WO2019200629A1 - 一种纳米层状横向同质pn二极管及其制备方法与应用 - Google Patents

一种纳米层状横向同质pn二极管及其制备方法与应用 Download PDF

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WO2019200629A1
WO2019200629A1 PCT/CN2018/085934 CN2018085934W WO2019200629A1 WO 2019200629 A1 WO2019200629 A1 WO 2019200629A1 CN 2018085934 W CN2018085934 W CN 2018085934W WO 2019200629 A1 WO2019200629 A1 WO 2019200629A1
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transition metal
metal chalcogenide
film
type
type transition
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曾祥斌
王文照
郭振宇
吴少雄
曾洋
胡一说
周广通
靳雯
任婷婷
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Huazhong University of Science and Technology
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F30/00—Individual radiation-sensitive semiconductor devices in which radiation controls the flow of current through the devices, e.g. photodetectors
    • H10F30/20—Individual radiation-sensitive semiconductor devices in which radiation controls the flow of current through the devices, e.g. photodetectors the devices having potential barriers, e.g. phototransistors
    • H10F30/21—Individual radiation-sensitive semiconductor devices in which radiation controls the flow of current through the devices, e.g. photodetectors the devices having potential barriers, e.g. phototransistors the devices being sensitive to infrared, visible or ultraviolet radiation
    • H10F30/22—Individual radiation-sensitive semiconductor devices in which radiation controls the flow of current through the devices, e.g. photodetectors the devices having potential barriers, e.g. phototransistors the devices being sensitive to infrared, visible or ultraviolet radiation the devices having only one potential barrier, e.g. photodiodes
    • H10F30/221—Individual radiation-sensitive semiconductor devices in which radiation controls the flow of current through the devices, e.g. photodetectors the devices having potential barriers, e.g. phototransistors the devices being sensitive to infrared, visible or ultraviolet radiation the devices having only one potential barrier, e.g. photodiodes the potential barrier being a PN homojunction
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F71/00—Manufacture or treatment of devices covered by this subclass
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F77/00—Constructional details of devices covered by this subclass
    • H10F77/10—Semiconductor bodies
    • H10F77/12—Active materials
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F77/00—Constructional details of devices covered by this subclass
    • H10F77/10—Semiconductor bodies
    • H10F77/14—Shape of semiconductor bodies; Shapes, relative sizes or dispositions of semiconductor regions within semiconductor bodies
    • H10F77/147—Shapes of bodies
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F77/00—Constructional details of devices covered by this subclass
    • H10F77/20—Electrodes
    • H10F77/206—Electrodes for devices having potential barriers
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Definitions

  • the invention belongs to the field of photodetectors, and more particularly to a nano-layered transition metal chalcogenide transverse homogenous PN diode and a preparation method and application thereof.
  • transition metal chalcogenide layered materials have attracted much attention due to their extremely high electron mobility and other excellent optical, electrical, mechanical, chemical, acoustic, and mechanical properties.
  • the transition metal chalcogenide has a similar chemical structure, and the transition metal chalcogenide exhibiting semiconductor characteristics has similar properties, for example, both have a band gap which varies with the number of layers.
  • MoS 2 is an intrinsic n-type semiconductor material and the band gap (1.29 eV-1.8 eV) varies with the number of layers.
  • MoS 2 has excellent carrier mobility, single-layer carrier mobility up to 410 cm 2 V -1 s -1 , and multilayer carrier mobility up to 500 cm 2 V -1 s -1 .
  • MoS 2 also has a strong light absorption capacity. It is reported that MoS 2 can absorb visible light to near-infrared incident light (350-950 nm), and about 1 nm thick MoS 2 can absorb about 5-10% of incident light, which absorbs it. The efficiency is about an order of magnitude higher than the absorption efficiency of GaAs and Si.
  • the MoS 2 film exhibits excellent characteristics on photodetectors.
  • the MoS 2 phototransistor detector using ferroelectrics as the gate dielectric has an optical response of 2570 A/W, and the shortest optical response time is only 1.8 ms.
  • the range is from visible light to near-infrared (1.55um) with a detection rate of 2.2 ⁇ 10 12 Jones.
  • transition metal chalcogenide photodetectors are phototransistor type and heterojunction type, but the performance of phototransistor-based transition metal chalcogenide photodetectors is affected by many factors, such as gate dielectric and transition metal sulfur.
  • the interfacial contact of the compound film, the performance of the heterojunction photodetector is subject to the good contact between different materials and the complex process of fixed-point transfer between different materials. Therefore, the structure is simpler, the process is controllable, easy to operate, the interface contact is better, and the homojunction transition metal chalcogenide photodetector with greater potential to exhibit excellent performance has become a research hotspot.
  • plasma-injection method is mainly used to prepare a homogenous lateral or longitudinal PN photodiode by doping a transition metal chalcogenide.
  • the ion implantation doping has the advantages of high selectivity and doping controllability, but due to transition metal chalcogenide It has weak bonding bond and strong chemical activity. Physical etching and chemical etching will destroy the physical structure of transition metal chalcogenide during ion bombardment, resulting in low doping success rate and preparation of transverse or longitudinal homogenous PN. Diode photodetectors have degraded performance.
  • the invention solves the technical problem that the prior art preparation of the transition metal chalcogenide homogenous PN diode has low success rate, complicated preparation process and slow light response.
  • a nano-layered transition metal chalcogenide transversely homogenous PN diode comprising a single crystal silicon, a dielectric layer, a p-type transition metal chalcogenide film, an n-type transition a metal chalcogenide film and an electrode layer;
  • the dielectric layer is on an upper surface of the single crystal silicon;
  • the p-type transition metal chalcogenide film and the n-type transition metal chalcogenide film are both located on an upper surface of the dielectric layer, and a transition metal chalcogenide compound and an n-type transition metal chalcogenide film are laterally connected;
  • the electrode layer is composed of two metal electrodes;
  • the electrode layer is located at a p-type transition metal chalcogenide film and an n-type transition metal chalcogenide
  • the upper surface of the film is longitudinally connected to the p-type transition metal chalcogenide film and the n-type transition metal chalcogenide
  • the single crystal silicon has a thickness of 300 ⁇ m to 500 ⁇ m; the dielectric layer has a thickness of 50 nm to 300 nm; and the p-type transition metal chalcogenide film and the n-type transition metal chalcogenide film each have a thickness of 0.65 nm. 2nm.
  • the upper layer of the electrode layer is an Au metal layer, and the Au metal layer has a thickness of 50 nm to 120 nm; and the electrode layer is in contact with the p-type transition metal chalcogenide film and the n-type transition metal chalcogenide film.
  • a Ti metal layer having a thickness of 5 nm to 15 nm.
  • the single crystal silicon is p-type single crystal silicon; the dielectric layer is a silicon dioxide dielectric layer; the p-type transition metal chalcogenide film is a p-type MoS 2 film; the n-type transition metal sulfur The compound film is an n-type MoS 2 film.
  • a method of preparing a nano-layered transition metal chalcogenide transversely homogenous PN diode comprising the steps of:
  • the surface of the n-type transition metal chalcogenide film of the sample B in the step (2) is spin-coated with a photoresist, exposed and developed by EBL, to obtain at least a portion of the n-type transition metal chalcogenide film is exposed, and Not all exposed samples C;
  • the sample D obtained in the step (4) is annealed at 400 ° C to 500 ° C under an inert gas atmosphere, and the annealing time is 50 min - 90 min; the partial doping of the n-type transition metal chalcogenide film is exposed. Oxygen ion, forming a p-type transition metal chalcogenide film, to obtain sample E;
  • the surface of the sample E obtained in the step (5) is spin-coated with a photoresist, and exposed and developed by EBL to obtain an electrode region on the surface of the n-type transition metal chalcogenide film and the p-type transition metal chalcogenide film. Or an electrode region outside the boundary of the n-type transition metal chalcogenide film and the p-type transition metal chalcogenide film to obtain a sample F;
  • the electrode layer is two layers of metal, to obtain a sample G;
  • the thickness of the single crystal silicon in step (1) is from 300 ⁇ m to 500 ⁇ m; the thickness of the dielectric layer in step (1) is from 50 nm to 300 nm; and the thickness of the n-type transition metal chalcogenide film in step (1) is 0.65 nm. -2 nm; the p-type transition metal chalcogenide film of the step (5) has a thickness of 0.65 nm to 2 nm; and the method for preparing the layered n-type transition metal chalcogenide film of the step (1) is a vapor phase deposition method.
  • the upper layer of the electrode layer in the step (7) is an Au metal layer, the Au metal layer has a thickness of 50 nm to 120 nm; the electrode layer and the p-type transition metal chalcogenide film and the n-type transition in the step (7)
  • the metal chalcogenide film is in contact with a Ti metal layer having a thickness of 5 nm to 15 nm.
  • the single crystal silicon in the step (1) is p-type single crystal silicon; the dielectric layer in the step (1) is a silicon dioxide dielectric layer; and the p-type transition metal chalcogenide film in the step (5) is p.
  • the MoS 2 film of the type; the n-type transition metal chalcogenide film of the step (1) is an n-type MoS 2 film.
  • the doping process in the step (4) is: introducing oxygen having a gas flow rate of 60 sccm-100 sccm into the magnetron sputtering device as a priming gas, and oxygen is ionized into an oxygen plasma after the fluorescing, the oxygen plasma
  • the body bombards the surface of the sample C under an electric field acceleration; the bombardment time is 10 seconds to 60 seconds; the oxygen pressure is 10 Pa-15 Pa; and the magnetron sputtering device has a radio frequency power of 10 W-40 W.
  • the nano-laminate transition metal chalcogenide transversely homogenous PN diode is provided for use in a photodetector.
  • the present invention discloses a nano-layered transition metal chalcogenide transverse homogenous PN diode and a preparation method and application thereof.
  • the nano-layered transition metal chalcogenide transverse homogenous PN junction adopts in-situ growth of n-type transition metal chalcogenide film, lithography of n-type transition metal chalcogenide film to leave p-type region, low power magnetron Sputter doping, annealing to form a p-type transition metal chalcogenide region, p-type transition metal chalcogenide and the original n-type transition metal chalcogenide constitute a homogeneous PN junction method synthesis.
  • the electrode layer is made of a double-layer metal and is prepared by an electron beam evaporation process. The electrode layer is in close contact with the surface of the transition metal chalcogenide, and the contact resistance is small.
  • the method for preparing a laterally homogeneous PN diode of a nano-layered transition metal chalcogenide according to the present invention eliminates the currently used directional transfer process, thereby making the preparation method simple; the diode of the present invention has a simple structure, and the prior art is transferred by stacking
  • the p-type transition metal chalcogenide and the n-type transition metal chalcogenide form a PN junction, and the PN junction of the invention is naturally formed by doping, so that the preparation method of the invention is simple, and the nano-layered transition metal chalcogen of the invention
  • the compound lateral homogenous PN diode has stable performance and good light response, and can realize high-efficiency detection of visible light.
  • the invention utilizes a magnetic field to control the doping ion composition and doping degree, so that the preparation process is controllable and easy to operate; the doping gas used is oxygen.
  • the preparation cost is low, the doping process has little damage to the transition metal chalcogenide film, and the prepared diode has stable performance and good light response, and can realize efficient detection of visible light.
  • the preparation method of the transversely homogeneous PN diode of the nano-layered transition metal chalcogenide of the present invention is simple and controllable, and the EBL lithography and electron beam evaporation of the metal are first performed on the sample on which the transition metal chalcogen compound is grown.
  • the metal coordinates are deposited on the surface, and the position of the transition metal chalcogenide is determined according to the coordinates.
  • the magnetron sputtering is used to adjust the composition of the oxygen plasma through the magnetic field, adjust the RF power and oxygen pressure, and the oxygen ion bombards the transition metal at low energy.
  • the transition metal chalcogenide layer of the present invention has a much higher interlayer mobility than the vertical mobility as a two-dimensional material, and the lateral mobility can be compared with the silicon material.
  • the invention is formed by doping and forming a homogenous PN junction. Different from the common vertical homojunction photodetector, the lateral homogenization PN junction has a larger lateral current and a better light response, and can realize efficient detection of visible light.
  • the nano-layered transition metal chalcogenide prepared by the present invention is a transversely homogeneous PN diode, the electrode layer is a double-layer metal, and the metal in contact with the transition metal chalcogenide film is titanium, and the transition metal chalcogenide Work function matching, forming a good ohmic contact, improving device performance.
  • gold has a high electrical conductivity to prevent the inner metal from being oxidized.
  • MoS work function of the metal material in contact with the work function matching film 2 MoS 2 can form a good ohmic contact with MoS 2.
  • Fig. 1 is a schematic view showing the structure of a laterally homogeneous PN diode of a nano-layered transition metal chalcogenide on the surface of a p-type transition metal chalcogenide film and an n-type transition metal chalcogenide film of the electrode layer of the present invention.
  • Fig. 2 is a schematic view showing the structure of a transversely homogeneous PN diode of a nano-layered transition metal chalcogenide in which an electrode layer of the present invention is bonded to a boundary of a p-type transition metal chalcogenide film and an n-type di-transition metal chalcogenide film.
  • FIG. 3 is a flow chart of a process for preparing a laterally homogeneous PN diode of a nano-layered transition metal chalcogenide according to the present invention.
  • FIG. 4 is a corresponding schematic diagram of a process flow chart for preparing a laterally homogeneous PN diode of a nano-layered transition metal chalcogenide according to the present invention.
  • FIG. 3 is a flow chart of a process for preparing a laterally homogeneous PN diode of a nano-layered transition metal chalcogenide according to the present invention.
  • 4 is a corresponding schematic diagram of a process flow chart for preparing a laterally homogeneous PN diode of a nano-layered transition metal chalcogenide according to the present invention.
  • the specific steps of the preparation method of the nano-layered transition metal chalcogenide transverse homogenous PN diode provided by the invention are as follows:
  • a substrate was washed with a buffer etchant BOE to remove the surface natural oxide layer, then rinsed with deionized water and blown dry with nitrogen.
  • a single crystal silicon wafer having a SiO 2 dielectric layer on the surface after cleaning is referred to as a substrate A.
  • n-type layered MoS 2 film was formed on the substrate A by chemical vapor deposition CVD on molybdenum trioxide powder MoO 3 and sulfur powder to form a sample B with an n-type MoS 2 film.
  • Sample D was obtained by preparing a gold film having a thickness of 80 nm to 300 nm by electron beam evaporation on the upper surface of the photoresist having C.
  • sample F placed in the center of the target position, pass oxygen as the igniting gas, flow rate of 60sccm-100sccm, adjust working pressure between 10Pa-15Pa, and RF power between 10W-40W. .
  • the oxygen plasma was bombarded on the surface of the sample F by an electric field for 10 seconds to 60 seconds, and the exposed portion of the n-type MoS 2 film was doped with oxygen ions to form a p-type MoS 2 film, and the doped sample was recorded as sample G.
  • Sample H was annealed under an Ar atmosphere.
  • the annealing temperature was 500 ° C and the annealing treatment time was 60 min; the annealed sample was designated as Sample I.
  • a photoresist was spin-coated on the surface of the sample I attached with a MoS 2 film, and subjected to EBL exposure and development to obtain a sample J having an electrode region on the upper surface.
  • the upper surface of the sample J contains MoS 2 on which a titanium thin film having a thickness of 5 nm to 15 nm is prepared by electron beam evaporation, and a gold thin film of 50 nm to 120 nm is formed thereon to constitute an upper electrode, and a sample K is obtained.
  • the invention provides a method for preparing a nano-layered transition metal chalcogenide transverse homogenous PN diode, comprising the following steps:
  • a 300 ⁇ m p-type single crystal silicon wafer having a thickness of 50 nm thick SiO 2 dielectric layer on the surface was subjected to ultrasonic cleaning using an acetone solution to remove organic dirt on the surface of the substrate, and the substrate was ultrasonically cleaned and removed by using alcohol.
  • the acetone on the surface of the substrate was rinsed 3 times with deionized water.
  • a substrate was washed with a buffer etchant BOE to remove the surface natural oxide layer, then rinsed with deionized water and blown dry with nitrogen.
  • a single crystal silicon wafer having a SiO 2 dielectric layer on the surface after cleaning is referred to as a substrate A.
  • n-type layered MoS 2 film was formed on the substrate A by chemical vapor deposition CVD on molybdenum trioxide powder MoO 3 and sulfur powder to form a sample B with an n-type MoS 2 film.
  • the surface of the MoS 2 film was spin-coated with a 4% PMMA photoresist, the rotation speed was 2000 r/min, and the rotation time was 60 s.
  • the sample B was uniformly covered with a layer of PMMA having a thickness of 400 nm. It was then placed on a hot plate and kept at 170 ° C for 3 minutes and 30 seconds. Then, the EBL exposure was carried out. After the exposure, the sample B was bubbled in the MIBK solution for 30 seconds, then transferred to an isopropyl alcohol solution for 70 seconds, finally rinsed with deionized water, and then blown dry with a nitrogen gun. A sample C having coordinate marks on the upper surface was obtained.
  • Sample D was obtained by preparing a gold film having a thickness of 80 nm by electron beam evaporation on the upper surface of C having a PMMA photoresist.
  • the sample D was de-geled by soaking the sample D in an acetone solution for 20 minutes to obtain a sample E having a metal coordinate mark on the surface.
  • the surface of the sample E with the gold mark on the surface was spin-coated with the zep520A stock solution photoresist, and the rotation speed was 4000 r/min, and the rotation time was 60 s, so that the sample E was uniformly covered with a layer of zep glue having a thickness of 340 nm. It was then placed on a hot plate and baked at 180 ° C for 3 minutes. According to the coordinate mark of the step (6), the exposed pattern of the n-type MoS 2 film is partially exposed, and the EBL exposure is performed. After the exposure, the sample B is bubbled in the xylene solution for 70 seconds and then transferred to the isopropanol solution to soak 30. After a second, it was blown dry with a nitrogen gun, and after development, the n-type transition metal chalcogenide film was at least partially exposed, and not all of the exposed samples.
  • the sample F is placed in the center of the target position, and oxygen is introduced as a priming gas, the gas flow rate is 60 sccm, the working pressure is adjusted to 10 Pa, and the radio frequency power is 10 W.
  • the oxygen plasma was bombarded on the surface of the sample F for 30 seconds under the acceleration of the electric field, and the exposed portion of the n-type MoS 2 film was doped with oxygen ions to form a p-type MoS 2 film, and the doped sample was recorded as sample G.
  • Sample H was annealed under an Ar atmosphere.
  • the annealing temperature was 500 ° C and the annealing treatment time was 60 min; the annealed sample was designated as Sample I.
  • the surface spin-coating concentration was 4% PMMA photoresist, the rotation speed was 2000r/min, and the rotation time was 60s, so that the sample I was uniformly covered with a layer of PMMA with a thickness of 400 nm. It was then placed on a hot plate and baked at 170 ° C for 3 minutes and 30 seconds.
  • the EBL exposure is performed by using an exposure pattern in which the electrode region is located on the upper surface of the boundary between the n-type MoS 2 film and the p-type MoS 2 film.
  • sample I was soaked in the MIBK solution for 30 seconds and then transferred to an isopropanol solution for 70 seconds, finally rinsed with deionized water, and then blown dry with a nitrogen gun.
  • a sample J of an electrode region on the surface of the n-type MoS 2 film and the p-type MoS 2 film was obtained.
  • the upper surface of the sample J contained MoS 2 on which a titanium thin film having a thickness of 5 nm was prepared by electron beam evaporation, and a 50 nm gold thin film was formed thereon to constitute an upper electrode to obtain a sample K.
  • the sample K was degassed by soaking the sample K in an acetone solution for 20 minutes, and the sample was removed by lift-off to obtain a sample L having an electrode on the surface.
  • the invention provides a method for preparing a nano-layered transition metal chalcogenide transverse homogenous PN diode, comprising the following steps:
  • a p-type single crystal silicon wafer having a thickness of 325 ⁇ m having an 80 nm thick SiO 2 dielectric layer on the surface was subjected to ultrasonic cleaning using an acetone solution to remove organic dirt on the surface of the substrate, and the substrate was ultrasonically cleaned by alcohol. Acetone on the surface of the substrate was rinsed 3 times with deionized water.
  • a substrate was washed with a buffer etchant BOE to remove the surface natural oxide layer, then rinsed with deionized water and blown dry with nitrogen.
  • a single crystal silicon wafer having a SiO 2 dielectric layer on the surface after cleaning is referred to as a substrate A.
  • n-type layered MoS 2 film was formed on the substrate A by chemical vapor deposition CVD on molybdenum trioxide powder MoO 3 and sulfur powder to form a sample B with an n-type MoS 2 film.
  • the surface of the MoS 2 film was spin-coated with a 4% PMMA photoresist, the rotation speed was 2000 r/min, and the rotation time was 60 s.
  • the sample B was uniformly covered with a layer of PMMA having a thickness of 400 nm. It was then placed on a hot plate and kept at 170 ° C for 3 minutes and 30 seconds. Then, the EBL exposure was carried out. After the exposure, the sample B was bubbled in the MIBK solution for 30 seconds, then transferred to an isopropyl alcohol solution for 70 seconds, finally rinsed with deionized water, and then blown dry with a nitrogen gun. A sample C having coordinate marks on the upper surface was obtained.
  • Sample D was obtained by preparing a gold film having a thickness of 100 nm by electron beam evaporation on the upper surface of C having a PMMA photoresist.
  • the sample D was de-geled by soaking the sample D in an acetone solution for 20 minutes to obtain a sample E having a metal coordinate mark on the surface.
  • the surface of the sample E with the gold mark on the surface was spin-coated with the zep520A stock solution photoresist, and the rotation speed was 4000 r/min, and the rotation time was 60 s, so that the sample E was uniformly covered with a layer of zep glue having a thickness of 340 nm. It was then placed on a hot plate and baked at 180 ° C for 3 minutes. According to the coordinate mark of the step (6), the exposed pattern of the partially exposed n-type MoS 2 film was used for EBL exposure. After exposure, the sample B was bubbled in a xylene solution for 70 seconds and then immersed in an isopropyl alcohol solution for 30 seconds, and then blown dry with a nitrogen gas gun. After development, the n-type transition metal chalcogenide film was at least partially exposed, and Not all samples that are exposed.
  • the sample F was placed in the center of the target position, and oxygen was introduced as a priming gas, the gas flow rate was 60 sccm, the working pressure was adjusted to 11 Pa, and the radio frequency power was 15 W.
  • the oxygen plasma was bombarded on the surface of the sample F for 30 seconds under the acceleration of the electric field, and the exposed portion of the n-type MoS 2 film was doped with oxygen ions to form a p-type MoS 2 film, and the doped sample was recorded as sample G.
  • Sample H was annealed under an Ar atmosphere.
  • the annealing temperature was 500 ° C and the annealing treatment time was 60 min; the annealed sample was designated as Sample I.
  • the surface of the MoS 2 film was spin-coated with a concentration of zep520A stock solution, the rotation speed was 4000 r/min, and the rotation time was 60 s, so that the sample I was uniformly covered with a layer of zep glue having a thickness of 340 nm. It was then placed on a hot plate and baked at 180 ° C for 3 minutes.
  • the EBL exposure is performed by using an exposure pattern in which the electrode region is located outside the boundary between the n-type MoS 2 film and the p-type MoS 2 film.
  • sample I was bubbled in a xylene solution for 70 seconds and then transferred to an isopropyl alcohol solution for 30 seconds, and then blown dry with a nitrogen gun.
  • a sample J having an electrode region whose lateral surface was laterally connected to the boundary between the n-type MoS 2 film and the p-type MoS 2 film was obtained.
  • the upper surface of the sample J contained MoS 2 on which a titanium thin film having a thickness of 6 nm was prepared by electron beam evaporation, and a gold thin film of 60 nm was formed thereon to constitute an upper electrode, and a sample K was obtained.
  • Example 1 is a transversely homogeneous PN diode of a nano-laminar transition metal chalcogenide prepared in Example 1.
  • the diode shown flows laterally in a transition metal chalcogenide homogeneous PN junction during operation, and flows vertically in the electrode.
  • 2 is a transversely homogeneous PN diode of the nano-layered transition metal chalcogenide prepared in Example 2. The diode is operated while the current flows laterally in the transition metal chalcogenide homogenous PN junction to the electrode and still flows laterally. .
  • a nano-layered transition metal chalcogenide transversely homogenous PN diode comprising single crystal silicon 1, dielectric layer 2, p-type transition metal chalcogenide film 3, n-type transition metal chalcogenide film 4 and The electrode layer 5;
  • the dielectric layer 2 is located on the upper surface of the single crystal silicon 1;
  • the p-type transition metal chalcogenide film 3 and the n-type transition metal chalcogenide film 4 are both located on the upper surface of the dielectric layer 2, and p
  • the transition metal chalcogenide 3 and the n-type transition metal chalcogenide film 4 are laterally connected;
  • the electrode layer 5 is composed of two layers of metal electrodes;
  • the electrode layer 5 is located at the p-type transition metal chalcogenide film 3 and n-type
  • the upper surface of the transition metal chalcogenide film 4 is longitudinally connected to the p-type transition metal chalcogenide film 3 and the n-type transition metal chalcogenide
  • the single crystal silicon 1 has a thickness of 300 ⁇ m; the dielectric layer 2 has a thickness of 50 nm; and the p-type transition metal chalcogenide film 3 and the n-type transition metal chalcogenide film 4 each have a thickness of 0.65 nm.
  • the upper layer of the electrode layer 5 is an Au metal layer having a thickness of 50 nm; the contact layer of the electrode layer 5 with the p-type transition metal chalcogenide film 3 and the n-type transition metal chalcogenide film 4 is a Ti metal layer, and the thickness It is 5 nm.
  • the single crystal silicon 1 is p-type single crystal silicon; the dielectric layer 2 is a silicon dioxide dielectric layer; the p-type transition metal chalcogenide film 3 is a p-type MoS 2 film; the n-type transition metal sulfur The compound film 4 is an n-type MoS 2 film.
  • a nano-layered transition metal chalcogenide transversely homogenous PN diode comprising single crystal silicon 1, dielectric layer 2, p-type transition metal chalcogenide film 3, n-type transition metal chalcogenide film 4 and The electrode layer 5;
  • the dielectric layer 2 is located on the upper surface of the single crystal silicon 1;
  • the p-type transition metal chalcogenide film 3 and the n-type transition metal chalcogenide film 4 are both located on the upper surface of the dielectric layer 2, and p
  • the transition metal chalcogenide 3 and the n-type transition metal chalcogenide film 4 are laterally connected;
  • the electrode layer 5 is composed of two layers of metal electrodes;
  • the electrode layer 5 is located at the p-type transition metal chalcogenide film 3 and n-type
  • the transition metal chalcogenide film 4 is outside the boundary and is laterally connected to the p-type transition metal chalcogenide film 3 and the n-type di-transition metal
  • the single crystal silicon 1 has a thickness of 400 ⁇ m; the dielectric layer 2 has a thickness of 100 nm; and the p-type transition metal chalcogenide film 3 and the n-type transition metal chalcogenide film 4 each have a thickness of 1 nm.
  • the upper layer of the electrode layer 5 is an Au metal layer having a thickness of 100 nm; the contact layer of the electrode layer 5 with the p-type transition metal chalcogenide film 3 and the n-type transition metal chalcogenide film 4 is a Ti metal layer, and the thickness It is 10 nm.
  • the single crystal silicon 1 is p-type single crystal silicon; the dielectric layer 2 is a silicon dioxide dielectric layer; the p-type transition metal chalcogenide film 3 is a p-type MoS 2 film; the n-type transition metal sulfur The compound film 4 is an n-type MoS 2 film.
  • a nano-layered transition metal chalcogenide transversely homogenous PN diode comprising single crystal silicon 1, dielectric layer 2, p-type transition metal chalcogenide film 3, n-type transition metal chalcogenide film 4 and The electrode layer 5;
  • the dielectric layer 2 is located on the upper surface of the single crystal silicon 1;
  • the p-type transition metal chalcogenide film 3 and the n-type transition metal chalcogenide film 4 are both located on the upper surface of the dielectric layer 2, and p
  • the transition metal chalcogenide 3 and the n-type transition metal chalcogenide film 4 are laterally connected;
  • the electrode layer 5 is composed of two layers of metal electrodes;
  • the electrode layer 5 is located at the p-type transition metal chalcogenide film 3 and n-type
  • the upper surface of the transition metal chalcogenide film 4 is longitudinally connected to the p-type transition metal chalcogenide film 3 and the n-type transition metal chalcogenide
  • the single crystal silicon 1 has a thickness of 500 ⁇ m; the dielectric layer 2 has a thickness of 300 nm; and the p-type transition metal chalcogenide film 3 and the n-type transition metal chalcogenide film 4 each have a thickness of 2 nm.
  • the upper layer of the electrode layer 5 is an Au metal layer having a thickness of 120 nm; the contact layer of the electrode layer 5 with the p-type transition metal chalcogenide film 3 and the n-type transition metal chalcogenide film 4 is a Ti metal layer, and the thickness It is 15 nm.
  • the single crystal silicon 1 is p-type single crystal silicon; the dielectric layer 2 is a silicon dioxide dielectric layer; the p-type transition metal chalcogenide film 3 is a p-type MoS 2 film; the n-type transition metal sulfur The compound film 4 is an n-type MoS 2 film.

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Abstract

本发明公开了一种纳米层状横向同质 PN 二极管及其制备方法与应用。所述 p 型过渡金属硫族化合物膜和n型过渡金属硫族化合物膜均位于介质层的上表面，且横向连接；电极层分别与 p 型过渡金属硫族化合物膜和n型过渡金属硫族化合物膜纵向连接或横向连接；所述 p 型过渡金属硫族化合物膜和 n 型过渡金属硫族化合物膜由相同过渡金属硫族化合物组成。本发明制备方法简单，采用磁控溅射使氧等离子体实现过渡金属硫族化合物高效率低损伤的 p 型掺杂，实现了有效、可控掺杂，得到的二极管用于光电探测器具有更快光响应和更高探测率。

Description

一种纳米层状横向同质PN二极管及其制备方法与应用 [技术领域]
本发明属于光探测器领域，更具体地，涉及一种纳米层状过渡金属硫族化合物横向同质PN二极管及其制备方法与应用。
[背景技术]
二维过渡金属硫族化合物层状材料(TMDs)，因具有极高的电子迁移率和其他优异的光、电、机械、化学、声、力学等特性而倍受关注。过渡金属硫族化合物化学结构类似，显示为半导体特性的过渡金属硫族化合物各项性能也相仿，例如都具有随层数变化的带隙。以MoS 2为例，MoS 2是一种本征为n型的半导体材料并且带隙(1.29eV-1.8eV)随层数变化。MoS 2有优良的载流子迁移率，单层载流子迁移率可达410cm 2V -1s -1，多层载流子迁移率高达500cm 2V -1s -1。MoS 2还具有很强的吸光能力，据报道MoS 2可吸收可见光到近红外波段的入射光(350-950nm)，约1nm厚的MoS 2就可以吸收约5-10％的入射光，其吸收效率比GaAs和Si的吸收效率大约高一个数量级。MoS 2薄膜在光电探测器上展现出优异的特性，最近报道的利用铁电体做栅介质的MoS 2光电晶体管探测器光响应度可以达到2570A/W，最短光响应时间只有1.8ms，探测波长范围从可见光到近红外(1.55um)，探测率达到2.2×10 12Jones。
目前大部分二维过渡金属硫族化合物光电探测器是光电晶体管型和异质结型，但是基于光电晶体管的过渡金属硫族化合物光探测器的性能受许多因素影响，如栅介质与过渡金属硫族化合物薄膜的界面接触，异质结型光电探测器性能受制于不同材料间接触良好与否和不同材料间定点转移的复杂工艺等等。因此结构更简单，工艺可控、易操作，界面接触更好，有更大潜能展现优异性能的同质结型过渡金属硫族化合物光电探测器成为研究热点。
目前主要采用等离子体注入方法对过渡金属硫族化合物掺杂制备同质横向或纵向PN光电二极管，离子体注入掺杂具有高度选择性和掺杂可控性的优点， 但是由于过渡金属硫族化合物具有较弱的结合键和较强的化学活性，在离子轰击过程中会产生物理刻蚀和化学刻蚀破坏过渡金属硫族化合物物理结构，使得掺杂成功率低且制备横向或纵向同质PN二极管光电探测器性能下降。
[发明内容]
本发明解决了现有技术制备过渡金属硫族化合物同质PN二极管成功率低、制备工艺复杂和光响应慢的技术问题。
根据本发明的第一方面，提供了一种纳米层状过渡金属硫族化合物横向同质PN二极管，所述PN二极管包括单晶硅、介质层、p型过渡金属硫族化合物膜、n型过渡金属硫族化合物膜和电极层；所述介质层位于单晶硅的上表面；所述p型过渡金属硫族化合物膜和n型过渡金属硫族化合物膜均位于介质层的上表面，且p型过渡金属硫族化合物和n型过渡金属硫族化合物膜横向连接；所述电极层由两层金属电极构成；所述电极层位于p型过渡金属硫族化合物膜和n型过渡金属硫族化合物膜的上表面，且分别与p型过渡金属硫族化合物膜和n型过渡金属硫族化合物膜纵向连接；或所述电极层位于p型过渡金属硫族化合物膜和n型过渡金属硫族化合物膜的边界外侧，且分别与p型过渡金属硫族化合物膜和n型二过渡金属硫族化合物膜横向连接；所述p型过渡金属硫族化合物膜和n型过渡金属硫族化合物膜由相同过渡金属硫族化合物组成。
优选地，所述单晶硅厚度为300μm-500μm；所述介质层厚度为50nm-300nm；所述p型过渡金属硫族化合物膜和n型过渡金属硫族化合物膜的厚度均为0.65nm-2nm。
优选地，所述电极层的上层为Au金属层，所述Au金属层厚度为50nm-120nm；所述电极层与p型过渡金属硫族化合物膜和n型过渡金属硫族化合物膜接触的是Ti金属层，所述Ti金属层厚度为5nm-15nm。
优选地，所述单晶硅为p型单晶硅；所述介质层为二氧化硅介质层；所述p型过渡金属硫族化合物膜为p型MoS 2膜；所述n型过渡金属硫族化合物膜为n型MoS 2膜。
按照本发明的另一方面，提供了一种纳米层状过渡金属硫族化合物横向同 质PN二极管的制备方法，包含以下步骤：
(1)选取上表面有介质层的单晶硅作为衬底，在介质层上制备层状n型过渡金属硫族化合物膜，形成样品A；
(2)在步骤(1)所述样品A的n型过渡金属硫族化合物膜上旋涂光刻胶，经EBL曝光及显影后，采用电子束蒸发在光刻胶上制备重金属膜，去胶后获得n型过渡金属硫族化合物膜表面留有坐标标记的样品B；
(3)在步骤(2)所述样品B的n型过渡金属硫族化合物膜表面旋涂光刻胶，经EBL曝光及显影，获得n型过渡金属硫族化合物膜至少有部分暴露在外，且不是全部暴露在外的样品C；
(4)采用磁控溅射使氧等离子体对步骤(3)所述的样品C进行掺杂，去除步骤(3)旋涂的光刻胶，得到样品D；
(5)在惰性气体环境下，将步骤(4)得到的样品D在400℃-500℃条件下退火，退火时间为50min-90min；使n型过渡金属硫族化合物膜暴露在外的部分掺杂氧离子，形成p型过渡金属硫族化合物膜，得到样品E；
(6)在步骤(5)得到的样品E上表面旋涂光刻胶，经EBL曝光及显影，获得n型过渡金属硫族化合物膜和p型过渡金属硫族化合物膜上表面分布的电极区域，或者n型过渡金属硫族化合物膜和p型过渡金属硫族化合物膜边界外侧的电极区域，得到样品F；
(7)在步骤(6)所述的样品F的电极区域采用电子束蒸发制备电极层；所述电极层为两层金属层，得到样品G；
(8)将步骤(7)所述的样品G去胶，即得到纳米层状过渡金属硫族化合物横向同质PN二极管。
优选地，步骤(1)所述单晶硅厚度为300μm-500μm；步骤(1)所述介质层厚度为50nm-300nm；步骤(1)所述n型过渡金属硫族化合物膜厚度为0.65nm-2nm；步骤(5)所述p型过渡金属硫族化合物膜厚度0.65nm-2nm；步骤(1)所述层状n型过渡金属硫族化合物膜的制备方法为气相沉积法。
优选地，步骤(7)所述电极层的上层为Au金属层，所述Au金属层厚度为 50nm-120nm；步骤(7)所述电极层与p型过渡金属硫族化合物膜和n型过渡金属硫族化合物膜接触的是Ti金属层，所述Ti金属层厚度为5nm-15nm。
优选地，步骤(1)所述单晶硅为p型单晶硅；步骤(1)所述介质层为二氧化硅介质层；步骤(5)所述p型过渡金属硫族化合物膜为p型MoS 2膜；步骤(1)所述n型过渡金属硫族化合物膜为n型MoS 2膜。
优选地，步骤(4)所述掺杂的过程为向磁控溅射装置中通入气流量为60sccm-100sccm的氧气作为起辉气体，起辉后氧气电离为氧等离子体，所述氧等离子体在电场加速下轰击样品C的表面；所述轰击的时间为10秒-60秒；所述氧气的压力10Pa-15Pa；所述磁控溅射装置的射频功率10W-40W。
按照本发明的另一方面，提供了所述的纳米层状过渡金属硫族化合物横向同质PN二极管用于光电探测器。
总体而言，通过本发明所构思的以上技术方案与现有技术相比，能够取得下列有益效果：
(1)本发明公开了一种纳米层状过渡金属硫族化合物横向同质PN二极管及其制备方法与应用。所述的纳米层状过渡金属硫族化合物横向同质PN结采用原位生长n型过渡金属硫族化合物薄膜、对n型过渡金属硫族化合物薄膜光刻留出p型区域、低功率磁控溅射掺杂、退火形成p型过渡金属硫族化合物区域、p型过渡金属硫族化合物与原n型过渡金属硫族化合物构成同质PN结方法合成。所述的电极层为双层金属，采用电子束蒸发工艺制备而成，电极层与过渡金属硫族化合物表面接触紧密，接触电阻小。
(2)本发明制备纳米层状过渡金属硫族化合物横向同质PN二极管的方法，省去目前常用的定向转移工艺，使得制备方法简单；本发明所述二极管结构简单，现有技术通过转移堆叠p型过渡金属硫族化合物和n型过渡金属硫族化合物形成PN结，本发明PN结通过掺杂后自然形成，使得本发明制备方法简单，且本发明所述的纳米层状过渡金属硫族化合物横向同质PN二极管性能稳定、光响应好，能够实现对可见光的高效探测；本发明利用磁场调控掺杂离子成分与掺杂程度，使得制备工艺可控易操作；使用的掺杂气体为氧气，使得制备成本 较低，掺杂过程对过渡金属硫族化合物膜损坏小，制备得到的二极管性能稳定、光响应好，能够实现对可见光的高效探测。
(3)本发明所述纳米层状过渡金属硫族化合物横向同质PN二极管的制备方法工艺简单可控，采用EBL光刻和电子束蒸发金属，先在生长有过渡金属硫族化合物的样品上表面沉积金属坐标，再根据坐标确定过渡金属硫族化合物位置进行定点光刻，采用磁控溅射通过磁场调控氧等离子的成分、调节射频功率与氧气压强使氧离子体在低能量下轰击过渡金属硫族化合物，实现低损耗掺杂，使得制备成功率提高。
(4)本发明所述纳米层状过渡金属硫族化合物横向同质PN二极管的制备方法，由于采用磁控溅射工艺，采用具有较低化学活性且较高掺杂效率的氧等离子体实现过渡金属硫族化合物高效率低损伤的p型掺杂，实现了有效、可控掺杂，得到的二极管应用于光电探测器时，具有更快光响应和更高探测率。
(5)本发明过渡金属硫族化合物层作为二维材料层间迁移率远大于垂直迁移率，且横向迁移率可与硅材料比拟。本发明经过定位掺杂构成同质PN结，与常见垂直同质结光电探测器不同的是横向同质PN结内横向电流更大，光响应更好，可以实现对可见光高效探测。
(6)本发明所制备的纳米层状过渡金属硫族化合物横向同质PN二极管，电极层采用双层金属，且与过渡金属硫族化合物薄膜接触的金属为钛，与过渡金属硫族化合物的功函数匹配，形成良好欧姆接触，提高器件性能。同时金具有很高的导电性，防止内层金属被氧化。与MoS 2薄膜接触的金属材料的功函数与MoS 2的功函数匹配，可以与MoS 2形成良好的欧姆接触。
[附图说明]
图1是本发明电极层位于p型过渡金属硫族化合物膜和n型过渡金属硫族化合物膜上表面的纳米层状过渡金属硫族化合物横向同质PN二极管结构示意图。
图2是本发明电极层与p型过渡金属硫族化合物膜和n型二过渡金属硫族化合物膜边界相连接的纳米层状过渡金属硫族化合物横向同质PN二极管结构示 意图。
图3是本发明制备纳米层状过渡金属硫族化合物横向同质PN二极管工艺流程图。
图4是本发明制备纳米层状过渡金属硫族化合物横向同质PN二极管工艺流程图的对应示意图。
其中1-单晶硅；2-介质层；3-p型过渡金属硫族化合物膜；4-n型过渡金属硫族化合物物膜；5-金属层。
[具体实施方式]
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合附图及实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。此外，下面所描述的本发明各个实施方式中所涉及到的技术特征只要彼此之间未构成冲突就可以相互组合。
图3是本发明制备纳米层状过渡金属硫族化合物横向同质PN二极管工艺流程图。图4是本发明制备纳米层状过渡金属硫族化合物横向同质PN二极管工艺流程图的对应示意图。本发明提供的纳米层状过渡金属硫族化合物横向同质PN二极管的制备方法具体步骤如下：
(1)采用丙酮溶液对表面有SiO 2介质层的p型单晶硅片，进行超声清洗，去除衬底表面的有机污垢，并采用酒精对所述衬底进行超声清洗去除所述衬底表面的丙酮，去离子水冲洗3次。
(2)采用缓冲蚀刻液BOE清洗上述衬底，去除表面自然氧化层，然后去离子水冲洗，用氮气吹干。清洗后的表面有SiO 2介质层的单晶硅片记作衬底A。
(3)对三氧化钼粉末MoO 3和硫粉采用化学气相沉积法CVD在衬底A上制备n型层状MoS 2薄膜，形成附有n型MoS 2薄膜的样品B。
(4)在样品B附有MoS 2薄膜上表面旋涂光刻胶，经EBL曝光及显影获得上表面有坐标标记的样品C。
(5)在C的具有光刻胶的上表面采用电子束蒸发制备厚度为80nm-300nm的金薄膜获得样品D。
(6)采用专用去胶液对样品D去胶，获得表面留有金属标记的样品E。
(7)表面留有金标的样品E上表面旋涂光刻胶，经EBL曝光及显影获得上表面MoS 2晶体有一半遮挡层一半暴露在外的样品F。
(8)采用磁控溅射设备，将样品F放置在靶材位中心，通入氧气作为起辉气体，气流量60sccm-100sccm，调节工作压力10Pa-15Pa之间，射频功率10W-40W之间。使氧等离子体在电场加速下轰击样品F表面10秒-60秒，n型MoS 2膜暴露在外的部分掺杂氧离子，形成p型MoS 2膜，掺杂后的样品记样品G。
(9)采用专用去胶液对样品G去胶，获得样品H。
(10)将样品H在Ar气氛下退火。退火温度为500℃，退火处理时间为60min；退火后的样品记作样品I。
(11)在样品I附有MoS 2薄膜上表面旋涂光刻胶，经EBL曝光及显影获得上表面有电极区域的样品J。
(12)样品J上表面含有MoS 2，其上采用电子束蒸发制备厚度为5nm-15nm的钛薄膜，再在其上制备50nm-120nm的金薄膜构成上电极，获得样品K。
(13)采用专用去胶液对样品K去胶，经过lift-off去胶，获得表面留有电极的的样品L。
现借助具体实施例进一步详细说明本发明提供的纳米层状过渡金属硫族化合物横向同质PN二极管光电探测器制备方法。
实施例1
本发明一种制备纳米层状过渡金属硫族化合物横向同质PN二极管的方法，包括以下步骤：
(1)采用丙酮溶液对表面有50nm厚SiO 2介质层的厚度300μm p型单晶硅片，进行超声清洗，去除衬底表面的有机污垢，并采用酒精对所述衬底进行超声清洗去除所述衬底表面的丙酮，去离子水冲洗3次。
(2)采用缓冲蚀刻液BOE清洗上述衬底，去除表面自然氧化层，然后去离子水冲洗，用氮气吹干。清洗后的表面有SiO 2介质层的单晶硅片记作衬底A。
(3)对三氧化钼粉末MoO 3和硫粉采用化学气相沉积法CVD在衬底A上制备 n型层状MoS 2薄膜，形成附有n型MoS 2薄膜的样品B。
(4)在样品B附有MoS 2薄膜上表面旋涂浓度为4％PMMA光刻胶，保持转速为2000r/min，旋转时间为60s，使样品B上均匀覆盖一层厚度为400nm的PMMA。再放在加热板保持170℃烘烤3分30秒。再进行EBL曝光，曝光后将样品B泡于MIBK溶液中30秒再移至异丙醇溶液中浸泡70秒，最后用去离子水冲洗干净，再用氮气枪吹干。获得上表面有坐标标记的样品C。
(5)在C的具有PMMA光刻胶的上表面采用电子束蒸发制备厚度为80nm的金薄膜获得样品D。
(6)将样品D泡于丙酮溶液中20分钟对样品D去胶，获得表面留有金属坐标标记的样品E。
(7)表面留有金标的样品E上表面旋涂zep520A原液光刻胶，保持转速为4000r/min，旋转时间为60s，使样品E上均匀覆盖一层厚度为340nm的zep胶。再放在加热板上保持180℃烘烤3分钟。根据步骤(6)的坐标标记，采用n型MoS 2薄膜有部分暴露在外的曝光版图，进行EBL曝光，曝光后将样品B泡于二甲苯溶液中70秒再移至异丙醇溶液中浸泡30秒，再用氮气枪吹干，显影后获得n型过渡金属硫族化合物膜至少有部分暴露在外，且不是全部暴露在外的样品。
(8)采用磁控溅射设备，将样品F放置在靶材位中心，通入氧气作为起辉气体，气流量60sccm，调节工作压力10Pa，射频功率10W。使氧等离子体在电场加速下轰击样品F表面30秒，n型MoS 2膜暴露在外的部分掺杂氧离子，形成p型MoS 2膜，掺杂后的样品记样品G。
(9)用NMP浸泡G片5分钟后，用去离子水冲洗干净，再用氮气枪吹干获得样品H。
(10)将样品H在Ar气氛下退火。退火温度为500℃，退火处理时间为60min；退火后的样品记作样品I。
(11)在样品I附有MoS 2薄膜上表面旋涂浓度为4％PMMA光刻胶，保持转速为2000r/min，旋转时间为60s，使样品I上均匀覆盖一层厚度为400nm的PMMA。再放在加热板上保持170℃烘烤3分30秒。根据步骤(6)的坐标标记，采用使 电极区域位于n型MoS 2膜和p型MoS 2膜边界上表面的曝光版图，进行EBL曝光。曝光后将样品I泡于MIBK溶液中30秒再移至异丙醇溶液中浸泡70秒，最后用去离子水冲洗干净，再用氮气枪吹干。获得n型MoS 2膜和p型MoS 2膜上表面分布的电极区域的样品J。
(12)样品J上表面含有MoS 2，其上采用电子束蒸发制备厚度为5nm的钛薄膜，再在其上制备50nm的金薄膜构成上电极，获得样品K。
(13)将样品K泡于丙酮溶液中20分钟对样品K去胶，经过lift-off去胶，获得表面留有电极的的样品L。
实施例2
本发明一种制备纳米层状过渡金属硫族化合物横向同质PN二极管的方法，包括以下步骤：
(1)采用丙酮溶液对表面有80nm厚SiO 2介质层的厚度325μm的p型单晶硅片，进行超声清洗，去除衬底表面的有机污垢，并采用酒精对所述衬底进行超声清洗去除所述衬底表面的丙酮，去离子水冲洗3次。
(2)采用缓冲蚀刻液BOE清洗上述衬底，去除表面自然氧化层，然后去离子水冲洗，用氮气吹干。清洗后的表面有SiO 2介质层的单晶硅片记作衬底A。
(3)对三氧化钼粉末MoO 3和硫粉采用化学气相沉积法CVD在衬底A上制备n型层状MoS 2薄膜，形成附有n型MoS 2薄膜的样品B。
(4)在样品B附有MoS 2薄膜上表面旋涂浓度为4％PMMA光刻胶，保持转速为2000r/min，旋转时间为60s，使样品B上均匀覆盖一层厚度为400nm的PMMA。再放在加热板保持170℃烘烤3分30秒。再进行EBL曝光，曝光后将样品B泡于MIBK溶液中30秒再移至异丙醇溶液中浸泡70秒，最后用去离子水冲洗干净，再用氮气枪吹干。获得上表面有坐标标记的样品C。
(5)在C的具有PMMA光刻胶的上表面采用电子束蒸发制备厚度为100nm的金薄膜获得样品D。
(6)将样品D泡于丙酮溶液中20分钟对样品D去胶，获得表面留有金属坐标标记的样品E。
(7)表面留有金标的样品E上表面旋涂zep520A原液光刻胶，保持转速为4000r/min，旋转时间为60s，使样品E上均匀覆盖一层厚度为340nm的zep胶。再放在加热板上保持180℃烘烤3分钟。根据步骤(6)的坐标标记，采用n型MoS 2薄膜有部分暴露在外的曝光版图，进行EBL曝光。曝光后将样品B泡于二甲苯溶液中70秒再移至异丙醇溶液中浸泡30秒，再用氮气枪吹干，显影后获得n型过渡金属硫族化合物膜至少有部分暴露在外，且不是全部暴露在外的样品。
(8)采用磁控溅射设备，将样品F放置在靶材位中心，通入氧气作为起辉气体，气流量60sccm，调节工作压力11Pa，射频功率15W。使氧等离子体在电场加速下轰击样品F表面30秒，n型MoS 2膜暴露在外的部分掺杂氧离子，形成p型MoS 2膜，掺杂后的样品记样品G。
(9)用NMP浸泡G片5分钟后，用去离子水冲洗干净，再用氮气枪吹干获得样品H。
(10)将样品H在Ar气氛下退火。退火温度为500℃，退火处理时间为60min；退火后的样品记作样品I。
(11)在样品I附有MoS 2薄膜上表面旋涂浓度为zep520A原液光刻胶，保持转速为4000r/min，旋转时间为60s，使样品I上均匀覆盖一层厚度为340nm的zep胶。再放在加热板上保持180℃烘烤3分钟。根据步骤(6)的坐标标记，采用使电极区域位于n型MoS 2膜和p型MoS 2膜边界外侧的曝光版图，进行EBL曝光。曝光后将样品I泡于二甲苯溶液中70秒再移至异丙醇溶液中浸泡30秒，再用氮气枪吹干。获得上表面有与n型MoS 2膜和p型MoS 2膜边界横向相连接的电极区域的样品J。
(12)样品J上表面含有MoS 2，其上采用电子束蒸发制备厚度为6nm的钛薄膜，再在其上制备60nm的金薄膜构成上电极，获得样品K。
(13)将样品K泡于NMP溶液中5分钟对样品K去胶，经过lift-off去胶，获得表面留有电极的的样品L。
由于制备步骤是相同的，各个实施例之间的区别仅仅是各个参数的区别的，上述实施例仅仅给出了个别实施例中的参数；具体实施例如下表所示，下表示 出了纳米层状过渡金属硫族化合物横向同质PN二极管的制备方法所用参数及光刻胶。
Figure PCTCN2018085934-appb-000001
图1为实施例1制备得到的纳米层状过渡金属硫族化合物横向同质PN二极管，所示的二极管在工作时电流在过渡金属硫族化合物同质PN结中横向流动，在电极中垂直流动；图2为实施例2制备得到的纳米层状过渡金属硫族化合物横向同质PN二极管，所示的二极管工作时电流在过渡金属硫族化合物同质PN结中横向流动到达电极处仍横向流动。
实施例3
一种纳米层状过渡金属硫族化合物横向同质PN二极管，所述PN二极管包括单晶硅1、介质层2、p型过渡金属硫族化合物膜3、n型过渡金属硫族化合物膜4和电极层5；所述介质层2位于单晶硅1的上表面；所述p型过渡金属硫族化合物膜3和n型过渡金属硫族化合物膜4均位于介质层2的上表面，且p型 过渡金属硫族化合物3和n型过渡金属硫族化合物膜4横向连接；所述电极层5由两层金属电极构成；所述电极层5位于p型过渡金属硫族化合物膜3和n型过渡金属硫族化合物膜4的上表面，且分别与p型过渡金属硫族化合物膜3和n型过渡金属硫族化合物膜4纵向连接；所述p型过渡金属硫族化合物膜3和n型过渡金属硫族化合物膜4由相同过渡金属硫族化合物组成。所述单晶硅1厚度为300μm；所述介质层2厚度为50nm；所述p型过渡金属硫族化合物膜3和n型过渡金属硫族化合物膜4的厚度均为0.65nm。所述电极层5的上层为Au金属层，厚度为50nm；所述电极层5与p型过渡金属硫族化合物膜3和n型过渡金属硫族化合物膜4的接触层为Ti金属层，厚度为5nm。所述单晶硅1为p型单晶硅；所述介质层2为二氧化硅介质层；所述p型过渡金属硫族化合物膜3为p型MoS 2膜；所述n型过渡金属硫族化合物膜4为n型MoS 2膜。
实施例4
一种纳米层状过渡金属硫族化合物横向同质PN二极管，所述PN二极管包括单晶硅1、介质层2、p型过渡金属硫族化合物膜3、n型过渡金属硫族化合物膜4和电极层5；所述介质层2位于单晶硅1的上表面；所述p型过渡金属硫族化合物膜3和n型过渡金属硫族化合物膜4均位于介质层2的上表面，且p型过渡金属硫族化合物3和n型过渡金属硫族化合物膜4横向连接；所述电极层5由两层金属电极构成；所述电极层5位于p型过渡金属硫族化合物膜3和n型过渡金属硫族化合物膜4的边界外侧，且分别与p型过渡金属硫族化合物膜3和n型二过渡金属硫族化合物膜4横向连接；所述p型过渡金属硫族化合物膜3和n型过渡金属硫族化合物膜4由相同过渡金属硫族化合物组成。所述单晶硅1厚度为400μm；所述介质层2厚度为100nm；所述p型过渡金属硫族化合物膜3和n型过渡金属硫族化合物膜4的厚度均为1nm。所述电极层5的上层为Au金属层，厚度为100nm；所述电极层5与p型过渡金属硫族化合物膜3和n型过渡金属硫族化合物膜4的接触层为Ti金属层，厚度为10nm。所述单晶硅1为p型单晶硅；所述介质层2为二氧化硅介质层；所述p型过渡金属硫族化合物膜3为p型MoS 2膜；所述n型过渡金属硫族化合物膜4为n型MoS 2膜。
实施例5
一种纳米层状过渡金属硫族化合物横向同质PN二极管，所述PN二极管包括单晶硅1、介质层2、p型过渡金属硫族化合物膜3、n型过渡金属硫族化合物膜4和电极层5；所述介质层2位于单晶硅1的上表面；所述p型过渡金属硫族化合物膜3和n型过渡金属硫族化合物膜4均位于介质层2的上表面，且p型过渡金属硫族化合物3和n型过渡金属硫族化合物膜4横向连接；所述电极层5由两层金属电极构成；所述电极层5位于p型过渡金属硫族化合物膜3和n型过渡金属硫族化合物膜4的上表面，且分别与p型过渡金属硫族化合物膜3和n型过渡金属硫族化合物膜4纵向连接；或所述电极层5位于p型过渡金属硫族化合物膜3和n型过渡金属硫族化合物膜4的边界外侧，且分别与p型过渡金属硫族化合物膜3和n型二过渡金属硫族化合物膜4横向连接；所述p型过渡金属硫族化合物膜3和n型过渡金属硫族化合物膜4由相同过渡金属硫族化合物组成。所述单晶硅1厚度为500μm；所述介质层2厚度为300nm；所述p型过渡金属硫族化合物膜3和n型过渡金属硫族化合物膜4的厚度均为2nm。所述电极层5的上层为Au金属层，厚度为120nm；所述电极层5与p型过渡金属硫族化合物膜3和n型过渡金属硫族化合物膜4的接触层为Ti金属层，厚度为15nm。所述单晶硅1为p型单晶硅；所述介质层2为二氧化硅介质层；所述p型过渡金属硫族化合物膜3为p型MoS 2膜；所述n型过渡金属硫族化合物膜4为n型MoS 2膜。
本领域的技术人员容易理解，以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。

Claims (10)

  1. 一种纳米层状过渡金属硫族化合物横向同质PN二极管，其特征在于，所述PN二极管包括单晶硅(1)、介质层(2)、p型过渡金属硫族化合物膜(3)、n型过渡金属硫族化合物膜(4)和电极层(5)；所述介质层(2)位于单晶硅(1)的上表面；所述p型过渡金属硫族化合物膜(3)和n型过渡金属硫族化合物膜(4)均位于介质层(2)的上表面，且p型过渡金属硫族化合物(3)和n型过渡金属硫族化合物膜(4)横向连接；所述电极层(5)由两层金属电极构成；所述电极层(5)位于p型过渡金属硫族化合物膜(3)和n型过渡金属硫族化合物膜(4)的上表面，且分别与p型过渡金属硫族化合物膜(3)和n型过渡金属硫族化合物膜(4)纵向连接；或所述电极层(5)位于p型过渡金属硫族化合物膜(3)和n型过渡金属硫族化合物膜(4)的边界外侧，且分别与p型过渡金属硫族化合物膜(3)和n型二过渡金属硫族化合物膜(4)横向连接；所述p型过渡金属硫族化合物膜(3)和n型过渡金属硫族化合物膜(4)由相同过渡金属硫族化合物组成。
  2. 如权利要求1所述的纳米层状过渡金属硫族化合物横向同质PN二极管，其特征在于，所述单晶硅(1)厚度为300μm-500μm；所述介质层(2)厚度为50nm-300nm；所述p型过渡金属硫族化合物膜(3)和n型过渡金属硫族化合物膜(4)的厚度均为0.65nm-2nm。
  3. 如权利要求1所述的纳米层状过渡金属硫族化合物横向同质PN二极管，其特征在于，所述电极层(5)的上层为Au金属层，所述Au金属层厚度为50nm-120nm；所述电极层(5)与p型过渡金属硫族化合物膜(3)和n型过渡金属硫族化合物膜(4)接触的是Ti金属层，所述Ti金属层厚度为5nm-15nm。
  4. 如权利要求1所述的纳米层状过渡金属硫族化合物横向同质PN二 极管，其特征在于，所述单晶硅(1)为p型单晶硅；所述介质层(2)为二氧化硅介质层；所述p型过渡金属硫族化合物膜(3)为p型MoS 2膜；所述n型过渡金属硫族化合物膜(4)为n型MoS 2膜。
  5. 一种纳米层状过渡金属硫族化合物横向同质PN二极管的制备方法，其特征在于，包含以下步骤：
    (1)选取上表面有介质层的单晶硅作为衬底，在介质层上制备层状n型过渡金属硫族化合物膜，形成样品A；
    (2)在步骤(1)所述样品A的n型过渡金属硫族化合物膜上旋涂光刻胶，经EBL曝光及显影后，采用电子束蒸发在光刻胶上制备重金属膜，去胶后获得n型过渡金属硫族化合物膜表面留有坐标标记的样品B；
    (3)在步骤(2)所述样品B的n型过渡金属硫族化合物膜表面旋涂光刻胶，经EBL曝光及显影，获得n型过渡金属硫族化合物膜至少有部分暴露在外，且不是全部暴露在外的样品C；
    (4)采用磁控溅射使氧等离子体对步骤(3)所述的样品C进行掺杂，去除步骤(3)旋涂的光刻胶，得到样品D；
    (5)在惰性气体环境下，将步骤(4)得到的样品D在400℃-500℃条件下退火，退火时间为50min-90min；使n型过渡金属硫族化合物膜暴露在外的部分掺杂氧离子，形成p型过渡金属硫族化合物膜，得到样品E；
    (6)在步骤(5)得到的样品E上表面旋涂光刻胶，经EBL曝光及显影，获得n型过渡金属硫族化合物膜和p型过渡金属硫族化合物膜上表面分布的电极区域，或者n型过渡金属硫族化合物膜和p型过渡金属硫族化合物膜边界外侧的电极区域，得到样品F；
    (7)在步骤(6)所述样品F的电极区域采用电子束蒸发制备电极层；所述电极层为两层金属层，得到样品G；
    (8)将步骤(7)所述的样品G去胶，即得到纳米层状过渡金属硫族化合物横向同质PN二极管。
  6. 如权利要求5所述的纳米层状过渡金属硫族化合物横向同质PN二极管的制备方法，其特征在于，步骤(1)所述单晶硅厚度为300μm-500μm；步骤(1)所述介质层厚度为50nm-300nm；步骤(1)所述n型过渡金属硫族化合物膜厚度为0.65nm-2nm；步骤(5)所述p型过渡金属硫族化合物膜厚度0.65nm-2nm；步骤(1)所述层状n型过渡金属硫族化合物膜的制备方法为气相沉积法。
  7. 如权利要求5所述的纳米层状过渡金属硫族化合物横向同质PN二极管的制备方法，其特征在于，步骤(7)所述电极层的上层为Au金属层，所述Au金属层厚度为50nm-120nm；步骤(7)所述电极层与p型过渡金属硫族化合物膜和n型过渡金属硫族化合物膜接触的是Ti金属层，所述Ti金属层厚度为5nm-15nm。
  8. 如权利要求5所述的纳米层状过渡金属硫族化合物横向同质PN二极管的制备方法，其特征在于，步骤(1)所述单晶硅为p型单晶硅；步骤(1)所述介质层为二氧化硅介质层；步骤(5)所述p型过渡金属硫族化合物膜为p型MoS 2膜；步骤(1)所述n型过渡金属硫族化合物膜为n型MoS 2膜。
  9. 如权利要求5所述的纳米层状过渡金属硫族化合物横向同质PN二极管的制备方法，其特征在于，步骤(4)所述掺杂的过程为向磁控溅射装置中通入气流量为60sccm-100sccm的氧气作为起辉气体，起辉后氧气电离为氧等离子体，所述氧等离子体在电场加速下轰击样品C的表面；所述轰击的时间为10秒-60秒；所述氧气的压力10Pa-15Pa；所述磁控溅射装置的射频功率10W-40W。
  10. 如权利要求1所述的纳米层状过渡金属硫族化合物横向同质PN二极管用于光电探测器。
PCT/CN2018/085934 2018-04-20 2018-05-08 一种纳米层状横向同质pn二极管及其制备方法与应用 Ceased WO2019200629A1 (zh)

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