CN112279301A - Preparation of centimeter-level 2H-phase CrS2-WS2Method for horizontal heterojunction - Google Patents

Preparation of centimeter-level 2H-phase CrS2-WS2Method for horizontal heterojunction Download PDF

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CN112279301A
CN112279301A CN202011169934.XA CN202011169934A CN112279301A CN 112279301 A CN112279301 A CN 112279301A CN 202011169934 A CN202011169934 A CN 202011169934A CN 112279301 A CN112279301 A CN 112279301A
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temperature
crs
phase
centimeter
heterojunction
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聂安民
康梦克
向建勇
牟从普
柳忠元
田永君
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Yanshan University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G41/00—Compounds of tungsten
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G37/00—Compounds of chromium
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    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
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Abstract

The invention discloses centimeter-level 2H-phase CrS2‑WS2A preparation method of a horizontal heterojunction belongs to the field of inorganic semiconductor nano material preparation, and comprises the following steps: cr, NaCl, WO3S is taken as a raw material, and Si/SiO is used in a multi-temperature-zone tubular furnace2Heating and vulcanizing under the protection of argon for serving as a substrate, and preparing centimeter-level 2H-phase CrS by a one-step chemical vapor deposition method2‑WS2A horizontal heterojunction; the method has the advantages of simple steps, convenient operation, high synthesis speed and low cost, and the prepared 2H-phase CrS2‑WS2The horizontal heterojunction has good crystallinity.

Description

Preparation of centimeter-level 2H-phase CrS2-WS2Method for horizontal heterojunction
Technical Field
The invention relates to a method for preparing centimeter-level 2H-phase CrS2-WS2A horizontal heterojunction method, belonging to inorganic semiconductor nano materialThe technical field of material preparation.
Background
Heterojunctions are important in the modern semiconductor industry, are regarded as an important substrate for semiconductor processes, play an important role in high-speed optoelectronic devices, and unlike conventional semiconductor heterojunctions, two-dimensional semiconductor heterojunctions made of two-dimensional materials such as graphene, boron nitride, transition metal chalcogenides, and the like have more excellent optical and electrical properties. Among them, the vertical heterojunction can be synthesized by hand tearing and chemical vapor deposition, but the horizontal heterojunction can only be synthesized by chemical vapor deposition, and the like, and the preparation process is more severe compared with the N-type or P-type semiconductor, so that only a small amount of horizontal heterojunction is prepared at present. We further explore on the basis of uniform doping, and further optimize the preparation process, thereby adding a new member to the few chalcogenide horizontal heterojunction families at present. Its abundant structural features open a new door for subsequent more advanced electronic research and wider application of optoelectronic devices.
The invention provides a novel rapid and effective synthesis method of a heterojunction, the operation is simple, and the synthesized sample can reach the centimeter-level width.
Disclosure of Invention
The invention aims to provide a method for preparing centimeter-level 2H-phase CrS2-WS2The method for the horizontal heterojunction has the advantages of simple steps, convenience in operation, high synthesis speed and low cost.
In order to achieve the purpose, the invention adopts the technical scheme that:
preparation of centimeter-level 2H-phase CrS2-WS2A method of horizontal heterojunction comprising the steps of: cr, NaCl, WO3S is taken as a raw material, and Si/SiO is used in a multi-temperature-zone tubular furnace2Heating and vulcanizing under the protection of argon for serving as a substrate, and preparing centimeter-level 2H-phase CrS by a one-step chemical vapor deposition method2-WS2A horizontal heterojunction; during the reaction, the S simple substance is arranged in a corundum boat and is arranged at the upstream of a multi-temperature-zone tubular furnace, WO3Placing the mixture of NaCl and the Cr powder in a corundum boat and placing the corundum boat and the Cr powder at the downstream of a multi-temperature-zone tube furnace, uniformly spreading the Cr powder at the bottom of the corundum boat and placing the Cr powder at the downstream of the multi-temperature-zone tube furnace and WO3And the other side of the mixture of NaCl, the position of the corundum boat of the Cr powder is adjusted, and the reaction temperature of the Cr powder is kept at 930-970 ℃.
The technical scheme of the invention is further improved as follows: the upstream temperature of the multi-temperature-zone tubular furnace is 150-210 ℃.
The technical scheme of the invention is further improved as follows: the downstream temperature of the multi-temperature-zone tubular furnace is 940-.
The technical scheme of the invention is further improved as follows: the flow rate of the argon is 20-50 sccm.
The technical scheme of the invention is further improved as follows: the pressure in the multi-temperature zone tubular furnace tube is 50-200Pa during the reaction.
The technical scheme of the invention is further improved as follows: the temperature rise time of the vulcanization reaction is 30-50min, and the reaction time is 20-50 min.
The technical scheme of the invention is further improved as follows: the method also includes depositing a substrate Si/SiO on the sample before the sulfurization reaction2Ultrasonic cleaning with acetone, cleaning with ethanol, and cleaning with N2And (5) drying.
The technical scheme of the invention is further improved as follows: the method also comprises cleaning the multi-temperature-zone tube furnace and the corundum boat by using argon gas before the vulcanization reaction.
Due to the adoption of the technical scheme, the invention has the following technical effects:
the method can synthesize centimeter-level continuous 2H-phase CrS within about two hours by only one-step reaction2-WS2The method is characterized in that a horizontal heterojunction sample is prepared by using simple and easily-obtained tungsten oxide, Cr simple substance, sulfur simple substance and sodium chloride as reaction raw materials, the cost is low, and centimeter-level 2H-phase CrS is prepared2-WS2The horizontal heterojunction is proved to have good crystallinity and stable chemistry and stability by the characterization of various technical means such as Raman spectrum, XPS spectrum, AFM, scanning transmission electron microscope and the likeThermodynamic property.
The invention is prepared by mixing S simple substance and WO3The mixture of NaCl and uniformly spread Cr powder are put into a multi-temperature-zone tubular furnace together for a vulcanization reaction, and the WO is treated by the S simple substance3And the uniformly spread Cr powder is gradually vulcanized to form 2H-phase CrS2Followed by epitaxial growth of WS2Thereby forming a 2H phase CrS2-WS2Horizontal heterojunction, and centimeter-level 2H-phase CrS prepared from the same2-WS2The horizontal heterojunction has stable chemical and thermodynamic properties and has great application prospect in the fields of high-speed photoelectronic devices and the like
Drawings
FIG. 1 shows the preparation of centimeter-sized 2H-phase CrS according to the invention2-WS2Experimental schematic of horizontal heterojunctions;
FIG. 2 shows centimeter-sized 2H-phase CrS prepared by the embodiment of the invention2-WS2An optical photograph of a horizontal heterojunction;
FIG. 3 shows centimeter-sized 2H-phase CrS prepared by the embodiment of the invention2-WS2Optical photographs of horizontal heterojunctions with the edges of the horizontal heterojunction sample distributed dispersedly;
FIG. 4 shows 2H phase CrS prepared according to an embodiment of the present invention2-WS2Fluorescence photographs of horizontal heterojunctions;
FIG. 5 shows centimeter-sized 2H-phase CrS prepared by the example of the invention2-WS2AFM pictures of horizontal heterojunctions;
FIG. 6 shows centimeter-sized 2H-phase CrS prepared by the example of the invention2-WS2A Raman line scan of the horizontal heterojunction at the junction;
FIGS. 7-9 centimeter-sized 2H-phase CrS prepared according to an embodiment of the invention2-WS2XPS data plot of horizontal heterojunction.
Detailed Description
The invention is described in further detail below with reference to the following figures and specific embodiments:
the invention discloses a method for preparing centimeter-level 2H-phase CrS2-WS2The method of horizontal heterojunction, as shown in FIG. 1, is an experimental schematic of the present invention, which comprises the following stepsThe method comprises the following steps:
1. ultrasonic cleaning of SiO with acetone and ethanol2a/Si substrate using N2Drying;
2. cleaning a quartz tube and a corundum boat of the multi-temperature-zone tube furnace by adopting argon;
3. mixing S simple substance with WO3The mixture of NaCl and the uniformly spread Cr powder are respectively placed at the upstream and the downstream of the multi-temperature-zone tubular furnace by a corundum boat for heating and vulcanizing reaction, and the Cr powder is uniformly spread at the bottom of the corundum boat;
4. in the step 3, the upstream temperature of the multi-temperature-zone tubular furnace is raised to 150-;
5. keeping the flow rate of argon of the multi-temperature-zone tubular furnace at 20-50sccm and the pressure in the tube at 50-200 Pa;
6. controlling the temperature rise time of the vulcanization reaction in the steps 3 and 4 to be 30-50min, controlling the time of the vulcanization reaction to be 25-50min, and naturally cooling to room temperature to obtain centimeter-level 2H-phase CrS2-WS2A horizontal heterojunction.
The following are specific examples of the present invention:
example 1
The method comprises the following steps:
1. ultrasonic cleaning of SiO with acetone and ethanol2a/Si substrate using N2Drying;
2. cleaning a quartz tube and a corundum boat of the multi-temperature-zone tube furnace by adopting argon;
3. mixing S simple substance with WO3The mixture of NaCl and the Cr powder are respectively placed at the upstream and the downstream of the multi-temperature-zone tubular furnace by a corundum boat for heating and vulcanizing reaction, and the Cr powder is evenly paved at the bottom of the corundum boat;
4. in the step 3, the upstream temperature of the multi-temperature-zone tubular furnace is raised to 150 ℃, the downstream temperature is raised to 940 ℃, and the position of the Cr powder corundum boat is adjusted to keep the reaction temperature of the Cr powder at 930 ℃;
5. keeping the flow rate of argon of the multi-temperature-zone tubular furnace at 20sccm and the pressure in the tube at 50 Pa;
6. controlling the vulcanization reaction in the steps 3 and 4The heating time is 30min, the vulcanization reaction time is 25min, and then the mixture is naturally cooled to room temperature to obtain centimeter-level 2H-phase CrS2-WS2A horizontal heterojunction.
Example 2
The method comprises the following steps:
1. ultrasonic cleaning of SiO with acetone and ethanol2a/Si substrate using N2Drying;
2. cleaning a quartz tube and a corundum boat of the multi-temperature-zone tube furnace by adopting argon;
3. mixing S simple substance with WO3The mixture of NaCl and Cr are respectively placed at the upstream and the downstream of the multi-temperature-zone tubular furnace by a corundum boat for heating and vulcanizing reaction, and Cr powder is evenly spread at the bottom of the corundum boat;
4. in the step 3, the upstream temperature of the multi-temperature-zone tubular furnace is raised to 210 ℃, the downstream temperature is raised to 980 ℃, and the position of the Cr powder corundum boat is adjusted to keep the reaction temperature of the Cr powder at 950 ℃;
5. keeping the flow rate of argon of the multi-temperature-zone tubular furnace at 50sccm and the pressure in the tube at 200 Pa;
6. controlling the temperature rise time of the vulcanization reaction in the steps 3 and 4 to be 40min and the time of the vulcanization reaction to be 50min, and then naturally cooling to room temperature to obtain centimeter-level 2H-phase CrS2-WS2A horizontal heterojunction.
Example 3
Which comprises the following steps:
1. ultrasonic cleaning of SiO with acetone and ethanol2a/Si substrate using N2Drying;
2. cleaning a quartz tube and a corundum boat of the multi-temperature-zone tube furnace by adopting argon;
3. mixing S simple substance with WO3The NaCl mixture and the uniformly spread Cr powder are respectively placed at the upstream and the downstream of the multi-temperature-zone tubular furnace by corundum boats for heating and vulcanizing reaction;
4. in the step 3, the upstream temperature of the multi-temperature-zone tubular furnace is raised to 170 ℃, the downstream temperature is raised to 950 ℃, and the position of the Cr powder corundum boat is adjusted to keep the reaction temperature of the Cr powder at 940 ℃;
5. keeping the flow rate of argon of the multi-temperature-zone tubular furnace at 25sccm and the pressure in the tube at 72 Pa;
6. controlling the temperature rise time of the vulcanization reaction in the steps 3 and 4 to be 35min and the time of the vulcanization reaction to be 40min, and then naturally cooling to room temperature to obtain centimeter-level 2H-phase CrS2-WS2A horizontal heterojunction.
Centimeter-sized 2H-phase CrS obtained by the method steps of the invention2-WS2The horizontal heterojunction is characterized by an optical microscope, a Raman spectrometer, an X-ray photoelectron spectrometer (XPS), an Atomic Force Microscope (AFM), a Scanning Transmission Electron Microscope (STEM) and other equipment, and the synthesized sample is determined to be 2H-phase CrS2-WS2Horizontal heterojunction, and its crystallinity, thermal stability are good. Has great application potential in the fields of photoelectric detector devices, flexible films, electrochemical hydrogen evolution and the like.
FIG. 2 shows centimeter-sized 2H-phase CrS prepared by the above example2-WS2The optical photograph of the horizontal heterojunction can see a sample with a large area and continuous distribution.
FIG. 3 shows the 2H-phase CrS with scattered edges of centimeter-level large-area continuous sample prepared in the above example2-WS2Optical photograph of horizontal heterojunction with obvious visible WS2And CrS2With different optical contrast, the sample obtained was proved to be WS2-CrS2The heterojunction of (2).
FIG. 4 shows a fluorescence photograph corresponding to the sample shown in FIG. 3, as seen in WS2And CrS2Has stronger fluorescence at the boundary, and CrS2Some of the fluorescence was barely visible and was further demonstrated to be WS2And CrS2The heterostructure is formed.
FIG. 5 shows 2H phase CrS2-WS2AFM pictures of horizontal heterojunctions with a thickness of 0.92nm measured by AFM, which is comparable to the single-layer WS2Is uniform and WS2And CrS2No significant fluctuation at the interface, indicating that 2H phase CrS was produced by the process steps of the invention2-WS2The horizontal heterojunction is single-layered.
As shown in FIG. 6, 2H phase CrS2-WS2Raman line scan at horizontal heterojunction interface, Raman peak from WS2Gradual transition to CrS2And further proves that the prepared sample is a horizontal heterostructure.
FIG. 7-FIG. 9 shows 2H phase CrS2-WS2XPS data of horizontal heterojunctions, and analysis of the data reveals the presence of CrS in the synthesized sample2And WS2Two components, further confirming CrS2-WS2The presence of a heterojunction.
The embodiments of the present invention are preferred embodiments of the present invention, and the scope of the present invention is not limited by these embodiments, so: all equivalent changes made according to the structure, shape, principle and the like of the invention are covered by the protection scope of the invention.
Alternative materials for the various components are listed in the description of the invention, but it will be understood by those skilled in the art that: the above list of component materials is not intended to be limiting and non exhaustive, and the various components may be replaced by other equivalent materials not mentioned in the present description, while still achieving the objects of the present invention. The specific embodiments mentioned in the description are to be construed as merely illustrative, and not limitative of the remainder of the disclosure in any way whatsoever.
In addition, the range of the amount of each component of the present invention includes any combination of any lower limit and any upper limit mentioned in the specification, and also includes any range where the specific content of the component in each specific example is made up as a combination of the upper limit or the lower limit: all such ranges are intended to be included within the scope of the present invention for brevity and clarity only and are not intended to be exhaustive or to limit the scope of the invention to the precise forms disclosed. Each feature of the invention described in this specification may be combined with any other feature of the invention which combination is not specifically disclosed in the specification for the sake of brevity.

Claims (8)

1. Preparation of centimeter-level 2H-phase CrS2-WS2A method of horizontal heterojunction, comprising the steps of: cr, NaCl, WO3S is taken as a raw material, and Si/SiO is used in a multi-temperature-zone tubular furnace2Heating and vulcanizing under the protection of argon for serving as a substrate, and preparing centimeter-level 2H-phase CrS by a one-step chemical vapor deposition method2-WS2A horizontal heterojunction; during the reaction, the S simple substance is arranged in a corundum boat and is arranged at the upstream of a multi-temperature-zone tubular furnace, WO3Placing the mixture of NaCl and the Cr powder in a corundum boat and placing the corundum boat and the Cr powder at the downstream of a multi-temperature-zone tube furnace, uniformly spreading the Cr powder at the bottom of the corundum boat and placing the Cr powder at the downstream of the multi-temperature-zone tube furnace and WO3And the other side of the mixture of NaCl, the position of the corundum boat of the Cr powder is adjusted, and the reaction temperature of the Cr powder is kept at 930-970 ℃.
2. The method of claim 1, wherein the method is used to produce centimeter-sized 2H-phase CrS2-WS2A method of horizontal heterojunction, characterized by: the upstream temperature of the multi-temperature-zone tubular furnace is 150-210 ℃.
3. The method of claim 1, wherein the method is used to produce centimeter-sized 2H-phase CrS2-WS2A method of horizontal heterojunction, characterized by: the downstream temperature of the multi-temperature-zone tubular furnace is 940-.
4. The method of claim 1, wherein the method is used to produce centimeter-sized 2H-phase CrS2-WS2A method of horizontal heterojunction, characterized by: the flow rate of the argon is 20-50 sccm.
5. The method of claim 1, wherein the method is used to produce centimeter-sized 2H-phase CrS2-WS2A method of horizontal heterojunction, characterized by: the pressure in the multi-temperature zone tubular furnace tube is 50-200Pa during the reaction.
6. The method of claim 1, wherein the method is used to produce centimeter-sized 2H-phase CrS2-WS2A method of horizontal heterojunction, characterized by: the temperature rise time of the vulcanization reaction is 30-50min,the reaction time is 20-50 min.
7. The method of claim 1, wherein the method is used to produce centimeter-sized 2H-phase CrS2-WS2A method of horizontal heterojunction, characterized by: the method also includes depositing a substrate Si/SiO on the sample before the sulfurization reaction2Ultrasonic cleaning with acetone, cleaning with ethanol, and cleaning with N2And (5) drying.
8. The method of claim 1, wherein the method is used to produce centimeter-sized 2H-phase CrS2-WS2A method of horizontal heterojunction, characterized by: the method also comprises cleaning the multi-temperature-zone tube furnace and the corundum boat by using argon gas before the vulcanization reaction.
CN202011169934.XA 2020-10-28 2020-10-28 Preparation of centimeter-level 2H-phase CrS2-WS2Method for horizontal heterojunction Pending CN112279301A (en)

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US20160314968A1 (en) * 2015-04-22 2016-10-27 Samsung Electronics Co., Ltd. Composition for layered transition metal chalcogenide compound layer and method of forming layered transition metal chalcogenide compound layer
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CN109868454A (en) * 2017-12-05 2019-06-11 浙江大学 A kind of preparation method of two dimension chromic sulfide material
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Application publication date: 20210129