KR101770235B1 - Preparing method of two-dimensional transition metal dichalcogenide - Google Patents

Preparing method of two-dimensional transition metal dichalcogenide Download PDF

Info

Publication number
KR101770235B1
KR101770235B1 KR1020150107443A KR20150107443A KR101770235B1 KR 101770235 B1 KR101770235 B1 KR 101770235B1 KR 1020150107443 A KR1020150107443 A KR 1020150107443A KR 20150107443 A KR20150107443 A KR 20150107443A KR 101770235 B1 KR101770235 B1 KR 101770235B1
Authority
KR
South Korea
Prior art keywords
transition metal
containing precursor
mos
dimensional
chalcogen
Prior art date
Application number
KR1020150107443A
Other languages
Korean (ko)
Other versions
KR20170014319A (en
Inventor
강상우
송재용
김태성
문지훈
Original Assignee
한국표준과학연구원
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 한국표준과학연구원 filed Critical 한국표준과학연구원
Priority to KR1020150107443A priority Critical patent/KR101770235B1/en
Priority claimed from JP2017561638A external-priority patent/JP2018525516A/en
Publication of KR20170014319A publication Critical patent/KR20170014319A/en
Application granted granted Critical
Publication of KR101770235B1 publication Critical patent/KR101770235B1/en

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00Sulfur; Compounds thereof
    • C01B17/20Methods for preparing sulfides or polysulfides, in general
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00Compounds of molybdenum
    • C01G39/06Sulfides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/80Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/04Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM

Abstract

The present invention relates to a method for producing a two-dimensional transition metal decalcogenide.

Description

TECHNICAL FIELD [0001] The present invention relates to a method for producing a two-dimensional transition metal dicalcogenide,

The present invention relates to a process for preparing a two-dimensional transition metal decalcogenide.

Various studies have shown that graphene is a promising candidate material that can replace materials used in conventional electronic devices. Despite the excellent properties of high electron mobility, elasticity, thermal conductivity and flexibility, graphene is suitable for transistors and optical devices due to the lack of bandgap (0 eV for pure graphenes) not. Molybdenum disulfide (MoS 2 ), which is a laminated structure material agglomerated by covalent bonds and interlaminar van der Waals forces of one molybdenum atom located between two sulfur atoms, has an adjustable band gap [1.2 eV (Direct bandgap of 1.8 eV (single layer) from the bandgap] and peripheral stability.

The fabrication of the MoS 2 monolayer was first attempted by a micromechanical exfoliation method similar to the approach used for the fabrication of graphene, and its applicability as a channel material for a field effect transistor (FET) . Since the study of improving the electrical properties of MoS 2 using a dielectric screening method has been published, it has become possible to use a variety of materials such as micro-mechanical and chemical exfoliation, lithiation, thermolysis, and two-step thermal evaporation Various synthetic processes have been studied. Subsequently, sulphurization of the pre-deposited Mo has been developed, and it has been found that the sulfuration is a somewhat suitable method for the synthesis of large area MoS 2 . However, the MoS 2 produced by the sulfidation of the pre-deposited Mo exhibits non-uniformity and low field effect mobility compared to the peeled sample, and the MoS 2 sometimes contains pre-deposited Mo and sulfur Due to incomplete bonding, they grow vertically on the substrate. Chemical vapor deposition (CVD) is a well-known method for large-area MoS 2 growth. Lee et al. [Lee, Y.-H. et al. Synthesis of large-area MoS 2 atomic layers with chemical vapor deposition. Adv . Mater. 24, 2320-2325 that (2012) molybdenum trioxide (MoO 3), a highly effective method for the molybdenum oxysulfide (MoO 3 -x) and CVD using sulfur powder Reduction from growth of MoS 2 atomic layer on a dielectric substrate . Using similar methods, studies on large area high quality MoS 2 with larger crystal size or layer number control were conducted.

However, a suitable growth method for MoS 2 at a low temperature of 400 캜 or below has not yet been reported, and still requires the sulfuration of MoO 3 -x at a high temperature of 550 캜 to 850 캜. Despite some studies using molybdenum pentachloride (MoCl 5 ) and molybdenum hexacarbonyl [Mo (CO) 6 ] as novel precursors for growing MoS 2 , the synthesis at low temperature has been limited to three- 3D) structure of MoS 2 . Typically, higher temperatures facilitate the growth of high quality films due to the small number of nuclei, long diffusion length on the surface, and effective desorption of volatiles. However, at low temperatures, the growth of high quality films is difficult due to the small critical radius for nucleation and the short diffusion length of the surface, and is particularly challenging for single layer growth.

The present invention provides a process for preparing a two-dimensional transition metal decalcogenide.

However, the problems to be solved by the present invention are not limited to the above-mentioned problems, and other problems not mentioned can be clearly understood by those skilled in the art from the following description.

According to a first aspect of the present invention, there is provided a method of manufacturing a semiconductor device, comprising: pre-treating a substrate in a deposition chamber; And providing a chalcogen-containing precursor and a transition metal-containing precursor in the deposition chamber to deposit a two-dimensional transition metal decalcogenide on the substrate. do.

According to one embodiment of the present invention, by controlling the size and nucleation position of the clusters of the two-dimensional transition metal decalcogenide, it is possible to produce a large-area, high-quality two-dimensional transition metal decalcogenide at a low temperature of about 600 ° C or less Since it is possible to grow at low temperatures, it is possible to grow a large-area, high-quality two-dimensional transition metal decalcogenide directly on a flexible substrate (substrate).

The two-dimensional transition metal decalcogenide according to one embodiment of the present invention can be used as an element, and has a polycrystalline single layer and a two-dimensional structure, thereby being advantageous as a next generation flexible device and a wearable device.

Figures 1 (a) and 1 (b) are graphs depicting the vapor pressure of a transition metal-containing precursor of a two-dimensional transition metal dicalcium nodide according to an embodiment of the present invention and the two-dimensional transition metal dicalcogenide FT-IR < / RTI >
Figures 2 (a) and 2 (b) are schematic diagrams illustrating a showerhead-type reactor connected to a gas-flow line and a load-lock chamber for deposition of a two-dimensional transition metal dicalcogenide in one embodiment of the present invention .
Figures 3 (a) - (d) show, in one embodiment of the present invention, that the two-dimensional transition metal dicar, measured at various partial pressure ratios (P SR / P MoP ) of the sulfur-containing precursor and the molybdenum metal- (A) to (c) and the Raman spectrum (d).
Figure 4 is a graph showing the ratio of S-versus-Mo in a two-dimensional transition metal decalcogenc coaginid according to various types of edge types, in one embodiment of the present invention.
FIG. 5A is a graph showing the growth window of a two-dimensional transition metal decahydronium oxide grown at low temperature, in one embodiment of the present invention. FIG.
Figure 5b is a micrographic image of a two-dimensional transition metal decalcogenide grown in various P SR / P MoPs, in one embodiment of the invention.
Figures 6 (a) through 6 (h) show, in an embodiment of the present invention, the structure (a) of the two-dimensional transition metal decanoic acid grown in various P SR / P MoPs , the schematic of the cluster- (b) and (c)], the Raman spectrum [(d) and (e)], the photoluminescence spectrum (f), and the XPS spectrum [g and h].
Figure 7 is an AFM image of a two-dimensional transition metal dicalcogenide grown over time on various substrates in one embodiment of the invention.
Figures 8 (a) - (c) are AFM images of two-dimensional transition metal dicalcogenides grown on various substrates in one embodiment of the invention.
9 (a) through 9 (f) are, in an embodiment of the present invention, a microscope image of a two-dimensional transition metal decahonocurine grown according to various growth times and a Raman spectrum of the two-dimensional transition metal decahonocinide .
10 (a) and 10 (b) are cross-sectional views of an embodiment of the present invention wherein an image (a) of a single-layer two-dimensional transition metal decalcogenide grown on a large- The result of the elipsometry mapping analysis (b).
11 (a) to 11 (d) illustrate an image (a) of a two-dimensional transition metal dicalcium longeon layer laminated from a single layer to a five-layer in an embodiment of the present invention, Spectra [(b) and (c)], and the photoluminescence spectrum (d) of the two-dimensional transition metal decalcogenide.
12 (a) to 12 (d) are cross-sectional views illustrating a low-power HRTEM image (a) of a transferred three-dimensional structure of a transition metal dicalcogenide in an embodiment of the present invention, (B) to (d).
13 (a) - (d) illustrate, in an embodiment of the invention, a low-power STEM-HAADF image (a) of a two-dimensional transition metal decahan- (D) showing the STEM-HAADF image (b), the smoothed and Fourier-filtered image (c) in FIG. 13 b, and the electrical characteristics of the fabricated FET device.

Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings so that those skilled in the art can easily carry out the present invention. It should be understood, however, that the present invention may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. In the drawings, the same reference numbers are used throughout the specification to refer to the same or like parts.

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 " on " another member, it includes not only when the member is in contact with the other member, but also when there is another member 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. The terms " about ", " substantially ", etc. used to the extent that they are used throughout the specification are intended to be taken to mean the approximation of the manufacturing and material tolerances inherent in the stated sense, Accurate or absolute numbers are used to help prevent unauthorized exploitation by unauthorized intruders of the referenced disclosure. The word " step (or step) " or " step " used to the extent that it is used throughout the specification does not mean " step for.

Throughout this specification, the term " combination (s) thereof " included in the expression of the machine form means a mixture or combination of one or more elements selected from the group consisting of the constituents described in the expression of the form of a marker, Quot; means at least one selected from the group consisting of the above-mentioned elements.

Throughout this specification, the description of "A and / or B" means "A or B, or A and B".

Hereinafter, embodiments and examples of the present invention will be described in detail with reference to the accompanying drawings. However, the present invention is not limited to these embodiments and examples and drawings.

According to a first aspect of the present invention, there is provided a method of manufacturing a semiconductor device, comprising: pre-treating a substrate in a deposition chamber; And providing a chalcogen-containing precursor and a transition metal-containing precursor in the deposition chamber to deposit a two-dimensional transition metal decalcogenide on the substrate. do.

In one embodiment of the present invention, by controlling the cluster size and nucleation site of the two-dimensional transition metal decalcogenide, high-quality large-area two-dimensional transition metal decalcogenide can be produced at a low temperature of about 600 ° C or less, By using the two-dimensional transition metal decalcogenide, a device having excellent electrical performance can be manufactured.

In one embodiment of the present invention, the deposition may be performed at a low temperature of about 600 DEG C or less, but may not be limited thereto. For example, the temperature range may be about 600 ° C or less, about 500 ° C or less, about 400 ° C or less, about 100 ° C to about 600 ° C, about 200 ° C to about 600 ° C, To about 400 < 0 > C, or from about 200 < 0 > C to about 400 < 0 > C.

In one embodiment of the present invention, the deposition may be performed by, for example, chemical vapor deposition, without limitation, using deposition methods known in the art. For example, the chemical vapor deposition may be performed by low pressure chemical vapor deposition (LPCVD), atmospheric pressure chemical vapor deposition (APCVD), metal organic chemical vapor deposition (MOCVD) ), Plasma-enhanced chemical vapor deposition (PECVD), inductively coupled plasma-chemical vapor deposition (ICP-CVD), atomic layer deposition, or plasma atomic layer deposition, But may not be limited thereto.

In one embodiment, the transition metal-containing precursor is selected from the group consisting of Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Nb, Ta, Mo, W, Tc, Re, A transition metal selected from the group consisting of Ir, Pt, Ag, Au, Cd, In, Tl, Sn, Pb, Sb, Bi, Zr, Te, Pd, Hf, , But may not be limited thereto. For example, the transition metal-but could be to include those containing precursor is selected from Mo (CO) 6, Mo ( Cl) 5, MoO (Cl) 4, MoO 3, and the group consisting of a combination thereof, But may not be limited thereto.

In one embodiment of the invention, the chalcogen-containing precursor is selected from the group consisting of H 2 S, CS 2 , SO 2 , S 2 , H 2 Se, H 2 Te, R 1 SR 2 wherein R 1 and R 2 are (NH 4 ) 2 S, C 6 H 8 OS, S (C 6 H 4 NH 2 ) 2 (wherein each of R 1 and R 2 is independently an alkyl having 1 to 6 carbon atoms, an alkenyl having 2 to 6 carbon atoms, or an alkynyl having 2 to 6 carbon atoms) , Na 2 SH 2 O, and combinations thereof, but it is not limited thereto.

In one embodiment of the present invention, by controlling the partial pressure ratio ( CPP / PMP ) of the chalcogen-containing precursor (hereinafter referred to as CP ') and the transition metal-containing precursor But the present invention is not limited thereto, and the cluster size of the two-dimensional transition metal decanoic acid deposited may be controlled. As the cluster size is controlled, the structural change of the deposited two-dimensional transition metal decalcogenide may occur but may not be limited thereto.

In one embodiment of the present invention, in the deposition process, the chalcogen-containing precursor and / or the chalcogen-containing precursor supplied into the deposition chamber by controlling the pressure in the deposition chamber by using no carrier gas or finely adjusting the flow rate of the carrier gas, By controlling the amount of the transition metal-containing precursor finely, the partial pressure ratio of the chalcogen-containing precursor to the transition metal-containing precursor may be finely controlled, but the present invention is not limited thereto.

In one embodiment, the size of the clusters formed by the gas phase reaction during the deposition of the transition metal decalcogenide is controlled by controlling the partial pressure ratio of the chalcogen-containing precursor to the transition metal-containing precursor, Energy may be controlled to induce the two-dimensional growth of the transition metal dicalcium cyanide, but the present invention is not limited thereto.

In one embodiment of the present application, in the deposition step, for example, in a chemical vapor deposition step, a gas phase reaction and a reaction on the substrate surface occur, and in the gas phase reaction, And these clusters are transferred to the substrate surface to cause a surface reaction. The cluster is formed in a larger size as the partial pressure ratio (P CP / P MP ) of the chalcogen-containing precursor to the transition metal-containing precursor is lower and is transferred to the substrate surface, in which case nucleation occurs at the substrate surface The gaseous materials stick to the side and grow in the form of an island (up to a certain size, it is called a nucleus, and when it gets bigger, it is called an island). At this time, clusters generated in the gas phase are also transferred to the substrate surface by diffusion. At this time, when the substrate surface temperature is high, the clusters can grow into a two-dimensional structure due to the surface diffusion effect. However, since the energy is insufficient at low temperatures, such a reaction does not actively occur, It is possible to control the structure of the two-dimensional transition metal decalcogenide deposited by controlling the generated cluster size and surface energy by increasing the partial pressure ratio (P CP / P MP ) of the precursor containing the precursor.

In one embodiment of the present invention, as the partial pressure ratio (P CP / P MP ) of the chalcogen-containing precursor to the transition metal precursor increases, the deposited two-dimensional transition metal decalcogenide increases in a two- But the present invention is not limited thereto. For example, the higher the partial pressure ratio (P CP / P MP ) of the chalcogen-containing precursor to the transition metal precursor, the lower the surface energy of the resulting transition metal decalcogenide, The two-dimensional growth of the metal dicalcogenide may be induced, but may not be limited thereto. In one embodiment herein, the more the partial pressure ratio (P CP / P MP ) of the chalcogen-containing precursor to the transition metal-containing precursor is further increased, the larger the grain size of the two-dimensional transition metal dicalcogenide And can be completely changed into a two-dimensional triangular area, but it may not be limited thereto.

In one embodiment herein, the feed partial pressure ratio of the chalcogen-containing precursor to the transition metal-containing precursor may be about 1: about 2 or more, but may not be limited thereto. For example, the feed partial pressure ratio of the chalcogen-containing precursor to the transition metal-containing precursor may be at least about 1: at least about 2: at least about 1: at least about 3: at least about 1: about 4: About 1: about 10 or more, but may not be limited thereto. Preferably, the feed partial pressure ratio of the chalcogen-containing precursor to the transition metal-containing precursor ranges from about 1: about 2 to about 600, about 1: about 2 to about 500, about 1: about 2 to about 400, From about 2 to about 300, from about 1: from about 2 to about 200, or from about 1: from about 2 to about 100.

In one embodiment of the present invention, in the deposition process, a gas phase reaction and a reaction on the surface of the substrate occur, and the gaseous materials react with each other in the gas phase reaction to form clusters, And the surface reaction occurs. At this time, the size of the cluster and the surface energy of the substrate can be controlled by controlling the partial pressure ratio (P CP / P MP ) of the chalcogen-containing precursor to the transition metal-containing precursor, The two-dimensional growth of the nide can be controlled and induced. For example, when increasing the partial pressure ratio (P CP / P MP ) of the chalcogen-containing precursor to the transition metal-containing precursor, the size of the cluster is reduced and the surface energy of the substrate is reduced, The two-dimensional growth of the co-nitrogen can be controlled and induced.

In one embodiment of this application, as the partial pressure ratio (P CP / P MP ) of the chalcogen-containing precursor to the transition metal-containing precursor increases, the volatile byproducts are desorbed and grown in the pseudo- But it may not be limited thereto.

In one embodiment of the present invention, when the partial pressure ratio (P CP / P MP ) of the chalcogen-containing precursor to the transition metal-containing precursor is low, an irregular three-dimensional region having a small grain size can be grown, But may not be limited. For example, when the transition metal decalcogenide is grown under conditions where the partial pressure ratio of the chalcogen-containing precursor to the transition metal-containing precursor is low, a large amount of transition metal-containing precursor vapor and large size clusters are produced, The clusters are adsorbed on the surface of the substrate to grow a three-dimensional region, so that the partial pressure ratio is preferably increased.

In one embodiment of the present invention, the nucleation site of the two-dimensional transition metal dicalcogenide deposited on the substrate may be artificially controlled by pretreating the substrate, but may not be limited thereto. For example, the grain size of the two-dimensional transition metal decalcogenide with limited grain size may be controlled by adjusting the nucleation site, but may not be limited thereto.

In one embodiment of the invention, the pretreatment of the substrate may include, but is not limited to, a process selected from the group consisting of vacuum heat treatment, annealing or high vacuum annealing treatment, chemical treatment, and combinations thereof have. For example, the pretreatment may be a high vacuum annealing process, wherein the nucleation site can be suppressed by decomposing a dangling bond that provides a reactive surface location on the substrate by the high vacuum annealing, Large-area two-dimensional transition metal dicalcogenides may be prepared, but are not limited thereto.

In one embodiment of the invention, the substrate is Si, SiO 2, Ge, GaN, AlN, GaP, InP, GaAs, SiC, Al 2 O 3, LiAlO 3, MgO, glass, quartz, sapphire, graphite, graphene , Plastics, polymers, boron nitride (h-BN), and combinations thereof, but the present invention is not limited thereto. The substrate may be a material that is difficult to synthesize due to problems such as atomic arrangement, a material that is advantageous for a price or a large area, and may function as a substrate capable of regulating a catalyst or nucleation site for growing the cluster.

In one embodiment of the present invention, before the step of pretreating the substrate, it may further include pre-cleaning the substrate to prevent unnecessary nucleation near the grain, but is not limited thereto . For example, the pre-cleaning step may be but is not limited to being performed under atmospheric conditions.

In one embodiment of the invention, the pre-cleaning may be, but not limited to, performed by water, ethanol, acidic substances, alcohols, or RCA cleaning methods. For example, the alcohols may include, but are not limited to, methanol, ethanol, propanol, butanol, or isomers thereof. For example, the acidic material may include, but is not limited to, selected from the group consisting of H 2 SO 4 , HCl, HNO 3 , and combinations thereof. For example, the acidic substance may be diluted in various ratios, but may not be limited thereto.

In one embodiment of the invention, the RCA cleaning process may be performed using a combination of NH 4 OH, H 2 O 2 , and / or HCl, depending on the combination of ammonia SC-1 rinsing or acidic SC- But it may not be limited thereto.

In one embodiment of the invention, the deposition of the two-dimensional transition metal decalcogenide can be controlled by controlling the chamber pressure by using a vacuum equipment feeding system, but not limited thereto.

In one embodiment of the invention, the grain size of the two-dimensional transition metal decalcogenide may be about 50 nm or more, but may not be limited thereto. For example, the grain size of the two-dimensional transition metal decalcogenide may be at least about 50 nm, at least about 70 nm, at least about 100 nm, at least about 50 nm to about 100 nm, at least about 50 nm to about 90 nm, at least about 50 nm, About 60 nm to about 80 nm, about 60 nm to about 70 nm, about 70 nm to about 100 nm, about 60 nm to about 60 nm, about 60 nm to about 100 nm, about 60 nm to about 90 nm, nm, about 70 nm about 90 nm, about 70 nm about 80 nm, or about 80 nm to about 100 nm.

In one embodiment of the present application, the two-dimensional transition metal decalcogenide may be applied to all electronic circuits and electronic devices, but is not limited thereto. For example, it is possible to manufacture a field effect transistor, an optical sensor, a light emitting device, a photodetector, a photomagnetic memory device, a photocatalyst, a flat panel display, a flexible device, .

In one embodiment of the present invention, the field effect transistor including the two-dimensional transition metal decalcogenide is excellent in electrical performance and exhibits a tendency of a conventional n-type semiconductor.

EXAMPLES Hereinafter, the present invention will be described in more detail with reference to the following examples. However, the following examples are given to aid understanding of the present invention, and the present invention is not limited to the following examples.

[ Example ]

Growth process

MoS 2 , a two-dimensional transition metal dicalcogenide, was grown by a showerhead-type reactor using Mo (CO) 6 (= 99.9%, Sigma Aldrich, CAS number 13939-06-5) as a transition metal-containing precursor . Highly-doped (<0.005 ohm-cm) p-type Si with a 300 nm-thick SiO 2 layer was used as the substrate. The substrate has been pre-cleaned and placed on a silicon carbide (SiC) -coated susceptor in a load-lock chamber within a short time to prevent any contamination in the environment. The heating blocks in the CVD were preheated to 350 占 폚 before growth. The susceptor with the substrate was transferred to the reactor, and the substrate temperature was increased over 10 minutes in argon flow. The growth was carried out using only the H 2 S and sublimed precursors during the growth time at a constant pressure of 0.5 Torr. After growth, the substrate was transferred to a load-lock chamber and cooled for 1 hour using an argon flow of 100 sccm. The post-growth treatment was not performed by any known methods (such as argon and H 2 S annealing at high temperature). All analyzes and characterization were performed using the grown samples.

AFM  Measure

The surface morphology, grain size, nucleation and growth process of the prepared two-dimensional transition metal dicalcogenides were measured using AFM (XE-150, Park Systems). For better quality, AFM images were measured using a very sharp silicon tip with a radius of curvature of less than 5 nm (<5 nm). A soft X-ray ionizer module was applied to prevent static electricity during measurement. The image was taken over an area of 1 μm 2 to 2 μm 2 with a resolution of 512 × 512 pixels and a measurement speed of 0.5 Hz. The image was adjusted to 750 nm 2 .

Spectroscopic measurement

The Raman spectroscopic measurement of the two-dimensional transition metal decalcogenides prepared in the above examples was carried out using a DXR Raman microscope (Thermo Scientific). A laser with an excitation wavelength of 532 nm, a spot size of 0.7 μm, and a power of 8 mW was used. The estimated spectral resolution is 0.5 cm - was a 1, the Si peak of 520.8 cm -1 were used for normalization (normalization). The photoluminescence (LabRam ARAMIS, Horiba Jobin Yvon) measurement of the grown sample was performed with a wavelength of 514 nm and a laser power of 10 mW. Ellipsoometry (M2000D, JA Woollam Co.) mapping measurements were performed with a step size of 0.5 cm. The thickness results were extracted by a four-layer model (air / MoS 2 / SiO 2 / Si). XPS measurements (SES-100, VG-SCIENTA) were performed using a non-monochromatic magnesium Kα source under ultra-high vacuum conditions (<10 -8 Torr).

TEM  Sample preparation

Poly (methyl methacrylate) (poly (methyl methacrylate) ( PMMA) (950 A2, MicroChem) spin for 60 seconds onto the MoS 2 / SiO 2 / Si samples grown at 4,000 rpm -. Were coated with the SiO 2 layer Was etched by immersing the coated sample in a buffered oxide etch (BOE) solution (6: 1, JT Baker). The separated PMMA / MoS 2 was washed several times with deionized water and then cleaned with a carbon grid (HC300- Electron Microscopy Sciences). PMMA was removed by annealing at 300 占 폚 for 30 minutes under high vacuum conditions (<10 -5 Torr).

HAADF -STEM image measurement

The HAADF-STEM image of the two-dimensional transition metal decalcogenide prepared in the above example was analyzed using Cs-STEM (Titan cubed) operating at 300 kV using a mrad convergence angle of 19.3 and a screen current of 50-100 pA G2 60-300, FEI). The image was smoothed and Fourier-filtered to improve contrast.

Electrical performance measurement

Back-gate FET devices were fabricated by depositing Ti / Au (5/50 nm) electrodes directly on the MoS 2 monolayers grown using electron-beam evaporation. The electrode morphology was patterned using electron-beam lithography of a PMMA (950 C4, MicroChem) layer and developed with a diluted MIBK (MIBK: IPA = 1: 1, MicroChem) solution. The lift-off process was carried out by immersion in dichloromethane (DCM) and IPA and drying with high purity N 2 (99.999%). The electrical performance of the device was measured at room temperature under ambient conditions using an in-house four-probe station with a precision semiconductor parameter analyzer (4156A, Hewlett-Packard). The device was not annealed.

Measurement of vapor pressure and decomposition properties of transition metal-containing precursors

The vapor pressure and decomposition properties of the precursor are important parameters when considering its suitability for CVD processes. For vapor pressure measurements, a self-made measurement system was used. A vessel of a certain volume was first held under high vacuum conditions by a turbomolecular pump (TMP), then a connected quartz tube containing the precursor was opened and the pressure was maintained It was maintained for several hours. 30, 50, and in the precursor temperature of 70 ℃ vapor pressure of Mo (CO) 6 was measured as 0.31, 1.27, and 5.24 Torr [(a) of Fig. 1, respectively, a simplified form of the Clapeyron equation, ln (P sat / Pa) = AB / (T / K), where P sat and T are the saturation vapor pressure and the precursor temperature, respectively. The decomposition properties of Mo (CO) 6 were evaluated using FT-IR (Nicolet 6700, Thermo Scientific). The main absorption peaks of Mo (CO) 6 were measured at 2,000 cm &lt; -1 &gt; consistent with previous studies and the precursor was completely decomposed at about 250 &lt; 0 &gt; C and a pressure of 0.5 Torr (Fig. The high vapor pressure and low decomposition temperature characteristics make Mo (CO) 6 a suitable precursor for low temperature CVD processes.

CVD set up

Low-temperature growth of the deposited MoS 2 , which is a two-dimensional transition metal dicalcogenide, is achieved by using a showerhead-type reactor connected to the gas flow line and the load-lock chamber, as shown in Figures 2 (a) . The SiO 2 substrate pre-cleaned or treated (by piranha or high vacuum annealing) was placed into a load-lock chamber, and then the sample was transferred to the main chamber. The partial pressure of Mo (CO) 6 was precisely controlled using a chiller-heater unit (the adjustable range is -20 ° C to 80 ° C). The flow rate of H 2 S was controlled using a mass flow controller. The use of carrier gases (Ar or H 2 ) has been ruled out to prevent the formation of large size clusters.

Example  1: Various P SR / P MoP Transition metal depending on the value Dicalcogenide  Growth analysis

1-1: Transition metal of three-dimensional structure Dicalcogenide

As shown in FIG. 3, the present inventors used sulfur-containing precursors and fluorine-containing precursors using a scanning electron microscope (SEM, S-4800, HITACHI), a high resolution transmission electron microscope (HRTEM, Tecnai G2 F30 S- Twin, FEI) The MoS 2 grown at various partial pressure ratios (P SR / P MoP ) of the molybdenum metal-containing precursor was evaluated. MoS 2 of large size three - dimensional structure was grown by large size clusters formed by vapor phase reaction. MoS 2 (P SR / P MoP = 1, 0.5 Torr) with large amounts of carbides and oxides was grown and identified by Raman spectroscopy (285 cm -1 for oxides, 1350 and 1580 cm -1 for carbides) . The presence of carbide in the grown MoS 2 under increased pressure conditions was not observed and only the MoO 3 and MoS 2 peaks were measured. Despite the decrease in the partial pressure of Mo (CO) 6 as the chamber pressure increased, the partial pressure of H 2 S did not decrease. As a result, the P SR / P MoP was increased, which led to the formation of small size clusters. This preliminary experiment shows the effect of the partial pressure ratio on the cluster size controlled structure change and easy decarbonylation method.

1-2: MoS 2  Edge type, Yellow Coverage , And related S Mo Ratio

It is known that two types of edge structures (Mo and S edges) can be formed under various conditions. The sulfur coverage according to the associated parameters of the edge type and S-to-Mo ratio generated accounts for the triangular monolayer domain often found in high-quality MoS 2 . A perfect, regular, triangular domain is present for an S-edge 2D MoS 2 cluster covered with 100% sulfur atoms. This structure is often formed under high sulfiding conditions. In FIG. 4, the calculated S-to-Mo ratio is expressed as a function of cluster size for various edge types and sulfur coverage. The XPS measurement results and AFM images of MoS 2 grown at various P SR / P MoP values indicate that high P SR / P MoP facilitates two-dimensional growth as the surface energy decreases.

1-3: Various P SR / P MoP  Transition metal depending on the value Dicalcogenide  Growth mechanism

Figures 5a and 5b are microscope images (Figure 5b) for samples grown at various P SR / P MoP values representing a growth window at low temperature (Figure 5a). The triangular two-dimensional MoS 2 region was grown under a specific P SR / P MoP of 73. The scale bar is 200 nm. 6 (a) shows the AFM of MoS 2 with different structures grown in various values of P SR / P MoP (three dimensions: cases 1 and 2, three dimensions + two dimensions: case 3, two dimensions: case 4) Image. The scale bar is 200 nm. The measured height profile of the area is shown in the inset indicated by the open yellow squares. Figures 6 (b) and 6 (c) are schematic diagrams of the cluster-size control mechanism of the present invention. The formation of the clusters was restricted in the higher P SR / P MoP (c), while the larger MoS 2 clusters were formed by the vapor phase reaction in the lower P SR / P MoP (b). 6 (d) and 6 (e) corresponded to the Raman spectrum of each sample. The value of Δk decreased from 21.7 to 18.8 cm - 1 at P SR / P MoP = 73 (d). The two predominant modes of FWHM were reduced from 17.84 to 6.27 cm -1 (E 1 2 g ) and from 8.68 to 6.75 cm -1 (A 1 g ) (e), respectively. A silicon peak (520.8 cm -1 ) was used for normalization. FIG. 6 (f) is a photoluminescence spectrum of each sample. Higher intensity indicates that high quality MoS 2 was grown. 6 (g) and 6 (h) are XPS spectra of the respective samples. The presence of MO + 6 in Case 1 indicates that the oxide was incorporated with Mo.

Example  2: High vacuum On annealing  Transition metal Dicalcogenide  Growth analysis

As shown in FIG. 7, growth processes on different substrates for different growth times were observed using AFM (P SR / P MoP = 146). For this treatment, untreated SiO 2 was first washed with acetone, IPA, and deionized water. The substrate was then immersed in the piranha solution for 10 minutes to hydrolyze the dangling bonds and then washed with deionized water. The untreated SiO 2 substrate was annealed at 750 ° C for 140 minutes under high vacuum conditions (<10 -5 Torr) to de-passivate hydrogen-passivated dangling bonds. A large number of MoS 2 nuclei were observed at nucleation sites on the piranha-treated substrate compared to the other two substrates, and new nucleation sites were not created during growth. Instead, the MoS 2 nuclei were attached to the edge of the pre-grown MoS 2 . Because of this growth mechanism, an increase in grain size can be achieved by limiting nucleation sites even at low temperatures. The grain size of the MoS 2 grown in the other substrate is 50 nm (piranha treated), 70 nm (untreated), and 100 nm (high vacuum annealed). The limitation of the nucleation site slightly inhibits the growth time for a fully covered monolayer. The scale bar is 100 nm. 8A to 8C are AFM images of the MoS 2 monolayers grown on different substrates, respectively: (a) Piranha-treated MoS 2 , (b) bare MoS 2 , and (c) High Vacuum Annealed MoS 2 . High vacuum annealing de-passivates the passivated dangling bonds in untreated SiO 2 while the piranha treatment passivates the dangling bonds. Large size islands were grown on high vacuum annealed SiO 2 substrates due to limited nucleation sites. The growth time was 12 hours and P SR / P MoP = 314. The scale bar is 100 nm.

Example  3: transition metal Dicalcogenide  Laminated growth

3-1: Laminated  Transition metal Dicalcogenide  growth

Figure 9 (a) shows the initial phase of growth. The small triangular area of the monolayer MoS 2 was grown at the nucleation site on the SiO 2 substrate. 9 (b) to 9 (d), the MoS 2 region was further grown, and polycrystalline single-layer MoS 2 was formed by merging with each other. 9 (e) and (f), the triangular MoS 2 bilayer region was grown in a fully covered monolayer. The corresponding value of? K in the Raman spectrum for each growth time was measured as a single layer, 18.8, and 19.3 to 20.3 cm -1 for each of the monolayers with bilayer regions. In the intermediate phase (phase) between the fully covers single-layer and double-layer, the average value of Δk is 18.8 and 22.4 cm for the MoS 2 single layer and double layer each completely cover-1. The scale bar is 100 nm. 11 (a) is a photograph of single-layer to five-layer MoS 2 grown on untreated SiO 2 and 1 x 1 cm 2 SiO 2 substrates. The layer was controlled according to growth time and no other conditions were changed. 11 (b) to 11 (c) are Raman spectra of the deposited MoS 2 . The E 1 2g and A 1g modes were red- and blue-shifted, respectively, as the number of layers increased. Value of Δk was measured as 18.8, respectively, 22.6, 23.6, 24.5, and 25 cm -1 with respect to the single layer of MoS 2 to 5 layers. 11 (d) shows the photoluminescence of the laminated MoS 2 . Two dominant absorption peaks (near 670 nm and 620 nm) consistent with two direct excitonic transitions (A1 and B1) were observed and their intensity decreased with increasing number of layers. The indirect bandgap transition was not observed in multilayer-laminated samples, which is a common phenomenon for SiO 2 substrates.

3-2: Wafer-scale growth

10 (a) shows a photograph of a single layer MoS 2 grown on a 4 "SiO 2 / Si wafer. The uniformity of the grown MoS 2 was evaluated by ellipsometry mapping analysis (Fig. 10 (b) The thickness was 0.7 to 0.8 nm. MoS 2 was successfully grown over the 3 "region. In FIG. 10 (b), the unit of the insertion value is nanometer.

Example  4: transition metal Dicalcogenide  Electrical performance measurement

12 (a) is a low magnification HRTEM image of MoS 2 of the transferred three-dimensional structure (Fig. 1 (a), case 1). 12 (b) to 12 (d) show a high magnification image selected at an arbitrary position in FIG. 12 (a) having a corresponding FFT pattern. Multilayered polycrystalline MoS 2 is composed of domains of small size three-dimensionally laminated structure, and it is difficult to distinguish grain boundaries due to interference of overlapped layers and small grain size. 13 (a) is a low magnification STEM-HAADF image of polycrystalline single layer MoS 2 . A single domain of a triangle with an approximate size of 100 nm can be observed and produce grain boundaries (yellow dashed triangles). 13 (a) is a low magnification STEM-HAADF image of polycrystalline single layer MoS 2 . A single domain of a triangle with an approximate size of 100 nm can be observed and produce grain boundaries (yellow dashed triangles). 13 (b) is a high magnification STEM-HAADF image of the grain boundary. Two adjacent single crystal domains form a grain boundary with an inclination angle of 31 [deg.]. The inset shows an FFT pattern showing the hexagonal structure of the MoS 2 monolayer. Figure 13 (c) is the smoothed and Fourier-filtered image in Figure 13 (b). A highly uniform and defect-free structure was observed for the brighter Mo atoms and the darker S atoms. Figure 13 (d) shows the electrical characteristics of FET devices fabricated to have channel lengths and widths (insertion degree, scale bar: 5 μm) of 5 μm and 10 μm. The mobility of 0.15 cm 2 V -1 s -1 and the maximum on / off ratio of 10 5 at 5 V were measured at applied back-gate voltages in the range of -150 V to 150 V. The monolayer of MoS 2 was not patterned.

A transition metal - CVD Process Using containing precursor of Mo (CO) 6 is, depending on the deposition conditions, containing a significant amount of the carbide or oxide such as large aggregates, Mo- based 3-D structure film, and Mo 2 C, or MoOC &Lt; / RTI &gt; is known to have a tendency to form a film that is &lt; RTI ID = Despite the many drawbacks caused by the carbonyl (CO) ligand released from the central Mo atom, the lower deposition temperature (FIG. 1) makes Mo (CO) 6 a suitable precursor for low temperature growth. In order to achieve two-dimensional growth of MoS 2 deposited at 350 ° C, the present inventors have developed a novel method of controlling the cluster size by supplying precise amounts of Mo precursors and controlling the nucleation sites on SiO 2 substrates by high vacuum annealing Respectively. Although the prior art has found that a large amount of carrier gas (Ar or H 2 ) facilitates decarbonylation, the use of carrier gas is, in the experiments of the present application, advantageous, since a large amount of carrier gas eventually increases the absolute amount of precursor vapor Were excluded. In order to investigate the strategic approach of the present application, experiments were conducted using various P SR / P MoP Lt; / RTI &gt; The P MoP was precisely controlled using a cooling-heater unit connected to a precursor canister (Fig. 2 (a)). Growth was performed using a showerhead-type reactor to assist in the generation of a uniform flow (Fig. 2 (b)). Before growth, the SiO 2 base material is first pre using acetone, isopropyl alcohol (IPA), and deionized water (DI) in order to prevent nucleation areas around dust (dust) grain-were washed. The substrate was then loaded into the load-lock chamber for several seconds under ambient conditions to prevent any surface contamination and was transported to the main reactor and then transferred to various Mo (CO) 6 sublimation temperatures (0-80 ° C) and H 2 S flow rate (10-100 sccm) at a substrate temperature of 350 &lt; 0 &gt; C for a certain period of time. In our preliminary experiments performed at lower P SR / P MoP , structural changes of MoS 2 were observed depending on cluster size and this partial pressure ratio was proved to be a major parameter for two-dimensional growth a)]. Figure 6 (a) shows atomic force microscope (AFM) photographs of various samples grown at different values of P SR / P MoP . In the low P SR / P MoP ( cases 1 and 2), an irregular three-dimensional region with a small grain size was grown. As the P SR / P MoP (case 3) increases, the morphology is changed to a mixed structure consisting of irregular three-dimensional islands and two-dimensional triangular regions. At much higher P SR / P MoP , the structure was completely changed to a two-dimensional triangular area with a larger grain size (case 4). This structural change can be explained by the hypothetical cold growth mechanism for cluster size-controlled growth (Figs. 6 (b) and (c)). In low P SR / P MoP , large amounts of Mo (CO) 6 vapor sublimate and large size MoS 2 clusters are formed by gas phase reactions. Consequently, the formed clusters were adsorbed on the surface, and a three-dimensional MoS 2 region was grown (Fig. 6 (b)). In the high P SR / P MoP , a pseudo- two dimensional MoS 2 region is grown on the surface by desorption of volatile byproducts and is converted to a MoS 2 monolayer by surface diffusion (FIG. 6 (c)). The result of the Raman spectroscopic analysis of the grown MoS 2 corresponds to the corresponding atomic structure measurement result (Fig. 6 (d)). Plane vibration (in-plane vibration) (E 1 2g) and a difference (Δk) between the out-of-plane vibration (out-of-plane vibration) (A 1g) the two Raman mode due to the, single-layer and double-layer overlapping of the MoS 2 (coincidence) as a result, low P SR / P MoP (cases 1 to 3) on the 21.7 cm -1 for the MoS 2 in the growth were measured, high P SR / P MoP (case 4), the E 2g mode 1 Fig. 6 (e)] half value width (full width at half maximum, FWHM ) further decreased to 18.8 cm -1 with a decrease and increase in the light emission [(f)] in Fig. 6 in the. These results indicate that high quality laminated MoS 2 can be grown under high P SR / P MoP conditions. The formation of the two-dimensional region is characterized by a theoretical consideration of chemical potential and surface energy. Schweiger, etc. [Schweiger, H., Raybaud, P. , Kresse, G. & Toulhoat, H. Shape and edge sites modifications of MoS 2 catalytic nanoparticles induced by working conditions: A theoretical study. J. Catal . 207, 76-87 (2002) have shown that the type of edge-termination (Mo- or S-edge) and the coverage by sulfur atoms in a single layer MoS 2 cluster correspond to the chemical potential of sulfur and the ratio of S to Mo (Fig. 4). &Lt; / RTI &gt; Under enhanced sulfiding conditions (high H 2 S partial pressure), the low chemical potential of the sulfur causes 100% coverage of the Mo edge (or S edge) by 100% sulfur with the lowest surface energy. Under these conditions, the layer atoms are attracted more strongly to the substrate than themselves, thus facilitating two-dimensional growth. S Mo Mo ratios of 1.37, 1.99, 1.95, and 2.27 were determined from X-ray photoelectron spectroscopy (XPS) for MoS 2 grown from low to high values of P SR / P MoP g) and (h). These observations illustrate structural changes and demonstrate that cluster size and strong sulphiding conditions are important factors for the growth of MoS 2 at low temperatures.

The grain size of the polycrystalline two-dimensional material is the most important characteristic that determines its physical and electrical characteristics. At low temperatures, the grain size of the two-dimensional material is much smaller than the grain size at high temperatures due to the small diffusion length at the surface. We have observed the growth of monocrystalline monolayer MoS 2 domains grown at various values of P SR / P MoP by AFM. However, no grain size greater than 50 nm was observed even under strong sulphiding conditions (P SR / P MoP = 594). These experiments show the presence of a grain-size limit at 350 ° C. To overcome this limitation due to the short diffusion length on the surface, nucleation sites were artificially manipulated by annealing the substrate in a high vacuum. To investigate the effect of nucleation-position manipulation on grain size, the inventors grown monolayers of MoS 2 on three different substrates, as shown in Figure 8: as shown in Figure 8, piranha ) -Treated (H 2 SO 4 : H 2 O 2 = 3: 1) SiO 2 , bare SiO 2 , and high vacuum annealed SiO 2 substrates. A small number of regions having a large grain size are formed in the vacuum-annealed substrate as compared with those of the untreated SiO 2 substrate (FIG. 8B) (FIG. 8C), while the piranha- A larger number of triangular MoS 2 regions having a smaller grain size were formed (Fig. 8 (a)). Hydroxylated or hydrogen-passivated dangling bonds of amorphous SiO 2 are known to provide a number of reactive surface areas compared to non-saturated surfaces. In contrast, the high vacuum annealing process decomposes the hydrogen-passivated dangling bonds. To identify the nucleation and growth mechanisms on different substrates, the AFM images obtained at different growth times show that the edges of the monolayer region grown after the MoS 2 nucleus occupied all the desired nucleation sites during the initial phase of growth adheres to the edge and proves that no further nucleation is observed during growth (FIG. 7). The monolayer MoS 2 region was grown to 100 nm on a nucleation-position-restricted substrate. For the growth of high quality MoS 2 at low temperatures it is important to control the affinity of the nucleus and substrate so that the grain-size limit can be overcome.

The number of MoS 2 layers, which are the two-dimensional transition metal decanoides, has been conventionally controlled by controlling the thickness, surface energy, or supersaturation of the pre-deposited Mo. The grown MoS 2 using the method of the present application is characterized by lamination growth (a detailed growth process is shown in Figures 9 (a) to (f)). As was observed in the different stories 11 degrees different surface colors for, also was a 11 a is very uniform large area MoS 2 grown on a 1 x 1 cm 2 SiO 2 substrate, confirmed by ellipsometry mapping analysis, (FIG. 10). We also used Raman spectroscopy and photoluminescence to confirm the thickness of the grown MoS 2. The Raman spectra of each of the above samples were measured using a scanning electron microscope with increasing number of layers, E 1 2g and. Δk values [(b) of FIG. 11] a 1g each showed a red and blue displacements were 18.8 in a single layer to five-layer, 22.6, 23.6, 24.5, and 25 cm -1 . The two dominant absorption peaks (near 670 nm and 620 nm) correspond to the two direct exciton transitions observed in the photoluminescence measurements (A1 and B1, respectively) It is a match. The original cluster-size control method provides a suitable method for stack growth of MoS 2 on the wafer scale.

The atomic structure of the grown monolayers MoS 2 was evaluated using a high-angle annular dark-field (HAADF) imaging by aberration-corrected scanning transmission electron microscopy (Cs-STEM) . 13 (a) shows a low magnification STEM-HAADF image of a MoS 2 monolayer transferred onto a carbon grid by a conventional wet-etching method. The white area represents the overlapped MoS 2 monolayers during transfer, and the gray area represents the polycrystalline MoS 2 monolayer. The size of the approximate domain indicated by the yellow dotted triangle is 100 nm, and the size of this domain coincides with the previous observation using AFM (Fig. 9 (b)). The high-power HAADF image of the selected region shows the atomic structure of the grain boundary by two triangular domains (Fig. 13 (b)). In the inset of FIG. 13 (b), the fast Fourier transform (FFT) pattern shows a hexagonal structure of two monocrystalline MoS 2 domains with an inclination angle of 31 °. From the image reconstructed by smoothing and Fourier filtering (Fig. 13 (c)), a uniform monocrystalline MoS 2 domain was observed and formation of a polycrystalline MoS 2 monolayer was observed by the merge forming grain boundaries. In addition, the sample grown at high P SR / P MoP showed better quality compared to the sample grown at low P SR / P MoP (FIG. 12). This microscopic observation shows that a very homogeneous and large grain MoS 2 polycrystalline monolayer is grown even at 350 ° C. In addition, the domain structure and grain boundaries are very similar to MoS 2 grown at higher temperatures. To investigate the electrical performance, the cold-grown monolayer MoS 2 was used to fabricate a back-gate FET. The device was fabricated using MoS 2 monolayers without patterning, with channel lengths and widths of 5 and 10 μm, respectively (FIG. 13 (d)). The MoS 2 monolayer was not treated after growth, and measurements were taken at room temperature under ambient conditions. The FET device exhibits a conventional n-type semiconductor behavior with a mobility of 0.15 cm 2 V -1 s -1 (Fig. 13 (d)). The maximum on / off ratio was 10 5 within a gate voltage range of -150 V to 150 V using a source-drain bias voltage of 5V.

As a result, the inventors have found that by controlling the cluster size and a nucleation position, transition metal-new for containing precursor of Mo (CO) 6 high-quality two-dimensional transition metal laminate growth radical Koji arsenide at a low temperature of 350 ℃ using One method was developed. Structural transfer from a three-dimensional cluster to a two-dimensional fault has been demonstrated by controlling the grain size using the change in P SR / P MoP and the limited nucleation site. These two parameters are key factors for the low temperature growth of MoS 2 with large grains with high electrical performance. The low-temperature growth of two-dimensional materials represented by graphene and transition metal dichalcogenides is important in the application of next-generation flexible and wearable devices. Thus, the present results suggest a novel approach to the production of high quality two-dimensional materials under low temperature conditions.

It will be understood by those of ordinary skill in the art that the foregoing description of the embodiments is for illustrative purposes and that those skilled in the art can easily modify the invention without departing from the spirit or essential characteristics thereof. It is therefore to be understood that the above-described embodiments are illustrative in all aspects and not restrictive. For example, each component described as a single entity may be distributed and implemented, and components described as being distributed may also be implemented in a combined form.

The scope of the present invention is defined by the appended claims rather than the detailed description, and all changes or modifications derived from the meaning and scope of the claims and their equivalents should be construed as being included within the scope of the present invention.

Claims (10)

  1. Pretreating the substrate in the deposition chamber; And
    Providing a chalcogen-containing precursor and a transition metal-containing precursor in the deposition chamber and depositing a two-dimensional transition metal decalcogenide on the substrate
    A method for producing a two-dimensional transition metal decalcogenide,
    The ratio of the partial pressure of the chalcogen-containing precursor to the transition metal-containing precursor is 1: 2 or more,
    By controlling the partial pressure ratio of the chalcogen-containing precursor to the transition metal-containing precursor, the size of the cluster formed by the gas phase reaction in the deposition process of the transition metal decalcogenide is controlled and the surface energy is controlled, The two-dimensional growth of the nide is induced,
    The deposition is performed at a low temperature of 600 DEG C or less,
    The pretreatment includes a vacuum heat treatment, an annealing treatment, a high vacuum annealing treatment or a chemical treatment,
    Wherein the nucleation position of the transition metal decanoic acid deposited on the substrate is controlled by the pretreatment.
    (Method for producing two - dimensional transition metal dicalcogenide).
  2. The method according to claim 1,
    The transition metal-containing precursor may be selected from the group consisting of Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Nb, Ta, Mo, W, Tc, Re, Ru, Os, Rh, Wherein the transition metal comprises a transition metal selected from the group consisting of Cd, In, Tl, Sn, Pb, Sb, Bi, Zr, Te, Pd, Hf, Gt;
  3. delete
  4. The method according to claim 1,
    Wherein the chalcogen-containing precursor comprises an S-containing organic or inorganic compound.
  5. delete
  6. The method according to claim 1,
    Wherein the deposition is performed by a chemical vapor deposition process. &Lt; RTI ID = 0.0 &gt; 11. &lt; / RTI &gt;
  7. The method according to claim 6,
    Wherein the chemical vapor deposition process includes a low pressure chemical vapor deposition process, an atmospheric pressure chemical vapor deposition process, a metal organic chemical vapor deposition process, a plasma chemical vapor deposition process, an inductively coupled plasma process, an atomic layer deposition process, or a plasma atomic layer deposition process. A process for the preparation of kojnide.
  8. delete
  9. delete
  10. The method according to claim 1,
    In the deposition process, the pressure in the deposition chamber is controlled to adjust the amount of the chalcogen-containing precursor and the transition metal-containing precursor to be fed into the deposition chamber, so that the chalcogen-containing precursor to the transition metal- Wherein the partial pressure ratio is controlled.
KR1020150107443A 2015-07-29 2015-07-29 Preparing method of two-dimensional transition metal dichalcogenide KR101770235B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
KR1020150107443A KR101770235B1 (en) 2015-07-29 2015-07-29 Preparing method of two-dimensional transition metal dichalcogenide

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
KR1020150107443A KR101770235B1 (en) 2015-07-29 2015-07-29 Preparing method of two-dimensional transition metal dichalcogenide
JP2017561638A JP2018525516A (en) 2015-07-29 2016-07-28 Method for producing two-dimensional transition metal dichalcogenide thin film
PCT/KR2016/008303 WO2017018834A1 (en) 2015-07-29 2016-07-28 Method for manufacturing two-dimensional transition metal dichalcogenide thin film
US15/562,545 US10309011B2 (en) 2015-07-29 2016-07-28 Method for manufacturing two-dimensional transition metal dichalcogemide thin film

Publications (2)

Publication Number Publication Date
KR20170014319A KR20170014319A (en) 2017-02-08
KR101770235B1 true KR101770235B1 (en) 2017-08-22

Family

ID=58155785

Family Applications (1)

Application Number Title Priority Date Filing Date
KR1020150107443A KR101770235B1 (en) 2015-07-29 2015-07-29 Preparing method of two-dimensional transition metal dichalcogenide

Country Status (1)

Country Link
KR (1) KR101770235B1 (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019117559A1 (en) * 2017-12-13 2019-06-20 한양대학교 에리카산학협력단 Transition metal-dichalcogenide thin film and manufacturing method therefor

Also Published As

Publication number Publication date
KR20170014319A (en) 2017-02-08

Similar Documents

Publication Publication Date Title
US9963343B2 (en) Transition metal dichalcogenide alloy and method of manufacturing the same
Rong et al. Controlling sulphur precursor addition for large single crystal domains of WS 2
Yu et al. Synthesis of high quality two-dimensional materials via chemical vapor deposition
US9343533B2 (en) Direct formation of graphene on semiconductor substrates
Zhang et al. Dendritic, transferable, strictly monolayer MoS2 flakes synthesized on SrTiO3 single crystals for efficient electrocatalytic applications
Liu et al. Vapor-phase growth and characterization of Mo 1− x W x S 2 (0≤ x≤ 1) atomic layers on 2-inch sapphire substrates
US9355842B2 (en) Direct and sequential formation of monolayers of boron nitride and graphene on substrates
George et al. Wafer scale synthesis and high resolution structural characterization of atomically thin MoS2 layers
Lee et al. Synthesis of wafer-scale uniform molybdenum disulfide films with control over the layer number using a gas phase sulfur precursor
Lin et al. Wafer-scale MoS 2 thin layers prepared by MoO 3 sulfurization
EP3037569B1 (en) Mos2 thin film and method for manufacturing same
US9527062B2 (en) Process for scalable synthesis of molybdenum disulfide monolayer and few-layer films
Bosi Growth and synthesis of mono and few-layers transition metal dichalcogenides by vapour techniques: a review
Kumar et al. A predictive approach to CVD of crystalline layers of TMDs: the case of MoS 2
Park et al. ZnO nanoneedles grown vertically on Si substrates by non‐catalytic vapor‐phase epitaxy
Gaiduk et al. Chemical bath deposition of PbS nanocrystals: Effect of substrate
US9637839B2 (en) Synthesis and transfer of metal dichalcogenide layers on diverse surfaces
Zhang High-quality oriented ZnO films grown by sol–gel process assisted with ZnO seed layer
McDonnell et al. Atomically-thin layered films for device applications based upon 2D TMDC materials
US20110091647A1 (en) Graphene synthesis by chemical vapor deposition
US20110256386A1 (en) Fabrication of Large-Area Hexagonal Boron Nitride Thin Films
Jang et al. Wafer-scale, conformal and direct growth of MoS2 thin films by atomic layer deposition
Huang et al. Scalable high-mobility MoS 2 thin films fabricated by an atmospheric pressure chemical vapor deposition process at ambient temperature
US9028919B2 (en) Epitaxial graphene surface preparation for atomic layer deposition of dielectrics
US9984874B2 (en) Method of producing transition metal dichalcogenide layer

Legal Events

Date Code Title Description
A201 Request for examination
E902 Notification of reason for refusal
E701 Decision to grant or registration of patent right
GRNT Written decision to grant