CN114959635A - Preparation method of tin sulfide/molybdenum disulfide mixed dimension van der waals heterojunction - Google Patents
Preparation method of tin sulfide/molybdenum disulfide mixed dimension van der waals heterojunction Download PDFInfo
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 102
- AFNRRBXCCXDRPS-UHFFFAOYSA-N tin(ii) sulfide Chemical compound [Sn]=S AFNRRBXCCXDRPS-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000000758 substrate Substances 0.000 claims abstract description 37
- 239000000843 powder Substances 0.000 claims abstract description 30
- 229910052786 argon Inorganic materials 0.000 claims abstract description 22
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims abstract description 16
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000012159 carrier gas Substances 0.000 claims abstract description 14
- 239000002356 single layer Substances 0.000 claims abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 56
- 238000004321 preservation Methods 0.000 claims description 13
- 239000010453 quartz Substances 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 10
- 238000000137 annealing Methods 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 238000005086 pumping Methods 0.000 claims description 7
- 238000007605 air drying Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000011010 flushing procedure Methods 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000463 material Substances 0.000 abstract description 27
- 239000002070 nanowire Substances 0.000 abstract description 14
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 10
- 238000010438 heat treatment Methods 0.000 abstract description 6
- 238000000926 separation method Methods 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 2
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- 239000002243 precursor Substances 0.000 abstract 2
- 239000000126 substance Substances 0.000 abstract 1
- 101100069231 Caenorhabditis elegans gkow-1 gene Proteins 0.000 description 37
- 229910052961 molybdenite Inorganic materials 0.000 description 35
- 235000012239 silicon dioxide Nutrition 0.000 description 30
- 229910052681 coesite Inorganic materials 0.000 description 22
- 229910052906 cristobalite Inorganic materials 0.000 description 22
- 239000000377 silicon dioxide Substances 0.000 description 22
- 229910052682 stishovite Inorganic materials 0.000 description 22
- 229910052905 tridymite Inorganic materials 0.000 description 22
- 230000003287 optical effect Effects 0.000 description 9
- 239000007789 gas Substances 0.000 description 7
- 239000004065 semiconductor Substances 0.000 description 7
- 238000012876 topography Methods 0.000 description 6
- 230000007547 defect Effects 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 238000001237 Raman spectrum Methods 0.000 description 4
- 238000000089 atomic force micrograph Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 150000004770 chalcogenides Chemical class 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000000969 carrier Substances 0.000 description 3
- 238000000407 epitaxy Methods 0.000 description 3
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- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- -1 chalcogenide compound Chemical class 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
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- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000002052 molecular layer Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
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- 230000000704 physical effect Effects 0.000 description 1
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- 238000011160 research Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/305—Sulfides, selenides, or tellurides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/52—Controlling or regulating the coating process
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/56—After-treatment
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Abstract
The invention discloses a preparation method of a tin sulfide/molybdenum disulfide mixed dimension Van der Waals heterojunction, which comprises the following steps: firstly, molybdenum oxide powder and sulfur powder are used as reaction precursors, argon is used as carrier gas, and a single-layer molybdenum disulfide is grown by heating reaction in a double-temperature-zone tubular furnace; and then taking tin sulfide powder and sulfur powder as reaction precursors, argon as carrier gas, taking a substrate with molybdenum disulfide as a growth substrate, and heating and reacting in a double-temperature-zone tubular furnace to grow the tin sulfide/molybdenum disulfide mixed dimension Van der Waals heterojunction. The heterojunction prepared by the invention is composed of one-dimensional tin sulfide and two-dimensional single-layer molybdenum disulfide, wherein the tin sulfide nanowire grows on the surface of the molybdenum disulfide in an epitaxial manner; the heterojunction material has stable chemical property and wide spectral response range, has an energy band structure of type II, is convenient for photon-generated carrier separation, and has wide application prospect in the field of photoelectric devices. The step-by-step chemical vapor deposition method adopted by the invention for preparing the tin sulfide/molybdenum disulfide mixed dimension van der Waals heterojunction has the advantages of high crystal quality, low preparation cost, simple process, repeatability and the like.
Description
Technical Field
The invention belongs to the field of low-dimensional semiconductor heterojunction materials and devices, and particularly relates to a preparation method of a tin sulfide/molybdenum disulfide mixed dimension van der Waals heterojunction.
Background
The low-dimensional layered metal chalcogenide compound has high structural stability and excellent optical, electronic and electrochemical properties, and has wide application prospects in the fields of nano-electronics, photoelectric devices, energy conversion and storage. Among these metal chalcogenide materials, tin sulfide (SnS) is a narrow-band semiconductor material which is abundant, non-toxic and stable, has a band gap value of about 1.1 eV, and shows p-type characteristics due to easy formation of tin vacancy defects during the preparation and synthesis process; molybdenum disulfide (MoS 2) is the most extensively studied two-dimensional semiconductor material and has a direct bandgap in the case of a single layer, with a bandgap value of about 1.86 eV; molybdenum disulfide exhibits intrinsic n-type characteristics due to the tendency to generate sulfur vacancy defects during manufacture. Therefore, Van der Waals integration of tin sulfide and molybdenum disulfide into a SnS/MoS2 heterojunction not only enables the spontaneous formation of a p-n junction, but also can broaden the range of spectral response of the two materials by taking advantage of the difference in band gap. In addition, the molybdenum disulfide and the tin sulfide show a type II band offset when combined, and can effectively promote the separation of photon-generated carriers, so that the tin sulfide/molybdenum disulfide Van der Waals heterojunction has great application potential in the fields of solar cells, photoelectric detectors and photocatalysis.
In order to realize the application of the tin sulfide/molybdenum disulfide Van der Waals heterojunction on the photoelectric device, the preparation of a high-crystallization, morphology and size-controllable tin sulfide/molybdenum disulfide heterojunction material is an important prerequisite. However, most of the previous researches focused on the preparation of the van der waals heterojunction of tin sulfide and molybdenum disulfide single materials or two-dimensional SnS/MoS2 and SnS2/MoS2, and the SnS/MoS2 mixed-dimension van der waals heterojunction composed of one-dimensional tin sulfide nanowires and two-dimensional single-layer molybdenum disulfide has not been reported yet. Compared with the two-dimensional SnS/MoS2 and SnS2/MoS2 Van der Waals heterojunction, the one-dimensional tin sulfide/two-dimensional molybdenum disulfide mixed dimension Van der Waals heterojunction has the following advantages in structure and property in several aspects: (1) the restriction and regulation on the space distribution of the current carriers are facilitated; (2) the energy band structure of the heterojunction composition material is beneficial to independently regulating and controlling the grid voltage; (3) the preparation of devices and electrode contact are facilitated; (4) the one-dimensional tin sulfide shows a phase structure different from that of the two-dimensional tin sulfide, and has low defect density and small dark current. The current method for preparing the layered metal chalcogenide and the heterojunction material thereof mainly comprises the following steps: mechanical peel transfer, hydrothermal synthesis, and Chemical Vapor Deposition (CVD) methods, among others. Among these methods, the mechanical peeling method, in which tin sulfide and molybdenum disulfide are firstly peeled off from a single crystal sample and then these two-dimensional materials are stacked by dry or wet transfer to form a heterojunction, has advantages in that intrinsic physical properties of these materials can be secured, and has disadvantages in that surface contamination is easily formed and the yield is low. The hydrothermal synthesis method is to obtain the metal chalcogenide through chemical reaction and annealing treatment process in a solution environment, and has the advantages of high yield; however, the obtained heterojunction nano material has small size and poor controllability of structure and appearance. In contrast, Chemical Vapor Deposition (CVD) is currently the most efficient method for producing large area, high quality layered metal chalcogenide materials and heterojunction materials. However, at present, the method is difficult to directly synthesize the one-dimensional/two-dimensional mixed-dimension van der waals heterojunction. In a Te/MoS2 Van der Waals heterostructure, a preparation method and application thereof (application publication No. CN 109065662A), although the Te nanowire is epitaxially grown on the surface of the MoS2 nano-layer by Chemical Vapor Deposition (CVD) to form a mixed-dimension Van der Waals heterojunction, the Te nanowire which is epitaxially grown is distributed on the surface of the MoS2 in a large quantity, and the size and the shape of the nanowire are small, so that the contact application of a device is not facilitated. Therefore, it is of great significance to develop a preparation method capable of realizing high-quality tin sulfide/molybdenum disulfide mixed dimension heterojunction material.
Disclosure of Invention
In order to overcome the defects of the existing preparation method, the invention provides a preparation method of a tin sulfide/molybdenum disulfide mixed dimension van der Waals heterojunction. The tin sulfide/molybdenum disulfide mixed dimension Van der Waals heterojunction prepared by the invention is a mixed dimension semiconductor heterojunction formed by vertically stacking one-dimensional tin sulfide nanowires and two-dimensional single-layer molybdenum disulfide. The invention adopts a step-by-step chemical vapor deposition method to realize the high-quality controllable and stable growth of the tin sulfide/molybdenum disulfide mixed dimension Van der Waals heterojunction on the substrates of SiO2/Si, mica and the like, and has the following advantages:
(1) the invention provides a tin sulfide/molybdenum disulfide mixed dimension Van der Waals heterojunction material which is formed by vertically stacking a one-dimensional tin sulfide nanowire and a two-dimensional single-layer molybdenum disulfide and is beneficial to gate voltage regulation and control; the heterojunction material shows a type II band offset, and is beneficial to the separation of photon-generated carriers;
(2) the tin sulfide/molybdenum disulfide mixed dimension Van der Waals heterojunction prepared by the invention has the characteristics of high crystallinity, good dispersibility, low impurity and defect density and the like;
(3) the preparation method uses sulfur powder, molybdenum trioxide and tin sulfide as reaction growth sources, adopts a two-step CVD method to prepare the tin sulfide/molybdenum disulfide mixed dimension van der Waals heterojunction, and has the advantages of simple preparation process, mild reaction and high repeatability.
The invention provides a preparation method of a tin sulfide/molybdenum disulfide mixed dimension Van der Waals heterojunction, which is carried out by a two-step chemical vapor deposition method according to the following steps:
step 1: wiping the double-temperature-zone tubular furnace clean by absolute ethyl alcohol, annealing the tubular furnace at the high temperature of 600 ℃, and flushing by using high-purity argon of 300sccm during annealing;
step 2: selecting a SiO2/Si substrate of 1cm multiplied by 1cm, sequentially soaking in acetone, deionized water and absolute ethyl alcohol solution, ultrasonically cleaning, and then washing and air-drying for later use;
and step 3: respectively placing sulfur powder and molybdenum oxide powder in the center of a first temperature area and the center of a second temperature area of a double-temperature-area tubular furnace; placing the cleaned substrate in a quartz boat containing molybdenum oxide powder, opening a vacuum pump to pump the pressure in the double-temperature-zone tubular furnace to be below 10pa, introducing argon of 300sccm into the tubular furnace to clean after the pumping is finished, and repeating for 2-3 times;
and 4, step 4: setting carrier gas flow rate after the washing is finished, enabling two temperature areas of the tubular furnace to respectively rise to target growth temperature at the stable carrier gas flow rate, carrying out heat preservation growth to obtain a single-layer molybdenum disulfide sample, waiting for the tubular furnace to naturally cool to room temperature after the reaction is finished, and taking out the molybdenum disulfide sample for later use;
and 5: respectively placing sulfur powder and tin sulfide powder in the center of a first temperature area and the center of a second temperature area of a double-temperature-area tubular furnace; placing the substrate with the molybdenum disulfide grown on a quartz boat containing tin sulfide powder, opening a vacuum pump to pump the pressure in the dual-temperature-zone tubular furnace to be below 10pa, introducing 300sccm argon into the tubular furnace to clean after the pumping is finished, and repeating for 2-3 times;
and 6: setting carrier gas flow rate after the washing is finished, raising the second temperature zone of the tube furnace to the target growth temperature at constant speed at the stable carrier gas flow rate, carrying out heat preservation growth on the mixed dimension van der Waals heterojunction of tin sulfide/molybdenum disulfide, and naturally cooling the tube furnace to room temperature after the reaction is finished;
preferably, the mass ratio of the sulfur powder to the molybdenum oxide powder in the step 3 is 2.6: 1;
preferably, in the step 3, the growth substrate is positioned 2cm behind the molybdenum oxide powder;
preferably, the carrier gas in the step 4 is argon, and the flow rate of the argon is 60 sccm;
preferably, the target growth temperature of the first temperature zone in the step 4 is 200 ℃;
preferably, the target growth temperature of the second temperature zone in the step 4 is 680-720 ℃, and particularly preferably 700 ℃;
preferably, the heat preservation growth time in the step 4 is 15min;
preferably, the mass ratio of the sulfur powder to the tin sulfide powder in the step 5 is 3: 1;
preferably, the substrate grown with the molybdenum disulfide in the step 5 is 6cm behind the tin sulfide powder;
preferably, in the step 6, the carrier gas is argon, and the argon flow is 60 sccm;
preferably, the first temperature zone does not work in step 6;
preferably, in the step 6, the target growth temperature of the second temperature zone is 680-720 ℃, and particularly preferably 700 ℃;
preferably, the incubation growth time in step 6 is 30 min.
Compared with the prior art, the technical scheme of the invention has the following advantages:
(1) the mass ratio of the sulfur powder to the molybdenum oxide powder in the step 3 is 2.6:1, and the mass ratio of the sulfur powder to the tin sulfide powder in the step 5 is 3:1, so that molybdenum disulfide and tin sulfide are generated in the reaction process;
(2) in the step 4 and the step 6, the argon flow is 60sccm, which is beneficial to uniform and stable growth of materials on the substrate;
(3) in the step 4, the target growth temperature of the first temperature zone is 200 ℃, the target growth temperature of the second temperature zone is 680-720 ℃, and particularly 700 ℃; in the step 6, the first temperature zone does not work, the target growth temperature of the second temperature zone is 680-720 ℃, and particularly 700 ℃ is preferred, so that the nucleation growth of the material on the substrate is facilitated, and the material can grow in a large size and high quality at a proper growth temperature;
(4) the substrate on which the molybdenum disulfide grows in the step 5 is 6cm behind the tin sulfide powder, so that the stable growth of the material is facilitated;
(5) the heat preservation growth time in the step 4 is 15min, and the heat preservation growth time in the step 6 is 30min, so that the preparation of a sample with large size, good appearance and no impurities is facilitated.
Drawings
FIG. 1 is a schematic diagram of the preparation process of example 4, example 5 and example 6 of the present invention.
FIG. 2 is an optical topography of molybdenum disulfide prepared on a SiO2/Si substrate in example 1 of the present invention.
FIG. 3 is an optical topographic map of molybdenum disulfide prepared on SiO2/Si substrate in example 2 of the present invention.
FIG. 4 is a Raman spectrum of molybdenum disulfide prepared on a SiO2/Si substrate in example 2 of the present invention.
FIG. 5 is an Atomic Force Microscope (AFM) image of molybdenum disulfide prepared on a SiO2/Si substrate in example 2 of the present invention.
FIG. 6 is an optical topography of molybdenum disulfide prepared on a SiO2/Si substrate in example 3 of the present invention.
FIG. 7 is an optical topography of a tin sulfide/molybdenum disulfide mixed dimension Van der Waals heterojunction fabricated on a SiO2/Si substrate in example 4 of the present invention.
FIG. 8 is an optical topography of a mixed dimension Van der Waals heterojunction of tin sulfide/molybdenum disulfide prepared on a SiO2/Si substrate according to example 5 of the present invention.
Figure 9 is an Atomic Force Microscope (AFM) image of a tin sulfide/molybdenum disulfide mixed dimension van der waals heterojunction fabricated on a SiO2/Si substrate in example 5 of the present invention.
FIG. 10 is a Raman spectrum of a mixed dimension van der Waals heterojunction of tin sulfide/molybdenum disulfide prepared on a SiO2/Si substrate in example 5 of the present invention.
FIG. 11 is an optical topography of a tin sulfide/molybdenum disulfide mixed dimension Van der Waals heterojunction fabricated on a SiO2/Si substrate in example 6 of the present invention.
Detailed Description
Example 1 preparation of a molybdenum disulfide sample with a first temperature zone targeted at 200 deg.C and a second temperature zone targeted at 680 deg.C
(1) Wiping the double-temperature-zone tubular furnace clean by absolute ethyl alcohol, annealing the tubular furnace at the high temperature of 600 ℃, and flushing by using high-purity argon of 300sccm during annealing;
(2) sequentially soaking a SiO2/Si substrate which is divided into 1cm multiplied by 1cm in acetone, deionized water and absolute ethyl alcohol solution, ultrasonically cleaning surface stains, and then washing and air-drying for later use;
(3) weighing 150mg of sulfur powder and 40mg of molybdenum oxide powder, placing the sulfur powder and the molybdenum oxide powder in a quartz boat, respectively placing the quartz boat in the first temperature zone and the central position of the first temperature zone of the two-temperature-zone tube furnace, and then placing a cleaned SiO2/Si substrate about 2cm behind the molybdenum oxide powder;
(4) pumping the pressure in the tubular furnace to be below 10pa by using a vacuum pump, then introducing argon gas of 300sccm into the tubular furnace for cleaning, repeating for 3 times, and setting the argon gas flow to be 60sccm after the cleaning is finished;
(5) and under the condition of 60sccm argon gas, respectively heating the first temperature zone and the second temperature zone to 200 ℃ and 680 ℃ within 60min, then carrying out heat preservation growth for 15min, naturally cooling to room temperature after the reaction is finished, and taking out a molybdenum disulfide sample for later use.
FIG. 2 shows that the MoS2 sample obtained in this example, although it was formed, was too small to facilitate heterojunction preparation.
Example 2 preparation of a molybdenum disulfide sample with a first temperature zone targeted at 200 ℃ and a second temperature zone targeted at 700 ℃
This example provides a process for the preparation of a MoS2 material on a SiO2/Si substrate, which is essentially the same as in example 1. The difference from example 1 is that: the second temperature zone target temperature is raised from 680 c to 700 c in step 5.
FIG. 3 is an optical morphology of MoS2 prepared in this example, which shows that MoS2 grains have uniform morphology and size (about 15 μm) and good dispersibility.
FIG. 4 is a Raman spectrum of a sample of MoS2 prepared in this example, showing two Raman peaks at 381cm-1 and 410cm-1, corresponding to the E2g and A1g modes of monolayer MoS2, respectively.
FIG. 5 is an Atomic Force Microscope (AFM) image of MoS2 prepared in this example, the height map showing that the thickness of the prepared MoS2 was 0.98nm, demonstrating a monolayer sample.
Example 3 preparation of a molybdenum disulfide sample with a first temperature zone targeted at 200 deg.C and a second temperature zone targeted at 720 deg.C
This example provides a process for the preparation of a MoS2 material on a SiO2/Si substrate, which is essentially the same as in example 1. The difference from example 1 is that: the second temperature zone target temperature is raised from 680 c to 720 c in step 5.
FIG. 6 shows a sample of MoS2 prepared in this example, where the molybdenum disulfide surface and surrounding impurities are higher at higher temperatures.
Example 4 the first temperature zone was not operated and the second temperature zone was targeted at 680 c to produce a tin sulfide/molybdenum disulfide mixed dimension van der waals heterojunction sample
The embodiment provides an SnS/MoS2 mixed-dimension Van der Waals heterojunction material, and particularly relates to a mixed-dimension semiconductor heterojunction formed by van der Waals epitaxy of a one-dimensional SnS nanowire and a two-dimensional single-layer MoS2 on an SiO2/Si substrate. This example provides a method for preparing the above heterojunction material (as shown in fig. 1), including the following steps:
(1) wiping the double-temperature-zone tubular furnace clean by absolute ethyl alcohol, annealing the tubular furnace at the high temperature of 600 ℃, and flushing by using high-purity argon of 300sccm during annealing;
(2) cutting into SiO2/Si substrates of 1cm multiplied by 1cm, soaking in acetone, deionized water and absolute ethyl alcohol solution in sequence, ultrasonically cleaning surface stains, and then washing and air-drying for standby;
(3) weighing 150mg of sulfur powder and 40mg of molybdenum oxide powder, placing the sulfur powder and the molybdenum oxide powder in a quartz boat, respectively placing the quartz boat in the center positions of a first temperature zone and a first temperature zone of a double-temperature-zone tube furnace, and then placing a cleaned SiO2/Si substrate about 2cm behind the molybdenum oxide powder;
(4) pumping the pressure in the tubular furnace to be below 10pa by using a vacuum pump, then introducing argon gas of 300sccm into the tubular furnace for cleaning, repeating for 3 times, and setting the argon gas flow to be 60sccm after the cleaning is finished;
(5) under the argon atmosphere of 60sccm, respectively heating the first temperature zone and the second temperature zone to 200 ℃ and 700 ℃ within 60min, then carrying out heat preservation growth for 15min, naturally cooling to room temperature after the reaction is finished, and taking out a molybdenum disulfide sample for later use;
(6) weighing 150mg of sulfur powder and 50mg of tin sulfide powder, placing the quartz boat containing the sulfur powder and the quartz boat containing the tin sulfide powder in the centers of a first temperature zone and a second temperature zone of a tube furnace respectively, and then placing a SiO2/Si substrate on which a molybdenum disulfide sample grows 6cm behind the tin sulfide powder;
(7) pumping the pressure in the tubular furnace to be below 10pa by adopting a vacuum pump, introducing argon gas of 300sccm into the tubular furnace for cleaning, repeating for 3 times, and setting the argon gas flow to be 60sccm after the cleaning is finished;
(8) heating the second temperature zone to 680 ℃ under the argon atmosphere of 60sccm, wherein the heating time is 60min, and the heat preservation growth time is 30 min; and in the temperature rise process of the second temperature zone, the first temperature zone does not work to keep trace sulfur powder to participate in the reaction, so that the SnS nanowire is formed on the surface of the MoS2, and after the reaction is finished, the tubular furnace is naturally cooled to room temperature to obtain the SnS/MoS2 mixed dimension Van der Waals heterojunction.
Fig. 7 is a van der waals heterojunction sample with mixed dimensions of SnS/MoS2 prepared in this example, and it can be seen that under the conditions of this example, SnS nanowires are difficult to nucleate and grow on the surface of MoS2, and no heterojunction can be formed.
Example 5 the first temperature zone was not operated and the second temperature zone was targeted at 700 c to produce a tin sulfide/molybdenum disulfide mixed dimension van der waals heterojunction sample
The embodiment provides an SnS/MoS2 mixed-dimension van der Waals heterojunction material, in particular to a mixed-dimension semiconductor heterojunction formed by one-dimensional SnS nanowires and two-dimensional single-layer MoS2 through van der Waals epitaxy on an SiO2/Si substrate, and the process is basically the same as that of embodiment 4. The difference from example 4 is that: the target temperature of the second temperature zone in step 8 is raised from 680 c to 700 c.
Fig. 8 is an optical topography of the SnS/MoS2 mixed-dimension van der waals heterojunction prepared in this example, and it can be seen that the heterojunction is formed by stacking one-dimensional SnS and two-dimensional single-layer MoS 2.
Fig. 9 is an atomic force microscope image of the SnS/MoS2 mixed-dimension van der waals heterojunction fabricated in this example, and it can be seen that the thickness of the SnS nanowire is 27.6nm and the thickness of the molybdenum disulfide is 0.98 nm.
Fig. 10 is a comparison graph of raman spectra of the SnS/MoS2 mixed-dimension van der waals heterojunction and the independent SnS and MoS2 prepared in this example, and it can be seen that the raman peaks of the heterojunction are both provided by the SnS nanowire and MoS2, which indicates that the prepared sample is a heterojunction material.
Example 6 the first temperature zone was not operated and the second temperature zone was targeted at 720 deg.c to produce a tin sulfide/molybdenum disulfide mixed dimension van der waals heterojunction sample
The embodiment provides an SnS/MoS2 mixed-dimension Van der Waals heterojunction material, in particular to a mixed-dimension semiconductor heterojunction formed by van der Waals epitaxy of a one-dimensional SnS nanowire and a two-dimensional single-layer MoS2 on an SiO2/Si substrate, and the process is basically the same as that of embodiment 4. The difference from example 4 is that: the target temperature of the second temperature zone in step 8 is raised from 680 ℃ to 720 ℃.
Fig. 11 shows the mixed dimension van der waals heterojunction sample of SnS/MoS2 prepared in this example, which shows that although the heterojunction is formed, there are many impurities.
Claims (3)
1. A preparation method of a tin sulfide/molybdenum disulfide mixed dimension Van der Waals heterojunction comprises the following steps:
step 1: wiping the double-temperature-zone tubular furnace clean by absolute ethyl alcohol, annealing the tubular furnace at the high temperature of 600 ℃, and flushing by using high-purity argon of 300sccm during annealing;
step 2: selecting SiO 1cm x 1cm 2 Soaking the Si substrate in acetone, deionized water and absolute ethyl alcohol solution in sequence, ultrasonically cleaning, and then washing and air-drying for later use;
and step 3: respectively placing sulfur powder and molybdenum oxide powder in the center of a first temperature area and the center of a second temperature area of a double-temperature-area tubular furnace; placing the cleaned substrate in a quartz boat containing molybdenum oxide powder, opening a vacuum pump to pump the pressure in the double-temperature-zone tubular furnace to be below 10pa, introducing argon of 300sccm into the tubular furnace to clean after the pumping is finished, and repeating for 2-3 times;
and 4, step 4: setting carrier gas flow rate after the washing is finished, enabling two temperature areas of the tubular furnace to respectively rise to target growth temperature at the stable carrier gas flow rate, carrying out heat preservation growth to obtain a single-layer molybdenum disulfide sample, waiting for the tubular furnace to naturally cool to room temperature after the reaction is finished, and taking out the molybdenum disulfide sample for later use;
and 5: respectively placing sulfur powder and tin sulfide powder in the center of a first temperature area and the center of a second temperature area of a double-temperature-area tubular furnace; placing the substrate with the molybdenum disulfide grown on a quartz boat containing tin sulfide powder, opening a vacuum pump to pump the pressure in the double-temperature-zone tubular furnace to be below 10pa, introducing argon of 300sccm into the tubular furnace to clean after the pumping is finished, and repeating for 2-3 times;
step 6: setting carrier gas flow rate after the washing is finished, raising the second temperature zone of the tube furnace to the target growth temperature at constant speed at the stable carrier gas flow rate, carrying out heat preservation growth on the mixed dimension van der Waals heterojunction of tin sulfide/molybdenum disulfide, and naturally cooling the tube furnace to room temperature after the reaction is finished;
the method is characterized in that in the step 3, the mass ratio of the sulfur powder to the molybdenum oxide powder is 2.6:1, placing a substrate 2cm behind a quartz boat containing molybdenum oxide powder; in the step 4, the flow rate of the carrier gas is 60sccm, the target temperature of the first temperature zone is 200 ℃, and the target temperature of the second temperature zone is 680-700 ℃; in the step 5, the mass ratio of the sulfur powder to the tin sulfide powder is 3:1, placing a substrate with molybdenum disulfide growing on a quartz boat containing tin sulfide powder 6cm behind the substrate; in the step 6, the flow rate of the carrier gas is 60sccm, the first temperature zone does not work, and the target temperature of the second temperature zone is 680-720 ℃.
2. The method for preparing a mixed-dimension van der waals heterojunction of tin sulfide/molybdenum disulfide as claimed in claim 1, wherein in the step 4, the target temperature of the second temperature zone is optimally 700 ℃; in step 6, the target temperature of the second temperature zone is optimally 700 ℃.
3. The method for preparing a tin sulfide/molybdenum disulfide mixed dimension van der waals heterojunction as claimed in claim 1, wherein in step 4, the temperature rise time of the first temperature zone is 40min, the heat preservation time is 15min, the temperature rise time of the second temperature zone is 40min, and the heat preservation time is 15min; in step 6, the temperature rise time of the second temperature zone is 60min, and the heat preservation time is 30 min.
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| CN115504510B (en) * | 2022-09-27 | 2023-11-07 | 华南理工大学 | 3R-MoS 2 Preparation method of powder |
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