CN114497196B - Se-Cr2S3Two-dimensional material, preparation method and application - Google Patents
Se-Cr2S3Two-dimensional material, preparation method and application Download PDFInfo
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- 239000012159 carrier gas Substances 0.000 claims abstract description 36
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- 239000002135 nanosheet Substances 0.000 claims description 42
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- 230000005669 field effect Effects 0.000 claims description 18
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- 229910052573 porcelain Inorganic materials 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 4
- 229910021556 Chromium(III) chloride Inorganic materials 0.000 claims description 3
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229960000359 chromic chloride Drugs 0.000 claims description 3
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Abstract
The invention provides a Se-Cr 2S3 two-dimensional material, a preparation method and application, wherein the preparation method comprises the following steps: dividing a cavity of the quartz tube into an upstream high-temperature constant-temperature region and a downstream high-temperature constant-temperature region according to the direction of carrier gas flow; placing S powder and Se powder in an upstream high-temperature constant-temperature area, and placing CrCl 3 powder in a downstream high-temperature constant-temperature area; pre-introducing a protective gas to purge the cavity before heating to remove impurities in the cavity of the quartz tube, and then heating the S powder, the Se powder and the CrCl 3 powder to the corresponding volatilization temperature at a heating rate of 30 ℃/min; the protector is then converted to a hydrogen-containing carrier gas Ar/H 2, and growth is controlled at a preset carrier gas flow rate in a deposition temperature range to obtain Se-Cr 2S3 two-dimensional material. The method successfully improves the mobility of the Cr 2S3 two-dimensional material through Se doping, shortens the photoresponse time and regulates and controls the magnetic performance of the Cr 2S3 two-dimensional material.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a Se-Cr 2S3 two-dimensional material, a preparation method and application.
Background
In classical semiconductor theory, doping techniques refer to the introduction of impurity atoms into a material for tuning semiconductor properties. Doped semiconductors can change their band structure, such as the size of the band gap, the location of the fermi level, and further tailor the corresponding electrical, optical, and magnetic properties. Since these properties are closely related to the doping concentration, it is crucial to achieve a controllable doping concentration in semiconductor technology.
Generally, two-dimensional (2D) materials, including layered and non-layered materials, having atomic scale thickness have shown unique electrical, optical, and magnetic properties. Such as superconductivity, anomalous quantum hall effect, and valley electronics. In order to maximize the use of two-dimensional materials, it is necessary to develop methods to tailor their properties, such as building heterostructures, fabricating new devices, and doping.
Cr 2X3 (x=s, se) is a non-layered magnetic material with a monoclinic NiAs crystal structure, and can be considered as 1/3Cr atoms embedded in the van der waals gap of 1T layered CrX 2. Wherein Cr 2Se3 is a ferromagnetic or spin-on glassy metal. The thickness-controllable Cr 2S3 nano-sheet synthesized by chemical vapor deposition method is a ferrimagnetic semiconductor, the Neille temperature is 75K, and the Curie temperature is 120K. The conductivity behavior of Cr 2S3 nanoplatelets is reported to vary with increasing thickness, from p-type to bipolar to n-type. In addition, the Cr 2S3 nanoplatelets exhibit excellent environmental stability and high responsiveness under laser irradiation at 520nm, 808nm, and 1550 nm. The Cr 2S3 nano-sheet is used as a spin injection layer and a high-performance broadband photoelectric detector, and has potential application in a semiconductor spin device.
However, ultra-thin Cr 2S3 nanoplatelets have hole mobility as low as 6.3x10 -3cm2·V-1·s-1 and a photo response time as long as 1.65s, severely limiting their development in electronics, spintronics and optoelectronics. Based on this, it is necessary to propose an effective method to improve the mobility of Cr 2S3.
Disclosure of Invention
Based on the above, the invention aims to solve the problems that in the prior art, the hole mobility of an ultrathin Cr 2S3 nano-sheet is too low, and the development of the ultrathin Cr 2S3 nano-sheet in electronics, spintronics and optoelectronics is severely limited due to too long photo-response time.
The invention provides a preparation method of Se-Cr 2S3 two-dimensional material, wherein the preparation method is used for preparing by a vapor deposition device, the vapor deposition device comprises a quartz tube, the quartz tube comprises an upstream high-temperature constant-temperature region and a downstream high-temperature constant-temperature region, the upstream high-temperature constant-temperature region is provided with a first porcelain boat loaded with sulfur powder and selenium powder, the downstream high-temperature constant-temperature region is provided with a second porcelain boat loaded with chromium trichloride and fluorophlogopite, the vapor deposition device also comprises a heating device for heating the upstream high-temperature constant-temperature region and the downstream high-temperature constant-temperature region, and the vapor deposition device is a double-temperature-region reaction device;
The method comprises the following steps:
The method comprises the steps that firstly, an inlet for inputting carrier gas into a cavity of a quartz tube is arranged at one end of the quartz tube, and an outlet for outputting cavity gas of the quartz tube is arranged at the other end of the quartz tube; dividing a cavity of the quartz tube into an upstream high-temperature constant-temperature region and a downstream high-temperature constant-temperature region according to the direction of carrier gas flow;
step two, placing S powder and Se powder in the upstream high-temperature constant-temperature area, and placing CrCl 3 powder in the downstream high-temperature constant-temperature area;
step three, pre-introducing a protective gas of 300sccm to purge the cavity for 5min before heating to remove impurities in the cavity of the quartz tube, and then heating the S powder, the Se powder and the CrCl 3 powder to the corresponding volatilization temperature at a heating rate of 30 ℃/min under the carrier gas flow rate of 110-130 sccm of the protective gas;
And step four, converting the protector into hydrogen-containing carrier gas Ar/H 2, controlling the growth of the carrier gas Ar/H 2 in a deposition temperature range under the preset carrier gas flow rate for 10-30 min, enabling the volatilized S powder, se powder and CrCl 3 powder to react with each other, depositing the S powder, se powder and CrCl 3 powder on a substrate, and growing on the substrate to obtain the Se-Cr 2S3 two-dimensional material.
In the third step, the volatilization temperature of the S powder is controlled to be 180-220 ℃, the volatilization temperature of the Se powder is controlled to be 280-320 ℃ and the volatilization temperature of the CrCl 3 powder is controlled to be 750-800 ℃ during heating.
In the fourth step, the hydrogen-containing carrier gas comprises Ar and H 2, wherein the flow rate of the preset carrier gas corresponding to Ar is controlled to be 110-130 sccm, and the flow rate of the preset carrier gas corresponding to H 2 is controlled to be 5-25 sccm.
The preparation method of the Se-Cr 2S3 two-dimensional material comprises the steps that the volatilization temperature of S powder is 150-240 ℃, the volatilization temperature of Se powder is 217-340 ℃, the volatilization temperature of CrCl 3 powder is 720-1152 ℃, and the volatilization temperature of CrCl 3 powder is equal to the deposition temperature.
In the third step, the shielding gas is at least one of inert gases, and the mass ratio of the added S powder to the Se powder to the CrCl 3 powder is 6.7-21:1:5.
In the fourth step, the corresponding deposition temperature is 750-850 ℃ during the deposition reaction.
The invention also provides a Se-Cr 2S3 two-dimensional material, wherein the Se-Cr 2S3 two-dimensional material is prepared according to the preparation method, the Se-Cr 2S3 two-dimensional material is a nano sheet, and the corresponding thickness is 1.8-50 nm.
The invention also provides an application of the Se-Cr 2S3 two-dimensional material, wherein the Se-Cr 2S3 two-dimensional material prepared by the preparation method is used for preparing Se-Cr 2S3 field effect transistors.
The application of the Se-Cr 2S3 two-dimensional material, wherein the preparation method of the Se-Cr 2S3 field effect transistor comprises the following steps:
And evaporating Cr/Au electrode on the Se-Cr 2S3 two-dimensional material prepared by adopting the vapor deposition method, wherein the thickness of the Cr/Au electrode is 10nm/50nm.
The preparation method of the Se-Cr 2S3 two-dimensional material provided by the invention obtains the single-layer single-crystal Se-Cr 2S3 two-dimensional material with the thickness reaching a single layer through a simple normal pressure chemical vapor deposition method, has the thickness as thin as 1.8nm and the size of 4-30 mu m, is single crystal, has high quality, controllable doping concentration and good reproducibility, and is simple and feasible, thereby providing reference for the preparation of other two-dimensional metallic materials. The method successfully improves the mobility of the Cr 2S3 two-dimensional material through Se doping, shortens the photoresponse time and regulates and controls the magnetic performance of the Cr 2S3 two-dimensional material. In addition, the ultrathin Se-Cr 2S3 two-dimensional material prepared by the method provides new possibility for the research in the two-dimensional electric, photoelectric and magnetic fields.
Additional features and advantages of the disclosure will be set forth in the description which follows, or in part will be obvious from the description, or may be learned by practice of the techniques of the disclosure.
In order to make the above objects, features and advantages of the present invention more comprehensible, preferred embodiments accompanied with figures are described in detail below.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of an atmospheric pressure chemical vapor deposition apparatus for preparing Se-Cr 2S3 nano sheets in the present invention;
FIG. 2 is a Raman diagram of Se-Cr 2S3 nanosheets prepared in example 1 of the present invention;
FIG. 3 is an EDS diagram of Se-Cr 2S3 nanosheets prepared in example 1 of the present invention;
FIG. 4 is a graph of HRTEM and SAED of Se-Cr 2S3 nano-sheets prepared in example 1 of the present invention;
FIG. 5 is an optical image of Se-Cr 2S3 nanosheets prepared in example 1 of the present invention;
FIG. 6 is an optical image of Se-Cr 2S3 nanosheets prepared in example 2 of the present invention;
FIG. 7 is a graph showing the relationship between the doping concentration of Se-Cr 2S3 nano-sheets and the mass ratio of Se prepared in example 3 of the present invention;
FIGS. 8, 9, 10, 11, 12, 13 and 14 are optical schematic diagrams of Se-Cr 2S3 nanoplatelets prepared in comparative examples 1, 2, 3, 4, 5, 6 and 7, respectively;
FIG. 15 is an optical photograph of Se-Cr 2S3 nanosheets transferred to a silicon wafer in example 4 of the present invention;
FIG. 16 is an optical schematic diagram of a Se-Cr 2S3 field effect transistor prepared in example 5 of the present invention;
FIG. 17 is a graph showing the output and transfer characteristics of Cr 2S3 FETs of different thicknesses according to the present invention;
FIG. 18 shows the output and transfer characteristics of 2.05% -Se-Cr 2S3 FETs of different thicknesses according to the present invention;
FIG. 19 is an enlarged view of one time resolved photoresponse period of a Cr 2S3 field effect transistor and a 2.05% -Se-Cr 2S3 field effect transistor in accordance with the present invention;
FIG. 20 shows the magnetization curves of the Cr 2S3 and Se-Cr 2S3 two-dimensional materials of example 6 of the present invention at Zero Field Cooling (ZFC) and Field Cooling (FC) for a parallel magnetic field of 1000 Oe.
Detailed Description
In order that the invention may be readily understood, a more complete description of the invention will be rendered by reference to the appended drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
The invention provides a preparation method of Se-Cr 2S3 two-dimensional material, which is used for preparing by a vapor deposition device.
Referring to fig. 1, the vapor deposition apparatus includes a quartz tube 1, wherein the quartz tube 1 includes an upstream high temperature constant temperature region 2 and a downstream high temperature constant temperature region 3, the upstream high temperature constant temperature region 2 is provided with a first porcelain boat 4 loaded with sulfur powder and selenium powder, and the downstream high temperature constant temperature region 3 is provided with a second porcelain boat 5 loaded with chromium trichloride and fluorophlogopite. Furthermore, the vapor deposition apparatus further comprises heating means for heating the upstream high temperature constant temperature zone 2 and the downstream high temperature constant temperature zone 3. In the present invention, the vapor deposition apparatus is preferably a double temperature zone reaction apparatus.
Specifically, the method for preparing the Se-Cr 2S3 two-dimensional material provided by the invention comprises the following steps:
S101, an inlet for inputting carrier gas into a cavity of the quartz tube is arranged at one end of the quartz tube, and an outlet for outputting cavity gas of the quartz tube is arranged at the other end of the quartz tube; according to the direction of carrier gas flow, the chamber of the quartz tube is divided into an upstream high-temperature constant-temperature region and a downstream high-temperature constant-temperature region.
As shown in fig. 1, an inlet for inputting carrier gas into the chamber of the quartz tube 1 is provided at the left end of the quartz tube 1, and an outlet for outputting chamber gas of the quartz tube 1 is provided at the other end.
S102, placing S powder and Se powder in the upstream high-temperature constant-temperature area, and placing CrCl 3 powder in the downstream high-temperature constant-temperature area.
Wherein, S powder and Se powder are placed on the first porcelain boat 4, and CrCl 3 powder and fluorophlogopite are placed on the second porcelain boat 5. As described above, the first boat 4 is located in the upstream high temperature constant temperature zone, and the second boat 5 is located in the downstream high temperature constant temperature zone. It should be noted that the S powder, se powder and CrCl 3 powder used in the invention are provided by Alpha company, and the purity is more than 99.99%.
S103, pre-introducing a protective gas of 300sccm to purge the cavity for 5min before heating to remove impurities in the cavity of the quartz tube, and then heating the S powder, the Se powder and the CrCl 3 powder to the corresponding volatilization temperature at a heating rate of 30 ℃/min under the carrier gas flow rate of 110-130 sccm of the protective gas.
In this step, the preferred volatilization temperature of the S powder is controlled to be 180-220 ℃, the preferred volatilization temperature of the Se powder is controlled to be 280-320 ℃, and the preferred volatilization temperature of the CrCl 3 powder is controlled to be 750-800 ℃ during heating.
In addition, it should be noted that the protective gas is at least one of inert gases, and the mass ratio of the added S powder, se powder and CrCl 3 powder is 6.7-21:1:5.
S104, then converting the protector into hydrogen-containing carrier gas Ar/H 2, controlling the growth of the carrier gas Ar/H 2 in a deposition temperature range for 10-30 min under the preset carrier gas flow rate, enabling the volatilized S powder, se powder and CrCl 3 powder to react with each other, depositing the volatile S powder, se powder and CrCl 3 powder on a substrate, and growing on the substrate to obtain the Se-Cr 2S3 two-dimensional material.
In this step, the hydrogen-containing carrier gas includes Ar and H2, wherein the flow rate of the preset carrier gas corresponding to Ar is controlled to be 110-130 sccm, and the flow rate of the preset carrier gas corresponding to H 2 -25 sccm.
In addition, the volatilization temperature of the S powder is 150-240 ℃, the volatilization temperature of the Se powder is 217-340 ℃, the volatilization temperature of the CrCl 3 powder is 720-1152 ℃, and the volatilization temperature of the CrCl 3 powder is equal to the deposition temperature. When the deposition reaction is carried out, the corresponding deposition temperature is 750-850 ℃.
The invention also provides a Se-Cr 2S3 two-dimensional material, wherein the Se-Cr 2S3 two-dimensional material is prepared according to the preparation method, the Se-Cr 2S3 two-dimensional material is a nano sheet, and the corresponding thickness is 1.8-50 nm.
The invention also provides an application of the Se-Cr 2S3 two-dimensional material, wherein the Se-Cr 2S3 two-dimensional material prepared by the preparation method is used for preparing Se-Cr 2S3 field effect transistors.
The preparation method of the Se-Cr 2S3 field effect transistor comprises the following steps:
And evaporating Cr/Au electrode on the Se-Cr 2S3 two-dimensional material prepared by adopting the vapor deposition method, wherein the thickness of the Cr/Au electrode is 10nm/50nm.
The preparation method of the Se-Cr 2S3 two-dimensional material provided by the invention obtains the single-layer single-crystal Se-Cr 2S3 two-dimensional material with the thickness reaching a single layer through a simple normal pressure chemical vapor deposition method, has the thickness as thin as 1.8nm and the size of 4-30 mu m, is single crystal, has high quality, controllable doping concentration and good reproducibility, and is simple and feasible, thereby providing reference for the preparation of other two-dimensional metallic materials. The method successfully improves the mobility of the Cr 2S3 two-dimensional material through Se doping, shortens the photoresponse time and regulates and controls the magnetic performance of the Cr 2S3 two-dimensional material. In addition, the ultrathin Se-Cr 2S3 two-dimensional material prepared by the method provides new possibility for the research in the two-dimensional electric, photoelectric and magnetic fields.
The preparation method of Se-Cr 2S3 two-dimensional material proposed by the present invention is described in more detail below with several specific examples and comparative examples.
Example 1
Preparation of Se-Cr 2S3 nano-sheets:
The first porcelain boat 4 with two sides respectively loaded with S powder and Se powder is placed in an upstream high-temperature constant-temperature area 2 of a quartz tube 1 (the volatilization temperature of the S powder is preferably 200 ℃ and the volatilization temperature of the Se powder is preferably 300 ℃), the second porcelain boat 5 with CrCl 3 powder is placed in the center of a downstream high-temperature constant-temperature area 3 (the volatilization temperature of CrCl 3 powder is preferably 750 ℃), and one fluorophlogopite is used as a growth substrate of Se-Cr 2S3, wherein the mass ratio of the S powder to the Se powder to the CrCl 3 powder is 15:1:5 (0.015 g/0.001g/0.005 g);
Before heating, the air in the quartz tube 1 is exhausted by argon, then the upstream high-temperature constant temperature region 2 and the downstream high-temperature constant temperature region 3 are respectively heated to 300 ℃ and 750 ℃ (deposition temperature), the flow of argon-hydrogen mixed gas is 120/15sccm, the constant temperature is 15min, H 2 is only introduced in the constant temperature stage, and single-crystal Se-Cr 2S3 nano-sheets are generated on the silicon wafer.
In the invention, the Raman, EDS, TEM and optical pictures of the Se-Cr 2S3 nano sheet are shown in figures 2, 3, 4 and 5. Specific:
FIG. 2 is a Raman diagram of a 4.8nm 2.05% -Se-Cr 2S3 nanosheet, with 2 peaks (246.6 cm -1 and 285.7cm -1) corresponding to an in-plane E g mode and an out-of-plane A g mode, respectively. The raman peak intensity mapping at 246.6cm -1 and 285.7cm -1 was uniform, indicating high quality and uniform doping of the samples.
EDS in fig. 3 shows that: the synthesized Se-Cr 2S3 nano sheet only contains three elements of Se, S and Cr, and the ratio is 2.05:36.85:61.1. In FIG. 4, the synthesized Se-Cr 2S3 nanoplatelets have high resolution and electron diffraction patterns with lattices of 0.30nm and 0.17nm corresponding to the (110) and (300) planes of Se-Cr 2S3, respectively. FIG. 5 is an optical schematic diagram of a Se-Cr 2S3 nano-sheet prepared, fluorophlogopite is taken as a substrate, an off-white triangle represents Se-Cr 2S3 nano-sheets with uniform thickness distribution, a white irregular pattern is slightly thicker Se-Cr 2S3 (less), and the Se-Cr 2S3 nano-sheet obtained under the condition has good crystallinity, thickness of 1.8-7.6 nm and size of 10-30 μm. Wherein the scale in FIG. 5 is 20 μm.
Example 2
Compared with example 1, the difference is that: the substrate temperature (volatilization temperature of CrCl 3 powder) is 800 ℃ (namely the deposition temperature is 800 ℃), the mass ratio of Se powder, S powder and CrCl 3 powder is 1:15:5 (0.001 g/0.015g/0.005 g), the corresponding flow is 120/15sccm, the deposition time is 15min, and H 2 is only introduced in the constant temperature stage. FIG. 6 is an optical schematic diagram of the Se-Cr 2S3 nano sheet prepared, wherein the Se-Cr 2S3 nano sheet has uniform thickness distribution, corresponding thickness of 10-30 nm and size of 10-20 μm. Wherein the scale in FIG. 6 is 20 μm.
Example 3
Compared with example 1, the difference is that: a series of experiments with different mass ratios are carried out, the mass ratio of Se powder, S powder and CrCl 3 powder is 1:10-21:5 (0.001 g/0.01-0.021 g/0.005 g), the flow is 120/15sccm, the deposition time is 15min, and H 2 is only introduced in a constant temperature stage. FIG. 7 is a graph showing the relationship between the doping concentration and the mass ratio obtained by statistics of Se-Cr 2S3 nano sheets prepared by a series of different doping, and can be seen from FIG. 7: the doping concentration has an approximate quadratic relation with the mass ratio.
Comparative example 1
The effect of lower airflow than in example 1 is mainly discussed as follows:
Compared with example 1, the difference is that: the substrate temperature (volatilization temperature of CrCl 3 powder) is 750 ℃ (i.e. deposition temperature is 750 ℃), the mass ratio of Se powder, S powder and CrCl 3 powder is 1:15:5 (0.001 g/0.015g/0.005 g), the flow rate is 90/15sccm, the deposition time is 15min, and H 2 is only introduced in the constant temperature stage. FIG. 8 is an optical schematic of a prepared Se-Cr 2S3 nano sheet, and the Se-Cr 2S3 nano sheet has a non-uniform thickness. Wherein the scale in FIG. 8 is 20 μm.
Comparative example 2
The effect of higher airflow rates compared to example 1 was mainly examined, as follows:
compared with example 1, the difference is that: the substrate temperature (volatilization temperature of CrCl 3 powder) is 750 ℃ (deposition temperature 750 ℃), the mass ratio of Se powder, S powder and CrCl 3 powder is 1:15:5 (0.001 g/0.015g/0.005 g), the flow is 200/15sccm, the deposition time is 15min, and H 2 is only introduced in the constant temperature stage. FIG. 9 is an optical schematic of the prepared Se-Cr 2S3 nanosheets, the surface of the Se-Cr 2S3 product being non-uniform. Wherein the scale in FIG. 9 is 100 μm.
Comparative example 3
The effect of higher deposition temperatures compared to example 1 is mainly discussed as follows:
Compared with example 1, the difference is that: the substrate temperature (volatilization temperature of CrCl 3 powder) is 850 ℃ (deposition temperature is 850 ℃), the mass ratio of Se powder, S powder and CrCl 3 powder is 1:15:5 (0.001 g/0.015g/0.005 g), the flow is 120/15sccm, the deposition time is 15min, and H 2 is only in a constant temperature stage. FIG. 10 is an optical schematic diagram of a prepared Se-Cr 2S3 nano sheet, wherein hexagonal materials (part of which is black edges) are super-thick Se-Cr 2S3, and part of the hexagonal materials are irregular in shape; wherein the thickness is 50-300 nm. Wherein the scale in FIG. 10 is 10 μm.
Comparative example 4
The effect of lower deposition temperatures compared to example 1 is mainly discussed as follows:
Compared with example 1, the difference is that: the substrate temperature (volatilization temperature of CrCl 3 powder) is 700 ℃ (deposition temperature 700 ℃), the mass ratio of Se powder, S powder and CrCl 3 powder is 1:15:5 (0.001 g/0.015g/0.005 g), the flow is 120/15sccm, the deposition time is 15min, and H 2 is only introduced in the constant temperature stage. FIG. 11 is an optical schematic of a prepared Se-Cr 2S3 nanosheet, with thick particles of small size being CrCl 3 that are substantially unreacted. Wherein the scale in FIG. 11 is 10 μm.
Comparative example 5
Compared with example 1, the influence of the continuous introduction of H 2 during the experiment is mainly examined, and the method is as follows:
Compared with example 1, the difference is that: the substrate temperature (volatilization temperature of CrCl 3 powder) was 750 ℃ (deposition temperature 750 ℃), the mass ratio of Se powder, S powder and CrCl 3 powder was 1:15:5 (0.001 g/0.015g/0.005 g), the flow was 120/15sccm, the deposition time was 15min, and H 2 was introduced during both the heating and the constant temperature stages. FIG. 12 is an optical schematic diagram of a prepared Se-Cr 2S3 nano sheet, wherein the irregular material is Se-Cr 2S3, and etching occurs due to higher hydrogen content. Wherein the scale in FIG. 12 is 20 μm.
Comparative example 6
In comparison with example 1, the influence of the excessive deposition time during the experiment is mainly examined, specifically as follows:
Compared with example 1, the difference is that: the substrate temperature (volatilization temperature of CrCl 3 powder) is 750 ℃ (deposition temperature 750 ℃), the mass ratio of Se powder, S powder and CrCl 3 powder is 1:15:5 (0.001 g/0.015g/0.005 g), the flow is 120/15sccm, the deposition time is 40min, and H 2 is only introduced in the constant temperature stage. FIG. 13 is an optical schematic diagram of a prepared Se-Cr 2S3 nano sheet, wherein the triangular material is a Se-Cr 2S3 nano sheet, and one side of a part of the material is tilted to present a black and fuzzy shape. Wherein the scale in FIG. 13 is 20 μm.
Comparative example 7
In comparison with example 1, the influence of the substrate during the experiment is mainly examined, in particular as follows:
Compared with example 1, the difference is that: the Si/SiO 2 substrate is selected, the substrate temperature (the volatilization temperature of CrCl 3 powder) is 800 ℃ (the deposition temperature is 800 ℃), the mass ratio of Se powder, S powder and CrCl 3 powder is 1:15:5 (0.001 g/0.015g/0.005 g), the flow is 120/15sccm, the deposition time is 15min, and H 2 is only introduced in a constant temperature stage. FIG. 14 is an optical schematic diagram of a prepared Se-Cr 2S3 nano sheet, wherein the irregular material is Se-Cr 2S3 nano sheet, and the thickness is 10-30 nm. The black particles are essentially unreacted CrCl 3. Wherein the scale in FIG. 14 is 10 μm.
Example 4
The transfer method of Se-Cr 2S3 comprises the following steps:
Se-Cr 2S3 nano-sheets prepared on a fluorophlogopite substrate by a CVD method are transferred to a SiO 2/Si substrate by a polymethyl methacrylate (PMMA) auxiliary transfer method. FIG. 15 is an optical schematic of a transferred Se-Cr 2S3 nanosheets, with a triangular material being the Se-Cr 2S3 nanosheets. Wherein the scale in FIG. 15 is 20 μm.
Example 5
The preparation method of the Se-Cr 2S3 field effect transistor comprises the following steps:
and evaporating Cr/Au (10 nm/50 nm) metal electrodes on the Se-Cr 2S3 nano-sheets prepared by the CVD method to obtain the Se-Cr 2S3 field effect transistor. The picture of the prepared Se-Cr 2S3 field effect transistor is shown in figure 16. Wherein the scales in FIG. 16 are 5 μm, respectively.
In FIG. 16, se-Cr 2S3 is triangular, and two long rectangles on the Se-Cr 2S3 surface are transferred Cr/Au electrodes.
In fig. 17, a in fig. 17 is an output characteristic curve of Cr 2S3 field effect transistors with different thicknesses; b in fig. 17 is a transfer characteristic curve of Cr 2S3 field effect transistors of different thicknesses. Figures 17a-b demonstrate that Cr 2S3 nanoplatelets are semiconductor materials, have weakly bipolar p-type conductivity behavior and are poorly conductive.
In fig. 18, a in fig. 18 is an output characteristic curve of 2.05% -Se-Cr 2S3 field effect transistors with different thicknesses; b in fig. 18 is a transfer characteristic curve of 2.05% -Se-Cr 2S3 field effect transistors of different thicknesses. The Se-Cr 2S3 with different thicknesses also shows p-type conduction behavior, but when the thickness is larger than 6nm, the source leakage current (I ds) is greatly increased and is not effectively regulated by the grid voltage (V g), the metal is gradually presented, and the conductivity is greatly enhanced.
In fig. 19, a in fig. 19 is an enlarged view of one time-resolved photo-response period of the Cr 2S3 field effect transistor, and the rise time (t r) and decay time (t d) are 4.9s and 5.7s, respectively; b in fig. 19 is an enlarged view of one time-resolved photo-response period of the 2.05% -Se-Cr 2S3 field effect transistor, and the rise time (tr) and decay time (td) are both 28ms. In contrast, the response speed of 2.05% -Se-Cr 2S3 is about 200 times higher than that of Cr 2S3.
Example 6
The difference between the magnetic VSM test of Se-Cr 2S3 and that of example 1 is:
The substrate temperature (volatilization temperature of CrCl 3 powder) is 800 ℃ (deposition temperature 800 ℃), the mass ratio of Se powder, S powder and CrCl 3 powder is 1:15:5 (0.001 g/0.015g/0.005 g), the flow is 120/15sccm, the deposition time is 30min, and H 2 is only introduced in the constant temperature stage. Obtaining Se-Cr 2S3 nano sheets which are fully distributed on the substrate and have uniform thickness distribution; wherein the thickness is 10-50 nm, and the size is 10-20 mu m.
In fig. 20, a in fig. 20 is a magnetization curve of the Cr 2S3 material under Zero Field Cooling (ZFC) and Field Cooling (FC) at a parallel magnetic field of 1000Oe, showing a remarkable ferrimagnetic behavior, with a curie temperature of 120K and a nier temperature of 75K. B in FIG. 20 is a magnetization curve of Se-Cr 2S3 two-dimensional material under Zero Field Cooling (ZFC) and Field Cooling (FC) at a parallel magnetic field of 1000Oe, showing ferromagnetism, a Curie temperature of about 200K and a Neille temperature of about 80K.
It was found by the above examples and comparative examples:
The successful preparation of Se-Cr 2S3 two-dimensional material requires cooperative control of the volatilization temperature of the raw materials, the carrier gas components, the carrier gas flow, the mass ratio of the raw materials and the deposition temperature of the volatilized materials within a reasonable range. According to the invention, se-Cr 2S3 nano-sheets with good morphology and nano-scale thickness can be prepared under the cooperation of carrier gas components, carrier gas flow, raw material mass ratio and deposition temperature (also called as growth temperature) and carrier gas type and flow.
Finally, it should be noted that: the above examples are only specific embodiments of the present invention, and are not intended to limit the scope of the present invention, but it should be understood by those skilled in the art that the present invention is not limited thereto, and that the present invention is described in detail with reference to the foregoing examples: any person skilled in the art may modify or easily conceive of the technical solution described in the foregoing embodiments, or perform equivalent substitution of some of the technical features, while remaining within the technical scope of the present disclosure; such modifications, changes or substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention, and are intended to be included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (4)
1. The preparation method of the Se-Cr 2S3 two-dimensional material is characterized by comprising a vapor deposition device, wherein the vapor deposition device comprises a quartz tube, an upstream high-temperature constant-temperature region and a downstream high-temperature constant-temperature region are arranged in the quartz tube, a first porcelain boat loaded with sulfur powder and selenium powder is arranged in the upstream high-temperature constant-temperature region, a second porcelain boat loaded with chromium trichloride and fluorophlogopite is arranged in the downstream high-temperature constant-temperature region, the vapor deposition device further comprises a heating device for heating the upstream high-temperature constant-temperature region and the downstream high-temperature constant-temperature region, and the vapor deposition device is a double-temperature-region reaction device;
The method comprises the following steps:
The method comprises the steps that firstly, an inlet for inputting carrier gas into a cavity of a quartz tube is arranged at one end of the quartz tube, and an outlet for outputting cavity gas of the quartz tube is arranged at the other end of the quartz tube; dividing a cavity of the quartz tube into an upstream high-temperature constant-temperature region and a downstream high-temperature constant-temperature region according to the direction of carrier gas flow;
step two, placing S powder and Se powder in the upstream high-temperature constant-temperature area, and placing CrCl 3 powder in the downstream high-temperature constant-temperature area;
Step three, pre-introducing a protective gas of 300sccm to purge the cavity for 5min before heating to remove impurities in the cavity of the quartz tube, and then heating the S powder, the Se powder and the CrCl 3 powder to the corresponding volatilization temperature at a heating rate of 30 ℃/min under the carrier gas flow rate of 110-130 sccm of the protective gas;
Step four, converting the protective gas into a hydrogen-containing carrier gas Ar/H 2, controlling the growth of the carrier gas Ar/H 2 in a deposition temperature range under the preset carrier gas flow rate, enabling the volatilized S powder, se powder and CrCl 3 powder to react with each other, depositing the S powder, se powder and CrCl 3 powder on a substrate, and growing on the substrate to obtain Se-Cr 2S3 two-dimensional material;
In the third step, when heating, controlling the volatilization temperature of the S powder to be 180-220 ℃, the volatilization temperature of the Se powder to be 280-320 ℃ and the volatilization temperature of the CrCl 3 powder to be 750-800 ℃;
In the fourth step, the hydrogen-containing carrier gas includes Ar and H 2, wherein the flow rate of the preset carrier gas corresponding to Ar is controlled to be 110-130 sccm, and the flow rate of the preset carrier gas corresponding to H 2 is controlled to be 5-25 sccm;
In the third step, the shielding gas is at least one of inert gases, and the mass ratio of the added S powder, se powder and CrCl 3 powder is 6.7-21:1:5;
In the fourth step, the corresponding deposition temperature is 750-850 ℃ when the deposition reaction is carried out.
2. The Se-Cr 2S3 two-dimensional material is characterized in that the Se-Cr 2S3 two-dimensional material is prepared by the preparation method of claim 1, the Se-Cr 2S3 two-dimensional material is a nano sheet, and the corresponding thickness is 1.8-50 nm.
3. The application of the Se-Cr 2S3 two-dimensional material is characterized in that the Se-Cr 2S3 two-dimensional material prepared by the preparation method according to claim 1 is used for preparing Se-Cr 2S3 field effect transistors.
4. The use of a two-dimensional material of Se-Cr 2S3 as claimed in claim 3, wherein the method for preparing the Se-Cr 2S3 field effect transistor comprises the steps of:
And evaporating Cr/Au electrode on the Se-Cr 2S3 two-dimensional material prepared by adopting the vapor deposition method, wherein the thickness of the Cr/Au electrode is 10nm/50nm.
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