KR101503733B1 - Method of synthesis metal sulfide with 3d structure using atomic layer deposition metal oxide - Google Patents

Method of synthesis metal sulfide with 3d structure using atomic layer deposition metal oxide Download PDF

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KR101503733B1
KR101503733B1 KR20140006786A KR20140006786A KR101503733B1 KR 101503733 B1 KR101503733 B1 KR 101503733B1 KR 20140006786 A KR20140006786 A KR 20140006786A KR 20140006786 A KR20140006786 A KR 20140006786A KR 101503733 B1 KR101503733 B1 KR 101503733B1
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South Korea
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heat treatment
metal
sulfide
silicon
metal sulfide
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KR20140006786A
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Korean (ko)
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김형준
박주상
송정규
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연세대학교 산학협력단
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/40—Oxides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45523—Pulsed gas flow or change of composition over time
    • C23C16/45525—Atomic layer deposition [ALD]
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/56—After-treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites

Abstract

The present invention relates to a method for forming a metal sulfide steric structure, which comprises depositing a metal oxide on a three-dimensional shape by atomic layer deposition, and synthesizing a metal sulfide corresponding to a three-dimensional shape by sulfiding the deposited metal oxide.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for forming a three-dimensional structure of a metal sulfide using a metal oxide deposited by an atomic layer deposition method. BACKGROUND ART < RTI ID = 0.0 >

The present invention relates to a method for forming a three-dimensional structure of a metal sulfide using a metal oxide deposited by atomic layer deposition.

BACKGROUND ART Transition metal dicalcogenide compounds (TMDs), which are two-dimensional layered semiconductor materials, have recently attracted attention as new functional nanomaterials. The TMDs material is a structure (MX 2 ) in which a metal atom (M) layer is sandwiched between chalcogen atom (X) layers and has a three-dimensional structure through a covalent bond in the interior and a van der Waals force between the MX 2 layers. Recent studies on WS 2 among TMD materials are underway. WS 2 can control the optical and electrical properties according to the thickness, and WS 2 having a three-dimensional shape can be expected to have improved optical characteristics because of its wide surface area. However, in the conventional method, it is not easy to control the thickness of WS 2 and to deposit it in a large area.

An object of the present invention is to provide a method of forming a three-dimensional structure of tungsten disulfide using atomic layer deposition.

The technical problem of the present invention is not limited to the above-mentioned technical problems, and other technical problems which are not mentioned can be clearly understood by those skilled in the art from the following description.

A method of forming a three-dimensional structure of a metal sulfide according to an embodiment of the present invention includes the steps of depositing a metal oxide (MO x ) on a three-dimensional shape by atomic layer deposition, and sulfiding the deposited metal oxide, And synthesizing a metal sulfide ( MSy ).

In an embodiment, the step of depositing the metal oxide comprises the steps of: supplying the metal source gas into a deposition chamber to adsorb the metal source gas onto the substrate; a second step of supplying and purge a purge gas; A third step of supplying an oxidizing gas to induce a reaction with the adsorbed metal source gas to deposit a metal oxide, and a fourth step of supplying purge gas and purging the purge gas.

In the embodiment, the step of synthesizing the metal sulfide may include a first heat treatment step of heat-treating the three-dimensional shape in hydrogen and an inert gas atmosphere, a second heat treatment step of heat-treating the three-dimensional shape in hydrogen gas and an inert gas atmosphere, And cooling in an inert gas atmosphere.

The method for fabricating metal sulfide nanotubes according to an embodiment of the present invention includes depositing a metal oxide on a silicon nanowire using atomic layer deposition, synthesizing a metal sulfide by sulfiding the deposited metal oxide, As shown in FIG.

In an embodiment, the step of depositing the metal oxide may further include heat treating the silicon nanowire in an oxygen atmosphere to form a silicon oxide layer.

In an embodiment, the step of forming the silicon oxide layer may be performed by heat-treating at 800 to 1000 ° C for 30 to 90 minutes in an oxygen atmosphere.

In an embodiment, in the step of depositing the metal oxide using atomic layer deposition, the metal source gas may include a metal organic precursor (bisisopropylcyclopentadienyl tungsten dihydride (WH 2 (iPrCp) 2 ), W (CO) 6 , Mo (CO) 6 ) is used as the oxygen source, and water, ozone, and oxygen plasma are used as the oxygen source.

In an embodiment, the step of synthesizing the metal oxide may include a heat treatment in hydrogen and an inert gas atmosphere, a heat treatment in hydrogen gas and an inert gas atmosphere, and a cooling in an inert gas atmosphere.

In an embodiment, the step of removing the silicon nanowires may be performed by treating the silicon nanowires with hydrogen fluoride (HF) and etching the silicon nanowires and the silicon oxide layer.

The tungsten disulfide nanotube according to an embodiment of the present invention can be manufactured by the above method.

According to one aspect of the present invention, atomic layer deposition can be used to form a metal sulfide, for example, a ternary structure of tungsten disulfide.

According to one aspect of the present invention, thickness control can be facilitated when forming the three-dimensional structure of the metal sulfide.

The effects of the present invention are not limited to the above-mentioned effects, and the effects not mentioned can be clearly understood by those skilled in the art from the present specification and the accompanying drawings.

1 is a view for explaining a method of forming a three-dimensional structure of a metal sulfide according to an embodiment of the present invention.
FIGS. 2 and 3 are views for explaining a method of manufacturing a tungsten disulfide nanotube according to an embodiment of the present invention.
4 is a scanning electron microscope (SEM) image of a tungsten disulfide nanotube fabricated by the method of manufacturing a metal sulfide nanotube according to an embodiment of the present invention.
FIGS. 5 and 6 are photographs of a tungsten disulfide nanotube produced by the method of manufacturing a metal sulfide nanotube according to an embodiment of the present invention by a transmission electron microscope.
FIGS. 7 and 8 show results of EDS analysis to confirm the composition of tungsten disulfide nanotubes produced by the method of manufacturing a metal sulfide nanotube according to an embodiment of the present invention.

Other advantages and features of the present invention and methods of achieving them will become apparent with reference to the embodiments described below in detail with reference to the accompanying drawings. The present invention may, however, be embodied in many different forms and should not be construed as being limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of the invention to those skilled in the art. Is provided to fully convey the scope of the invention to those skilled in the art, and the invention is only defined by the scope of the claims.

Unless defined otherwise, all terms (including technical or scientific terms) used herein have the same meaning as commonly accepted by the generic art in the prior art to which this invention belongs. Terms defined by generic dictionaries may be interpreted to have the same meaning as in the related art and / or in the text of this application, and may be conceptualized or overly formalized, even if not expressly defined herein I will not.

The terminology used herein is for the purpose of illustrating embodiments and is not intended to be limiting of the present invention. In the present specification, the singular form includes plural forms unless otherwise specified in the specification. As used herein, the terms' comprise 'and / or various forms of use of the verb include, for example,' including, '' including, '' including, '' including, Steps, operations, and / or elements do not preclude the presence or addition of one or more other compositions, components, components, steps, operations, and / or components.

The term 'and / or' as used herein refers to each of the listed configurations or various combinations thereof.

The present invention relates to a method for forming a metal sulphide, for example tungsten disulfide, using metal oxide deposited using atomic layer deposition, for example tungsten dioxide. According to an embodiment of the present invention, a metal oxide (e.g., tungsten dioxide) is deposited on the steric structure using atomic layer deposition, and a metal sulfide (e.g., tungsten dioxide) Tungsten disulfide), a metal sulfide (for example, tungsten disulfide) capable of controlling the thickness and synthesizing in a large area can be obtained. Then, the deposited three-dimensional structure can be removed to form a three-dimensional structure of the metal sulfide (for example, tungsten disulfide).

1 is a view for explaining a method of forming a three-dimensional structure of a metal sulfide according to an embodiment of the present invention. The method of forming a three-dimensional structure of a metal sulfide according to an embodiment of the present invention can be applied to various metal sulfides such as tungsten disulfide and molybdenum disulfide.

As shown in FIG. 1, a method of forming a three-dimensional structure of a metal sulfide according to an embodiment of the present invention includes depositing a metal oxide on a three-dimensional shape using atomic layer deposition (S10), sulfiding the deposited metal oxide (S20) of synthesizing the metal sulfide corresponding to the metal sulfide and removing the three-dimensional shape (S30). The three-dimensional structure may be, for example, a three-dimensional structure having nanoscale such as nanowire, nano rod, and nanoparticle. However, the three-dimensional structure is not limited to this, and may include a three-dimensional structure of arbitrary shape. The material of the three-dimensional structure is not particularly limited.

The step S10 of depositing the metal oxide on the three-dimensional shape using the atomic layer deposition method includes a metal source gas adsorption step S12, an inert gas purging step S14, a step of depositing a metal oxide by supplying an oxygen source And an inert gas purging step (S18).

The metal source gas adsorption step (S12) is performed by supplying a source gas containing a metal into the deposition chamber. In an embodiment, the metal source gas may comprise tungsten or molybdenum. In an embodiment, a metal organic precursor (bisisopropylcyclopentadienyl tungsten dihydride (WH 2 (iPrCp) 2 ), W (CO) 6 can be used as a source gas comprising tungsten and a source gas comprising molybdenum (CO) 6 ) may be used as the metal organic precursor. The metal organic precursor may be carried by inert gas at about 25-100 < 0 > C. As the inert gas, for example, argon, nitrogen and the like can be used.

As an oxygen source, water, ozone, and oxygen plasma may be used as an example of the step of supplying the oxygen source and depositing the metal oxide (S16).

The inert gas purging step S14 removes the unadsorbed metal source gas in the metal source gas adsorption step S12 and the inactive gas purging step S18 in the step S16 of supplying the oxygen source to deposit the metal oxide The unreacted oxygen source and by-products present in the chamber can be removed.

The ratio of the processing time of the metal source gas adsorption step (S12), the inert gas purge step (S14), the supply of the oxygen source to the deposition of the metal oxide (S16) and the inert gas purge step (S18) ~ 5: 5 ~ 12: 3 ~ 5: 5 ~ 12.

The step (S20) of sulfiding the deposited metal oxide into a metal sulfide includes a first heat treatment step (S22) for performing heat treatment in hydrogen and an inert atmosphere, a second heat treatment step (S24) for heat treatment in a hydrogen gas atmosphere and an inert gas atmosphere, (S26). ≪ / RTI >

According to an embodiment of the present invention, the first heat treatment step (S22) is carried out at 300 to 500 DEG C for 30 to 60 minutes in the hydrogen and inert gas atmosphere. The hydrogen gas and the inert gas may be supplied at 10 to 30 sccm each, respectively.

According to an embodiment of the present invention, the second heat treatment step (S24) is conducted at 700 to 1000 DEG C for 30 to 60 minutes in the atmosphere of hydrogen sulfide and an inert gas. The hydrogen sulfide is supplied at 5 to 30 sccm and the inert gas is supplied at 30 to 50 sccm.

According to an embodiment of the present invention, the step of cooling (S26) in the argon atmosphere may be carried out by supplying 30 to 50 sccm of inert gas at room temperature.

According to embodiments of the present invention, nanostructures can be used in a three dimensional structure in which metal sulfides are deposited. For example, silicon nanowires can be used in a three-dimensional structure. 2 and 3, a method for producing metal sulfide nanotubes using nanostructures with a three-dimensional structure will be described. The steps of depositing a metal oxide using an atomic layer deposition method to form a metal sulfide nanotube, and synthesizing a metal oxide as a sulfide are described with reference to FIGS. 1 and 2.

FIGS. 2 and 3 are views for explaining a method of manufacturing a metal sulfide nanotube according to an embodiment of the present invention.

As shown in FIG. 2, a method of manufacturing a metal sulfide nanotube according to an embodiment of the present invention includes a step (S110) of forming a silicon oxide layer by annealing a nano wire, for example, a silicon nanowire in an oxygen atmosphere, A step S130 of depositing a metal oxide on the silicon oxide layer by using the metal oxide to be deposited on the silicon oxide layer, a step S130 of synthesizing a metal sulfide by sulfiding the deposited metal oxide on the silicon oxide layer, (S140).

The step of depositing a metal oxide on the silicon oxide layer using the atomic layer deposition method (S120) may be performed by depositing a metal oxide on the three-dimensional shape of FIG. 1 (S10).

Step S130 of synthesizing a metal sulfide by sulfiding the deposited metal oxide may be performed by the step of sulfiding the deposited metal oxide of FIG. 1 into a metal sulfide (S20).

Referring to FIGS. 2 and 3, a nanowire, for example, a silicon nanowire 10 is provided. When the silicon nanowire 10 is heat-treated in an oxygen atmosphere, a silicon oxide (SiO 2 ) layer is formed and a silicon oxide / silicon nanowire 20 is formed (S 110).

A metal oxide / silicon oxide / silicon nanowire is formed when the metal oxide is deposited on the formed silicon oxide / silicon nanowire 20 using atomic layer deposition (S120). Then, when the formed metal oxide is sulfided, it is formed on the metal sulfide / silicon oxide / silicon nanowire 30.

Finally, the metal sulfide tungsten nanotube 40 can be manufactured by immersing the formed metal oxide / silicon oxide / silicon nanowire 30 in hydrogen fluoride to remove silicon oxide / silicon nanowire by etching.

FIGS. 4 to 8 illustrate tungsten disulfide nanotubes produced by the method of manufacturing a metal sulfide nanotube according to an embodiment of the present invention.

Metallic organic precursors (bisisopropylcyclopentadienyl tungsten dihydride (WH 2 (iPrCp) 2 ) and W (CO) 6 were used as the metal source gas, RTI ID = 0.0 > argon < / RTI >

An oxygen plasma was used as the oxygen source.

4 is a scanning electron microscope (SEM) image of a tungsten disulfide nanotube fabricated by the method of manufacturing a metal sulfide nanotube according to an embodiment of the present invention. Transparency shows that the nanotubes are well formed.

FIGS. 5 and 6 are photographs of a tungsten disulfide nanotube produced by the method of manufacturing a metal sulfide nanotube according to an embodiment of the present invention by a transmission electron microscope. Referring to FIGS. 5 and 6, it can be seen that tungsten disulfide can be synthesized by adjusting the thickness. In the experiment, tungsten disulfide was synthesized to be four layers.

FIGS. 7 and 8 show results of energy dispersive X-ray spectroscopy (EDS) analysis to confirm the composition of the tungsten disulfide nanotubes produced by the method of manufacturing a metal sulfide nanotube according to an embodiment of the present invention. Referring to FIG. 7, the distribution of tungsten can be confirmed, and the distribution of sulfur can be confirmed with reference to FIG.

It is to be understood that the above-described embodiments are provided to facilitate understanding of the present invention, and do not limit the scope of the present invention, and it is to be understood that various modifications may be made within the scope of the present invention. For example, each component shown in the embodiment of the present invention may be distributed and implemented, and conversely, a plurality of distributed components may be combined. Therefore, the technical protection scope of the present invention should be determined by the technical idea of the claims, and the technical protection scope of the present invention is not limited to the literary description of the claims, The invention of a category.

Claims (19)

delete delete delete delete Depositing a metal oxide over the silicon nanowire using atomic layer deposition;
Sulfiding the deposited metal oxide to synthesize a metal sulfide; And
Removing the silicon nanowires;
≪ / RTI >
6. The method of claim 5,
Prior to the step of depositing the metal oxide,
Heat treating the silicon nanowires in an oxygen atmosphere to form a silicon oxide layer;
Wherein the metal sulfide nanotubes further comprise a metal sulfide nanotube.
The method according to claim 6,
The step of forming the silicon oxide layer
Followed by heat treatment at 800 to 1000 占 폚 for 30 to 90 minutes in an oxygen atmosphere.
6. The method of claim 5,
The step of depositing the metal oxide
Metalorganic precursor gas bis-isopropyl-cyclopentadienyl tungsten di-hydride as a metal source (WH 2 (iPrCp) 2) , W (CO) 6, or Mo (CO) using a 6, and water as the oxygen source, ozone, Method of fabricating metal sulfide nanotubes using oxygen plasma.
6. The method of claim 5,
The step of synthesizing the metal sulfide
A first heat treatment step of performing heat treatment at a first temperature; And,
And a second heat treatment step of performing heat treatment at a second temperature higher than the first temperature.
10. The method of claim 9,
And cooling the metal sulfide nanotubes in an inert atmosphere after the second heat treatment step.
11. The method of claim 9 or 10,
Wherein the first heat treatment step is carried out in an atmosphere of hydrogen and an inert gas,
Wherein the second heat treatment step is performed in a hydrogen sulfide and an inert gas atmosphere.
12. The method of claim 11,
Wherein the first heat treatment step is performed at the first temperature of 300 to 500 DEG C for 30 to 60 minutes.
12. The method of claim 11,
Wherein the second heat treatment step is performed at the second temperature of 700 to 1000 占 폚 for 30 to 60 minutes.
6. The method of claim 5,
The step of removing the silicon nanowires comprises:
Wherein the silicon nano-wire is treated with hydrogen fluoride (HF) to etch the silicon nano-wire and the silicon oxide layer.
A metal sulfide nanotube produced by the method of claim 14.
Depositing tungsten oxide over the silicon nanowire using atomic layer deposition;
Sulfiding the deposited tungsten oxide to synthesize tungsten sulfide; And
Removing the silicon nanowires;
≪ / RTI >
17. The method of claim 16,
The step of synthesizing the tungsten sulfide
Heat treating the substrate at a first temperature in a hydrogen and argon gas atmosphere; And,
And a heat treatment at a second temperature higher than the first temperature in an atmosphere of hydrogen sulfide and argon gas
Method for manufacturing tungsten sulfide nanotubes.
18. The method of claim 17,
Hydrogen gas and an inert gas are supplied at 10 to 30 sccm, respectively, in the first heat treatment step, and the first heat treatment step is performed at 300 to 500 ° C for 30 to 90 minutes.
The method according to claim 17 or 18,
Wherein the hydrogen gas is supplied at 5 to 30 sccm and the inert gas is supplied at 30 to 50 sccm in the second heat treatment step and the second heat treatment is performed at 700 to 1000 ° C for 30 to 60 minutes.


KR20140006786A 2014-01-20 2014-01-20 Method of synthesis metal sulfide with 3d structure using atomic layer deposition metal oxide KR101503733B1 (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100310461B1 (en) 1994-12-20 2001-12-15 박종섭 Method for forming silicon oxide
WO2002088024A1 (en) * 2001-04-30 2002-11-07 University Of Sussex Nanotubes
KR20030097125A (en) * 2002-06-19 2003-12-31 삼성전자주식회사 Manufacturing method of inorganic nano tube
KR20080009528A (en) * 2006-07-24 2008-01-29 삼성전자주식회사 Method for thin film

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100310461B1 (en) 1994-12-20 2001-12-15 박종섭 Method for forming silicon oxide
WO2002088024A1 (en) * 2001-04-30 2002-11-07 University Of Sussex Nanotubes
KR20030097125A (en) * 2002-06-19 2003-12-31 삼성전자주식회사 Manufacturing method of inorganic nano tube
KR20080009528A (en) * 2006-07-24 2008-01-29 삼성전자주식회사 Method for thin film

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