the invention is provided, but it should be understood that the scope of the invention is not limited to the specific embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. The experimental methods described in the examples of the present invention are all conventional methods unless otherwise specified.
Example 1
The preparation method of the SiC-graphene core-shell nanowire array comprises the following steps:
(1) Cutting SiC (produced by New materials of Shandong Tianyue) into pieces of 7mm multiplied by 7mm by laser, and cleaning and pretreating the SiC substrate, so that the pollution of organic matters, oxides, ions and the like on the surface of the substrate can be eliminated, wherein the cleaning treatment adopts a standard RCA cleaning method: ultrasonically washing the sample wafer in deionized water for 15min, taking out the sample wafer, and repeatedly washing in flowing deionized water; preparing ammonia water: hydrogen peroxide: deionized water =1, 2; preparing hydrochloric acid: hydrogen peroxide: deionized water =1, 2; placing the sample in 5% HF solution for 1min, taking out, repeatedly washing in flowing deionized water, and drying with nitrogen gun;
the cleaned surface of the SiC substrate has a large number of scratches, and the damage of the SiC surface caused by polishing is removed by a hydrogen etching process before growth, so that the SiC is etched by adopting high-purity hydrogen at 1580 ℃ for 30min (in a vacuum radio frequency induction chemical vapor deposition furnace), the scratches on the surface are removed, and the surface with a regular step structure is formed, wherein the step width is about 1 mu m, and the height is about 1nm;
after hydrogen etching is finished, protection treatment is carried out, 2L/min of hydrogen is introduced at the low vacuum degree of 1000 ℃ for maintaining for 15min, and low-speed slow cooling is carried out at the speed of 0.3L/min in the cooling process from 1580 ℃ to 1000 ℃, so that silicon derivatives formed in the etching process are prevented from depositing on the surface of SiC; then at 850 ℃ at 10 2 Introducing silane 0.5mL/min under low vacuum for 10min to balance Si content, and further at 1050 deg.C and 10 deg.C 2 Maintaining the vacuum degree for 5min;
(2) Preparing a 4H-SiC nanowire array film: and carrying out electrochemical corrosion on the treated SiC wafer, wherein the treated SiC wafer and the graphite sheet are respectively used as an anode and a cathode in the electrochemical corrosion process, and the volume ratio of hydrofluoric acid to ethanol to hydrogen peroxide is 2.5:6:1, etching the SiC wafer in etching solution for 20min at room temperature, then stripping the SiC nanowire array film by adopting a direct current stripping method, namely applying direct current to strip the nanowire array film, and finally washing and drying the obtained SiC nanowire array film by using ethanol and deionized water respectively to obtain a 4H-SiC nanowire array film;
(3) And (3) putting the 4H-SiC nanowire array prepared in the step (2) into a vacuum radio frequency induction chemical vapor deposition furnace, introducing argon gas with the flow rate of 2L/min into the vacuum radio frequency induction chemical vapor deposition furnace, maintaining the pressure of 5mbar in a reaction cavity, raising the temperature of the system to 1650 ℃, naturally cooling to 1420 ℃, and raising the temperature to 1650 ℃ again, so that the temperature field is more uniform by repeatedly raising and lowering the temperature, the temperature unevenness caused by the over-fast reaction is avoided, the whole reaction lasts for 1H, and the SiC-graphene core-shell nanowire array is prepared.
Example 2
The preparation method of the SiC-graphene core-shell nanowire array comprises the following steps:
the method is the same as the preparation steps of the example 1, except that in the step (3), the SiC wafer and the graphite sheet are subjected to electrochemical corrosion, the SiC wafer and the graphite sheet are respectively treated as an anode and a cathode in the electrochemical corrosion process, and the volume ratio of hydrofluoric acid to ethanol to hydrogen peroxide is 3:6:1, in an etching solution, etching the SiC wafer at room temperature; subsequently, stripping the SiC nanowire array film; and finally, washing the obtained SiC nanowire array film with ethanol and deionized water respectively, and drying to obtain the 4H-SiC nanowire array film.
Example 3
The preparation method of the SiC-graphene core-shell nanowire array comprises the following steps:
(1) Cutting SiC (produced by Shandong Tianyue New Material Co.) into 10mm × 10mm pieces with laser, cleaning the SiC substrate by RCA standard cleaning method, and drying with a nitrogen gun;
the cleaned surface of the SiC substrate has a large number of scratches, and the damage of the SiC surface caused by polishing is removed by a hydrogen etching process before growth, so that the SiC is etched by adopting high-purity hydrogen at 1300 ℃ for 30min (in a vacuum radio frequency induction chemical vapor deposition furnace), the scratches on the surface are removed, and the surface with a regular step structure is formed, wherein the step width is about 1 mu m, and the height is about 1nm;
after hydrogen etching is finished, protection treatment is carried out, 2L/min of hydrogen is introduced at the low vacuum degree of 900 ℃ for maintaining for 20min, and low-speed slow cooling is carried out at the speed of 0.3L/min in the cooling process from 1300 ℃ to 900 ℃, so that silicon derivatives formed in the etching process are prevented from depositing on the surface of SiC; then at 900 ℃ at 10 DEG 4 Introducing silane 0.5mL/min under low vacuum for 7min to balance Si content, and then at 1000 deg.C and 10 deg.C 4 Maintaining at low vacuum degree for 6min;
(2) Preparing a 4H-SiC nanowire array film: and carrying out electrochemical corrosion on the treated SiC wafer, wherein the treated SiC wafer and the graphite sheet are respectively used as an anode and a cathode in the electrochemical corrosion process, and the volume ratio of hydrofluoric acid to ethanol to hydrogen peroxide is 3.5:6:1, etching the SiC wafer in etching solution for 15min at room temperature, then stripping the SiC nanowire array film by adopting a direct current stripping method, namely applying direct current to strip the nanowire array film, and finally washing and drying the obtained SiC nanowire array film by using ethanol and deionized water respectively to obtain a 4H-SiC nanowire array film;
(3) And (3) putting the 4H-SiC nanowire array prepared in the step (2) into a vacuum radio frequency induction chemical vapor deposition furnace, introducing argon gas with the flow rate of 2L/min into the vacuum radio frequency induction chemical vapor deposition furnace, maintaining the pressure of 5mbar in a reaction cavity, raising the temperature of the system to 1300 ℃, and continuing the whole reaction for 1.5 hours to prepare the SiC-graphene core-shell nanowire array.
Example 4
The preparation method of the SiC-graphene core-shell nanowire array comprises the following steps:
(1) Cutting SiC (produced by Shandong Tianyue New Material Co.) into 10mm × 10mm pieces with laser, cleaning the SiC substrate by RCA standard cleaning method, and drying with a nitrogen gun;
the cleaned surface of the SiC substrate has a large number of scratches, and the damage of the SiC surface caused by polishing is removed by a hydrogen etching process before growth, so that the SiC is etched by adopting high-purity hydrogen at 1450 ℃ for 30min (in a vacuum radio frequency induction chemical vapor deposition furnace), the scratches on the surface are removed, and the surface with a regular step structure is formed, wherein the step width is about 1 mu m, and the height is about 1nm;
after hydrogen etching is finished, protection treatment is carried out, 2L/min of hydrogen is introduced at the low vacuum degree of 1100 ℃ for maintaining for 10min, and slow cooling is carried out at a low speed of 0.3L/min in the cooling process from 1450 ℃ to 1100 ℃, so that silicon derivatives formed in the etching process are prevented from depositing on the surface of SiC; then at 1100 ℃ at 10 5 Charging silane 0.5mL/min for 13min under low vacuum degree to balance Si content, and heating at 1100 deg.C and 10 deg.C 5 Maintaining the vacuum degree for 4min;
(2) Preparing a 4H-SiC nanowire array film: and carrying out electrochemical corrosion on the treated SiC wafer, wherein the treated SiC wafer and the graphite sheet are respectively used as an anode and a cathode in the electrochemical corrosion process, and the volume ratio of hydrofluoric acid to ethanol to hydrogen peroxide is 3:6:1, etching the SiC wafer in etching solution for 25min at room temperature, then stripping the SiC nanowire array film by adopting a direct current stripping method, namely applying direct current to strip the nanowire array film, and finally washing and drying the obtained SiC nanowire array film by using ethanol and deionized water respectively to obtain a 4H-SiC nanowire array film;
(3) And (3) putting the 4H-SiC nanowire array prepared in the step (2) into a vacuum radio frequency induction chemical vapor deposition furnace, introducing argon gas with the flow rate of 2L/min into the vacuum radio frequency induction chemical vapor deposition furnace, maintaining the pressure of 5mbar in a reaction cavity, raising the temperature of the system to 1700 ℃, and continuing the whole reaction for 1H to prepare the SiC-graphene core-shell nanowire array.
Example 5
The preparation method of the SiC-graphene core-shell nanowire array comprises the following steps:
the same procedure as in example 1 was followed except that in step (2), an imaging process was also performed on the SiC wafer, and the process was carried out by: dispersing polystyrene microspheres with the diameter of 1000nm in an ethanol solution to obtain a dispersion liquid with the mass percent of 1wt%, spin-coating the dispersion liquid on the treated SiC wafer in the step (1), and then adopting a thermal evaporation method to ensure that the vacuum degree is 3.0 multiplied by 10 -2 Metal tin is evaporated under pa, a tin catalyst is plated on the polystyrene microspheres, after the evaporation time is 1.5h, the polystyrene microspheres are removed by ultrasonic in absolute ethyl alcohol,placing the SiC wafer into a hydrofluoric acid solution with the volume fraction of 25%, and soaking for 15min to remove the tin catalyst to obtain an imaged SiC wafer;
then HF and C 2 H 5 OH、H 2 O 2 The formed etching solution is used as electrolyte, electrochemical corrosion treatment is carried out on the imaged SiC wafer by an anodic oxidation method, and then stripping treatment is carried out to obtain the 4H-SiC nanowire array film.
In the embodiments 1-5 of the present invention, siC-graphene core-shell nanowire arrays with good stability and heat dissipation capability are prepared, and the performances are similar, and the following researches are performed by taking the SiC-graphene core-shell nanowire array sample of the embodiments 1-2 as an example, and the SiC-graphene core-shell nanowire array sample is applied to the preparation of a self-powered photoelectric detector, wherein the structural schematic diagram of the self-powered photoelectric detector is shown in fig. 1, and the specific preparation method of the self-powered photoelectric detector is as follows: cleaning and drying the SiC-graphene core-shell nanowire array prepared in the step (3), filling the edge of the SiC-graphene core-shell nanowire array with polyimide for insulation, spin-coating PMMA (anisole) with the weight percentage of 4% on the top of graphene, reserving a window for contact in the middle of the graphene, curing on a hot plate, depositing Ti/Au on the SiC surface of the SiC-graphene core-shell nanowire array to serve as a back electrode of a device, and removing anisole with hot acetone.
The self-powered photoelectric detector is prepared by the following steps: the fabricated devices were measured electrically and electro-optically using a four probe station in conjunction with a semiconductor characterization system (Keithley 4200-CSC) and these data were recorded using a computer controlled by a Labview program. The light source was a 365nm UV lamp and the light intensity was measured with a CEL-NP2000 dynamometer.
Results and discussion
FIG. 1 is a view of the structure of the device thus obtained;
fig. 2 is an SEM cross-sectional view of the prepared SiC nanowire array, and the results of fig. 2 show that a perfectly aligned and vertically oriented SiC nanowire array structure with a uniform length of 25 μm was prepared. Many curved nanowires were observed on top of the SiC nanowire array, indicating that these etched nanowires were significantly flexible.
Fig. 3 is an SEM image of the prepared graphene, and the result of fig. 3 shows that ultra-thin graphene is prepared and slightly detached from the substrate, demonstrating its easy peelability.
FIG. 4 is a graph of IV curves of a self-powered photodetector prepared with a SiC-graphene core-shell nanowire array under a 365nm excitation light source in a dark state (dark); the results of fig. 4 show that the self-powered photodetector has a significant difference between photocurrent and dark current under 365nm ultraviolet illumination, and the device is highly sensitive to ultraviolet light. Ultraviolet light at 365nm (245 mW cm) -2 ) And under an external voltage of-5.0V, the light current of the heterojunction ultraviolet detector reaches 1.25 muA, which is 125 times of dark current (10 nA). Under the synergistic effect of the one-dimensional SiC nanowire array and the two-dimensional graphene, the device achieves ultrahigh light-dark ratio and quick response.
Fig. 5 is an IT curve graph of a self-powered photodetector prepared with a SiC-graphene core-shell nanowire array under 365nm excitation light source and 0V bias. The results of fig. 5 show that the self-powered photoelectric detector has a significant response current change under the periodical switching-on and switching-off of 365nm ultraviolet light, which shows that the self-powered photoelectric detector has excellent self-powered photoelectric response characteristics.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations. The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of protection is not limited thereto. The equivalents and modifications of the present invention which may occur to those skilled in the art are within the scope of the present invention as defined by the appended claims.
Claims (10)
- The preparation method of the SiC-graphene core-shell nanowire array is characterized by comprising the following steps:(1) Cleaning, drying, etching, protecting and balancing Si content of the SiC wafer to obtain a processed SiC wafer;(2) Preparing a 4H-SiC nanowire array film: taking the SiC wafer treated in the step (1) as an anode, taking a graphite sheet as a cathode, and taking HF and C 2 H 5 OH、H 2 O 2 The formed etching solution is used as electrolyte, electrochemical corrosion treatment is carried out on the SiC wafer by an anodic oxidation method, and then stripping treatment is carried out to obtain the 4H-SiC nanowire array film;(3) Preparing a SiC-graphene core-shell nanowire array: and (3) placing the 4H-SiC nanowire array film obtained in the step (2) into a vacuum radio frequency induction chemical vapor deposition furnace, introducing argon gas with the flow rate of 2L/min into the vacuum radio frequency induction chemical vapor deposition furnace, maintaining the pressure of 5mbar in a reaction cavity, maintaining the temperature of the system at 1300-1700 ℃, and reacting for 1-1.5 hours to obtain the SiC-graphene core-shell nanowire array.
- 2. The method for preparing the SiC-graphene core-shell nanowire array according to claim 1, wherein the cleaning treatment in the step (1) adopts an RCA standard cleaning method and nitrogen drying;the etching treatment method in the step (1) comprises the following steps: and etching the SiC wafer by adopting high-purity hydrogen at 1300-1580 ℃ in a vacuum radio frequency induction chemical vapor deposition furnace until the surface of the SiC wafer has no scratch, thereby forming the surface with a regular step structure.
- 3. The method for preparing the SiC-graphene core-shell nanowire array according to claim 1, wherein the protection treatment in the step (1) is as follows: at 900-1100 deg.C and 10 2 -10 5 Introducing 2L/min of hydrogen under Pa, and maintaining for 10-20min.
- 4. The method for preparing the SiC-graphene core-shell nanowire array according to claim 1, wherein the step (1) for balancing Si content comprises the following steps: at 10 2 -10 5 Introducing silane at 800-900 deg.C under Pa in an amount of 0.5mL/min for 7-13min, and maintaining at 1000-1100 deg.C for 4-6min.
- 5. The method for preparing the SiC-graphene core-shell nanowire array according to claim 1, wherein HF and C are used in the step (2) 2 H 5 OH、H 2 O 2 In a volume ratio of 2.5-3.5:6: the conditions of the electrochemical corrosion treatment are as follows: and performing electrochemical corrosion treatment at room temperature for 15-25min.
- 6. The method for preparing the SiC-graphene core-shell nanowire array according to claim 1, wherein the method for maintaining the system temperature in the step (3) comprises the following steps: the temperature is increased to 1600-1700 ℃, then the temperature is naturally reduced to 1300-1400 ℃, and the alternating temperature rise and fall operation is repeated.
- 7. The method for preparing the SiC-graphene core-shell nanowire array according to claim 1, wherein in the step (2), an imaging process of the SiC wafer can be performed, and the processing method comprises the following steps: dispersing polystyrene microspheres in an ethanol solution to obtain a dispersion solution, spin-coating the dispersion solution on the SiC wafer to be treated in the step (1), plating a tin catalyst on the polystyrene microspheres by a thermal evaporation method, ultrasonically removing the polystyrene microspheres in absolute ethanol, and then placing the polystyrene microspheres in a hydrofluoric acid solution to remove the tin catalyst to obtain an imaged SiC wafer;then HF and C 2 H 5 OH、H 2 O 2 The formed etching solution is used as electrolyte, electrochemical corrosion treatment is carried out on the imaged SiC wafer by an anodic oxidation method, and then stripping treatment is carried out to obtain the 4H-SiC nanowire array film.
- 8. The method for preparing the SiC-graphene core-shell nanowire array according to claim 7, wherein in the step (2), polystyrene microspheres with the diameter of 100-2000nm are dispersed in an ethanol solution to obtain a dispersion liquid with the mass percent of 0.01-1 wt%;the thermal evaporation method comprises the following steps: at a vacuum degree of 3.0X 10 -2 Metal tin is evaporated under pa, and the evaporation time is 1-1.5h;the method for removing the tin catalyst comprises the following steps: soaking in 25% hydrofluoric acid solution for 10-15min.
- 9. An SiC-graphene core-shell nanowire array prepared by the preparation method of any one of claims 1-8.
- 10. An application of the SiC-graphene core-shell nanowire array of claim 9 in the preparation of a self-powered photoelectric detector, wherein the application method is as follows:(1) Cleaning and drying the SiC-graphene core-shell nanowire array;(2) Filling the edge of the SiC-graphene core-shell nanowire array with polyimide for insulation, coating anisole with the weight percentage of 4wt% on the top of the SiC-graphene core-shell nanowire array in a circumferential direction in a rotating manner, and curing on a hot plate to obtain a top electrode;depositing Ti/Au on the SiC surface of the SiC-graphene core-shell nanowire array to be used as a back electrode of the electro-optical detector;and then removing anisole by hot acetone to prepare the self-powered photoelectric detector based on the SiC-graphene core-shell nanowire array.
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