KR101726507B1 - 2-dimensional material/metal composite having opening whose edge is deposited with metal and application of the composite - Google Patents

2-dimensional material/metal composite having opening whose edge is deposited with metal and application of the composite Download PDF

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KR101726507B1
KR101726507B1 KR1020150114923A KR20150114923A KR101726507B1 KR 101726507 B1 KR101726507 B1 KR 101726507B1 KR 1020150114923 A KR1020150114923 A KR 1020150114923A KR 20150114923 A KR20150114923 A KR 20150114923A KR 101726507 B1 KR101726507 B1 KR 101726507B1
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metal
dimensional material
composite
openings
dimensional
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KR20170020727A (en
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박원일
이재석
김수한
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한양대학교 산학협력단
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00—Processes for servicing or operating cells for electrolytic coating
    • C25D21/12—Process control or regulation
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/46—Electroplating: Baths therefor from solutions of silver
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/48—Electroplating: Baths therefor from solutions of gold
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/50—Electroplating: Baths therefor from solutions of platinum group metals
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/02—Electroplating of selected surface areas
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/34—Pretreatment of metallic surfaces to be electroplated
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/54—Electroplating of non-metallic surfaces
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/403—Cells and electrode assemblies
    • G01N27/406—Cells and probes with solid electrolytes
    • G01N27/407—Cells and probes with solid electrolytes for investigating or analysing gases
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/403—Cells and electrode assemblies
    • G01N27/406—Cells and probes with solid electrolytes
    • G01N27/407—Cells and probes with solid electrolytes for investigating or analysing gases
    • G01N27/4073—Composition or fabrication of the solid electrolyte

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  • Electrochemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
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Abstract

A two-dimensional material / metal composite with a metal coated on the edge of the opening and its application. The two-dimensional workpiece / metal composite includes a two-dimensional work layer having a plurality of openings and a metal coated on the edges of the openings.

Description

[0001] The present invention relates to a two-dimensional material / metal composite material coated with a metal at the edge of an opening and a two-dimensional material /

The present invention relates to a two-dimensional material, and more particularly, to a two-dimensional material / metal composite material.

A two-dimensional material generally means a material having a very thin thickness of not more than ten layers, preferably one atom layer, and representative two-dimensional materials include graphene.

Graphene has different thermal, mechanical and electrical properties than bulk materials in 3D. Specifically, it is known that it has excellent mechanical rigidity, strength and ductility, and has excellent electrical and thermal conductivity. Because of the excellent properties of graphene, graphene has been widely applied to energy storage devices, energy conversion devices, sensors, catalysts, and bio-application devices.

When applied to such devices, various functional materials can be bonded onto the graphene. As an example, Korean Patent No. 1331021 discloses a biosensor having an antibody bound to graphene.

A second object of the present invention is to provide a two-dimensional material / metal composite material having improved bonding strength with a functional material and an application thereof.

According to an aspect of the present invention, there is provided a two-dimensional material / metal composite material. The two-dimensional workpiece / metal composite includes a two-dimensional work layer having a plurality of openings and a metal coated on the edges of the openings.

The metal may be chemically bonded to the two-dimensional material. The metal may be a plurality of metal particles. The density of the metal particles formed on the edge of the opening may be larger than the density of the metal particles on the surface of the two-dimensional material. The two-dimensional material layer may be graphene, transition metal dichalcogenides, or a composite layer thereof. The metal may contain Ag, Pt, Au, Pd, or a composite metal thereof. The openings may penetrate the crystal plane of the two-dimensional material.

According to another aspect of the present invention, there is provided a method of manufacturing a two-dimensional material / metal composite material. First, a two-dimensional material is provided, which has a plurality of openings and dangling bonds are located at the edges of the respective openings. A metal is applied to the edge of the opening.

The metal may be a plurality of metal particles. The density of the metal particles formed on the edge of the opening may be larger than the density of the metal particles on the surface of the two-dimensional material. The two-dimensional material layer may be graphene, transition metal dichalcogenides, or a composite layer thereof. The metal may contain Ag, Pt, Au, Pd, or a composite metal thereof. The openings may penetrate the crystal plane of the two-dimensional material. The step of applying the metal to the edge of the opening may be performed using an electroplating method.

Wherein applying the metal using the electroplating method comprises: applying a positive voltage to the two-dimensional material to increase the density of the dangling bonds at the edge of the opening; Applying a negative voltage to the two-dimensional material to form a metal nucleus on the edge of the opening; And applying a negative voltage having a negative absolute value to the two-dimensional material in comparison with a negative voltage for forming the metal nucleus, thereby growing a metal on the metal nucleus.

According to another aspect of the present invention, there is provided a gas sensor. The gas sensor comprises a substrate and the two-dimensional material / metal composite disposed on the substrate. A pair of electrodes may be electrically connected to the two-dimensional workpiece / metal composite.

The two-dimensional material of the two-dimensional material / metal composite is graphene, and the metal may be Pd or Pt. Alternatively, the two-dimensional material of the two-dimensional workpiece / metal composite may be tungsten disulfide and the metal may be Ag.

As described above, according to the present invention, by selectively applying a metal to the edges of the openings having many dangling bonds, it is possible to obtain a two-dimensional material / metal composite material having improved bonding force between the metal and the two- / A device having improved performance in the application of a metal composite can be obtained.

The effects of the present invention are not limited to those mentioned above, and other effects not mentioned can be clearly understood by those skilled in the art from the following description.

FIGS. 1A to 1C are schematic views showing a method of manufacturing a two-dimensional material having a plurality of openings according to an embodiment of the present invention.
2 is a perspective view showing a two-dimensional material having a plurality of openings.
FIGS. 3 and 4 are schematic views showing a method of manufacturing a two-dimensional material / metal composite according to an embodiment of the present invention.
FIG. 5 is a graph showing a bias voltage applied to a two-dimensional material according to time in the plating process described with reference to FIG.
6 is a perspective view showing a gas sensor according to an embodiment of the present invention.
7 is an SEM photograph of a two-dimensional material according to a two-dimensional material production example.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. However, the present invention is not limited to the embodiments described herein but may be embodied in other forms. In the drawings, where a layer is referred to as being "on" another layer or substrate, it may be formed directly on another layer or substrate, or a third layer may be interposed therebetween.

FIGS. 1A to 1C are schematic views showing a method of manufacturing a two-dimensional material having a plurality of openings according to an embodiment of the present invention.

Referring to FIG. 1A, a two-dimensional material-forming catalyst layer 12 may be formed on a substrate 10. However, the present invention is not limited thereto, and the catalyst layer 12 may not be formed when the substrate 10 contains or is made of a catalyst material for forming a two-dimensional work. The catalyst layer 12 may be nickel, copper, or a combination thereof.

The particles 15 may be disposed on the catalyst layer 12. The particles 15 may be inorganic particles or organic particles. The inorganic particles may be silica particles or alumina particles, and the organic particles may be polystyrene particles, polyacrylate particles (e.g., poly (methyl methacrylate) particles), polyester particles, poly Acrylonitrile particles, or polycarbonate particles. The particles 15 may be beads having the shape of a sphere. In addition, disposing the particles 15 on the catalyst layer 12 can be achieved by a coating method such as a dip-coating method, a spin-coating method or a spray-coating method using the colloid solution in which the particles are dispersed; Printing methods such as inkjet printing, contact printing, and offset printing; Or an electrophoresis method or the like. The size of such particles 15 may have a diameter in the nanometer to micrometer size, e.g., 1 nm to 10 um.

Referring to FIG. 1B, a two-dimensional material layer 20 may be formed on the catalyst layer 12 between the particles 15. As an example, chemical vapor deposition (CVD) may be used.

The two-dimensional material layer 20 is a layer having a very thin thickness of 1 to 10, for example 1 to 5, 1 to 3, or 1 atomic layers, graphene; Transition metal dichalcogenides such as niobium disulfide (NbS2), tungsten disulfide (WS2), and molybdenum disulfide (MoS2); Or a composite layer thereof. The width of the two-dimensional material layer 20 may have a nanometer size or a micrometer size.

Referring to FIG. 1C, the particles 15 may be etched to obtain a two-dimensional material layer 20 having a plurality of openings 20a defined by the particles 15. The etching of the particles 15 may be performed using an appropriate etchant. For example, the particles 15 may be an HF solution buffered with NH 4 F when the particles are silica particles, or acetone if the particles 15 are organic particles.

2 is a perspective view showing a two-dimensional material having a plurality of openings.

Referring to FIG. 2, the two-dimensional material 20 is a material having a very thin thickness of 1 to 10, for example 1 to 5, 1 to 3, or 1 atomic layers, including graphene; Transition metal dichalcogenides such as niobium disulfide (NbS2), tungsten disulfide (WS2), and molybdenum disulfide (MoS2); Or a composite layer thereof. The width of the two-dimensional material 20 may have a nanometer size or a micrometer size.

The openings 20a may penetrate the two-dimensional material 20, specifically the crystal plane of the two-dimensional material 20, and may have a diameter of nanometer to micrometer size, for example, 1 nm to 10 um. In addition, a plurality of dangling bonds may be exposed at the edges of the openings 20a.

The method of manufacturing such a two-dimensional material is not limited to the method described with reference to Figs. 1A to 1C, but may be a method of laminating a two-dimensional material layer on a substrate, After forming the mask layer, the two-dimensional material layer exposed in the holes may be etched using the etch mask layer as a mask, and the etch mask layer may be removed to produce a two-dimensional material having a plurality of openings.

FIGS. 3 and 4 are schematic views showing a method of manufacturing a two-dimensional material / metal composite according to an embodiment of the present invention.

Referring to FIG. 3, a two-dimensional material 20 having a plurality of openings 20a may be disposed on the holder 30. FIG. Thereafter, the conductor 40 may be connected to a part of the two-dimensional workpiece 20. The two-dimensional material 20 to which the lead wire 40 is connected may be immersed in the plating liquid 50. The plating solution 50 may be a metal precursor, for example, an electrolyte solution containing metal ions or the like, and may further contain an additive. The counter electrode 60 and the reference electrode 70 may be further contained in the plating solution 50. [ The counter electrode 60 may be a gold electrode, and the reference electrode 70 may be Ag / AgCl. The metal precursor may be a metal salt.

4, a voltage is applied to the two-dimensional workpiece 20 through a conductor 40 to selectively apply a metal 25 to the edges of the opening 20a to form a two-dimensional workpiece / metal composite material 20 ' ) Can be obtained. The two-dimensional material / metal composite 20 'includes a two-dimensional material having a plurality of openings 20a and a metal 25 coupled to the edge of the opening 20a. The metal 25 is shown to be applied only to the edge of the opening 20a, but it is not limited thereto and may be formed at the edges of the two-dimensional material 20. [

The metal 25 may have an aggregate form of a plurality of metal particles. The metal 25 may be composed of, for example, Ag, Pt, Au, Pd, or a composite metal thereof, or may contain at least one of them.

FIG. 5 is a graph showing a bias voltage applied to a two-dimensional material according to time in the plating process described with reference to FIG.

Referring to FIGS. 3, 4, and 5, a relatively large positive voltage may be applied to the two-dimensional material 20, specifically, the oxidation voltage Eox. In this case, the voltage can be concentrated on the edge of the opening 20a of the two-dimensional material 20, so that the bonding of the portion can be broken, and as a result, the density of the dangling bond can be increased at the edge of the opening 20a. Also, oxygen-containing functional groups of -OH or -COOH may be generated in the dangling bonds. This positive voltage may be between 0.6V and 1.0V.

Thereafter, a nucleation generating voltage (Enu), specifically, a negative voltage having a relatively large absolute value can be applied to the two-dimensional material (20). In this case, metal ions in the electrolyte can form metal nuclei while bound to a dangling bond or an oxygen-containing functional group formed at the edge of the opening 20a, for example, chemically. This negative voltage may be from -0.6V to -1.0V.

Thereafter, the growth reduction voltage Egrow, specifically, a negative voltage having a relatively low absolute value can be applied to the two-dimensional material 20. This negative voltage may be -0.4V to -0.1V. Metal ions in the electrolytic solution on the metal nuclei generated at the edges of the openings 20a may be continuously reduced and stacked so that the metal 25 is exposed at the edges of the openings 20a, It can be grown. The metal (25) can be chemically bonded to the two-dimensional material (20). The size of the metal particles 25 may be nanometer size, for example, 1 to 100 nm, specifically 10 to 50 nm, more specifically 15 nm to 25 nm.

During the metal nucleus and metal growth process, the metal nuclei and metal may be grown on the edges of the two-dimensional material 20 in which the dangling bonds are present. In addition, when a dangling bond is present on the surface of the two-dimensional material 20, the metal can also grow on the dangling bond on the surface. However, since the density of the dangling bonds on the surface is smaller than the edge of the opening 20a, the density of the metal particles formed at the edge of the opening 20a, specifically, the density of the metal particles, .

6 is a perspective view showing a gas sensor according to an embodiment of the present invention.

Referring to FIG. 6, the gas sensor may include a two-dimensional workpiece / metal composite 20 'disposed on a support substrate 80. The two-dimensional material / metal composite material 20 'includes a two-dimensional material 20 having a plurality of openings 20a and a metal 25 coupled to an edge of the opening 20a.

The two-dimensional material 20 may be graphene; Transition metal dichalcogenides such as niobium disulfide (NbS2), tungsten disulfide (WS2), and molybdenum disulfide (MoS2); Or a composite layer thereof. The width of such a composite material 20 'may have a micrometer size. The metal 25 may have an aggregate form of a plurality of metal particles. The metal 25 may be composed of, for example, Ag, Pt, Au, Pd, or a composite metal thereof, or may contain at least one of them.

For example, if the two-dimensional material / metal composite 20 'is a graphene / Pd composite or a graphene / Pt composite, the gas sensor may be a hydrogen sensor. Alternatively, when the two-dimensional material / metal composite 20 'is a tungsten disulfide / Ag composite, the gas sensor may be a nitrogen dioxide sensor.

The sensing electrodes 81 and 83 may be disposed on the two-dimensional material / metal composite 20 '.

In such a gas sensor, the metal 25 can react with the gas to generate charge, and the generated charge can be delivered to the two-dimensional material chemically bonded to the metal 25 very quickly, and the two- It is very good so that the charge can be transferred quickly to the electrode. As a result, the sensitivity of the gas sensor can be greatly improved.

Hereinafter, preferred examples will be given to facilitate understanding of the present invention. It should be understood, however, that the following examples are for the purpose of promoting understanding of the present invention and are not intended to limit the scope of the present invention.

<Examples of two-dimensional material / metal composite production>

A silica bead array was deposited on a copper foil using a Langmuir-Blodgett assembly and then sinked in an oven. The copper foil on which the silica bead array was formed was placed in a quartz tube of a CVD (Chemical Vapor Deposition) equipment, and heat treatment was performed at 500 mtorr and 1000 ° C for 10 minutes while flowing H 2 . Thereafter, CH 4 and H 2 were flowed at 800 mtorr for 10 minutes, and all the gas was turned off, followed by cooling at -10 ° C / s to grow graphene. The graphene - grown copper foil was immersed in HF for 10 minutes to remove the silica beads to form a graphene mesh.

The grown graphene mesh was transferred onto a slide glass, the lead wire was attached, and the glass was immersed in a PdCl 3 0.01M electrolyte solution. Metal was electroplated on the edges of the openings of the graphene mesh using gold as the counter electrode and Ag / AgCl as the reference electrode. In the electroplating process, 0.8V was applied to the graphene mesh for 5 seconds to oxidize the edge of the opening, and then -0.8 V was applied for 0.01 second to generate nuclei at the edge of the opening. Then, And the nuclei formed at the edges of the openings were grown to form metal particles.

7 is an SEM photograph of a two-dimensional material according to a two-dimensional material production example.

Referring to FIG. 7, it can be seen that palladium particles 25 having a diameter of about 15 to 25 nm are mainly formed at the edge of the opening 20a of the graphene mesh.

While the present invention has been particularly shown and described with reference to preferred embodiments thereof, it will be understood by those skilled in the art that various changes and modifications may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (18)

A two-dimensional material layer having a plurality of openings; And
And a plurality of metal particles formed on edges of the openings,
The openings penetrating the crystal plane of the two-dimensional material,
Wherein the density of the metal particles formed on the edge of the opening is larger than the density of the metal particles on the surface of the two-dimensional material. The method according to claim 1,
Wherein the metal is chemically bonded to the two-dimensional material. delete delete The method according to claim 1,
Wherein the two-dimensional material layer is graphene, transition metal dichalcogenides, or a composite layer thereof. The method according to claim 1,
Wherein the metal comprises Ag, Pt, Au, Pd, or a composite metal thereof. delete Providing a two-dimensional material having a plurality of openings and dangling bonds disposed at edges of each of the openings; And
Applying a metal to an edge of the opening to form a plurality of metal particles,
The openings penetrating the crystal plane of the two-dimensional material,
Wherein the density of the metal particles formed on the edge of the opening is larger than the density of the metal particles on the surface of the two-dimensional material. delete delete 9. The method of claim 8,
Wherein the two-dimensional material layer is graphene, transition metal dichalcogenides, or a composite layer thereof. 9. The method of claim 8,
Wherein the metal comprises Ag, Pt, Au, Pd, or a composite metal thereof. delete 9. The method of claim 8,
Wherein the step of applying the metal to the edge of the opening is performed using an electroplating method. 15. The method of claim 14,
The step of applying the metal using the electroplating method
Applying a positive voltage to the two-dimensional material to increase the density of dangling bonds at the edges of the openings;
Applying a negative voltage to the two-dimensional material to form a metal nucleus on the edge of the opening; And
And applying a negative voltage having a lower absolute value to the two-dimensional material than the negative voltage for forming the metal nucleus, thereby growing a metal on the metal nucleus. Board;
The two-dimensional workpiece / metal composite of claim 1 disposed on the substrate; And
And a pair of electrodes electrically connected to the two-dimensional workpiece / metal composite. 17. The method of claim 16,
Wherein the two-dimensional material of the two-dimensional material / metal composite is graphene, and the metal is Pd or Pt. 17. The method of claim 16,
Wherein the two-dimensional material of the two-dimensional material / metal composite is tungsten disulfide and the metal is Ag.
KR1020150114923A 2015-08-13 2015-08-13 2-dimensional material/metal composite having opening whose edge is deposited with metal and application of the composite KR101726507B1 (en)

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