CN111509086A - Preparation method of two-dimensional non-laminar β -phase indium sulfide continuous film and optical detector - Google Patents

Preparation method of two-dimensional non-laminar β -phase indium sulfide continuous film and optical detector Download PDF

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CN111509086A
CN111509086A CN202010311816.1A CN202010311816A CN111509086A CN 111509086 A CN111509086 A CN 111509086A CN 202010311816 A CN202010311816 A CN 202010311816A CN 111509086 A CN111509086 A CN 111509086A
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dimensional non
continuous film
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余代者
魏爱香
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Guangdong University of Technology
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    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
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    • H01L31/08Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof in which radiation controls flow of current through the device, e.g. photoresistors
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Abstract

The invention belongs to the technical field of two-dimensional semiconductor films, and particularly relates to a preparation method of a two-dimensional non-layered β -phase indium sulfide continuous film and a photodetector, wherein the invention provides a two-dimensional non-layered β -In2S3The preparation method of the continuous film takes a horizontal tube furnace as a reaction furnace and In2S3The powder is used as raw material, inert gas or nitrogen is used as carrier gas, fluorophlogopite sheet is used as substrate, and the flow rate of inert gas or nitrogen and In are regulated based on Van der Waals epitaxial growth technology2S3Powder and fluorophlogopiteDistance between the sheets, In2S3Preparation of large-area two-dimensional non-laminar β -In by evaporation temperature and evaporation time of powder2S3The test result shows that In the preparation method, the film can continuously grow, the area can reach the centimeter-level size, and the two-dimensional non-lamellar β -In with stable phase and large area can be obtained2S3A continuous film of the two-dimensional non-layered β -In2S3Transfer of continuous film to SiO2After the/Si substrate, a field effect transistor is fabricated, which can be used as a photodetector.

Description

Preparation method of two-dimensional non-laminar β -phase indium sulfide continuous film and optical detector
Technical Field
The invention belongs to the technical field of two-dimensional semiconductor films, and particularly relates to a preparation method of a two-dimensional non-laminar β -phase indium sulfide continuous film and a photodetector.
Background
After two scientists of Andre Geim (Andre Geim) and consutant novo delov (Konstatin novoseov) from Manchester university in 2004 obtained single-layer graphene by a mechanical exfoliation method, two-dimensional materials were proven to exist in nature. Two-dimensional layered materials represented by graphene and transition metal sulfides have received great attention and have made breakthrough research progress. The concept of two-dimensional layered materials is that when the thickness of three-dimensional materials is reduced to nanometer size by mechanical or liquid phase exfoliation, the band structure and conductivity type of the materials are changed due to quantum confinement effect. For example, when MoS2When the thickness is reduced to a single layer, the band gap is changed from an indirect band gap to a direct band gap. The nano-scale thickness of the material obtained after exfoliation is referred to as a two-dimensional material. Two-dimensional layered materials share a common structural feature in that each monolayer is bonded by strong covalent bonds and the layers are bonded by weak van der waals forces, so that single-or multi-layered two-dimensional layered materials can be obtained from single-crystal bulk materials by mechanical or liquid-phase exfoliation. Meanwhile, researchers also develop chemical vapor deposition technology and physical vapor deposition technology to synthesize two-dimensional layered semiconductor materials. The specific performance and the mature preparation method which are continuously discovered make the layered material become the main object of the two-dimensional material research at present.
The two-dimensional structure of non-layered materials consisting of chemical bonds in all three dimensions is receiving increasing attention from researchers. Compared with a two-dimensional layered material, the two-dimensional non-layered material has the remarkable characteristic that a large number of suspended covalent bonds exist on the surface of the two-dimensional non-layered material, so that the surface of the two-dimensional non-layered material has very high-density active sites, and the two-dimensional non-layered material has certain advantages in the aspect of catalytic application. Meanwhile, the two-dimensional non-layered material has a high-density surface state, and the device design can be carried out by utilizing the unique rich surface state of the non-layered material, so that the efficient regulation and control of the interface state of the non-layered material are realized.
Indium sulfide (In)2S3) Is a typical non-layered semiconductor which can form three different crystal structures at different temperatures, namely α -phase indium sulfide (α -In)2S3Defect cube), β phase indium sulfide (β -In)2S3Defect spinel) and gamma-phase indium sulfide (gamma-In)2S3Layered structure) of β -In2S3Is a direct band gap n-type semiconductor which stably exists at room temperature, has a cubic or tetragonal spinel structure and has a band gap of 2.0-2.3 eV β -In2S3The tetrahedral cation sites have high-concentration vacancies, and have unique electrical and optical properties due to natural defect structures, so that the tetrahedral cation sites have good application prospects in the fields of electronics and optoelectronics in the future, such as photocatalysis, photodetectors, photovoltaic devices, light-emitting diodes and the like.
At present, the two-dimensional non-layered material is mainly synthesized by wet chemistry, such as hydrothermal synthesis method, template method and the like, the two-dimensional material obtained by the wet chemistry method has small area and has residues of active agents or impurities, the defects seriously affect the application of the two-dimensional non-layered material In the aspect of high-performance photoelectric devices, compared with the wet chemistry method, reactants used by the physical vapor deposition method do not contain organic solvents with strong toxicity (such as hydrazine hydrate and the like), the reaction time is shorter, no intermediate harmful products are generated In the reaction process, the safety and the efficiency of experiments are greatly improved, and the two-dimensional non-layered β -In obtained by the physical vapor deposition or the chemical vapor deposition technology is reported at present2S3The nano-sheet has an area of only several to several tens of micrometers, and is dispersedly distributed on the substrateAnd is not favorable for the preparation and integration of devices.
Disclosure of Invention
In view of the above, the present invention provides a two-dimensional non-layered β -In2S3A preparation method of a continuous film, which is used for solving the problem that the prior art can not obtain high-quality large-area two-dimensional non-laminar β -In2S3The problem of materials. And the continuous film is prepared into a field effect transistor which is used as a light detector.
The specific technical scheme of the invention is as follows:
two-dimensional non-layered β -In2S3A method of making a continuous film comprising the steps of:
a) first, In is mixed2S3Placing the powder and fluorophlogopite sheet In a horizontal tube furnace with a single temperature zone, wherein In2S3The powder is located In a central constant-temperature area of the horizontal tube furnace, the fluorophlogopite sheet is located In a downstream area of the horizontal tube furnace, the fluorophlogopite sheet is a stripped fluorophlogopite sheet, a stripping surface of the stripped fluorophlogopite sheet faces upwards, and the fluorophlogopite sheet and the In the central area2S3The distance between the powder is 3-10 cm; then, sealing the horizontal tube furnace, introducing air for 0.5-1 h by using inert gas or nitrogen with the flow rate of 200-300 sccm, discharging air in the horizontal tube furnace, and adjusting the flow rate of the inert gas or nitrogen to be 20-100 sccm after the air is discharged;
b) heating the central constant-temperature area of the horizontal tube furnace to 970-990 ℃ at the heating rate of 50-60 ℃/min to ensure that In is2S3Gasifying the powder, and transporting In by taking inert gas or nitrogen with the flow rate of 20-100 sccm as carrier gas2S3Gas molecules and conditioning In near the substrate2S3The concentration of gas molecules grows on the stripped fluorophlogopite sheet for 10-20 min to obtain two-dimensional non-laminar β -In2S3A continuous film.
The invention also provides a preparation method of the field effect transistor, the field effect transistor is mainly used for the optical detector, and the preparation method comprises the following steps:
A) the two-dimensional non-layered β -In the technical scheme2S3The continuous film is spin-coated with a toluene solution dissolved with polystyrene, and after being baked for 15min at 80 ℃, the fluorophlogopite sheet is a polystyrene film/two-dimensional non-lamellar β -In2S3Placing the polystyrene film/two-dimensional non-laminar β -In deionized water2S3Separating the continuous film from the fluorophlogopite sheet, and separating the polystyrene film/two-dimensional non-layered β -In2S3Continuous film sticking on SiO2Baking the Si substrate at 110-130 ℃ for 30-40 min to enable the Si substrate to be tightly and flatly adhered to the SiO substrate2a/Si substrate; then SiO2Polystyrene film on Si substrate/two-dimensional non-layered β -In2S3Immersing the continuous film In toluene to remove the polystyrene film, and blow-drying with nitrogen to realize that the two-dimensional non-laminar β -In2S3Transfer of continuous film from fluorophlogopite substrate to SiO2a/Si substrate;
B) at the transfer to SiO2Two-dimensional non-laminar β -In on a/Si substrate2S3Coating photoresist on the surface of the continuous film, aligning by a photoetching machine, exposing, developing to form a device pattern, plating gold on an electrode to obtain a field effect transistor, and using the field effect transistor as a light detector.
The invention also provides an optical detector, which comprises an optical detection device;
the optical detection device is the field effect transistor in the technical scheme.
In summary, the present invention provides a two-dimensional non-layered β -In2S3Method for producing continuous films, two-dimensional non-laminar β -In according to the invention2S3The preparation method of the continuous film takes a horizontal tube furnace as a reaction furnace and In2S3The powder is used as raw material, inert gas or nitrogen is used as carrier gas to facilitate epitaxial growth of two-dimensional non-laminated material, excellent van der Waals epitaxial substrate with flat and inert surface-fluorophlogopite sheet is used as substrate, and the flow rate of inert gas or nitrogen, In and In are regulated based on van der Waals epitaxial growth technology2S3Distance between powder and fluorophlogopite flakes, In2S3Preparation of large-area two-dimensional non-laminar β -In by evaporation temperature and evaporation time of powder2S3The experimental result shows that In the preparation method, the film can continuously grow, the area can reach the centimeter-level size, and the two-dimensional non-lamellar β -In with stable phase and large area can be obtained2S3A continuous film.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 shows the preparation of two-dimensional non-laminar β -In2S3Schematic view of an apparatus for continuous film;
FIG. 2 shows the two-dimensional non-laminar β -In obtained In example 1 of the present invention2S3Optical microscopy of continuous films;
FIG. 3 shows the two-dimensional non-laminar β -In obtained In example 2 of the present invention2S3Optical microscopy of continuous films;
FIG. 4 shows the two-dimensional non-laminar β -In obtained In example 3 of the present invention2S3Optical microscopy of continuous films;
FIG. 5 shows the two-dimensional non-laminar β -In obtained In example 1 of the present invention2S3XRD pattern of continuous film;
FIG. 6 shows example 4 of the present invention using example 1 two-dimensional non-laminar β -In2S3Optical microscopy of field effect transistors made from continuous films;
fig. 7 is a graph showing the photo-response characteristics measured by using the field effect transistor of example 4 of the present invention as a photo-detector.
Detailed Description
The invention provides a preparation method of a two-dimensional non-laminar β -phase indium sulfide continuous film and a photodetector, which are used for solving the problem that the prior art cannot obtain high-quality large-area two-dimensional non-laminar β -In2S3The problem of materials.
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment of the invention provides a two-dimensional non-layered β -In2S3The preparation method of the continuous film adopts the physical vapor deposition technology, and is prepared in a horizontal tube furnace with a single constant temperature area, wherein the length of a quartz tube is 55cm, and the inner diameter of the quartz tube is 2cm, and the preparation method comprises the following steps:
(1) weighing In2S3Putting the powder in a quartz boat, and placing the quartz boat in a central constant-temperature area of the horizontal tube furnace;
(2) peeling off the fluorophlogopite sheet with the specification size of (1-2) cm × (1-2) cm, namely firstly, sticking one side of the fluorophlogopite sheet on a transparent adhesive tape, and then cutting a small opening on the side edge of the fluorophlogopite sheet substrate by using a clean blade, wherein the fluorophlogopite sheet has good dissociation property and can be easily peeled into two clean fluorophlogopite sheets;
(3) using the freshly dissociated side as the front side of the fluorophlogopite sheet, placing the fluorophlogopite sheet In the downstream region of the horizontal tube furnace with the front side facing upward, the fluorophlogopite sheet and In2S3The distance between the powders is 3-10 cm.
(4) When In2S3After the powder and fluorophlogopite flakes were placed in the quartz tube, the quartz tube was sealed. And opening inert gas or nitrogen, adjusting the flow to be 200-300 sccm, and setting the ventilation time to be 0.5-1 h so as to achieve the purpose of discharging the air in the quartz tube. Then, the flow rate of the inert gas or nitrogen gas is adjusted to be 20-100 sccm, and heating is started.
(5) Adjusting a temperature controller of the tube furnace to increase the temperature of the central constant-temperature area from room temperature to 970-990 ℃, wherein the temperature increase rate is 50-60 ℃/min, keeping the constant temperature for 10-20 min after the temperature reaches 970-990 ℃, and performing two-dimensional non-laminar β -In2S3ContinuousAnd (5) growing the thin film. And after the reaction is finished, closing the heater, and keeping the flow of the inert gas or the nitrogen gas to be 20-100 sccm until the furnace tube is cooled to the room temperature.
The two-dimensional non-layered β -In of the embodiment of the invention2S3The preparation method of the continuous film takes a single constant temperature zone horizontal tube furnace as a reaction furnace and In2S3The powder is used as raw material, inert gas or nitrogen is used as carrier gas to facilitate epitaxial growth of two-dimensional non-laminated material, excellent Van der Waals epitaxial substrate with flat and inert surface-fluorophlogopite sheet is used as substrate, and the flow rate of inert gas or nitrogen, In and the like are regulated based on physical vapor deposition Van der Waals epitaxial growth technology2S3Distance between powder and fluorophlogopite flakes, In2S3Preparation of large-area two-dimensional non-laminar β -In by evaporation temperature and evaporation time of powder2S3The experimental result shows that In the preparation method of the embodiment of the invention, the film can continuously grow, the area can reach the centimeter-level size, and the two-dimensional non-lamellar β -In with stable phase and large area can be obtained2S3Continuous film, and the resulting two-dimensional non-laminar β -In2S3The continuous film can be transferred to other substrates by wet transfer method, and has good adhesion with other substrates, which is β -In2S3Subsequent application of the semiconductor film provides assurance.
The embodiment of the invention also provides a preparation method of the field effect transistor, which comprises the following steps:
the two-dimensional non-lamellar β -In prepared by the preparation method2S3Transfer of continuous films to SiO Using Wet transfer Process2The specific transfer method of the/Si substrate is that two-dimensional non-layered β -In is grown on the substrate2S3Spin-coating a toluene solution (PS solution) dissolved with polystyrene on a fluorophlogopite sheet of the continuous film, and then baking at 80-90 ℃ for 10-15 min, wherein the fluorophlogopite sheet is a PS film/two-dimensional non-laminar β -In2S3Continuous film, then place the sample In deionized water and gently stir the edges of fluorophlogopite flakes with tweezers to make PS film/two-dimensional non-lamellar β -In2S3Stripping the continuous film from the fluorophlogopite sheet, suspending the film on the surface of deionized water, and carrying out two-dimensional non-laminar β -In treatment on the PS film2S3The continuous film is stuck on the cleaned SiO2Baking the Si substrate at 110-130 ℃ for 30-40 min to enable the Si substrate to be tightly and flatly attached to SiO2a/Si substrate is immersed into toluene to be dissolved and removed with the PS film, and finally, nitrogen is used for blow drying, thus completing the two-dimensional non-laminar β -In2S3Transfer of continuous film from fluorophlogopite substrate to SiO2On a/Si substrate.
Then β -In two-dimensional non-laminar state2S3Spin-coating photoresist on the surface of the continuous film, aligning by a photoetching machine, exposing, developing to form a device pattern, and finally evaporating the gold electrode by a thermal evaporation coating apparatus to obtain the field effect transistor, wherein the field effect transistor is a two-dimensional β -In field effect transistor2S3The channel is formed by gold as an electrode, silicon oxide as an insulating layer and a silicon substrate as a bottom gate. The field effect transistor is used as a light detector. The test result shows that the optical detector shows good optical response sensitivity under the irradiation of laser with different wavelengths.
For a further understanding of the invention, reference will now be made in detail to the following examples.
In a specific embodiment, In2S3The powder was purchased from alatin and had a purity of 99.99%.
Example 1
This example was carried out two-dimensionally non-laminar β -In2S3The preparation of the continuous film comprises the following steps:
1) and the glass instruments such as quartz boats and quartz tubes are wiped by using the dust-free cloth dipped with the wet absolute ethyl alcohol, so that the cleanness of the experimental equipment is ensured. Wherein, the length of the quartz tube is 55cm, and the inner diameter is 2 cm. Then, 20mg of In was weighed2S3Placing the powder In a quartz boat, and filling In2S3Placing a quartz boat of powder In a central constant temperature zone of a horizontal tube furnace, placing a 1cm × 2cm size freshly peeled fluorophlogopite sheet downstream of the horizontal tube furnace with the peel side of the peeled fluorophlogopite sheet facing upward, and peeling the fluorophlogopite sheet from In the central zone2S3The distance of the powder was 10 cm.
2) Sealing the quartz tube, introducing argon gas with the flow rate of 200sccm to exhaust air In the quartz tube, adjusting the argon gas flow rate to 50sccm after 1 hour of ventilation, setting a temperature raising program, heating the temperature of a central constant temperature region of the horizontal tube furnace from room temperature to 980 ℃ at the speed of 60 ℃/min, and carrying out physical vapor growth at 980 ℃ for 15min to prepare the two-dimensional non-lamellar β -In2S3A continuous film. After the growth process is finished, the heater is closed, and the argon flow is still kept at 50sccm until the furnace tube is cooled to the room temperature.
Referring to FIG. 2, there is shown a two-dimensional non-layered β -In prepared In example 1 of the present invention2S3FIG. 2 shows the two-dimensional non-laminar β -In obtained In this example2S3The continuous film is composed of smooth surface and irregular polygon β -In2S3A continuous growth stack is formed.
Referring to FIG. 5, there is shown a two-dimensional non-layered β -In prepared In accordance with example 1 of the present invention2S3XRD Pattern of continuous film FIG. 5 shows that two-dimensional non-layered β -In was produced2S3In continuous thin film2S3β phase.
Example 2
This example was carried out two-dimensionally non-laminar β -In2S3Preparation of a continuous film, the procedure is as in example 1, but with the following differences: stripping off the fluorophlogopite sheet from In the center region2S3The distance of the powder is 3 cm; after 1 hour of aeration, the argon flow was adjusted to 20 sccm; setting a temperature rise program, heating the temperature of the central constant-temperature area of the horizontal tube furnace from room temperature to 990 ℃ at the speed of 60 ℃/min, and carrying out physical vapor growth at 990 ℃ for 10 min.
Referring to FIG. 3, a two-dimensional non-layered β -In is shown, which is obtained In accordance with example 2 of the present invention2S3FIG. 3 shows the two-dimensional non-laminar β -In obtained In this example2S3The continuous film is mainly composed of smooth-surfaced regular-shaped triangles β -In with smaller size2S3Continuously growing stacksAnd (4) forming.
Example 3
This example was carried out two-dimensionally non-laminar β -In2S3Preparation of a continuous film, the procedure is as in example 1, but with the following differences: after 1 hour of aeration, the argon flow was adjusted to 100 sccm; setting a temperature rise program, heating the temperature of the central constant-temperature area of the horizontal tube furnace from room temperature to 970 ℃ at the speed of 60 ℃/min, and carrying out physical vapor growth at 970 ℃ for 20 min.
FIG. 4 shows two-dimensional non-layered β -In obtained In example 3 of the present invention2S3FIG. 4 shows the two-dimensional non-laminar β -In obtained In this example2S3The continuous film is composed of smooth surface, regular shape and larger size triangle β -In2S3A continuous growth stack is formed.
Example 4
In this example, the field effect transistor was fabricated, including the following steps:
the two-dimensional non-layered β -In prepared In example 1 was used2S3Transfer of continuous films to SiO Using Wet transfer Process2The specific transfer method of the/Si substrate is that two-dimensional non-layered β -In is grown on the substrate2S3Spin-coating polystyrene-dissolved toluene solution (PS solution) on fluorophlogopite sheet of continuous film, baking at 80 deg.C for 15min to obtain PS film/two-dimensional non-laminar β -In2S3Continuous film, placing the sample In deionized water, and gently poking the edge of fluorophlogopite sheet with tweezers to make PS film/two-dimensional non-laminar β -In2S3Stripping the continuous film from fluorophlogopite sheet, suspending the film on the surface of deionized water, and preparing PS film/two-dimensional non-laminated β -In2S3The continuous film is stuck on the cleaned SiO2Baking the substrate/Si at 130 ℃ for 30min, immersing the substrate In toluene to dissolve and remove the PS film, and finally blowing the substrate by nitrogen to dry, thereby realizing the purpose of drying the two-dimensional non-laminar β -In2S3Transfer of continuous film from fluorophlogopite substrate to SiO2On a/Si substrate.
Then β -In two-dimensional non-laminar state2S3Spin-coating photoresist on the surface of the continuous film, aligning by a photoetching machine, exposing, developing to form a device pattern, and finally evaporating the gold electrode by a thermal evaporation coating apparatus to obtain the field effect transistor, wherein the field effect transistor is formed In a two-dimensional non-layered β -In manner2S3The channel is formed by gold as an electrode, silicon oxide as an insulating layer and a silicon substrate as a bottom gate.
Referring to FIG. 6, there is shown two-dimensional non-layered β -In prepared In example 1 as In example 4 of the present invention2S3Optical microscopy of field effect transistors made from continuous films.
Fig. 7 shows a photo-response characteristic curve diagram of a field effect transistor as a photo-detector in embodiment 4 of the present invention. Fig. 7 shows that, under the irradiation of laser light with 5mw of optical power intensity and with wavelengths of 405nm blue light, 532nm green light and 635nm red light respectively, the switching period of the laser light source is 3s, and the laser light source has good photoresponse sensitivity.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that modifications can be made by those skilled in the art without departing from the principle of the present invention, and these modifications should also be construed as the protection scope of the present invention.

Claims (3)

1. Two-dimensional non-layered β -In2S3The preparation method of the continuous film is characterized by comprising the following steps:
a) in is mixed with2S3Placing the powder and fluorophlogopite sheet In a horizontal tube furnace with a single temperature zone, wherein In2S3The powder is located In a central constant-temperature area of the horizontal tube furnace, the fluorophlogopite sheet is located In a downstream area of the horizontal tube furnace, the fluorophlogopite sheet is a stripped fluorophlogopite sheet, a stripping surface of the stripped fluorophlogopite sheet faces upwards, and the fluorophlogopite sheet and the In the central area2S3The distance between the powder is 3-10 cm; sealing the horizontal tube furnace, introducing inert gas or nitrogen with the flow of 200-300 sccm for 0.5-1 h, and introducing the waterDischarging air in the flat tube furnace, and adjusting the flow of inert gas or nitrogen to be 20-100 sccm after the air is discharged;
b) heating the central constant-temperature area of the horizontal tube furnace to 970-990 ℃ at the heating rate of 50-60 ℃/min to ensure that In is2S3Gasifying the powder, and transporting In by taking inert gas or nitrogen with the flow rate of 20-100 sccm as carrier gas2S3Gas molecules and conditioning In near the substrate2S3The concentration of gas molecules grows on the stripped fluorophlogopite sheet for 10-20 min to obtain two-dimensional non-laminar β -In2S3A continuous film.
2. A preparation method of a field effect transistor is characterized by comprising the following steps:
A) the two-dimensional non-layered β -In of claim 12S3The continuous film is spin-coated with a toluene solution dissolved with polystyrene, and after being baked for 15min at 80 ℃, the fluorophlogopite sheet is a polystyrene film/two-dimensional non-lamellar β -In2S3Placing the polystyrene film/two-dimensional non-laminar β -In deionized water2S3Separating the continuous film from the fluorophlogopite sheet, and separating the polystyrene film/two-dimensional non-layered β -In2S3Continuous film sticking on SiO2Baking the Si substrate at 110-130 ℃ for 30-40 min; then SiO2Polystyrene film on Si substrate/two-dimensional non-layered β -In2S3Immersing the continuous film In toluene to remove the polystyrene film, and blow-drying with nitrogen to realize that the two-dimensional non-laminar β -In2S3Transfer of continuous film from fluorophlogopite substrate to SiO2a/Si substrate;
B) at the transfer to SiO2Two-dimensional non-laminar β -In on a/Si substrate2S3And coating photoresist on the surface of the continuous film, aligning by using a photoetching machine, exposing, developing to form a device pattern, and plating gold electrode to obtain the field effect transistor.
3. A photodetector, comprising a photodetector device;
the photodetecting device is a field effect transistor according to claim 2.
CN202010311816.1A 2020-04-20 2020-04-20 Preparation method of two-dimensional non-laminar β -phase indium sulfide continuous film and optical detector Pending CN111509086A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105463580A (en) * 2016-01-07 2016-04-06 中国科学院理化技术研究所 Preparation method of cadmium selenide or cadmium sulfide two-dimensional monocrystal nanosheet
CN106129112A (en) * 2016-07-04 2016-11-16 华为技术有限公司 A kind of electronic device based on two-dimensional semiconductor and manufacture method thereof
CN108048900A (en) * 2017-12-17 2018-05-18 华中科技大学 A kind of method and product for preparing non-laminar two-dimensional nano cadmium sulfide crystalline material
CN108531981A (en) * 2018-03-09 2018-09-14 广东工业大学 A method of preparing two-dimentional indium trisulfide monocrystalline in mica substrate
CN110473925A (en) * 2019-07-09 2019-11-19 广东工业大学 A kind of two dimension molybdenum sulfide/indium sulfide transverse direction hetero-junctions and its preparation method and application
CN110528072A (en) * 2019-07-09 2019-12-03 广东工业大学 A kind of two dimension indium trisulfide coupling tellurium quantum dot composite material and its preparation method and application
CN110846719A (en) * 2019-11-28 2020-02-28 华中科技大学 Two-dimensional non-layered In2SnS4Crystalline material and method for producing same

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105463580A (en) * 2016-01-07 2016-04-06 中国科学院理化技术研究所 Preparation method of cadmium selenide or cadmium sulfide two-dimensional monocrystal nanosheet
CN106129112A (en) * 2016-07-04 2016-11-16 华为技术有限公司 A kind of electronic device based on two-dimensional semiconductor and manufacture method thereof
CN108048900A (en) * 2017-12-17 2018-05-18 华中科技大学 A kind of method and product for preparing non-laminar two-dimensional nano cadmium sulfide crystalline material
CN108531981A (en) * 2018-03-09 2018-09-14 广东工业大学 A method of preparing two-dimentional indium trisulfide monocrystalline in mica substrate
CN110473925A (en) * 2019-07-09 2019-11-19 广东工业大学 A kind of two dimension molybdenum sulfide/indium sulfide transverse direction hetero-junctions and its preparation method and application
CN110528072A (en) * 2019-07-09 2019-12-03 广东工业大学 A kind of two dimension indium trisulfide coupling tellurium quantum dot composite material and its preparation method and application
CN110846719A (en) * 2019-11-28 2020-02-28 华中科技大学 Two-dimensional non-layered In2SnS4Crystalline material and method for producing same

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
LU JIANTING ET.AL: "Epitaxial growth of large-scale In2S3 nanoflakes and the construction of a high performance In2S3/Si photodetector", 《JOURNAL OF MATERIALS CHEMISTRY C》 *

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