KR101360997B1 - Preparing method of chacogenide metal thin film - Google Patents

Abstract

The present application relates to a method for producing a metal chalcogenide thin film, a method for transferring a metal chalcogenide thin film and a metal chalcogenide thin film produced by the production method.

Description

Manufacturing method of metal chalcogenide thin film {PREPARING METHOD OF CHACOGENIDE METAL THIN FILM}

The present application relates to a method for producing a metal chalcogenide thin film, a method for transferring a metal chalcogenide thin film and a metal chalcogenide thin film produced by the production method.

Chalcogenide materials are materials that generally contain one or more additional elements that act to modify chalcogen elements and electrical or structural properties. In recent years, chalcogenide materials have been applied in various manufacturing fields such as light emitting devices, photodetectors, catalysts, chemical sensors, biological markers, and nonlinear optical materials. Chalcogenide materials have been widely studied for applications in various fields of manufacture because of their wide bandgap properties and the potential for providing short wavelength light emission. US Patent No. 6,875,661 and US Patent Publication No. 2005/0009225 disclose solution deposition of metal chalcogenide films using precursor solutions comprising metal chalcogenide and hydrazine compounds. Here, soluble chalcogenide hydrazinium salts are prepared to form thin films by spin coating. However, such chalcogenide hydrazinium salts are chemically unstable and have a problem of deteriorating long-term stability of the solution, which makes it difficult to apply them to actual device manufacturing lines.

The present application provides a method for producing a metal chalcogenide thin film, a method for transferring a metal chalcogenide thin film and a metal chalcogenide thin film manufactured by the method.

However, the problem to be solved by the present application is not limited to the above-mentioned problem, and other problems not mentioned will be clearly understood by those skilled in the art from the following description.

A first aspect of the present disclosure can provide a method for producing a metal chalcogenide thin film, comprising:

Forming a metal thin film on the substrate;

Supplying a chalcogen atom-containing gas onto the metal thin film; And

Reacting the metal and the chalcogen atom-containing gas to form a metal chalcogenide thin film represented by Formula 1 below:

[Formula 1]

M _a X _b

Wherein M = Mo, W, Bi, Mg, Al, Si, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, Sr, Y, Zr, Nb, Tc, Ru, Rh, Pd, Ag, Cd, In Sn, Sb, Ba, La, Hf, Ta, Re, Os, Ir, Pt, Au, Hg, Tl, Pb, or Po And X = S, Se, or Te, and a and b are each independently integers of 1 to 3.

The second aspect of the present application can provide a metal chalcogenide thin film, which is produced by the manufacturing method according to the first aspect of the present application.

A third aspect of the present disclosure may provide a device, comprising a metal chalcogenide thin film according to the second aspect of the present disclosure.

A fourth aspect of the present disclosure can provide a method of transferring a metal chalcogenide thin film, comprising:

Forming a metal thin film on the substrate;

Supplying a chalcogen atom-containing gas onto the metal thin film;

Reacting the metal and the chalcogen atom-containing gas to form a metal chalcogenide thin film represented by Formula 1 below;

Separating the metal chalcogenide thin film by removing the substrate and the metal thin film; And

Transferring the separated metal chalcogenide thin film onto a target substrate

Including, the method of transferring the metal chalcogenide thin film:

[Formula 1]

M _a X _b

Wherein M = Mo, W, Bi, Mg, Al, Si, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, Sr, Y, Zr, Nb , Tc, Ru, Rh, Pd, Ag, Cd, In Sn, Sb, Ba, La, Hf, Ta, Re, Os, Ir, Pt, Au, Hg, Tl, Pb, or Po And X = S, Se, or Te, and a and b are each independently integers of 1 to 3.

A fifth aspect of the present disclosure can provide a metal chalcogenide thin film laminate comprising a single or multiple layers of the metal chalcogenide thin film according to the second aspect of the present application.

According to the present application, the metal chalcogenide thin film may be easily manufactured using the chemical vapor deposition method, and the metal chalcogenide thin film may be formed from the single layer to the multilayer using the chemical vapor deposition method. In addition, the metal chalcogenide thin film of the present application can be applied to various applications such as a field effect transistor, an optical sensor, a light emitting device, a photodetector, a magneto-optical memory device, a photocatalyst, a flat panel display, a flexible device, and a solar cell.

1 is a process chart showing a method of manufacturing a metal chalcogenide thin film according to an embodiment of the present application.
2 is a process chart showing a method of transferring a metal chalcogenide thin film according to an embodiment of the present application.
Figure 3 is a photograph of the equipment used for the production of metal chalcogenide thin film according to an embodiment of the present application.
Figure 4 shows the manufacturing process of the metal chalcogenide thin film according to an embodiment of the present application.
FIG. 5 shows a binary phase diagram of a Mo-S system according to one embodiment of the present disclosure.
Figure 6 shows an optical microscope image (a) and Raman mapping image (b) of the MoS ₂ thin film according to an embodiment of the present application.
7 is a graph (a) showing the average spectrum of the MoS ₂ thin film according to an embodiment of the present application and a graph (b) showing uniformity.
Figure 8 shows the optical microscope image (a) and Raman mapping image (b) of the MoS ₂ thin film after the injection of a small amount of gas on the MoS ₂ thin film according to an embodiment of the present application.
9 is a graph (a) showing the average spectrum of the MoS ₂ thin film and a graph (b) showing the uniformity after the injection of a small amount of gas on the MoS ₂ thin film according to an embodiment of the present application.
10 is an optical microscope image showing a specific position of the MoS ₂ thin film for measuring the uniformity of the MoS ₂ thin film according to an embodiment of the present application.
11 is a graph (b) showing an optical microscope image (a) and spectrum of a MoS ₂ thin film according to an embodiment of the present application.
12 is a graph (b) showing an optical microscope image (a) and spectrum of a MoS ₂ thin film according to an embodiment of the present application.
13 is a process chart showing the transfer process of the metal chalcogenide thin film according to an embodiment of the present application.

Hereinafter, embodiments and examples of the present invention will be described in detail with reference to the accompanying drawings, which will be readily apparent to those skilled in the art to which the present invention pertains.

It should be understood, however, that the present invention may be embodied in many different forms and is not limited to the embodiments and examples described herein. In order to clearly illustrate the present invention, parts not related to the description are omitted, and similar parts are denoted by like reference characters throughout the specification.

Throughout this specification, when a part is referred to as being "connected" to another part, it is not limited to a case where it is "directly connected" but also includes the case where it is "electrically connected" do.

Throughout this specification, when a member is located "on" another member, this includes not only when one member is in contact with another member but also when another member exists between the two members.

Throughout this specification, when an element is referred to as "including " an element, it is understood that the element may include other elements as well, without departing from the other elements unless specifically stated otherwise.

As used herein, the terms "about," " substantially, "and the like are used herein to refer to or approximate the numerical value of manufacturing and material tolerances inherent in the stated sense, Accurate or absolute numbers are used to prevent unauthorized exploitation by unauthorized intruders of the mentioned disclosure. Also, throughout the present specification, the phrase " step "or" step "does not mean" step for.

Throughout this specification, the term "combination of these" included in the expression of the makushi form means one or more mixtures or combinations selected from the group consisting of constituents described in the expression of the makushi form, wherein the constituents It means to include one or more selected from the group consisting of.

Hereinafter, a method of manufacturing the metal chalcogenide thin film of the present application, a method of transferring the metal chalcogenide thin film and the metal chalcogenide thin film by the above-described manufacturing method will be described in detail with reference to embodiments, examples, and drawings. However, the present invention is not limited to these embodiments and examples and drawings.

A first aspect of the present disclosure can provide a method for producing a metal chalcogenide thin film, comprising:

Forming a metal thin film on the substrate;

Supplying a chalcogen atom-containing gas onto the metal thin film; And

Reacting the metal and the chalcogen atom-containing gas to form a metal chalcogenide thin film represented by Formula 1 below:

[Formula 1]

M _a X _b

Wherein M = Mo, W, Bi, Mg, Al, Si, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, Sr, Y, Zr, Nb, Tc, Ru, Rh, Pd, Ag, Cd, In Sn, Sb, Ba, La, Hf, Ta, Re, Os, Ir, Pt, Au, Hg, Tl, Pb, or Po And X = S, Se, or Te, and a and b are each independently integers of 1 to 3.

1 is a process chart showing a method of manufacturing a metal chalcogenide thin film according to an embodiment of the present application.

First, as shown in FIG. 1A, the metal thin film 20 may be formed on the substrate 10.

According to one embodiment of the present application, the substrate 10 is Si, SiO ₂ , Ge, GaN, AlN, GaP, InP, GaAs, SiC, Al ₂ O ₃ , LiAlO ₃ , MgO, glass, quartz, sapphire, graphite , But may be selected from the group consisting of graphene and combinations thereof, but is not limited thereto.

According to one embodiment of the present application, the metal thin film 20 is Mo, W, Bi, Mg, Al, Si, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga , Ge, Sr, Y, Zr, Nb, Tc, Ru, Rh, Pd, Ag, Cd, In Sn, Sb, Ba, La, Hf, Ta, Re, Os, Ir, Pt, Au, Hg, Tl, Pb, Po And combinations thereof, but is not limited thereto.

According to the exemplary embodiment of the present application, the metal thin film 20 may be sputtered, E-beam evaporator, thermal evaporation, ion cluster beam, or pulsed laser deposition. laser deposition (PLD) method and combinations thereof may be formed on the substrate by a method selected from the group consisting of, but is not limited thereto.

Subsequently, as shown in FIG. 1B, the chalcogen atom-containing gas may be supplied onto the metal thin film 20 to form the metal chalcogenide thin film 30.

According to one embodiment of the present application, the chalcogen atom-containing gas may be selected from the group consisting of S ₂ , Se ₂ , Te ₂ , H ₂ S, H ₂ Se, H ₂ Te, and combinations thereof. However, the present invention is not limited thereto.

The metal thin film 20 and the chalcogen atom-containing gas react on the metal thin film 20 by the supply of the chalcogen atom-containing gas such that M _a X _b (wherein, M = Mo, W , Bi, Mg, Al, Si, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, Sr, Y, Zr, Nb, Tc, Ru, Rh, Pd Ag, Cd, In Sn, Sb, Ba, La, Hf, Ta, Re, Os, Ir, Pt, Au, Hg, Tl, Pb, or Po , X = S, Se, or Te, and a and b are each independently integers of 1 to 3, and a metal chalcogenide thin film 30 represented by the chemical formula of Formula 1 may be formed.

According to an embodiment of the present disclosure, the reaction temperature at which the metal thin film 20 and the chalcogen atom-containing gas react is about 20 ° C. to about 1,800 ° C., about 100 ° C. to about 1,700 ° C., about 200 ° C. to about 1,600 ° C, about 300 ° C to about 1,500 ° C, about 400 ° C to about 1,400 ° C, about 500 ° C to about 1,300 ° C, about 600 ° C to about 1,200 ° C, about 700 ° C to about 1,100 ° C, about 800 ° C to about 1,000 ° C, About 900 ° C. to about 1,000 ° C., about 400 ° C. to about 1,800 ° C., about 400 ° C. to about 1,700 ° C., about 400 ° C. to about 1,500 ° C., about 400 ° C. to about 1,300 ° C., about 400 ° C. to about 1,000 ° C., about 500 ℃ to about 1,700 ℃, about 500 ℃ to about 1,500 ℃, about 500 ℃ to about 1,300 ℃, about 500 ℃ to about 1000 ℃, about 100 ℃ to about 1,800 ℃, about 100 ℃ to about 1,700 ℃ or about 100 ℃ It may be about 1,600 ℃, but is not limited thereto.

The metal chalcogenide thin film 30 may be further formed by forming a metal chalcogenide thin film by adjusting the appropriate number of layers according to a use to form a sulfide chalcogenide laminate (not shown) stacked in multiple layers. Specifically, in the method for producing a sulfide chalcogenide laminate laminated in multiple layers of the metal chalcogenide thin film 30 according to the present application, the chalcogen atom-containing gas is supplied onto the metal chalcogenide thin film By further forming the additional metal chalcogenide thin film one or more times, the number or thickness of the metal chalcogenide thin film can be easily adjusted.

The metal chalcogenide thin film laminated in multiple layers may have a thickness ranging from about 1 layer to about 100 layers, which is a single layer of metal chalcogenide thin film, but is not limited thereto.

The second aspect of the present application may provide a metal chalcogenide thin film, which is prepared by the method according to the first aspect of the present application.

According to one embodiment of the present application, the metal chalcogenide thin film may be stacked to include about 1 layer to about 100 metal chalcogenide thin films, but is not limited thereto.

The third aspect of the present application can provide a device, comprising a metal chalcogenide thin film according to the second aspect of the present application.

The metal chalcogenide thin film can be utilized in various applications. When the metal chalcogenide thin film is utilized as a semiconductor layer, it becomes possible to manufacture a field effect transistor, an optical sensor, a light emitting element, a photodetector, a magneto-optical memory element, a photocatalyst, a flat panel display, a flexible element, a solar cell, and the like.

A fourth aspect of the present disclosure can provide a method of transferring a metal chalcogenide thin film, comprising:

Forming a metal thin film on the substrate;

Supplying a chalcogen atom-containing gas onto the metal thin film;

Reacting the metal and the chalcogen atom-containing gas to form a metal chalcogenide thin film represented by Formula 1 below;

Separating the metal chalcogenide thin film by removing the substrate and the metal thin film; And

Transferring the separated metal chalcogenide thin film onto a target substrate:

 [Formula 1]

M _a X _b

Wherein M = Mo, W, Bi, Mg, Al, Si, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, Sr, Y, Zr, Nb, Tc, Ru, Rh, Pd, Ag, Cd, In Sn, Sb, Ba, La, Hf, Ta, Re, Os, Ir, Pt, Au, Hg, Tl, Pb, or Po And X = S, Se, or Te, and a and b are each independently integers of 1 to 3.

2 is a process chart showing a method of manufacturing a metal chalcogenide thin film according to an embodiment of the present application.

First, as illustrated in FIG. 2A, the metal thin film 20 may be formed on the substrate 10.

According to one embodiment of the present application, the substrate 10 is Si, SiO ₂ , Ge, GaN, AlN, GaP, InP, GaAs, SiC, Al ₂ O ₃ , LiAlO ₃ , MgO, glass, quartz, sapphire, graphite , But may be selected from the group consisting of graphene and combinations thereof, but is not limited thereto.

According to one embodiment of the present application, the metal thin film 20 is Mo, W, Bi, Mg, Al, Si, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga , Ge, Sr, Y, Zr, Nb, Tc, Ru, Rh, Pd, Ag, Cd, In Sn, Sb, Ba, La, Hf, Ta, Re, Os, Ir, Pt, Au, Hg, Tl, It may include one selected from the group consisting of Pb, Po and combinations thereof, but is not limited thereto. According to the exemplary embodiment of the present application, the metal thin film 20 may be sputtered, E-beam evaporator, thermal evaporation, ion cluster beam, or pulsed laser deposition. laser deposition (PLD) method and combinations thereof may be formed by a method selected from the group consisting of, but is not limited thereto.

Subsequently, as shown in FIG. 2 (b), the chalcogen atom-containing gas is supplied onto the metal thin film 20 to supply the chalcogen atom-containing gas to the metal and the chalcogen atom-based gas. The containing gas reacts with M _a X _b (wherein M = Mo, W, Bi, Mg, Al, Si, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, Sr, Y, Zr, Nb, Tc, Ru, Rh, Pd, Ag, Cd, In Sn, Sb, Ba, La, Hf, Ta, Re, Os, Ir, Pt, Au, Hg, Tl , Pb, or Po , X = S, Se, or Te, and a and b are each independently integers of 1 to 3, and a metal chalcogenide thin film 30 represented by the chemical formula of Formula 1 may be formed. The chalcogen atom-containing gas may be selected from, for example, S ₂ , Se ₂ , Te ₂ , H ₂ S, H ₂ Se, H ₂ Te, and combinations thereof, but is not limited thereto. It is not.

According to an embodiment of the present disclosure, the reaction temperature at which the metal thin film 20 and the chalcogen atom-containing gas react is about 20 ° C. to about 1,800 ° C., about 100 ° C. to about 1,700 ° C., about 200 ° C. to about 1,600 ° C, about 300 ° C to about 1,500 ° C, about 400 ° C to about 1,400 ° C, about 500 ° C to about 1,300 ° C, about 600 ° C to about 1,200 ° C, about 700 ° C to about 1,100 ° C, about 800 ° C to about 1,000 ° C, About 900 ° C. to about 1,000 ° C., about 400 ° C. to about 1,800 ° C., about 400 ° C. to about 1,700 ° C., about 400 ° C. to about 1,500 ° C., about 400 ° C. to about 1,300 ° C., about 400 ° C. to about 1,000 ° C., about 500 ℃ to about 1,700 ℃, about 500 ℃ to about 1,500 ℃, about 500 ℃ to about 1,300 ℃, about 500 ℃ to about 1000 ℃, about 100 ℃ to about 1,800 ℃, about 100 ℃ to about 1,700 ℃ or about 100 ℃ It may be about 1,600 ℃, but is not limited thereto.

Then, as shown in Fig. 2 (c) Likewise, the polymer support layer 40 may be formed on the metal chalcogenide thin film 30.

In order to apply the metal chalcogenide thin film 30 to the device to be finally applied, it may be necessary to remove the metal thin film 20. The metal thin film 20 is removed by an etching method such as wet or dry. For example, in the case of wet etching, the metal thin film 20 is removed by reacting with an acid which is an etchant. In the process of removing the metal thin film 20, the metal chalcogenide thin film 30 may be damaged. Thus, the polymer support layer 40 may be formed to protect the metal chalcogenide thin film 30 from the etching process.

The polymer support layer 40 may include polymethylmethacrylate (PMMA), polydimethylsiloxanes (PDMS), polyvinylalcohol (PVA), polyvinyl chloride (PVC), polycarbonate (polycarbonate; PC), polytetrafluoroethylene (PTFE), benzylmetha-acrylate (benzylmetha-acrylate), heat-peelable tape, UV peeling tape, and combinations thereof. However, it is not limited thereto.

Subsequently, as illustrated in FIG. 2 (d), the metal chalcogenide thin film 30 may be separated by removing the metal thin film 20. Removal of the metal thin film 20 may include, for example, reactive ion etching (RIE), inductively coupled plasma RIE (ICP-RIE), electron cyclotron resonance RIE (ECR-RIE), reactive ion beam etching (RIBE), or CAIBE. dry etching using an etching apparatus such as (chemical assistant ion beam etching); Potassium hydroxide (KOH), tetra methyl ammonium hydroxide (TMAH), ethylene diamine pyrocatechol (EDP), burred red oxide etch (BOE), FeCl ₃ , Fe (NO ₃ ) ₃ , HF, H ₂ SO ₄ , HNO ₃ , HPO ₄ Wet etching with etchants such as, HCL, NaF, KF, NH ₄ F, AlF ₃ , NaHF ₂ , KHF ₂ , NH ₄ HF ₂ , HBF ₄ and NH ₄ BF ₄ ; Or a chemical mechanical polishing process using an oxide etchant.

Subsequently, as shown in FIG. 2E, the metal chalcogenide thin film 30 and the polymer support layer 40 may be formed on the target substrate 50 by being transferred. The target substrate 50 may be one selected from the group consisting of glass, quartz, sapphire, SiC, MgO, plastic, ceramic, rubber, and combinations thereof, as the substrate of various materials, but is not limited thereto. no.

According to one embodiment of the present application, the target substrate 50 may be a transparent substrate, a flexible substrate, or a transparent flexible substrate, but is not limited thereto. Specifically, the target substrate may be, for example, a transparent inorganic substrate such as glass, quartz, sapphire, SiC, MgO, polyethylene terephthalate (PET), polystyrene (PS), polyimide (PI), polyvinyl chloride (PVC). ), Transparent flexible organic substrates such as polyvinylpyrrolidone (PVP) and polyethylene (PE) or Si, Ge, GaAs, InP, InSb, InAs, AlAs, AlSb, CdTe, ZnTe, ZnS, CdSe, CdSb, GaP Base materials, such as these, can be used. When a plastic substrate such as PET is used as a substrate for a device, an electronic device can be manufactured as a flexible device.

Subsequently, as illustrated in FIG. 2F, the polymer support layer 40 formed on the metal chalcogenide thin film 30 may be removed. After the transfer process of the metal chalcogenide thin film 30 to the target substrate 50, the metal chalcogenide thin film 30 to protect the metal chalcogenide thin film 30 during the etching process of the metal chalcogenide thin film 20 The polymer support layer 40 formed on the chalcogenide thin film 30 may be removed by acetone or the like.

All of the contents described with respect to the method according to the first aspect of the present application can be applied to the second to the fourth aspect of the present application, and duplicate description thereof is omitted for convenience.

Hereinafter, the present invention will be described in more detail with reference to the following examples. However, the following examples are for illustrative purposes only and are not intended to limit the scope of the present invention.

[ Example  One]

3 nm of metal Mo was deposited on an Si / SiO ₂ substrate using an e-beam evaporation method using the equipment shown in FIG. 3. Then, as shown in FIG. 4, H ₂ S was injected at a temperature of about 750 ° C. for 1 hour and quenched in an argon atmosphere to form a MoS ₂ layer. The binary phase diagram of Mo-S is shown in FIG. 5. 5 is a two-phase state diagram of Mo and S; The region where MoS ₂ is formed by CVD is shown on the display FIG. 5. It can be seen that Mo and MoS ₂ are produced when the temperature ranges from about 0 ° C. to about 550 ° C. and the S content is about 65% or less. In addition, when the temperature ranges from about 444.6 ° C. to about 1750 ± 50 ° C., and the S content is about 70% or more, MoS ₂ and 1 atm of gas are generated. Here, the S content refers to the S atom content when the Mo atom and the entire S atom are 100%. An average of about 5 layers of MoS ₂ layers formed were observed (see FIG. 7 below).

6 (a) is an optical micrograph of the substrate and MoS ₂ , with a small portion in the upper left corner showing the substrate surface. MoS ₂ White cracks on the surface were observed, in order to confirm the cracks, the MoS ₂ Raman mapping images of the surface (FIG. 6 (b)) were analyzed. MoS ₂ of FIG. 6 (a) White cracks on the surface were also observed in FIG. 6 (b). The upper surface of the substrate was black because no peak was detected at all, and the crack on the MoS ₂ surface had a color difference but the peak was detected. It was confirmed that it was formed obscured.

7 (a) is Atom of MoS ₂ as the distance between the E ¹ _2g peak and the A ¹ _1g peak as shown in the average spectra of FIG. 6 (b) The number of floors can be estimated. As shown in Fig. 7A, the peaks were clearly observed even in the cracked portion. 7B is References (Source C.Lee ACS Nano , 4 (5), 2695 , (2011)) is a graph showing the uniformity of MoS ₂ thin film. Referring to FIG. 7B, the distance between the E ¹ _2g peak and the A ¹ _1g peak is about 24.5 cm ⁻¹ , representing atoms of MoS ₂ . It can be assumed that the floor is five floors. The rectangle in Fig. 7 (b) is the peak position of E ¹ _2g and the triangle shows the peak position of A ¹ _1g (left scale). Red color indicates the distance between peaks (right scale).

Figure 8, even if after injecting the H ₂ S gas in a very small amount on the MoS ₂ thin film shows a light microscopy image of (a) and Raman mapping image (b) of MoS ₂ thin film, injecting the H ₂ S gas in a very small amount Uniform cracks were formed as shown in FIG. 8. Fig. 8 (a) The upper part represents the substrate surface and the lower part is MoS ₂ A thin film is shown (synthesis condition H2S 1sccm, 10 min). The red square means the position measured in FIG. 8 (b). Of Fig. 8 (b) The part shown in black represents the substrate surface, and the yellow part represents the MoS ₂ thin film. It can be assumed that the MoS ₂ thin film is formed uniformly from the peaks appearing evenly.

Figure 9 (a) shows the average spectra of Figure 8 (b), the atom of MoS ₂ as the distance between the E ¹ _2g peak and the A ¹ _1g peak The number of floors can be estimated. 9 (b) is a reference (Source C.Lee ACS). Nano , 4 (5), 2695 , (2011)) is a graph showing the uniformity of MoS ₂ thin film. Figure 9 (b) the reference time, the distance is about 22 cm between the E ^{1 1} A _{1g 2g} peak and ^{peak-as 1} atom of MoS ₂ It can be assumed that the layer is two layers. The square in Fig. 9B shows the peak position of E ¹ _2g and the triangle shows the peak position of A ¹ _1g (left scale). Red color indicates the distance between peaks (right scale).

10 is a light microscope image showing a location (position) of MoS ₂ thin film for the uniformity measurement of MoS ₂ thin film. The distance between the E ¹ _2g peak and the A ¹ _1g peak was measured at any three points with the specimen as shown in FIG. 6. The distance between the peaks for each point shown in FIGS. 10 (a) (sample 1) and 10 (b) (sample 2) is shown in Table 1 below.

In terms of uniformity, the distance between the peaks was reproducible with the second sample in two layers. Therefore, it can be seen that by applying the chemical vapor deposition method according to the present embodiment, it is possible to grow on a thin film. The synthesized samples can be used for FETs.

[ Example  2]

H ₂ S was injected for 15 minutes in a Mo foil at a temperature of 750 ° C. to form a MoS ₂ layer. Figure 11 (a) is an optical micrograph of the MoS ₂ sample. Near the right side, purple is the substrate surface. It can be seen that the MoS ₂ formed was significantly affected by the surface state of the Mo foil. The red cross mark on Fig. 11 (a) indicates a point that is assumed to be the thinnest layer. The red cross-marked portion was measured in Raman and shown in FIG. 11 (b). 23.5 cm distance between E ¹ and A ¹ _{1g 2g} peak peak ^- a ^1, it is possible to estimate that the Figure 7 (b) or even when the reference 9 (b), the MoS ₂ is formed on the third floor.

12 (a) is also an optical micrograph of the MoS ₂ sample. The red cross mark on FIG. 12 (a) indicates the point that is assumed to be the thinnest layer. The red cross marked portion was measured in Raman and shown in FIG. 12 (b). The distance of about 22 cm between E ¹ and A ¹ _{1g 2g} peak peak ^- a ^1, it is possible to estimate that the Figure 7 (b) or even when the reference 9 (b), the formed MoS ₂ is a double-layer.

[ Example  3]

13 shows a transfer process of a metal chalcogenide thin film It is a process chart. 3 nm of metal Mo was deposited on an Si / SiO ₂ substrate using an e-beam evaporation method. next, As shown in FIG. 13, H ₂ S was injected for 15 minutes at a temperature of 750 ° C. to form a MoS ₂ layer. PMMA was coated on the MoS ₂ layer as a polymer support layer, and the MoS ₂ layer was separated by etching the Mo layer and the substrate SiO ₂ using a KOH solution (˜15 M). The separated MoS ₂ layer / PMMA layer was transferred onto the target substrate. After transfer, the PMMA layer was removed using acetone.

Hereinbefore, the present invention has been described in detail with reference to the embodiments and examples, but the present invention is not limited to the above embodiments and embodiments, and may be modified in various forms, and is commonly used in the art within the technical spirit of the present application. It is evident that many variations are possible by those of skill in the art.

Claims (15)

Forming a metal thin film on the substrate;
Supplying a chalcogen atom-containing gas onto the metal thin film; And
Reacting the metal and the chalcogen atom-containing gas to form a metal chalcogenide thin film represented by Chemical Formula 1
In the, Method for producing a metal chalcogenide thin film,
The metal thin film is Mo, W, Bi, Mg, Al, Si, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, Sr, Y, Zr, Nb, Tc, Ru, Rh, Pd, Ag, Cd, In Sn, Sb, Ba, La, Hf, Ta, Re, Os, Ir, Pt, Au, Hg, Tl, Pb, Po, and combinations thereof It includes what is selected from the group,
Wherein the chalcogen atom-containing gas comprises one selected from the group consisting of S ₂ , Se ₂ , Te ₂ , H ₂ S, H ₂ Se, H ₂ Te, and combinations thereof.
Method for producing a metal chalcogenide thin film.
[Chemical Formula 1]
M _a X _b
Wherein M = Mo, W, Bi, Mg, Al, Si, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, Sr, Y, Zr, Nb, Tc, Ru, Rh, Pd, Ag, Cd, In Sn, Sb, Ba, La, Hf, Ta, Re, Os, Ir, Pt, Au, Hg, Tl, Pb, or Po And X = S, Se, or Te, and a and b are each independently integers of 1 to 3.
delete The method of claim 1,
The metal thin film may be formed by a sputtering method, an E-beam evaporator method, a thermal evaporation method, an ion cluster beam, a pulsed laser deposition (PLD) method, and combinations thereof. Formed by a method selected from the group consisting of, a metal chalcogenide thin film manufacturing method.
delete The method of claim 1,
And supplying a chalcogen atom-containing gas onto the metal chalcogenide thin film to form the metal chalcogenide thin film at least once.
The method of claim 1,
The substrate is a group consisting of Si, SiO ₂ , Ge, GaN, AlN, GaP, InP, GaAs, SiC, Al ₂ O ₃ , LiAlO ₃ , MgO, glass, quartz, sapphire, graphite, graphene and combinations thereof Including the one selected from, Metal chalcogenide thin film manufacturing method.
A metal chalcogenide thin film prepared by the method according to any one of claims 1, 3, 5, and 6.
Device comprising a metal chalcogenide thin film according to claim 7.
Forming a metal thin film on the substrate;
Supplying a chalcogen atom-containing gas onto the metal thin film;
Reacting the metal and the chalcogen atom-containing gas to form a metal chalcogenide thin film represented by Formula 1 below;
After forming the metal chalcogenide metal thin film, forming a polymer support layer on the metal chalcogenide thin film;
Separating the metal chalcogenide thin film on which the polymer support layer is formed by removing the substrate and the metal thin film; And
Transferring the thin metal chalcogenide thin film on which the separated polymer support layer is formed on a target substrate;
Including, the method of transferring the metal chalcogenide thin film:
[Chemical Formula 1]
M _a X _b
Wherein M = Mo, W, Bi, Mg, Al, Si, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, Sr, Y, Zr, Nb, Tc, Ru, Rh, Pd, Ag, Cd, In Sn, Sb, Ba, La, Hf, Ta, Re, Os, Ir, Pt, Au, Hg, Tl, Pb, or Po And X = S, Se, or Te, and a and b are each independently integers of 1 to 3.
delete The method of claim 9,
And after removing the metal chalcogenide thin film on which the polymer support layer is formed on the target substrate, removing the polymer support layer.
The method of claim 9,
The polymer support layer may include polymethylmethacrylate (PMMA), polydimethylsiloxanes (PDMS), polyvinylalcohol (PVA), polyvinyl chloride (PVC), polycarbonate; PC), polytetrafluoroethylene (PTFE), benzylmetha-acrylate (benzylmetha-acrylate), heat peeling tape, UV peeling tape and metal knife, including those selected from the group consisting of Transfer method of cogenide thin film.
The method of claim 9,
The substrate is a group consisting of Si, SiO ₂ , Ge, GaN, AlN, GaP, InP, GaAs, SiC, Al ₂ O ₃ , LiAlO ₃ , MgO, glass, quartz, sapphire, graphite, graphene and combinations thereof Transfer method of a metal chalcogenide thin film, comprising the one selected from.
The method of claim 9,
The object substrate is glass, quartz, sapphire, SiC, MgO, plastics, ceramics, rubber, and combinations thereof will be selected from the group consisting of, metal chalcogenide thin film transfer method.
A metal chalcogenide thin film laminate comprising the metal chalcogenide thin film according to claim 7 as a singular or plural layer.

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