KR101851578B1 - Preparing method single-crystal two-dimensional materlial having large-area - Google Patents

Preparing method single-crystal two-dimensional materlial having large-area Download PDF

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KR101851578B1
KR101851578B1 KR1020150054239A KR20150054239A KR101851578B1 KR 101851578 B1 KR101851578 B1 KR 101851578B1 KR 1020150054239 A KR1020150054239 A KR 1020150054239A KR 20150054239 A KR20150054239 A KR 20150054239A KR 101851578 B1 KR101851578 B1 KR 101851578B1
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single crystal
graphene
seeds
substrate
crystal
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KR1020150054239A
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Korean (ko)
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KR20160123725A (en
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황동목
이재현
임재영
장현식
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성균관대학교산학협력단
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/182—Graphene
    • C01B32/184—Preparation
    • C01B32/186—Preparation by chemical vapour deposition [CVD]
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/36—Carbides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Metallurgy (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Nanotechnology (AREA)

Abstract

Peeling the single crystal two-dimensional material grown on the first metal substrate to obtain a seed; Transferring the seeds to a second substrate; And a step of growing the transferred seed to obtain a large-area single-crystal two-dimensional material.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention [0001] The present invention relates to a method for manufacturing a large-area single crystal two-dimensional material,

The present invention relates to a method for producing large-area single crystal two-dimensional materials.

Two-dimensional materials composed of mono-layers are considered as next-generation materials because they have various characteristics. Mainly, the properties of two-dimensional materials are confirmed using a scotch tape stripping method, but a large area synthesis method is required for practical use. Conventionally, a two-dimensional material is synthesized through a process such as chemical vapor deposition (CVD). However, in this synthesis method, since the crystal orientation is not controlled during nucleation in the course of synthesis of two-dimensional materials, crystal grains grow in different crystal directions, and when grown crystals meet, crystal grains at various angles are formed. As a result, a polycrystalline two-dimensional material is formed, and defects are generated from the grain boundaries of the polycrystal, resulting in degradation of the properties of the two-dimensional material.

Examples of two-dimensional materials include graphenes. Currently, methods for producing graphene films include mechanical peeling of graphite, chemical peeling by graphene oxidation-reduction reaction, epitaxial growth on a silicon carbide substrate, Chemical vapor deposition on a metal catalyst layer, and the like. Among them, the CVD method can be regarded as a method of commercialization by manufacturing a large-area graphene at a low cost. In general, when a graphene film is manufactured by a CVD method, graphene is formed on a polycrystalline transition metal catalyst layer It is known that it is difficult for the grown graphene to become a single crystal over a large area.

On the other hand, Korean Patent Laid-Open No. 10-2009-0065206 discloses a single crystal graphene sheet using a lamination growth method and a manufacturing method thereof.

The present invention seeks to provide a method for producing a large-area single crystal two-dimensional material.

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.

One aspect of the present invention relates to a method of manufacturing a semiconductor device, comprising: peeling a single crystal two-dimensional material grown on a first metal substrate to obtain a seed; Transferring the seeds to a second substrate; And growing the transferred seed to obtain a large-area single-crystal two-dimensional material.

According to an embodiment of the present invention, it is possible to suppress the nucleation by controlling the temperature and the amount of the gas to form a single-crystal two-dimensional material on a desired growth substrate in a large area, and to provide a high-quality, large- Lt; / RTI >

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a flowchart schematically illustrating a process of forming a large-area single-crystal two-dimensional material in one embodiment of the present invention.
Figure 2 is an optical microscope image of a peeled seed transferred onto a copper foil, in one embodiment of the invention.
3 is an electron microscope image of a single-crystal two-dimensional material grown and encountered in one embodiment of the present invention.
4 is an electron microscope image of a large-area single-crystal two-dimensional material according to one embodiment of the present invention.

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 "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.

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.

The term " step " or " step of ~ " as used throughout the specification does not imply " 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".

Throughout this specification, the term "graphene " means that a plurality of carbon atoms are linked together by a covalent bond to form a polycyclic aromatic molecule, wherein the carbon atoms linked by the covalent bond are 6-membered rings A 5-membered ring, and / or a 7-membered ring. Thus, the sheet formed by graphene can be seen as a single layer of carbon atoms covalently bonded to each other, but is not limited thereto. The sheet formed by the graphene may have various structures, and the structure may vary depending on the content of the 5-membered ring and / or the 7-membered ring which may be contained in the graphene. When the sheet formed by the graphene is a single layer, they may be laminated to form a plurality of layers, and the side end portion of the graphene sheet may be saturated with hydrogen atoms, but the present invention is not limited thereto.

Hereinafter, a manufacturing method of the large-area single crystal two-dimensional material of the present invention will be described in detail with reference to the embodiments, examples and drawings. However, the present invention is not limited to these embodiments and examples and drawings.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a flowchart schematically illustrating a manufacturing process of a large-area single-crystal two-dimensional material according to one embodiment of the present invention.

One aspect of the present invention is a method of fabricating a semiconductor device, comprising: (S10) peeling a single crystal two-dimensional material 200 grown on a first metal substrate 100 to obtain a seed 210; Transferring the seed 210 to the second substrate 300 (S20); And a step (S30) of growing the transferred seed to obtain a large-area single-crystal two-dimensional material (S30).

In one embodiment of the present invention, the first metal substrate 100 is made of a metal such as Ge, Cu, Ni, Co, Fe, Pt, Au, Al, Cr, Mg, Mn, Mo, Rh, Si, , U, V, Zr, and combinations thereof, but is not limited thereto. The first metal substrate 100 is a material capable of forming the single crystal two-dimensional material 200, and the atoms are aligned with the atoms of the single-crystal two-dimensional material 200, May be used without limitation as long as the seeds do not form crystal grains when they are combined, and may act as a catalyst for growing the single crystal two-dimensional material 200.

In one embodiment of the present invention, the single crystal two-dimensional material 200 may be grown by chemical vapor deposition (CVD), but the present invention is not limited thereto. , Rapid thermal chemical vapor deposition (RTCVD), inductively coupled plasma-chemical vapor deposition (ICP-CVD), low pressure chemical vapor deposition (LPCVD) (APCVD), metal organic chemical vapor deposition (MOCVD), or plasma-enhanced chemical vapor deposition (PECVD), etc. However, But is not limited thereto.

In one embodiment of the present invention, the seeds 210 may be peeled from the single-crystal two-dimensional material, but the present invention is not limited thereto.

In one embodiment of the present invention, the single crystal two-dimensional material 200 may be graphene, hexagonal boron nitride (h-BN), or transition metal dichalcogenide (TMD) , But is not limited thereto. The transition metal dicalcogenide may be represented by the formula MX 2 , where M may be a transition metal material, for example, Mo, Ti, V, or W, As the cogent material, there may be, but is not limited to, for example, S, Se, or Te. The transition metal radical chalcogenides include, for example, MoS 2, TiS 2, VS 2, WS 2, MoSe 2, TiSe 2, VSe 2, WSe 2, MoTe 2, TiTe 2, VTe 2, or WTe 2 is in But is not limited thereto. The seed 210 and the large-area single-crystal two-dimensional material 220 may be the same material as the single-crystal two-dimensional material 200.

In one embodiment of the invention, the second substrate 300 may be one comprising a metal or an insulator, e.g., Pt, Cu, Ni, Ru, SiO 2, Al 2 O 3, SnO 2, AlO x N x , and combinations thereof. < / RTI > The second base material 300 may be made of the same material as the first base material, but is preferably a material difficult to synthesize a single crystal of a single-crystal two-dimensional material due to problems such as atomic arrangement or a material favorable for a price or a large area. And may act as a catalyst for growing the seed 210. In addition, the second substrate may be in the form of a thin film or a foil, but is not limited thereto.

In one embodiment of the present invention, the method may further include forming a metal layer on the second substrate before transferring the seed 210, but the present invention is not limited thereto. The metal layer may be formed to minimize impurities. For example, the metal layer may be Au or Ni, but is not limited thereto.

In one embodiment of the present invention, the step (S30) of growing the seed 210 to obtain a large-area single-crystal two-dimensional material 220 includes: a step of forming a plurality of seeds 210 in the same crystal orientation To grow the seeds, but the present invention is not limited thereto. The seeds 210 may be arranged in two or more identical crystal directions. The seed 210 may be grown by growing the seed 210 by supplying a reactive gas or a reactive powder.

In one embodiment of the present invention, the step of removing the impurities of the second substrate 300 to which the seed 210 has been transferred by an acid or etching treatment before growing the seed 210 But is not limited thereto. The acid may be, but is not limited to, an acidic material selected from the group consisting of, for example, nitric acid (HNO 3 ), hydrochloric acid (HCl), hydrofluoric acid (HF), and combinations thereof. The etch process may be performed using an etchant to remove the formed metal layer. For example, the etchant may include Au etchant or Ni etchant. However, It is not.

In one embodiment of the invention, the method further comprises heat treating the second substrate 300, onto which the seed 210 has been transferred, before growing the seed 210 at a temperature ranging from about 500 ° C to about 2,000 ° C But it is not limited thereto and can be applied without limitation if it is at a temperature of about 500 ° C or higher and lower than the melting point of the second substrate. For example, the heat treatment temperature may range from about 500 ° C to about 2,000 ° C, from about 500 ° C to about 1,800 ° C, from about 500 ° C to about 1,600 ° C, from about 500 ° C to about 1,400 ° C, From about 500 ° C to about 800 ° C, from about 500 ° C to about 600 ° C, from about 600 ° C to about 2,000 ° C, from about 700 ° C to about 1,500 ° C, or from about 800 ° C to about 1,000 ° C But is not limited thereto.

In an embodiment of the present invention, the H 2 gas and the inert gas may be supplied during the heat treatment, and the reaction gas or the reaction powder may be supplied during the growth of the seed 210. However, the present invention is not limited thereto. The seed 210 is grown by supplying the reaction gas or the reactive powder to the second substrate 300 to which the seed 210 having been thermally treated while supplying the H 2 gas and the inert gas is transferred to form a large- (220) can be obtained. Before the growth of the seed 210, nucleation can be suppressed by pretreatment by heat treatment using the H 2 gas and an inert gas. As a result, the seed 210 can be grown without grain boundaries, Dimensional material 220 can be produced. Also, the energy state of the edge of the single-crystal two-dimensional material can be controlled through the heat treatment. The inert gas may be, for example, Ar, N 2 , He, Ne, or Xe, but is not limited thereto.

In one embodiment of the invention, the reaction gas or reactive powder may comprise a gas selected from the group consisting of a carbon source, a transition metal source, a chalcogen source, a boron source, a nitrogen source, and combinations thereof , But is not limited thereto. The carbon source may be, for example, carbon monoxide, carbon dioxide, methane, ethane, ethylene, ethanol, acetylene, propane, butane, butadiene, pentane, pentene, cyclopentadiene, hexane, cyclohexane, benzene, But is not limited thereto. The transition metal source or chalcogen source may include, for example, Zr, Se, Ta, S, Nb, V, W, Mo, Ti, Te, Ga, no.

In one embodiment of the invention, the reaction gas, H 2 gas, and inert gas may be supplied at a flow rate ranging from about 0.01 to about 1: about 200 to about 400: about 200 to about 400, But is not limited thereto. For example, the feed flow rate of the reactive gas, H 2 gas, and inert gas comprising the carbon source may be from about 0.01 to about 1: about 200 to about 400: about 200 to about 400, about 0.05 to about 1: about 250 From about 250 to about 400, from about 0.3 to about 1: from about 300 to about 400: from about 300 to about 400, from about 0.5 to about 400, from about 250 to about 350, from about 0.1 to about 1: 1: about 350 to about 400: about 350 to about 400, about 0.01 to about 0.5: about 200 to about 350: about 200 to about 350, about 0.01 to about 0.1: about 200 to about 300: Or from about 0.01 to about 0.05: from about 200 to about 250: from about 200 to about 250, but are not limited thereto.

In one embodiment of the invention, the gas supply pressure may range from about 1 Torr to about 760 Torr, but is not limited thereto. For example, the pressure may range from about 1 Torr to about 760 Torr, from about 10 Torr to about 760 Torr, from about 100 Torr to about 760 Torr, from about 150 Torr to about 760 Torr, from about 200 Torr to about 760 Torr, About 700 Torr to about 700 Torr, about 100 Torr to about 700 Torr, about 100 Torr to about 760 Torr, about 600 Torr to about 760 Torr, about 700 Torr to about 760 Torr, But is not limited to, about 600 Torr, about 100 Torr to about 500 Torr, about 100 Torr to about 400 Torr, about 100 Torr to about 300 Torr, or about 100 Torr to about 200 Torr.

In one embodiment of the present invention, the growth of the seed 210 may be performed by chemical vapor deposition (CVD), but the present invention is not limited thereto. The chemical vapor deposition may be performed, for example, (RTCVD), inductively coupled plasma-chemical vapor deposition (ICP-CVD), low pressure chemical vapor deposition (LPCVD), atmospheric pressure chemical vapor deposition (APCVD), metal organic chemical vapor deposition (MOCVD), or plasma-enhanced chemical vapor deposition (PECVD), and the like. But is not limited to.

In one embodiment of the present invention, large-area single crystal two-dimensional material 220 having no defects and grain boundaries can be produced by suppressing nucleation by controlling the heat treatment temperature and controlling the amount of gas. The grain boundary refers to a boundary between single crystals, and the inhibition of nucleation may mean inhibition of nucleation at a portion excluding the seed. The large-area monocrystalline two-dimensional material 220 formed on the second substrate 300 may be the same single-crystal two-dimensional material as the monocrystalline two-dimensional material 200 grown on the first metal substrate 100 .

Hereinafter, the present invention will be described in detail with reference to examples, but the present invention is not limited thereto.

[ Example ]

The single crystal graphene seeds were peeled from the single crystal graphene synthesized on the germanium (110) wafer as the first metal base material and transferred to the copper foil as the second base material. The graphene seed transferred onto the copper foil can be confirmed through an optical microscope (Olympus, BX51M) image of FIG. The impurities generated during the transferring process were removed through nitric acid treatment, and the copper foil from which the impurities were removed was annealed at 1,000 DEG C while supplying H 2 gas under an Ar atmosphere and a pressure of 100 torr in order to prevent nucleation of the graphene. Thereafter, the substrate was oxidized in a hot plate at 200 ° C. for 6 hours in air to form a condition that the seeds transferred onto the copper foil could be well grown. Thereafter, LPCVD was performed using CH 4 gas as a reaction gas Large - area single crystal two - dimensional material was grown.

The growth was inhibited by nucleation of the graphene by the manufacturing method according to the present embodiment. Thus, it was confirmed by the image of the battery microscope of FIGS. 3 and 4 that the grain boundaries were not formed. 3 shows an electron microscope image (JEOL-Korea, FE-SEM 7601) when graphene seeds grow on the copper base material and meet each other. As shown in FIG. 4, As an electron microscope image of the area single crystal two-dimensional material, it can be confirmed that the finally obtained large area single crystal two-dimensional material and grain boundary system are not present.

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 interpreted as being included in the scope of the present invention .

100: First metal substrate
200: single crystal two-dimensional substance 210: seed
220: large-area single crystal two-dimensional substance 300: second substrate

Claims (9)

Peeling a portion of the monocrystalline graphene grown on the monocrystalline first metal substrate to obtain a plurality of single crystal graphene seeds;
Aligning the separated plurality of single crystal graphene seeds in the same crystal direction on the second polycrystalline substrate and transferring the same;
Annealing and pretreating the polycrystalline second substrate to which the plurality of single crystal graphene seeds have been transferred; And
And a step of growing the transferred plurality of single crystal graphene seeds to obtain a large-area single crystal graphene,
Wherein the large-area single-crystal graphene suppresses nucleation during growth of a plurality of single-crystal graphene seeds transferred to the polycrystalline second substrate, so that defects and grain boundaries are not formed.
Method of manufacturing large area single crystal graphene.
The method according to claim 1,
The first monocrystalline first metal substrate may be at least one of Ge, Cu, Ni, Co, Fe, Pt, Au, Al, Cr, Mg, Mn, Mo, Rh, Si, Ta, Ti, W, ≪ / RTI > and combinations thereof.
delete The method according to claim 1,
The polycrystalline second substrate of, large area single crystal graphene comprises a material selected from the group consisting of Pt, Cu, Ni, Ru, SiO 2, Al 2 O 3, SnO 2, and combinations thereof Gt;
delete The method according to claim 1,
And removing the impurities of the polycrystalline second base material onto which the plurality of monocrystalline graphene seeds have been transferred by acid or etching treatment before growing the plurality of monocrystalline graphene seeds, ≪ / RTI >
The method according to claim 1,
Wherein the annealing is performed at a temperature in the range of 500 < 0 > C to 2,000 < 0 > C.
The method according to claim 1,
And supplying the H 2 gas and the inert gas during the annealing and supplying the reaction gas or the reaction powder during the growth of the plurality of single crystal graphene seeds.
9. The method of claim 8,
And supplying the reaction gas, the H 2 gas, and the inert gas at a flow rate in the range of 0.01 to 1: 200 to 400: 200 to 400.
KR1020150054239A 2015-04-17 2015-04-17 Preparing method single-crystal two-dimensional materlial having large-area KR101851578B1 (en)

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