KR101742388B1 - Method for Synthesizing Transition Metal Chalcogenide Using CVD - Google Patents

Method for Synthesizing Transition Metal Chalcogenide Using CVD Download PDF

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KR101742388B1
KR101742388B1 KR1020150149510A KR20150149510A KR101742388B1 KR 101742388 B1 KR101742388 B1 KR 101742388B1 KR 1020150149510 A KR1020150149510 A KR 1020150149510A KR 20150149510 A KR20150149510 A KR 20150149510A KR 101742388 B1 KR101742388 B1 KR 101742388B1
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transition metal
cocl2
cvd
vacuum chamber
compound
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KR20170048873A (en
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김형준
김영준
송정규
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연세대학교 산학협력단
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00—Sulfur; Compounds thereof
    • C01B17/20—Methods for preparing sulfides or polysulfides, in general
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00—Selenium; Tellurium; Compounds thereof
    • C01B19/007—Tellurides or selenides of metals
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00—Compounds of molybdenum
    • C01G39/04—Halides
    • 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

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Abstract

A method of synthesizing a transition metal chalcogen compound using CVD is disclosed. The disclosed method comprises: (a) preparing a vacuum chamber loaded with an alkali metal salt; And (b) injecting a precursor having a halide ligand and a reactant into the vacuum chamber to synthesize a transition metal chalcogenide compound by CVD. According to the disclosed method, it is possible to synthesize a transition metal chalcogenide compound by CVD at a high speed, and the carbon component can be efficiently removed when a substance having an organic ligand roll as a reaction material is used.

Description

[0001] The present invention relates to a method for synthesizing a transition metal chalcogenide compound using CVD,

Embodiments of the present invention are directed to methods for synthesizing chalcogen compounds, and more particularly to methods for synthesizing chalcogen compounds using a chemical vapor deposition (CVD) technique.

Transition metal chalcogen compounds have high electric mobility and excellent on-off characteristics and are expected to be used in various applications. In particular, the transition metal chalcogenide compound has an advantage of being suitable for use as a thin film transistor, flexible display to realize a flexible display due to its flexibility.

These transition metal chalcogen compounds can be synthesized in various ways, and when synthesized by CVD, there is a problem that the productivity is lowered due to the slow reaction rate.

Also, when a transition metal chalcogen compound is synthesized by CVD, a transition metal chalcogen compound is synthesized by a reaction between a reactant and a precursor. In the case where the reactant is a substance having an organic ligand, a transition metal chalcogen compound There is a problem that the carbon component can not be efficiently removed.

One aspect of the present invention is to propose a method for synthesizing transition metal chalcogen compounds by CVD at high speed.

Another aspect of the present invention is to propose a method of synthesizing a transition metal chalcogenide compound in which a carbon component can be efficiently removed when a substance having an organic ligand roll as a reaction material is used.

According to an aspect of the present invention, there is provided a method of manufacturing a semiconductor device, comprising: (a) preparing a vacuum chamber loaded with an alkali metal salt; And a step (b) of synthesizing a transition metal chalcogenide compound by CVD by injecting a precursor having a halide ligand and a reaction material into the vacuum chamber.

The alkali metal salt includes any one of NaCl, Na 2 CO 3 , KNO 3 , and LiBr.

The reactant may include a reactant having an organic ligand.

The transition metal chalcogen compound is deposited on an amorphous substrate in the vacuum chamber.

The precursor includes any one transition metal selected from Ti, Hf, Zr, V, Nb, Ta, Mo, W, Tc, Re, Co, Rh, Ir, Ni, Pd, Pt, Zn and Sn.

 The precursor may be selected from the group consisting of TiCl4, TiF4, TiI4, HfCl4, HfCp2Me2, HfI4, Hf (CpMe) 2 (OMe) Me, ZrCl4, ZrI4, VCl3, VoCl3, NbCl5, TaCl5, TaF5, TaI5, MoCl5, Mo CoCp2, CoCp2, RhCl5, IrCl3, NiCl2, Ni (acac) 2, NiCp2, PdCl2, Pd, CoCl2, CoCl2, CoCl2, CoCl2, CoCl2, CoCl2, CoCl2, CoCl2, CoCl2, CoCl2, RhCl5, IrCl3, WF4, WF6, WOCl4, TcCl4, ReCl4, ReCl5, ReCl6, (thd) 2, PtCl2, ZnCl2, ZnMe2, ZnEt2, ZnI2, SnCl2, SnCl4 and SnI4.

The reactive material comprises at least one chalcogenide element selected from S, Se and Te.

The reactant may be selected from the group consisting of sulfur powder, H2S, diethyl sulfide, dimethyl disulfide, ethyl methyl sulfide, Et3Si2S, selenium powder ), Selenium hydrogen sulphide (H2Se), diethyl selenide, dimethyl diselenide, ethyl methyl selenide, (Et3Si) 2Se, Telenium powder, And includes one of hydrogen peroxide (H2Te), dimethyl telluride, diethyl telluride, ethyl methyl telluride and (Et3Si) 2Te.

According to another aspect of the present invention, there is provided a method for preparing a catalyst, comprising: preparing an alkali metal salt as a catalyst; There is provided a method for synthesizing a transition metal chalcogenide compound, which comprises synthesizing a transition metal chalcogenide compound by CVD using a precursor and a reaction material with the prepared alkali metal salt as a catalyst.

According to the present invention, it is possible to synthesize a transition metal chalcogenide compound by CVD at a high speed, and the carbon component can be efficiently removed when a substance having an organic ligand roll as a reaction material is used.

BRIEF DESCRIPTION OF THE DRAWINGS Figure 1 is a schematic diagram of equipment for the synthesis of transition metal chalcogen compounds using CVD according to one embodiment of the present invention.
2 is a flow chart of a method of synthesizing a transition metal chalcogen compound using CVD according to one embodiment of the present invention.
FIG. 3 is a microscope image when the alkali metal salt is loaded into a vacuum chamber according to an embodiment of the present invention, followed by an image of a microscope when the CVD is performed for 15 minutes and an image obtained when the CVD is performed for 15 minutes without loading the alkali metal salt .
4 is a graph showing Raman measurement results of a transition metal chalcogen compound synthesized by a method according to an embodiment of the present invention and a transition metal chalcogen compound synthesized by a general CVD method.
FIG. 5 is a graph showing Raman measurement results for determining whether carbon components are detected in a transition metal chalcogen compound synthesized by a method according to an embodiment of the present invention.
6 is a graph showing PL intensities of transition metal chalcogen compounds synthesized by the method according to an embodiment of the present invention and transition metal chalcogen compounds synthesized by general CVD.
7 is a graph showing XPS measurement results of a transition metal chalcogen compound prepared according to an embodiment of the present invention.
8 is a graph showing the Raman measurement results of the transition metal chalcogen compounds prepared according to the method of the present invention at 600 ° C and the graph of Raman measurement results of the transition metal chalcogen compounds prepared according to the method of the present invention at 500 ° C .
9 is a graph showing Raman scattering graphs of transition metal chalcogen compounds prepared using alkali metal salts Na 2 CO 3 , KNO 3 and LiBr, respectively, according to the present invention.

While the invention is susceptible to various modifications and alternative forms, specific embodiments thereof are shown by way of example in the drawings and will herein be described in detail. It should be understood, however, that the invention is not intended to be limited to the particular embodiments, but includes all modifications, equivalents, and alternatives falling within the spirit and scope of the invention. Like reference numerals are used for like elements in describing each drawing.

Hereinafter, embodiments according to the present invention will be described in detail with reference to the accompanying drawings.

1 is a schematic diagram of an apparatus for synthesizing a transition metal chalcogenide compound using CVD according to an embodiment of the present invention.

The present invention basically synthesizes transition metal chalcogen compounds by using CVD, and CVD (Chemical Vapor Deposition) is a process for producing a chalcogen compound by chemical reaction and pyrolysis from gaseous elements or compounds, Or particles.

The CVD is performed in the vacuum chamber 100, and the substrate 110 is provided in the vacuum chamber 100. A transition metal chalcogenide compound to be synthesized is synthesized on the substrate 110 provided in the vacuum chamber 100. As an example, the substrate may be a substrate made of silicon oxide (SiO 2 ) or an amorphous substrate such as silicon nitride (Si 3 N 4 ).

In addition, a catalyst for promoting the reaction rate for synthesizing the transition metal chalcogenide compound is preliminarily injected into the vacuum chamber 100. According to a preferred embodiment of the present invention, a catalyst of an alkali metal salt is preloaded in the vacuum chamber 100 to promote the reaction rate of the transition metal chalcogenide compound by CVD.

In one example, the alkali metal salt is in some cases NaCl, Na 2 CO 3, KNO 3, may include LiBr, and in addition will be able to be used in a variety of alkali metal salt catalyst 1 has which NaCl is loaded is shown.

After setting the environment of the vacuum chamber to a preset environmental condition, the precursor, the reactant and the gas are injected into the vacuum chamber 100.

Here, the environmental condition of the vacuum chamber 100 for the reaction may include the temperature and the pressure in the vacuum chamber 100. According to an embodiment of the present invention, the temperature in the vacuum chamber may be set to be about 600 ° C or higher.

The precursor injected into the vacuum chamber 100 has the form of a transition metal having a halide ligand. The exemplary precursor of MoCl 5 is shown in Fig.

According to a preferred embodiment of the present invention, the transition metal constituting the precursor is selected from the group consisting of Ti, Hf, Zr, V, Nb, Ta, Mo, W, Tc, Re, Co, Rh, Ir, Ni, Pd, But is not limited thereto.

The reactive material injected into the vacuum chamber 100 may include at least one kind of chalcogenide selected from S, Se and Te. Particularly, the present invention can exert a superior effect when a reactive substance having an organic ligand is injected. In FIG. 1, a representative example of the reactant is dimethyl disulfide (DMS).

A gas is injected into the vacuum chamber 100 to remove unreacted precursor material, wherein the gas may be an inert gas. As shown in FIG. 1, the inert gas may include argon (Ar) and hydrogen (H 2 ) gas. After the reaction is completed, the gas is discharged from the chamomile chamber.

2 is a view showing a flow of a method of synthesizing a transition metal chalcogenide compound using CVD according to one embodiment of the present invention.

Referring to FIG. 2, a vacuum chamber including a substrate is first prepared (step 200).

Once the vacuum chamber containing the substrate is ready, the alkali metal salt is loaded into the vacuum chamber (step 202). The alkali metal salt acts as a catalyst for accelerating the reaction rate in the transition metal chalcogen compounds according to the present invention. In particular, the alkali metal salt functions as a catalyst capable of efficiently removing the carbon black when a reactant having an organic ligand is used.

Once the alkali metal salt is loaded, the process environment within the vacuum chamber is established (step 204). The process pressure and the process temperature are set, and according to a preferred embodiment of the present invention, the process temperature is set to be 600 ° C or higher.

Once the process environment is established, the reactants, precursors, and gases are injected into the vacuum chamber (step 206).

As described above, the precursor has a form of a transition metal having a ligand of a halide group, and a precursor thereof is TiCl4, TiF4, TiI4, HfCl4, HfCp2Me2, HfI4, Hf (CpMe) 2 (OMe) Me, ZrCl4, ZrI4 CoCl 2, CoCl 2, CoCl 2, CoCl 2, CoCl 2, CoCl 2, CoCl 2, CoCl 2, CoCl 2, CoCl 2, CoCl 2, CoCl 2, CoCl 2, CoCl 2, CoCl 2, CoCl 2, CoCl 2, CoCl 2, CoCl 2, CoCl 2, CoCl 2, CoCl 2, CoCl 2, ) 2, CoCp 2, RhCl 5, IrCl 3, NiCl 2, Ni (acac) 2, NiCp 2, PdCl 2, Pd (thd) 2, PtCl 2, ZnCl 2, ZnMe 2, ZnEt 2, ZnI 2, SnCl 2, SnCl 4 and SnI 4.

According to one embodiment of the present invention, the reactant is selected from the group consisting of sulfur powder, hydrogen sulfide (H2S), diethyl sulfide, dimethyl disulfide, ethyl methyl sulfide, Et3Si) 2S, selenium powder, H2Se, diethyl selenide, dimethyl diselenide, ethyl methyl selenide, (Et3Si) 2Se, It contains one of Telenium powder, H2Te, dimethyl telluride, diethyl telluride, Ethyl methyl telluride and (Et3Si) 2Te. can do.

Once precursors, reactants and gases have been introduced, a reaction for the synthesis of the transition metal chalcogenide compound takes place in the vacuum chamber (step 208).

When the precursor is MoCl 5 and the reactant is DMS, the transition metal chalcogen compound of MOS 2 is synthesized. As another example, transition metal chalcogen compounds of MOS 2 are synthesized even when the precursor is MoCl 5 and the reactants are H 2 S. As another example, when the precursor is WCl 3 and the reactant is H 2 S, a transition metal chalcogen compound of WS 2 is synthesized.

FIG. 3 is a microscope image when the alkali metal salt is loaded into a vacuum chamber according to an embodiment of the present invention, followed by an image of a microscope when the CVD is performed for 15 minutes and an image obtained when the CVD is performed for 15 minutes without loading the alkali metal salt to be.

FIG. 3 (a) shows a microscope image when the alkali metal salt is loaded under CVD for 15 minutes and scratches are generated, FIG. 3 (b) shows the case where CVD is carried out for 15 minutes without loading the alkali metal salt, And FIG.

3 (a) and 3 (b), when CVD was carried out with the alkali metal salt loaded, crystals were formed on the transition metal chalcogenide compound even in a short time of 15 minutes, Is significantly increased.

From FIG. 3, it is confirmed that the alkali metal salt can act as a catalyst for promoting the reaction of the transition metal chalcogen compound.

4 is a graph showing Raman measurement results of a transition metal chalcogen compound synthesized by a method according to an embodiment of the present invention and a transition metal chalcogen compound synthesized by a general CVD method.

Referring to FIG. 4, when a transition metal chalcogen compound is synthesized by carrying out CVD by loading an alkali metal salt as in the present invention, and when a transition metal chalcogen compound is synthesized by general CVD, It can be confirmed that it has a peak value.

From the Raman measurement results of FIG. 4, it can be seen that the alkali metal salt does not react and acts as a catalyst.

FIG. 5 is a graph of a Raman measurement result for confirming whether a carbon component is detected in a transition metal chalcogen compound synthesized by a method according to an embodiment of the present invention.

FIG. 5 shows that when a general DMS is used as a reactant, a carbon source is detected by synthesizing a transition-electron chalcogen compound by a general CVD method.

However, when a transition metal chalcogen compound is synthesized using an alkali metal salt as a catalyst as in the present invention, it can be confirmed that no carbon component is detected.

It can be seen from FIG. 5 that when the alkali metal salt is used as a catalyst according to the present invention, the carbon material can be efficiently removed by using the reactant having an organic ligand.

6 is a graph showing PL intensities of transition metal chalcogen compounds synthesized by a method according to an embodiment of the present invention and transition metal chalcogen compounds synthesized by general CVD.

Referring to FIG. 6, when a transition metal chalcogen compound is synthesized by general CVD, a PL peak is not detected, and it can be confirmed that a carbon component is contained in the transition metal chalcogen compound.

7 is a graph showing XPS measurement results of transition metal chalcogen compounds prepared according to one embodiment of the present invention.

7A is an XPS measurement result for detecting an Mo component, FIG. 7B is an XPS measurement result for detecting an S component, FIG. 7C is an XPS measurement result for detecting a carbon component, ) Is the XPS measurement result for detecting the Na component.

7 (a) and 7 (b), MO and S components are shown for both the case of synthesizing a transition metal chalcogen compound according to the present invention and the case of synthesizing a transition metal chalcogen compound by general CVD It can be confirmed that it is detected stably.

 Referring to FIG. 7 (c), when a transition metal chalcogen compound is synthesized by a general CVD method, a carbon component is detected in a transition metal chalcogen compound. However, when a transition metal chalcogen compound is synthesized according to the present invention, Can not be detected.

Referring to FIG. 7 (d), it can be seen that when the transition metal chalcogen compound is synthesized by the present invention, the Na component is not detected, and it can be confirmed that the alkali metal salt acts as a catalyst.

8 is a graph showing the Raman measurement results of the transition metal chalcogen compounds prepared according to the method of the present invention at 600 ° C and the graph of Raman measurement results of the transition metal chalcogen compounds prepared according to the method of the present invention at 500 ° C to be.

Referring to FIG. 8 (a), it can be confirmed that MoS 2 is appropriately synthesized at 600 ° C. or higher. However, MoS 2, regardless of whether Referring to (b) of 8, 500 ℃ below to determine that they do not properly MoS 2 are synthesized, and that the alkali metal salt is used It can be confirmed that the synthesis is not performed.

FIG. 9 is a graph showing Raman scattering graphs of transition metal chalcogen compounds prepared using alkali metal salts Na 2 CO 3 , KNO 3 and LiBr, respectively, in accordance with the present invention.

(A) of Figure 9 is MoS 2 (B) is a Raman measurement graph for carbon component detection.

Referring to FIG. 9 (a), it can be seen that MoS 2 was grown as a single layer as a result of Raman measurement even when any alkali metal salt among Na 2 CO 3 , KNO 3 and LiBr was used.

Also, referring to FIG. 9 (b), it can be confirmed that no carbon component is detected from the synthesized MoS 2 even when any alkali metal salt among Na 2 CO 3 , KNO 3 and LiBr is used.

As described above, the present invention has been described with reference to particular embodiments, such as specific elements, and limited embodiments and drawings. However, it should be understood that the present invention is not limited to the above- Various modifications and variations may be made thereto by those skilled in the art to which the present invention pertains. Accordingly, the spirit of the present invention should not be construed as being limited to the embodiments described, and all of the equivalents or equivalents of the claims, as well as the following claims, belong to the scope of the present invention .

Claims (11)

(A) preparing a vacuum chamber loaded with an alkali metal salt serving as a catalyst;
And (b) synthesizing a transition metal chalcogenide compound by CVD by injecting a precursor having a halide ligand and a reactant into the vacuum chamber. The method according to claim 1,
The alkali metal salt is NaCl, Na 2 CO 3, KNO 3, any of the transition metal chalcogenide synthesis method comprising the of LiBr. The method according to claim 1,
Wherein the reaction material is a reaction material having an organic ligand. The method according to claim 1,
Wherein the transition metal chalcogen compound is deposited on an amorphous substrate in the vacuum chamber. The method according to claim 1,
The precursor includes any one selected from Ti, Hf, Zr, V, Nb, Ta, Mo, W, Tc, Re, Co, Rh, Ir, Ni, Pd, Pt, ≪ / RTI > wherein the transition metal chalcogen compound is a transition metal. 6. The method of claim 5,
The precursor may be selected from the group consisting of TiCl4, TiF4, TiI4, HfCl4, HfCp2Me2, HfI4, Hf (CpMe) 2 (OMe) Me, ZrCl4, ZrI4, VCl3, VoCl3, NbCl5, TaCl5, TaF5, TaI5, MoCl5, Mo CoCp2, CoCp2, RhCl5, IrCl3, NiCl2, Ni (acac) 2, NiCp2, PdCl2, Pd, CoCl2, CoCl2, CoCl2, CoCl2, CoCl2, CoCl2, CoCl2, CoCl2, CoCl2, CoCl2, RhCl5, IrCl3, WF4, WF6, WOCl4, TcCl4, ReCl4, ReCl5, ReCl6, (thd) 2, PtCl2, ZnCl2, ZnMe2, ZnEt2, ZnI2, SnCl2, SnCl4 and SnI4.
The method according to claim 1,
Wherein the reactant comprises at least one chalcogenide element selected from S, Se and Te.
8. The method of claim 7,
The reactant may be selected from the group consisting of sulfur powder, H2S, diethyl sulfide, dimethyl disulfide, ethyl methyl sulfide, Et3Si2S, selenium powder ), Selenium hydrogen sulphide (H2Se), diethyl selenide, dimethyl diselenide, ethyl methyl selenide, (Et3Si) 2Se, Telenium powder, Characterized in that it comprises one of hydrogen peroxide (H2Te), dimethyl telluride, diethyl telluride, ethyl methyl telluride and (Et3Si) 2Te. Compound synthesis method.







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WO2019117559A1 (en) * 2017-12-13 2019-06-20 한양대학교 에리카산학협력단 Transition metal-dichalcogenide thin film and manufacturing method therefor
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CN110683522B (en) * 2019-10-08 2021-06-11 中南大学 Transition metal chalcogen family carbon-based heterostructure composite material with regular morphology and preparation method and application thereof
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KR20230151672A (en) 2022-04-26 2023-11-02 한국과학기술원 Method for manufacturing transition metal chalcogen film and promoter therefor

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