KR101708260B1 - Transitional metal dichalcogenides and method of preparing the same - Google Patents
Transitional metal dichalcogenides and method of preparing the same Download PDFInfo
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- KR101708260B1 KR101708260B1 KR1020150086763A KR20150086763A KR101708260B1 KR 101708260 B1 KR101708260 B1 KR 101708260B1 KR 1020150086763 A KR1020150086763 A KR 1020150086763A KR 20150086763 A KR20150086763 A KR 20150086763A KR 101708260 B1 KR101708260 B1 KR 101708260B1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F11/00—Compounds containing elements of Groups 6 or 16 of the Periodic Table
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The present invention relates to a transition metal chalcogenide structure and a process for preparing the same, and more particularly, to a process for preparing a transition metal chalcogenide structure using a dip coating process, Various types of transition metal chalcogenide structures can be prepared.
Description
The present invention relates to a transition metal chalcogenide structure that can be applied to an electronic device or a heterostructure device requiring mass production and a method for manufacturing the same.
For the purpose of developing new types of electronic and optoelectronic devices that can be made using existing materials, much research has been done on two-dimensional (2D) materials. In particular, the transition metal chalcogenide (TMD) represented by the general formula MX2 has attracted a great deal of attention due to its excellent optical and mechanical properties, and the electrical properties due to the atomic thickness and the finite band gap.
Studies on TMD have been performed mostly on mechanically exfoliated flakes or by transferring them onto a useful substrate such as SiO 2 and sapphire. However, this method is unsuitable for electronic devices and heterostructure devices capable of mass production in terms of scale and interface. Several synthetic methods have been used for the production of large area TMD films. For example, using chemical vapor deposition (CVD), which is currently the most successful method for synthesizing high quality TMD, a uniform film with a well-controlled number of layers can be obtained. Further, by using the CVD method, it is possible to easily manufacture a horizontal or vertical heterostructure by changing the gaseous reactant during the growth process. Various heterojunctions have been successfully synthesized by this method. The CVD method ensures excellent crystallinity and uniformity, but this method has the problem that the synthesis conditions are complicated and sensitive and the pattern formation required for the integrated device is difficult. Therefore, a solution-based method is desired in which the size and structure of the material can be changed through relatively simple and various changes of the synthesis parameters.
SUMMARY OF THE INVENTION The present invention has been made in view of the above problems, and it is an object of the present invention to provide a transition metal chalcogenide structure capable of producing various types of transition metal chalcogenide structures by easily controlling process conditions during a transition metal chalcogenide production process. And to provide a method for producing a chalcogenide.
Another object of the present invention is to provide a transition metal chalcogenide structure according to various embodiments of the present invention, and a device including the same.
One aspect of the present invention relates to a method for preparing a metal complex comprising: (A) adjusting the pH of an aqueous solution of a transition metal chalcogenide (TMD) precursor; (B) immersing the substrate in a pH-adjusted TMD precursor aqueous solution; And (C) drying the TMD precursor aqueous solution coated on the substrate to induce self-assembly of the TMD.
Another aspect of the present invention is a process for preparing a precursor solution comprising: (A) adjusting the pH of an aqueous solution of a first transition metal chalcogenide (TMD) precursor; (B) immersing the substrate in a pH-adjusted first TMD precursor aqueous solution; (C) drying the first TMD precursor aqueous solution coated on the substrate to induce self-assembly of the first TMD; (D) immersing the self-assembled first TMD structure in a second transition metal chalcogenide (TMD) precursor aqueous solution; And (E) drying the second TMD precursor aqueous solution coated on the first TMD structure to induce self-assembly of the second TMD.
Another aspect of the present invention relates to a transition metal chalcogenide structure produced by the above process.
Another aspect of the present invention relates to a transition metal chalcogenide heterostructure produced by the above process.
Yet another aspect of the present invention is a device comprising the transition metal chalcogenide structure, wherein the device is one selected from a field effect transistor (FET), a transparent electronic device, and a flexible device.
Yet another aspect of the present invention is a device comprising the transition metal chalcogenide heterostructure, wherein the device is one selected from a field effect transistor (FET), a transparent electronic device, and a flexible device.
The method of preparing the transition metal chalcogenide structure according to the present invention uses a dip coating method, and thus it is easy to control process conditions such as concentration, pH, and evaporation rate of a solution. In addition, various types of transition metal chalcogenide structures can be produced by controlling such process conditions, and the diversified transition metal chalcogenide structures can be produced in electronic devices requiring high volume production or devices requiring heterostructure Can be widely applied.
1 schematically illustrates a dip coating process for preparing a transition metal chalcogenide structure according to an embodiment of the present invention.
2 is an SEM (Scanning Electron Microscope) image and a schematic diagram of an MoS 2 structure according to an embodiment of the present invention.
FIG. 3 is a phase diagram of the MoS 2 structure according to the evaporation rate, humidity, and concentration of the precursor aqueous solution in the process of manufacturing the MoS 2 structure according to an embodiment of the present invention.
4 is an optical image showing a self-assembly process of a wire-shaped MoS 2 structure according to an embodiment of the present invention.
FIG. 5 is a characteristic analysis result of the MoS 2 structure according to an embodiment of the present invention.
FIG. 6 is a result of analyzing the characteristics of the MoS 2 structure by the IPA addition amount according to an embodiment of the present invention.
7 is an SEM image showing nucleation for self-assembly of an MoS 2 structure according to an embodiment of the present invention.
8 is a graph showing a correlation between wire density and light transmittance of an MoS 2 structure according to an embodiment of the present invention.
9 is a characteristic analysis result of a core-shell type WS 2 / MoS 2 heterostructure according to an embodiment of the present invention.
10 is a characteristic analysis result of a device to which a MoS 2 structure according to an embodiment of the present invention is applied.
Hereinafter, the present invention will be described in more detail with reference to the drawings.
One aspect of the present invention relates to a method for preparing a metal complex comprising: (A) adjusting the pH of an aqueous solution of a transition metal chalcogenide (TMD) precursor; (B) immersing the substrate in a pH-adjusted TMD precursor aqueous solution; And (C) drying the TMD precursor aqueous solution coated on the substrate to induce self-assembly of the TMD.
According to one embodiment, the TMD precursor is (NH 4 ) 2 MoS 4 , (NH 4 ) 2 WS 4 , NH 4 2 MoSe 4 , (NH 4 ) 2 WSe 4 , (NH 4 ) 2 WTe 4 and (NH 4 ) 2 MoTe 4 , Compound capable of inducing self-assembly of the TMD structure on a substrate by the method of the present invention can be widely used.
However, when (NH 4 ) 2 MoS 4 or (NH 4 ) 2 WS 4 is used as compared to other kinds of TMD precursors, the TMD self-assembly can be more easily induced, and the MoS 2 structure or the WS 2 structure Can be efficiently formed. Also, when (NH 4 ) 2 MoSe 4 or (NH 4 ) 2 WSe 4 is used as a TMD precursor, an MoSe 2 structure or a WSe 2 structure can be formed, and (NH 4 ) 2 WTe 4 as a TMD precursor or (NH 4 ) 2 MoTe 4 , a MoTe 2 structure or a WTe 2 structure can be formed.
According to another embodiment, the concentration of the TMD precursor aqueous solution may be 0.1 to 0.8 wt%, and the concentration of the TMD precursor aqueous solution may be adjusted according to the shape of the TMD structure to be obtained. For example, if the concentration of the TMD precursor aqueous solution is in the range of 0.2 to 0.8 wt%, a TMD structure in the form of a film can be formed (however, the evaporation rate must be significantly faster) and the concentration of the TMD precursor aqueous solution is 0.6 To about 0.8 wt%, a dendritic TMD structure may be formed, and when it is within the range of 0.1 to 0.6 wt%, a wire-shaped TMD structure may be formed, and when the concentration of the TMD precursor aqueous solution is less than 0.1 wt% , It is difficult to obtain a TMD structure applicable to a device because a cluster is formed. However, the shape of the TMD structure according to these concentrations is exemplary and may vary depending on other factors such as the pH of the aqueous TMD precursor solution as described below, and the rate of drying.
According to another embodiment, in step (A), the pH of the TMD precursor aqueous solution may be adjusted using an acid. The self-assembly of the TMD can be promoted by controlling the pH range from 4.5 to 6.5, preferably from 4.5 to 5.5. In addition, by appropriately adjusting the pH within the prescribed pH range, the shape of the TMD structure formed by self-assembly can be controlled. For example, a higher pH can form a dendritic TMD structure, and a lower pH can form a wire-shaped TMD structure, which is exemplary and can be determined by the concentration of the TMD precursor aqueous solution as described above, Speed, and other factors.
The acid may be at least one selected from hydrochloric acid, sulfuric acid and nitric acid, but an acid capable of controlling the pH of the aqueous solution can be widely used. However, when hydrochloric acid is used in comparison with other kinds of acids, the TMD structure can be easily formed by self-assembly.
According to another embodiment, at least one selected from the group consisting of alcohol, ether and acetone may be added to the TMD precursor aqueous solution of the step (B) as a material for controlling the thickness of the TMD precursor. The alcohol may be IPA (isopropyl alcohol), and the ether may be dimethyl ether.
For example, when the TMD precursor is in the form of a wire, the thickness of the TMD structure can be controlled by adjusting the distance between the wires by adding the isopropyl alcohol.
The thickness of the TMD structure may be in the range of 16 to 60 ppm, and the thickness of the TMD structure may be reduced by decreasing the distance between the TMD structure and the TMD structure.
According to another embodiment, the substrate of the step (B) may be one selected from the group consisting of a SiO 2 / Si substrate, a quartz substrate and a plastic substrate. However, since TMD nuclei are formed on the surface, A hydrophilic substrate which can be formed and a transparent substrate having good light transmittance can be widely used.
According to another embodiment, the substrate may be oxygen plasma treated to improve the hydrophilicity of the surface. On the surface of the substrate, the TMD precursor is agglomerated to form nuclei, and then the TMD self-assembly is induced to produce various types of TMD structures.
Therefore, it is important that nucleation occurs smoothly on the surface of the substrate. In the hydrophilic portion of the substrate surface, nuclei due to the agglomeration of the precursor may be generated. Therefore, by performing oxygen plasma treatment on the substrate surface to enhance hydrophilicity, .
According to another embodiment, in step (C), various types of TMD structures can be obtained by controlling the drying rate of the TMD precursor aqueous solution. The drying rate suitable for obtaining the TMD structure may be from 0.5 to 330 nl / s, and the drying rate may be from 0.5 to 330 nl / s, the TMD structure may be formed into a film form, and the drying speed may be slower A TMD structure in the form of a dendrite or a wire may be formed. For example, when a film is to be formed, the drying speed may be at least 320 nl / s, the drying speed may be 0.5-1.2 nl / s for a dendrite, and 1.2-2 nl / s for a wire, , As described above, can be appropriately adjusted according to the concentration and pH of the TMD precursor aqueous solution.
According to another embodiment, the drying rate may be controlled by changing at least one selected from humidity and temperature. The lower the humidity and the higher the temperature, the faster the drying rate. The higher the humidity and the lower the temperature, the slower the drying rate.
1 schematically illustrates a dip coating process for preparing a transition metal chalcogenide structure according to an embodiment of the present invention. Referring to FIG. 1, the substrate is immersed in (NH 4 ) 2 MoS 4 as a TMD precursor aqueous solution, coated, dried, and self-assembled from the nucleation formed on the surface of the substrate to obtain a TMD structure have.
According to another embodiment, the step (C) may further comprise: (D) a first heat treatment step of performing heat treatment at 400 to 600 ° C under hydrogen and argon atmosphere; And a second heat treatment step of performing heat treatment at 800 to 1200 ° C under an argon atmosphere. The first heat treatment step may be a reaction step to cause the TMD precursor formed after the dip coating to form a TMD structure, and the second heat treatment step may be a step to increase the crystallinity of the formed TMD structure. For example, the MoS 4 becomes MoS 2 in the first heat treatment step, and the crystallinity of MoS 2 can be improved in the second heat treatment step. Here, the heat treatment temperature range in the first and second heat treatment steps is set in consideration of whether or not the reaction can be optimized and appropriate crystallinity can be imparted.
Meanwhile, the second heat treatment step may be performed under argon and S atmosphere. Here, in the S atmosphere, the S powder is vaporized and flowed in the heat treatment to make the space to be heat-treated into the S atmosphere, thereby further improving the heat treatment efficiency and crystallinity.
Another aspect of the present invention is a process for the preparation of a first precursor chalcogenide (TMD) precursor comprising: (A) adjusting the pH of an aqueous solution of a first transition metal chalcogenide (TMD) precursor; (B) immersing the substrate in a pH-adjusted first TMD precursor aqueous solution; (C) drying the first TMD precursor aqueous solution coated on the substrate to induce self-assembly of the first TMD; (D) immersing the self-assembled first TMD structure in a second transition metal chalcogenide (TMD) precursor aqueous solution; And (E) drying the second TMD precursor aqueous solution coated on the first TMD structure to induce self-assembly of the second TMD.
In the method for producing the transition metal chalcogenide heterostructure, the steps (A) to (C) may be carried out in the same manner as the steps (A) to (C) of the method for producing the transition metal chalcogenide structure.
However, in the method of preparing the transition metal chalcogenide heterostructure, two different kinds of transition metal chalcogenide precursors can be used to form a heterostructure.
According to one embodiment, the first and second transition metal chalcogenide precursors are (NH 4 ) 2 MoS 4 , (NH 4 ) 2 WS 4 , (NH 4 ) 2 MoSe 4 , (NH 4 ) 2 WSe 4 , (NH 4 ) 2 WTe 4 and (NH 4 ) 2 MoTe 4 , And the second transition metal chalcogenide precursor may be different.
However, it is preferable to use (NH 4 ) 2 MoS 4 as the first transition metal chalcogenide precursor and (NH 4 ) 2 WS 4 as the second transition metal chalcogenide precursor. In this case, A transition metal chalcogenide heterostructure of a core-shell structure, wherein the core comprises MoS 2 and the shell comprises WS 2 , can be obtained.
According to another embodiment, after the step (E), (F) a first heat treatment step of performing heat treatment at 400 to 600 ° C under hydrogen and argon atmosphere; And a second heat treatment step of performing heat treatment at a temperature of 800 to 1200 ° C under an argon atmosphere. The heat treatment may be carried out in the same manner as the heat treatment in step (D) of the method for producing a transition metal chalcogenide structure have.
Another aspect of the present invention relates to a transition metal chalcogenide structure produced by the above method, wherein the transition metal chalcogenide structure may be selected from a thin film, a dendrite and a wire.
Another aspect of the present invention relates to a transition metal chalcogenide heterostructure produced by the above process, wherein the transition metal chalcogenide heterostructure comprises a wire having a core-shell structure, a wire having a core- And may be a form selected from a film of a dye and a heterostructure. Here, the heterostructure film may be a double-layered film, a surface of a film prepared from the first TMD precursor is surrounded by a film formed from the second TMD precursor, but the present invention is not limited thereto.
Yet another aspect of the invention relates to a device comprising the transition metal chalcogenide structure.
Yet another aspect of the present invention relates to a device comprising the transition metal chalcogenide heterostructure.
In the present invention, the device may include a semiconductor device, a transparent electronic device, and a flexible device. Also, the semiconductor device may be a field effect transistor (FET) or a hybrid transistor, where the hybrid transistor may be combined with a transistor of another material to implement a solar cell, a photodetector, etc. through a pn junction Is a generic term for a device. In addition, the transparent electronic device may include all devices requiring transparency, including a transparent transistor, and the flexible device may include all devices requiring flexibility.
Example
Hereinafter, the present invention will be described in more detail with reference to Examples and the like, but the scope and content of the present invention can not be construed to be limited or limited by the following Examples. In addition, it is apparent that, based on the teachings of the present invention including the following examples, those skilled in the art can easily carry out the present invention in which experimental results are not specifically shown.
material
In the following examples, (NH 4 ) 2 MoS 4 and (NH 4 ) 2 WS 4 were used as transition metal chalcogenide (TMD) precursors, and SiO 2 / Si substrates were used as substrates.
Example 1
(1) pH adjustment
(NH 4 ) 2 MoS 4 powder was dissolved in 130 mL of deionized water (DI) and sonicated for 40 minutes to prepare a 0.2 wt% (NH 4 ) 2 MoS 4 aqueous solution. The pH of the (NH 4 ) 2 MoS 4 aqueous solution was 6.41.
The (NH 4) 2 MoS while the dropwise addition of dilute HCl solution and the aqueous solution adjusted to pH 4, the (NH 4) 2 MoS 4 pH of the aqueous solution was adjusted to 5.02.
(2) coating the substrate with a TMD precursor aqueous solution (dip coating)
pH of 5.02 (NH 4) 2 MoS 4 After filtering the solution by a membrane filter of pore size of the 0.45㎛, H 2 O 2 / H 2
(3) Drying
The (NH 4 ) 2 MoS 4 aqueous solution coated on the SiO 2 / Si substrate was dried at a rate of 1.6 nl / s under a humidity of 20 to 25% to obtain an MoS 2 structure.
(4) Heat treatment
Treated at 500 ° C. for 60 minutes under H 2 (25 sccm) and Ar (100 sccm), and then heat-treated at 1000 ° C. for 30 minutes under Ar (100 sccm) and S atmosphere. MoS 2 structure was obtained.
Example 2
An MoS 2 structure was prepared in the same manner as in Example 1, except that IPA (isopropyl alcohol) was added to the (NH 4 ) 2 MoS 4 aqueous solution and the SiO 2 / Si substrate was immersed in the step ( 2 ).
Example 3
The MoS 2 structure was prepared in the same manner as in Example 1 except that the SiO 2 / Si substrate was washed in the step (2) and then subjected to oxygen plasma treatment.
Example 3
An MoS 2 structure was prepared in the same manner as in Example 1, except that a quartz substrate was used instead of the SiO 2 / Si substrate in the step (2).
Example 5
(1) to (3) were carried out in the same manner as in Example 1 to obtain an MoS 2 structure.
(4) coating the substrate with TMD precursor aqueous solution (dip coating)
(NH 4 ) 2 WS 4 powder was dissolved in 130 mL of deionized water (DI), and ultrasonicated for 40 minutes to prepare an aqueous solution of (NH 4 ) 2 WS 4 . The pH of the (NH 4 ) 2 WS 4 aqueous solution was 6.41.
The pH was adjusted while adding a dilute HCl solution to the (NH 4 ) 2 WS 4 aqueous solution to adjust the pH of the (NH 4 ) 2 WS 4 aqueous solution to 5.02.
pH of 5.02 (NH 4) 2 WS 4, and then filtered with a membrane filter of pore size is an
(5) Drying
The (NH 4 ) 2 WS 4 aqueous solution coated on the MoS 2 structure was dried at a rate of 1.6 nl / s under a humidity of 20 to 25% to obtain a MoS 2 / WS 2 heterostructure.
(6) Heat treatment
Treated at a temperature of 500 캜 for 60 minutes under H 2 (25 sccm) and Ar (100 sccm), and then heat-treated at a temperature of 1000 캜 for 30 minutes under Ar (100 sccm) for drying.
Experimental Example 1
1-1. Manufacture of thin film TMD structure
The pH was adjusted to 6.41 in step (2) of Example 1, and the temperature was raised to 80 ° C in step (3) to obtain a MoS 2 structure at a drying rate of 320 nL / s.
1-2. Manufacture of TMD structure in dendrite form
The MoS 2 structure was prepared by adjusting the pH to 6.41 in step (2) of Example 1 and setting the drying rate to 0.67-1.72 nL / s in step (3).
1-3. Manufacture of wire-shaped TMD structure
The MoS 2 structure was prepared by adjusting the pH to 5.02 in step (2) of Example 1 and setting the drying rate to 0.67-1.72 nL / s in step (3).
Table 1 below shows the evaporation rates, the pH of the (NH 4 ) 2 MoS 4 aqueous solution and the MoS 2 structure prepared in Examples 1-1 to 1-3, and FIG. 2 shows the results of Experimental Examples 1-1 to 1- 3 is an SEM (Scanning Electron Microscope) image and a schematic diagram of the MoS 2 structure manufactured in Example 3.
(nL / s)
As shown in Table 1 and FIG. 2, the MoS 2 structure of Experimental Example 1-1 prepared by accelerating the evaporation rate of the (NH 4 ) 2 MoS 4 aqueous solution coated on the substrate showed a thin film form, while the evaporation rate , The MoS 2 structure of Experimental Example 1-2 exhibits a dendritic shape, and the dendrites have many small branches and are formed by self-assembling randomly on a substrate having a large number of stems Able to know. In addition, it can be seen that the MoS 2 structure of Experimental Example 1-3 prepared using (NH 4 ) 2 MoS 4 aqueous solution having a relatively high acidity as compared with Experimental Example 1-2 spontaneously formed an aligned wire pattern.
Experimental Example 2: Reaction Conditions Affecting the Form of TMD Structure (Phase Equilibrium Diagram)
Example 1 and prepared in the MoS 2 structure in the same way, pH 5.02 in (NH 4) 2 MoS 4 solution by evaporation speed, the humidity, and the use of (NH 4) 2 MoS 4 solution of MoS prepared sikimyeo changing the concentration of 2 The shapes of the structures are examined, and their relationship is shown in Fig.
FIG. 3 is a phase diagram of the MoS 2 structure according to the evaporation rate, humidity, and concentration of (NH 4 ) 2 MoS 4 aqueous solution prepared according to the experimental example of the present invention. Referring to FIG. 3, (NH 4 ) 2 MoS 4 aqueous solution showed a low evaporation rate of 0.67 to -1.72 nL / s and a relative humidity of 80 to 20% at a fixed pH of 5.02. When the concentration of the (NH 4 ) 2 MoS 4 aqueous solution was less than 0.05% (w / v), it was confirmed that clusters composed of small particles agglomerated over the entire region regardless of the evaporation rate and humidity were formed (Region I). On the other hand, when the concentration of the (NH 4 ) 2 MoS 4 aqueous solution is 0.05% (w / v) or more, the MoS 2 structure changes depending on the drying rate. If the drying speed is slowed, the MoS 2 structure shows dendritic (Region II) and that the MoS 2 structure exhibits wire morphology when the drying rate slows down (region III). In addition, the (NH 4) 2 MoS 4, if the evaporation speed of the aqueous solution of not less than 1.2nL / s has the (NH 4) 2 MoS 4 in a high concentration region of aqueous (NH 4) 2 MoS 4 is separation promotion of fingering It can be seen that a wire-like MoS 2 structure is formed due to the periodic spacing between the nuclei due to instability.
The (NH 4 ) 2 MoS 4 aqueous solution promotes the precipitation of (NH 4 ) 2 MoS 4 in the solid phase in the region where the concentration of the aqueous solution is high due to the fingering instability, and nuclei having periodic intervals are generated, Is formed.
Experimental Example 3: Characterization of TMD structure in wire form
The characteristics of the wire-shaped MoS2 structure prepared in Example 1 were analyzed.
FIG. 4 are images showing the self-assembly process of the wire-shaped MoS 2 structure according to time during the evaporation of the solvent during drying in step (3) of Example 1. It can be confirmed that MoS 2 structures self-assembled at regular intervals of wires from (NH 4 ) 2 MoS 4 aqueous solution with time (0.0 sec, 0.8 sec, 1.6 sec and 2.4 sec) are formed.
5 is an analysis of the characteristics of the wire-shaped MoS 2 structure produced in Example 1. FIG.
FIGS. 5A and 5B are atomic force microscopy (AFM) images and graphs showing wire morphological changes due to heat treatment during drying in
FIGS. 5C and 5D are graphs showing the SEM image of the wire after the heat treatment during drying and the number of counts of the length of wire in the
5 (e) is a result of X-ray photoelectron spectroscopy (XPS) and X-ray diffractometry (XRD) of the wire-shaped MoS 2 structure produced in Example 1 .
Referring to FIG. 5 (e), as a result of X-ray photoelectron spectroscopic analysis, it can be seen that the wire manufactured in Example 1 clearly shows MoS 2 characteristics. Peaks corresponding to Mo 3d 5/2 and Mo 3d 3/2 were observed at 229.5 eV and 232.7 eV, respectively. As a result of X-ray diffraction analysis, it was confirmed that the wire exhibited a high crystallinity by strongly showing peaks corresponding to (002), (004), (103) and (006) crystal planes.
Experimental Example 4: Characterization of TMD structure according to IPA content
When the wire-shaped MoS 2 structure is applied to various devices, it is important to control the position of the wires and the periodic alignment on the substrate in terms of device fabrication. Experiments were conducted on controlling the characteristics of the wires in the wire-shaped MoS 2 structure.
Example 2 was prepared in a wire form of MoS 2 structure in the same way as, IPA at different (isopropyl alcohol) the addition amounts respectively to 16ppm, 33ppm and 60ppm, and analyzed the characteristics of the wire form of MoS 2 structure in accordance with IPA addition.
6 is a graph showing the characteristics of the wire-shaped MoS 2 structure produced in Example 2. FIG.
6 (a) and 6 (b) are transmission electron microscope (TEM) images of a wire-shaped MoS 2 structure section according to the amount of IPA added. Referring to FIG. 6 (a), wires with reduced number of layers and thickness were observed as the amount of IPA added increased. 6 (b), when the addition amount of IPA is 0 ppm, the thickness of the wire is 30 nm or more, 16 ppm, the wire thickness is 11 nm, the thickness is reduced to about 13 layers, It was found that the thickness of the wire was less than 10 nm and decreased to a thickness of about 3 layers, and the distance between the wires was decreased as the amount of IPA was increased.
7 is an SEM image showing nucleation for inducing MoS 2 self-assembly on a substrate in the process of manufacturing a wire-shaped MoS 2 structure according to Example 3. FIG.
Figure 7 (a) shows that the precursor was aggregated in a functionalized area due to oxygen plasma treatment on the substrate. Referring to FIGS. 7 (b) and 7 (c), it can be confirmed that the aggregate of the precursor functions as a nucleus capable of forming a wire-shaped MoS 2 structure by self-assembly, and the wire is self-assembled. The oxygen plasma treatment can be performed on the substrate in a desired position at a desired position, and is subjected to oxygen plasma treatment by positioning using photolithography commonly used in the art.
Fig. 8 shows the results of observing the light transmittance of the wire-shaped MoS 2 structure produced in Example 4. Fig.
8 (a) is an optical image of the wire-shaped MoS 2 structure manufactured in Example 4. FIG. 8 (a), a wire-shaped MoS 2 structure having a wire-to-wire spacing of 5 m (1), 10 m (2) and 40 m (3) It can be seen that both the wire and the quartz substrate have excellent light transmittance. FIG. 8 (b) is a graph showing transmittance and fill factor according to interspace. Referring to FIG. 8 (b), the fill factor is 22%, 11%, and 3%, respectively, when the wire spacing is 5 탆, 10 탆, and 40 탆, respectively, and the light transmittance is 79%, 85% 95%. It was confirmed that the filling factor of the wire and the light transmittance were inversely proportional to each other. The fill factor was calculated as the ratio of the area occupied by MoS 2 in the unit area.
Experimental Example 5: TMD heterostructure in core-shell form (WS 2 / MoS 2 )
9 is a characteristic analysis of the core-shell type WS 2 / MoS 2 heterostructure (WS 2 / MoS 2 ) prepared in Example 5. FIG.
9 (a) and 9 (b) are schematic and optical images of the core-shell type WS 2 / MoS 2 heterostructure produced in Example 5. Referring to Figure 9 (a) and (b), the core-shell type of WS 2 / MoS 2 hetero structure is self-assembled in a self-WS 2 wire (A) and MoS 2 phase formed is assembled on the substrate MoS 2 Core And WS 2 (B) formed in the form of a shell for the substrate.
9C is a Raman shift graph for MoS 2 wire, WS 2 wire and WS 2 / MoS 2 wire in the WS 2 / MoS 2 heterostructure produced in Example 5, and FIG. d) and (e) are TEM images of MoS 2 and WS 2 , respectively.
9 (c), (d), and (e), the WS 2 wire A self-assembled on the substrate has an E 2g mode of 350 cm -1 and an A 1g mode of about 418 cm -1 ), Indicating that the number of stacked WS 2 layers is small. In addition, WS 2 (B), self-assembled on the MoS 2 phase and formed in the form of a shell for the MoS 2 core, exhibits two distinct peaks at 382 cm -1 and 407 cm -1 , which correspond to the E 2 g mode of MoS 2 Corresponds to the A1g mode. Relative Raman intensities of E 2g and A 1g modes of MoS 2 were not significantly different before and after formation of WS 2 including heat treatment. From this, it can be seen that the WS 2 shell with a high sulfur content prevented the MoS 2 core from being damaged during the thermal decomposition of WS 2 .
9 (e) and 9 (f) are TEM images of the cross section of the WS 2 / MoS 2 heterostructure produced in Example 5, and FIG. 9 (g) is a TEM image of the WS 2 / MoS 2 heterostructure PL (photoluminescence) to be. 9 (e), due to the difference in atomic number, WS 2 exhibits a higher image contrast than MoS 2 , and can be used as a pick-up and transfer method or a manual integration method In the manufacturing process of the heterostructure by the conventional method, no interlayer separation which is often observed by the trapped molecules and the residual polymer was observed. In addition, the MoS 2 core (M), the WS 2 shell (W) and their interface (I), which are well aligned from the Fourier transformed image (FFT) Referring to FIG. 9 (f), a spatial defect is observed at the interface between MoS 2 and WS 2 , and referring to FIG. 9 (g), 640 nm (1.94 eV), 860 nm (1.44 eV) eV), three emission peaks were identified. It can be seen that a weak peak at 640 nm appears due to spatial defects at the interface between MoS 2 and WS 2 , that is, interlayer coupling at the incomplete MoS 2 / WS 2 interface.
Experimental Example 6: MoS 2 Analysis of device characteristics with structure
MoS 2 structures were prepared in the same manner as in Example 1 except that IPA was not added (W / O IPA) and IPA was added to produce MoS 2 structures having wire thicknesses of 32 nm and 5 nm, respectively, A field effect transistor in which the wire-shaped MoS 2 structure was applied as a channel was fabricated and the properties thereof were tested.
10 (a) is a graph showing the conductivity (σ = [L / W] x [Id / Vd] of the field effect transistor, L: channel length, W: channel width, Vd: Drain current) versus gate voltage (Vg) curve. Here, an electrolyte providing appropriate gate characteristics by conformal contact with the wire surface was used as a gate insulator. 10 (a), a MoS 2 structure composed of a thick wire having a thickness (t = 32 nm) exhibits a symmetrical ambipolar conduction characteristic while a MoS 2 layer having a thickness (t = 5 nm) The structure showed unipolar n-type characteristics.
10 (b) is a graph showing the effective electron mobility (μ FET ) according to the wire thickness of the wire-shaped MoS 2 structure. Referring to FIG. 10 (b), when the thickness of the wire is 5 nm, when the effective electron mobility is 7
FIGS. 10 (c) and 10 (d) show a field effect transistor in which MLG (multilayered graphene) is applied as a source / drain electrode so as to exhibit high light transmittance and mechanical flexibility. Referring to FIGS. 10 (c) and 10 (d), the number of nucleation seeds can be controlled by controlling the number of word lines between the channels, and the light transmittance of the field effect transistor is 78% .
FIG. 10E is a graph of a current vs. voltage at a small bias in the field effect transistor (I DS -V DS ). 10E, when the number of wires is 15 in a small bias (0.5V, 1V, 1.5V, and 2V), the current and the voltage exhibit a linear proportional relationship, from which wire and multilayer graphene It can be seen that this is a quasi-ohmic contact.
10 (f) is a graph of current vs. voltage according to the number of wires in the field-effect transistor (I DS -V DS ). Referring to (f) of FIG. 10, as the number of wires increases (3, 7 and 15), the currents to the same voltage increase, so that the output current can be controlled by adjusting the number of wires have.
10 (g) is a graph showing the number distribution according to the mobility of the field effect transistor. Referring to FIG. 10 (g), the average effective electron mobility (μFET) of the 42 field effect transistors formed on one substrate is 45
The average effective mobility (μFET) of the 42 devices fabricated on one device substrate was about 45
10 (h) is a graph showing results of bending and twisting experiments of the field-effect transistor. The PET substrate on which the field-effect transistor with the wire-shaped MoS2 structure was formed was bent to a radius of curvature (strain: 0.8%) of 20 mm in the direction perpendicular to the channel length. Referring to FIG. 10 (h), the transistor stably operated after bending and twisting (maximum twist angle: 30). Thus, it can be seen that the wire-shaped MoS 2 structure is suitable for applications requiring high mechanical properties such as flexible electronic devices.
As described above, the method of preparing the transition metal chalcogenide structure according to the present invention facilitates control of the concentration, pH and drying rate of the precursor solution during the production process, and can appropriately control the shape of the transitional metal chalcogenide structure can do. Accordingly, it can be confirmed that the transition metal chalcogenide structure having a controlled form depending on the application can be widely applied to various devices.
It will be apparent to those skilled in the art that the present invention is not limited to the embodiments described above and that various changes and modifications may be made without departing from the spirit and scope of the present invention as defined by the appended claims. As shown in FIG.
It will be understood by those skilled in the art that the present invention may be embodied in many other specific forms without departing from the spirit or scope of the invention as defined by the appended claims and their equivalents. .
Claims (23)
(B) immersing the substrate in a pH-adjusted TMD precursor aqueous solution; And
(C) drying the TMD precursor aqueous solution coated on the substrate to induce self-assembly of the TMD,
And the drying rate is controlled in the step (C) to prepare various types of transition metal chalcogenide structures,
When the drying rate is 0.5 to 1.2 nl / s, a dendritic transition metal chalcogenide structure is prepared,
Wherein the transition metal chalcogenide structure in wire form is prepared when the drying rate is from 1.2 to 2 nl / s.
(B) immersing the substrate in a pH-adjusted first TMD precursor aqueous solution;
(C) drying the first TMD precursor aqueous solution coated on the substrate to induce self-assembly of the first TMD;
(D) immersing the self-assembled first TMD structure in a second transition metal chalcogenide (TMD) precursor aqueous solution; And
(E) drying the second TMD precursor aqueous solution coated on the first TMD structure to induce self-assembly of the second TMD,
And the drying rate is controlled in the step (C) to prepare various types of transition metal chalcogenide heterostructures,
When the drying rate is 0.5 to 1.2 nl / s, a transition metal chalcogenide heterostructure in the form of dendrites is prepared,
Wherein the transition metal chalcogenide heterostructure in the form of a wire is produced when the drying rate is 1.2 to 2 nl / s.
Wherein the first and second transition metal chalcogenide precursors are different. ≪ RTI ID = 0.0 > 11. < / RTI >
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| KR20200056694A (en) | 2018-11-15 | 2020-05-25 | (주)아모레퍼시픽 | Composition for maintaining titer of antioxidants comprising functionalized transition metal dichalcogenides |
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