CN112850660B - alpha-MnSe nanosheet and preparation method and application thereof - Google Patents

alpha-MnSe nanosheet and preparation method and application thereof Download PDF

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CN112850660B
CN112850660B CN202110057412.9A CN202110057412A CN112850660B CN 112850660 B CN112850660 B CN 112850660B CN 202110057412 A CN202110057412 A CN 202110057412A CN 112850660 B CN112850660 B CN 112850660B
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何军
李宁宁
王振兴
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National Center for Nanosccience and Technology China
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Abstract

The invention relates to the field of photoelectric materials, in particular to an alpha-MnSe nanosheet and a preparation method and application thereof. The preparation method of the alpha-MnSe nanosheet comprises the following steps: se and manganese sources are taken as raw materials and prepared by a chemical vapor deposition method; the manganese source is MnO2Or MnCl2. According to the invention, alpha-MnSe nanosheet is prepared on a mica substrate by selecting specific raw materials and using a Chemical Vapor Deposition (CVD) method; the alpha-MnSe nanosheet is an antiferromagnetic wide band gap semiconductor. The preparation method provided by the invention has good controllability on the size and thickness of the alpha-MnSe nanosheet, and has the advantages of simple process, high synthesis speed, high crystal quality of the prepared alpha-MnSe nanosheet and good stability. The invention provides good material selection for two-dimensional magnetic research; the alpha-MnSe nanosheet prepared by the method is applied to a photoelectric detection device, and has excellent photodetection performance.

Description

alpha-MnSe nanosheet and preparation method and application thereof
Technical Field
The invention relates to the field of photoelectric materials, in particular to an alpha-MnSe nanosheet and a preparation method and application thereof.
Background
Atomic thin two-dimensional materials have attracted much attention from researchers due to their excellent electrical, optical, mechanical, and magnetic properties, as well as their wide application in the fields of electronics, optoelectronics, and spintronics. Among them, two-dimensional magnetic materials have been a research focus of attention in recent years due to their unique two-dimensional magnetic properties.
Currently, much research effort is devoted to the exploration and study of two-dimensional magnetic materials. E.g., crI in fewer layers3The giant tunneling magnetoresistance is realized, and the magnetoresistance ratio can reach 19000 percent, even higher than that of the traditional MgO-based magnetic tunneling junction. Two dimensional Fe3GeTe2Room temperature ferromagnetism is exhibited by the ion grid. These very interesting phenomena suggest a very promising prospect in spintronics and valley electronics. However, the above magnetic materials are all based on the conventional mechanical stripping method, which has very poor control on the thickness, size and mass production of the two-dimensional nanosheets, and inevitably limits the exploration and further practical application of the basic properties thereof.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a preparation method of alpha-MnSe nanosheets, which has good controllability on the size and the thickness of a sample, simple process and high synthesis speed; the invention also aims to provide an alpha-MnSe nanosheet, which has high crystalline quality and good stability; the invention also aims to provide application of the alpha-MnSe nanosheet.
Specifically, the invention provides the following technical scheme:
the invention provides a preparation method of an alpha-MnSe nanosheet, which comprises the following steps:
se and manganese sources are taken as raw materials and prepared by a chemical vapor deposition method;
the manganese source is MnO2Or MnCl2。
The invention discovers that when the nanosheet is prepared by using a chemical vapor deposition method, the thickness and the size of the two-dimensional nanosheet can be controlled by regulating and controlling the growth temperature and the growth time; further, the present inventors have unexpectedly discovered, in their research, that by controlling the manganese source (i.e., mnO)2Or MnCl2) When the specific selection is carried out, the growth orientation of the two-dimensional nanosheet can be controlled; namely, the invention can control the growth orientation, thickness and size of the obtained alpha-MnSe nanosheet by controlling the specific selection and growth conditions of the manganese source.
In order to further improve the controllability of the alpha-MnSe nanosheet, the conditions of the chemical vapor deposition method are optimized, and the conditions are as follows:
preferably, the reaction temperature of Se is 270-290 ℃; further, the reaction temperature of Se is 280 ℃.
Preferably, the MnO is2The reaction temperature of (2) is 680-750 ℃; further, the MnO2The reaction temperature of (2) was 720 ℃.
Preferably, the MnCl2The reaction temperature is 630-710 ℃; further, the MnCl2The reaction temperature of (2) is 660 DEG C
In the invention, when the chemical vapor deposition method is used for preparing the alpha-MnSe nanosheet, the reaction temperature of the raw materials is particularly important; specifically, when Se and MnO2Or MnCl2When the reaction temperature is in the range, the obtained alpha-MnSe nanosheet has higher controllability and better crystallization quality and stability.
Preferably, the carrier gas of the chemical vapor deposition method is a mixed gas of argon and hydrogen; the flow rate of the argon is 100-150 sccm; the flow rate of the hydrogen is 5-20 sccm.
Further, the flow rate of the argon gas is 120sccm; the flow rate of the hydrogen gas was 10sccm.
According to the invention, the mixed gas of argon and hydrogen is adopted, and the flow of argon and hydrogen are respectively controlled, so that the controllability of the alpha-MnSe nanosheet is improved.
Preferably, the reaction time of the chemical vapor deposition method is 15 to 55min.
Further, the reaction time of the chemical vapor deposition method is 30min.
Preferably, the substrate of the chemical vapor deposition process is mica.
Preferably, the preparation method comprises the following steps:
respectively placing Se and a manganese source in a low-temperature area and a high-temperature area of a double-temperature area tubular furnace, placing a substrate 2-6 cm behind the manganese source, continuously introducing mixed gas of argon and hydrogen into the double-temperature area tubular furnace, reacting by a chemical vapor deposition method, and cooling to room temperature after the reaction is finished.
Further, a furnace tube of the double-temperature-zone tube furnace is a quartz tube; after placing the Se and manganese sources, the quartz tube was purged with argon.
As a preferred technical solution of the present invention, the preparation method comprises:
placing Se in a low-temperature area of a double-temperature-area tubular furnace, placing a manganese source in a high-temperature area of the double-temperature-area tubular furnace, placing mica 2-6 cm behind the manganese source, cleaning the quartz tube with argon, raising the temperature of the low-temperature area to 280 ℃, raising the temperature of the high-temperature area to 680-750 ℃ or 630-710 ℃, and continuously introducing mixed gas of argon and hydrogen, wherein the flow of argon is 100-150 sccm, the flow of hydrogen is 5-20 sccm, the reaction time is 15-55 min, and after the reaction is finished, naturally cooling to room temperature to obtain the alpha-MnSe nanosheet growing on the mica.
In the technical schemeThe temperature of the high temperature zone is determined by the manganese source; when the manganese source is MnO2When the temperature of the high-temperature area is raised to 680-750 ℃; when the manganese source is MnCl2When the temperature of the high-temperature area is raised to 630-710 ℃.
The invention also provides an alpha-MnSe nanosheet, which is prepared by the method.
The alpha-MnSe nanosheet is a nanosheet growing on a substrate in parallel; specifically, nanosheets of different shapes can be obtained by selecting different manganese sources, specifically as follows:
preferably, when the manganese source is MnO2When the alpha-MnSe nanosheets are square nanosheets growing along the (001) plane;
furthermore, the transverse size of the square nanosheet is 12-119 μm, and the thickness is 3-50 nm.
Furthermore, the transverse dimension of the square nanosheet is 15-40 μm, and the thickness is 20-30 nm.
Preferably, when the manganese source is MnCl2When the alpha-MnSe nanosheets are triangular nanosheets growing along the (111) plane;
furthermore, the triangular nanosheet is 3-76 μm in transverse size and 5-48 nm in thickness.
Furthermore, the triangular nanosheet is 15-40 μm in transverse dimension and 20-30 nm in thickness.
The invention also provides application of the alpha-MnSe nanosheet in preparation of a photoelectric detector.
The invention has the beneficial effects that:
(1) According to the invention, alpha-MnSe nanosheet is prepared on a mica substrate by selecting specific raw materials and using a Chemical Vapor Deposition (CVD) method; the alpha-MnSe nanosheet is an antiferromagnetic wide band gap semiconductor.
(2) The preparation method provided by the invention has good controllability on the size and thickness of the alpha-MnSe nanosheet, and is simple in process and high in synthesis speed, and the prepared alpha-MnSe nanosheet is high in crystal quality and good in stability.
(3) The invention provides good material selection for two-dimensional magnetic research; the alpha-MnSe nanosheet prepared by the invention is applied to a photoelectric detection device, and has excellent light detection performance.
Drawings
Fig. 1 is an Optical Microscope (OM) picture of α -MnSe nanoplatelets grown on a mica substrate provided by the present invention; wherein a is an Optical Microscope (OM) picture of alpha-MnSe (001) square nanosheet growing on a mica substrate; b is an Optical Microscope (OM) picture of alpha-MnSe (111) triangular nanosheet growing on a mica substrate.
FIG. 2 is an Atomic Force Microscope (AFM) view of α -MnSe nanoplates provided by the present invention; wherein a is an Atomic Force Microscope (AFM) picture of an alpha-MnSe (001) square nanosheet; b is an Atomic Force Microscope (AFM) picture of an alpha-MnSe (111) triangular nanosheet.
Fig. 3 is an X-ray diffraction (XRD) pattern of the α -MnSe nanosheet provided by the present invention; wherein a is an X-ray diffraction (XRD) pattern of an alpha-MnSe (001) square nanosheet; b is an X-ray diffraction (XRD) pattern of the alpha-MnSe (111) triangular nanosheet.
FIG. 4 is a selected area electron diffraction pattern, high Resolution Transmission Electron Microscopy (HRTEM) pattern, and elemental distribution plot of an α -MnSe nanosheet provided by the present invention; wherein a is a selected area electron diffraction pattern of an alpha-MnSe (001) square nanosheet; b is a high-resolution transmission electron microscope (HRTEM) image of an alpha-MnSe (001) square nanosheet; c and d are element distribution maps of the alpha-MnSe (001) square nanosheets; e is a selected area electron diffraction pattern of the alpha-MnSe (111) triangular nanosheet; f is a High Resolution Transmission Electron Microscope (HRTEM) image of the alpha-MnSe (111) triangular nanosheets; g and h are element distribution maps of the alpha-MnSe (111) triangular nanosheets.
Fig. 5 is a schematic diagram of the alpha-MnSe (001) square nanosheet provided by the invention along with the change of growth temperature and time.
Fig. 6 is a schematic diagram of the alpha-MnSe (111) triangular nanosheet provided by the invention along with the change of growth temperature and time.
Fig. 7 is a diagram of a device based on α -MnSe (001) square nanoplates.
FIG. 8 shows responsivity of the output curve test, optical switching characteristic curve and photoelectric detection of the alpha-MnSe (001) square nanosheet under 473nm laser provided by the present invention; wherein a is the output characteristic curve of the photoelectric detector of the alpha-MnSe (001) square nanosheet under different laser intensities; b is the light switch characteristic of the alpha-MnSe photoelectric detector under different light intensities; and c is the responsivity of photoelectric detection of the alpha-MnSe (001) square nanosheet.
Fig. 9 is a diagram of a device based on alpha-MnSe (111) triangular nanosheets.
FIG. 10 shows responsivity of an output curve test, a photoswitch characteristic curve and a photodetection of the alpha-MnSe (111) triangular nanosheet under 473nm laser provided by the invention; wherein a is the output characteristic curve of the photoelectric detector of the alpha-MnSe (111) triangular nanosheet under different laser intensities; b is the light switch characteristic of the alpha-MnSe photoelectric detector under different light intensities; and c is the responsivity of photoelectric detection of the alpha-MnSe (111) triangular nanosheet.
Detailed Description
The following examples are intended to illustrate the invention, but are not intended to limit the scope of the invention.
Example 1
The embodiment provides an α -MnSe (001) square nanosheet, and a preparation method of the α -MnSe (001) square nanosheet comprises the following steps:
placing Se powder in a low-temperature area of a double-temperature-area tube furnace, mnO2Placing the powder in the high temperature region of a double-temperature-region tube furnace, and placing the mica substrate in MnO2Cleaning a quartz tube 2-6 cm behind the powder by argon, and then heating the low-temperature region to 280 ℃ and the high-temperature region to 720 ℃; and continuously introducing mixed gas of argon and hydrogen, wherein the flow of argon is 120sccm, the flow of hydrogen is 10sccm, the growth time is 30min, and then naturally cooling to room temperature.
Specifically, fig. 1a is an Optical Microscope (OM) picture of α -MnSe (001) square nanoplatelets grown on a mica substrate; FIG. 2a is an Atomic Force Microscope (AFM) image of α -MnSe (001) square nanoplates. As can be seen from FIGS. 1a and 2a, the nanosheets prepared in this example are square, with a size of 10-30 μm, and a typical α -MnSe (001) square nanosheet has a thickness of 5.63nm.
FIG. 3a is an X-ray diffraction (XRD) pattern of α -MnSe (001) square nanoplates; as can be seen from fig. 3a, the detected peaks correspond to (002) plane and (004) plane respectively, indicating that the growth orientation of the α -MnSe (001) square nanosheets is the (001) crystal plane.
FIG. 4a is a selected area electron diffraction pattern of a square nanosheet of α -MnSe (001); as can be seen from fig. 4a, only one set of square diffraction spots is shown demonstrating its single crystal nature and square lattice structure, and its [001] crystal axis again demonstrates the preferred growth orientation of the (001) plane. FIG. 4b is a High Resolution Transmission Electron Microscopy (HRTEM) image of α -MnSe (001) square nanoplates; as can be seen from FIG. 4b, the lattice fringes and the selected diffraction spots of the synthesized alpha-MnSe (001) square nanosheet are quite clear, and the crystallinity is very good. FIGS. 4c and 4d are elemental distribution diagrams of α -MnSe (001) square nanosheets; as can be seen from FIGS. 4c and 4d, the synthesized α -MnSe (001) square nanosheets have very uniform element distribution.
FIG. 5 is a schematic of α -MnSe (001) square nanoplates as a function of growth temperature and time; as can be seen from fig. 5, the nanoplatelets increase in size first and then decrease in size as the temperature increases, and the growth temperature is preferably 720 ℃; the maximum size of the synthesized alpha-MnSe nanosheets gradually increased from 16 μm to 119 μm with growth time increasing from 15min to 50min at a fixed growth temperature of 720 ℃.
Example 2
The embodiment provides an alpha-MnSe (111) triangular nanosheet, and the preparation method of the alpha-MnSe (111) triangular nanosheet comprises the following steps:
placing Se powder in a low-temperature area of a double-temperature-area tube furnace and MnCl2Placing the powder in the high temperature region of a double-temperature-region tube furnace, placing the mica substrate in MnCl2Cleaning a quartz tube 2-6 cm behind the powder by using argon, raising the temperature of a low-temperature region to 280 ℃, raising the temperature of a high-temperature region to 660 ℃, continuously introducing mixed gas of argon and hydrogen, wherein the flow of the argon is 100-150 sccm, the flow of the hydrogen is 5-20 sccm, the growth time is 15-50 min, and then naturally cooling to room temperature.
Specifically, fig. 1b is an Optical Microscope (OM) picture of alpha-MnSe (111) triangular nanosheets grown on a mica substrate, and fig. 2b is an Atomic Force Microscope (AFM) picture of alpha-MnSe (111) triangular nanosheets; as can be seen from FIGS. 1b and 2b, the synthesized nanosheets are triangular in shape, the size of the nanosheets is 5-20 μm, and the thickness of one typical alpha-MnSe (111) triangular nanosheet is 7.5nm.
FIG. 3b is an X-ray diffraction (XRD) pattern of α -MnSe (111) triangular nanoplates; as can be seen from fig. 3b, the detected peaks correspond to (111) plane and (222) plane respectively, indicating that the growth orientation of the α -MnSe (111) triangular nanosheets is the (111) crystal plane.
FIG. 4e is a selected area electron diffraction pattern of α -MnSe (111) triangular nanosheets; as can be seen in FIG. 4e, only one set of triangular diffraction spots is shown demonstrating its single crystal nature and triangular lattice structure, and its [111] crystallographic axis again demonstrates the preferential growth orientation of the (111) plane. FIG. 4f is a High Resolution Transmission Electron Microscopy (HRTEM) image of α -MnSe (111) triangular nanosheets; as can be seen from FIG. 4f, the lattice fringes and the selected diffraction spots of the synthesized alpha-MnSe (111) triangular nanosheets are quite clear, and the alpha-MnSe (111) triangular nanosheets have very good crystallinity. FIGS. 4g and 4h are elemental distribution plots of triangular α -MnSe (111) nanosheets; as can be seen from FIGS. 4g and 4h, the synthesized alpha-MnSe (111) triangular nanosheets have very uniform element distribution.
FIG. 6 is a schematic of α -MnSe (111) triangular nanosheets as a function of growth temperature and time; as can be seen from fig. 6, the nanoplatelets increase in size first and then decrease in size with increasing temperature, and the growth temperature is preferably 660 ℃; the maximum size of the synthesized alpha-MnSe (111) triangular nanosheets gradually increased from 9 μm to 75 μm as the growth time increased from 15min to 55min at a fixed growth temperature of 660 ℃.
Example 3
In this example, the α -MnSe nanosheets of examples 1 and 2 were fabricated into transistor devices by EBL and thermal evaporation, and the application performance thereof in the aspect of photodetection was tested, with the laser wavelength being 473nm.
Specifically, fig. 8a is an output characteristic curve of a photodetector of an α -MnSe (001) square nanosheet under different laser intensities, fig. 7 is a device diagram based on the α -MnSe (001) square nanosheet, and Cr/Au (8/60 nm) is thermally evaporated to form a source-drain electrode; as can be seen from FIGS. 7 and 8a, alpha-MnSe (00) is obtained after the light is applied1) The square nanoplatelets exhibit a pronounced photoresponse. Fig. 8b shows the optical switching characteristics of the α -MnSe photodetector under different light intensities, and it can be seen from fig. 8b that the device has good stability. FIG. 8c shows the responsivity of photoelectric detection of the square nanosheets of alpha-MnSe (001), and as can be seen from FIG. 8c, the square nanosheets of alpha-MnSe (001) have good photoresponse, and the responsivity of the square nanosheets of alpha-MnSe (001) can reach 1.21 multiplied by 102A/W。
FIG. 10a is an output characteristic curve of a photodetector with alpha-MnSe (111) triangular nanosheets under different laser intensities, FIG. 9 is a device diagram based on the alpha-MnSe (111) triangular nanosheets, and Cr/Au (8/60 nm) is thermally evaporated to form a source electrode and a drain electrode; from fig. 9 and fig. 10a, it can be seen that the alpha-MnSe (111) triangular nanosheets exhibit a distinct photoresponse after being illuminated with a good linear ohmic contact. FIG. 10b is the photo-switch characteristics of the α -MnSe photodetector at different light intensities; as can be seen from fig. 10b, the device has good stability. FIG. 10c is the responsivity of the photodetection of alpha-MnSe (111) triangular nanoplates; as can be seen from FIG. 10c, the alpha-MnSe (111) triangular nanosheet has good photoresponse, and the responsivity of the alpha-MnSe (111) triangular nanosheet can reach 2.52 multiplied by 103A/W。
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims (2)

1. A preparation method of an alpha-MnSe nanosheet is characterized by comprising the following steps:
se and a manganese source are taken as raw materials and prepared by a chemical vapor deposition method;
the method specifically comprises the following steps: placing Se in a low-temperature area of a double-temperature-area tubular furnace, placing a manganese source in a high-temperature area of the double-temperature-area tubular furnace, placing mica 2-6 cm behind the manganese source, cleaning the quartz tube with argon, raising the temperature of the low-temperature area to 280 ℃, raising the temperature of the high-temperature area to 680-750 ℃ or 630-710 ℃, and continuously introducing mixed gas of argon and hydrogen, wherein the flow of the argon is 100-150 sccm, the flow of the hydrogen is 5-20 sccm, the reaction time is 15-55 min, and after the reaction is finished, naturally cooling to room temperature to obtain alpha-nanosheet MnSe growing on the mica;
wherein the temperature of the high temperature zone is determined by the manganese source; when the manganese source is MnO2When the temperature is higher than 680 to 750 ℃, the temperature of the high-temperature area is raised to 680 ℃; when the manganese source is MnCl2When the temperature is higher than the set temperature, the temperature of the high-temperature region is raised to 630-710 ℃.
2. The application of the alpha-MnSe nanosheet prepared by the preparation method of claim 1 in preparing a photoelectric detector.
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