WO2022186423A1 - Method for preparing max precursor and mxene nanoink - Google Patents

Method for preparing max precursor and mxene nanoink Download PDF

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WO2022186423A1
WO2022186423A1 PCT/KR2021/004705 KR2021004705W WO2022186423A1 WO 2022186423 A1 WO2022186423 A1 WO 2022186423A1 KR 2021004705 W KR2021004705 W KR 2021004705W WO 2022186423 A1 WO2022186423 A1 WO 2022186423A1
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mxene
fluoride
ink
nano
precursor
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Korean (ko)
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오정민
권한중
서창열
김문성
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전북대학교산학협력단
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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
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/90—Carbides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • 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
    • C01B32/90—Carbides
    • C01B32/914—Carbides of single elements
    • C01B32/921—Titanium carbide
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00—Inks
    • C09D11/02—Printing inks
    • C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
    • C09D11/033—Printing inks characterised by features other than the chemical nature of the binder characterised by the solvent
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00—Inks
    • C09D11/02—Printing inks
    • C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
    • C09D11/037—Printing inks characterised by features other than the chemical nature of the binder characterised by the pigment
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/32—Carbon-based
    • H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer

Definitions

  • the present invention relates to a method for manufacturing MAX precursor and MXene nano ink, and more particularly, to a method for manufacturing MAX precursor and MXene nano ink capable of reducing manufacturing cost will be.
  • Graphene a single atomic layer material composed of carbon atoms in a honeycomb structure, has attracted a lot of attention worldwide due to its excellent physical properties. As such research on graphene is of explosive interest, interest in graphene-like two-dimensional materials has recently been expanding.
  • MXene has a hydrophilic surface and high electrical and thermal conductivity, so it shows excellent properties in the fields of electrodes, supercapacitors, biosensors, desalination systems, and electromagnetic wave shielding.
  • graphene does not have a bandgap despite its high characteristics, it is difficult to use it for semiconductor materials, whereas MXene forms a bandgap and is useful as a semiconductor material.
  • MXene is composed of transition metal carbides and nitrides or carbonitrides with the chemical formula M n+1 X n .
  • M is a transition metal such as Ti, Sc, Zr, Hf, V, Nb, Mo, Ta, Cr, and X is carbon and nitrogen.
  • MXenes are composed of a transition metal and a compound of carbon and nitrogen.
  • MXene is made from a MAX precursor, which has a chemical formula of M n+1 AX n , and consists of a compound of transition metal M, interlayer material A, and carbon or nitrogen.
  • a MAX precursor which has a chemical formula of M n+1 AX n , and consists of a compound of transition metal M, interlayer material A, and carbon or nitrogen.
  • the production cost is high because a transition metal in a metallic state is used. there was.
  • a metal oxide is used as a raw material, there is a problem in that the purity is deteriorated because oxides having a different composition than the MAX component such as alumina are simultaneously produced.
  • An object of the present invention is to solve the above problems, and to provide a method for manufacturing a MAX precursor and MXene nano-ink using a lower metal oxide.
  • the present invention comprises the steps of: a) reacting a lower metal oxide with carbon or nitrogen to prepare a carbide or nitride;
  • b) provides a method for producing a MAX precursor comprising the step of synthesizing the carbide or nitride prepared in step a) with aluminum or silicon.
  • the metal may be any one or more transition metals selected from Sc, Y, Lu, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, and W.
  • the present invention comprises the steps of 1) preparing a maxine (MXene) nanosheet by reacting the MAX precursor of claim 1 with an acid-based solution containing a fluorine atom; and
  • It provides a method for producing a maxine (MXene) nano ink comprising the step of dispersing the maxine (MXene) nanosheets in any one or more selected from water (H 2 O) and an organic solvent.
  • the acid-based solution containing a fluorine atom is hydrofluoric acid (HF), LiHF 2 , NaHF 2 , KHF 2 , lithium fluoride (LiF), sodium fluoride (NaF), magnesium fluoride ( MgF 2 ), strontium fluoride (SrF 2 ), beryllium fluoride (BeF 2 ) , calcium fluoride (CaF 2 ), ammonium fluoride (NH 4 F), ammonium difluoride (NH 4 HF 2 ), ammonium hexafluoroaluminate ( (NH 4 ) 3 AlF 6 ) It may include any one or more selected from.
  • the organic solvent may be any one or more selected from methyl acetate, ethyl acetate, acetone, and ethanol.
  • the present invention provides a transparent electrode or film prepared from the MXene nano ink.
  • the manufacturing method of the MAX precursor and the MXene nano ink according to the present invention can dramatically lower the production cost of the MXene nano ink by using a metal oxide instead of a transition metal, and a high-purity MAX precursor There are advantages to getting
  • the transparent electrode and the film prepared using the MXene nano ink prepared according to the present invention exhibit high electrical properties.
  • FIG. 1 is a flowchart illustrating a method of manufacturing MXene nano ink according to the present invention.
  • FIG. 2 is an image (a) of a vacuum filtering device used when manufacturing a high-density film using the MXene nano-ink prepared according to the present invention, an image (b) of the manufactured high-density film, and XRD of the film (X-ray diffraction)
  • the analysis result (c) is shown.
  • FIG 3 shows an image (a) of a transparent electrode prepared using MXene nano ink prepared according to the present invention and an SEM image (b) of the surface of the transparent electrode.
  • the present invention comprises the steps of: a) reacting a lower metal oxide with carbon or nitrogen to prepare a carbide or nitride; and b) synthesizing the carbide or nitride prepared in step a) with aluminum or silicon.
  • the metal may be any one or more transition metals selected from Sc, Y, Lu, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, and W.
  • the MAX precursor has a chemical formula of M n+1 AX n , wherein M is a transition metal, and A is an intermediate layer material such as aluminum (Al), silicon (Si), P, S, Ga, Ge, It may be any one selected from As, Cd, In, Sn, Tl, and Pb, wherein X is carbon (C) or nitrogen (N), and n is any one selected from 1 to 3.
  • lower generally means a purity of 99% or less, and examples of the lower metal oxide include TiO 2 , V 2 O 5 , NbO 2 and the like, but is not limited thereto.
  • pure aluminum metal powder or Al 2 O 3 may be used, and as the silicon, pure silicon metal powder or SiO 2 may be used.
  • examples of the MAX precursor include Ti 2 CdC, Sc 2 InC, Ti 2 AlC, Ti 2 GaC, Ti 2 InC, Ti 2 TIC, V 2 AlC, V 2 GaC, Cr 2 GaC, Ti 2 AlN, Ti 2 GaN, Ti 2 InN, V 2 GaN, Cr 2 GaN, Ti 2 GeC, Ti 2 SnC, Ti 2 PbC, V 2 GeC, Cr 2 AlC, Cr 2 GeC, V 2 PC, V 2 AsC, Ti 2 SC, Zr 2 InC, Zr 2 TlC, Nb 2 AlC, Nb 2 GaC, Nb 2 InC, Mo 2 GaC, Zr 2 InN, Zr 2 TlN, Zr 2 SnC, Zr 2 PbC, Nb 2 SnC, Nb 2 PC, Nb 2 AsC, Zr 2 SC, Nb 2 SC, Hf 2 InC, Hf 2 TlC, Ta 2 AlC, Ta 2 GaC, Hf 2 SnC, Hf 2 PbC, Hf 2
  • the production cost can be reduced by up to 80% by using a metal oxide instead of a transition metal, and a high-purity MAX precursor can be obtained.
  • the present invention comprises the steps of: 1) preparing a maxine nanosheet by reacting the MAX precursor of claim 1 with an acid-based solution containing a fluorine atom; and 2) dispersing the maxine (MXene) nanosheet in at least one selected from water (H 2 O) and an organic solvent.
  • MXene nanosheets which are high-purity MXene powders, are manufactured by removing the intermediate layer material from the MAX precursor using an acid-based solution containing the fluorine atom, and the MXene nanosheets Finally, MXene nano ink can be obtained by dispersing it in water or an organic solvent.
  • the acid-based solution containing a fluorine atom is hydrofluoric acid (HF), LiHF 2 , NaHF 2 , KHF 2 , lithium fluoride (LiF), sodium fluoride (NaF), magnesium fluoride ( MgF 2 ), strontium fluoride (SrF 2 ), beryllium fluoride (BeF 2 ) , calcium fluoride (CaF 2 ), ammonium fluoride (NH 4 F), ammonium difluoride (NH 4 HF 2 ), ammonium hexafluoroaluminate ( (NH 4 ) 3 AlF 6 ) It may include any one or more selected from, but is not limited thereto.
  • the organic solvent may be any one or more selected from methyl acetate, ethyl acetate, acetone, and ethanol, but is not limited thereto. .
  • FIG. 1 is a flowchart illustrating a method of manufacturing MXene nano-ink according to the present invention, and reaction conditions, reactants, and the like are illustratively and not limited thereto. It will be described in more detail using FIG. 1 as follows.
  • a low-grade metal oxide and carbon powder are mixed and reacted at 1200° C. for 4 hours to prepare a carbide, and then the carbide and aluminum powder are mixed and reacted at 1450° C. for 4 hours to prepare a MAX precursor.
  • MXene nanosheets are prepared by reacting the MAX precursor with an HF-based acid solution, and then dispersed in water to finally prepare MXene nanoinks.
  • the present invention provides a transparent electrode or film prepared from the MXene nano ink.
  • the transparent electrode and the film are formed by coating MXene nano ink on a glass substrate.
  • TiO 2 Alfa Aesar, 99.5 %, 45 ⁇ m
  • carbon powder Alfa Aesar, 99.9%, 3 ⁇ m
  • aluminum powder High Prity Chemical, 99.9%, 45 ⁇ m
  • Ti 3 C 2 nano-ink was prepared by dispersing Ti 3 C 2 nanosheets prepared by reacting 10 g of the Ti 3 AlC 2 powder with 100 ml of an HF solution for 10 hours in water at a concentration of 0.5 wt.%.
  • the Ti 3 C 2 nano ink prepared in Preparation Example 1 was subjected to vacuum filtering (FIG. 2, a) to prepare a high-concentration film.
  • the size of the filter used to manufacture the high-concentration film was 55 mm, and the pores were 1 ⁇ m.
  • a high-concentration film was prepared through vacuum filtering, it was dried at 45° C. for 1 hour through a vacuum heat treatment apparatus. The thickness of the high-concentration film prepared through this was 10 ⁇ m, and is shown in FIG. 2(b).
  • XRD X-ray diffraction
  • Example 1 For the films of Example 1 and Comparative Example 1, commercially available carbon-ukraine MXene (Carbon-Ukraine ltd., Ti 3 C 2 aqueous solutions), resistance, sheet resistance, specific resistance and electrical conductivity were measured in the following manner. are shown in Table 1.
  • Sheet resistance It was measured using a four-point probe resistivity-meter (Mitsubishi, MCP-T370, Japan).
  • Resistivity Measured using a four-point probe resistivity-meter (Mitsubishi, MCP-T370, Japan).
  • Electrical conductivity was calculated using the measured resistance, sheet resistance, resistivity, and film thickness.
  • Example 1 had a lower overall resistance value and increased electrical conductivity by 213.3% compared to Comparative Example 1.
  • a transparent electrode was prepared by coating the Ti 3 C 2 nano ink prepared in Preparation Example 1 on a glass substrate, thereby obtaining a transparent electrode as shown in (a) of FIG. 3 .
  • a spin coating method was used for coating, in which the rotation speed was 3,000 rpm and the holding time was 30 seconds, and about 5 ml of nano ink was used for one coating.

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Abstract

The present invention relates to a method for preparing a MAX precursor and a MXene nanoink, and, more specifically, to a method for preparing a MAX precursor and a MXene nanoink by using a low-grade metal oxide so that manufacturing costs can be reduced.

Description

맥스 전구체 및 맥신 나노 잉크의 제조 방법Methods for making Max precursors and Maxine nano inks
본 발명은 맥스(MAX) 전구체 및 맥신(MXene) 나노 잉크의 제조 방법에 관한 것으로, 보다 상세하게는 제조 원가를 감소시킬 수 있는 맥스(MAX) 전구체 및 맥신(MXene) 나노 잉크의 제조 방법에 관한 것이다.The present invention relates to a method for manufacturing MAX precursor and MXene nano ink, and more particularly, to a method for manufacturing MAX precursor and MXene nano ink capable of reducing manufacturing cost will be.
벌집 모양 구조의 탄소 원자들로 이루어진 단일 원자층 물질인 그래핀은 뛰어난 물리적 성질로 전 세계적으로 수많은 관심이 집중되어 왔다. 이와 같은 그래핀에 대한 연구가 폭발적으로 관심을 갖고 있어 최근 들어 그래핀과 유사한 2차원 물질들에 대하여 관심이 확대되어 가는 추세이다.Graphene, a single atomic layer material composed of carbon atoms in a honeycomb structure, has attracted a lot of attention worldwide due to its excellent physical properties. As such research on graphene is of explosive interest, interest in graphene-like two-dimensional materials has recently been expanding.
이러한 2차원 물질 중 하나인 맥신(MXene)은 친수성 표면과 높은 전기·열 전도도를 갖고 있어, 전극, 수퍼캐패시터, 바이오센서, 담수화 시스템, 전자파 차폐 분야에 탁월한 특성을 나타낸다. 또한 그래핀이 높은 특성에도 불구하고 밴드갭이 없어서 반도체 재료에 사용하기 어려운 반면, MXene은 밴드갭을 형성하여 반도체 재료로써 활용 가치가 있다. One of these two-dimensional materials, MXene, has a hydrophilic surface and high electrical and thermal conductivity, so it shows excellent properties in the fields of electrodes, supercapacitors, biosensors, desalination systems, and electromagnetic wave shielding. In addition, although graphene does not have a bandgap despite its high characteristics, it is difficult to use it for semiconductor materials, whereas MXene forms a bandgap and is useful as a semiconductor material.
일반적으로 MXene은 Mn+1Xn의 화학공식을 가진 전이금속 탄화물 및 질화물 또는 탄질화물로 구성된다. 여기서 M은 Ti, Sc, Zr, Hf, V, Nb, Mo, Ta, Cr 등의 전이금속이며, X는 탄소 및 질소이다. 이러한 MXene은 전이금속과 탄소 및 질소의 화합물로 이루어져 있다.In general, MXene is composed of transition metal carbides and nitrides or carbonitrides with the chemical formula M n+1 X n . Here, M is a transition metal such as Ti, Sc, Zr, Hf, V, Nb, Mo, Ta, Cr, and X is carbon and nitrogen. These MXenes are composed of a transition metal and a compound of carbon and nitrogen.
또한 MXene은 맥스(MAX) 전구체로부터 만들어지며, MAX 전구체는 Mn+1AXn의 화학공식을 가지고, 전이금속 M, 중간층 물질 A 및 탄소 또는 질소의 화합물로 이루어져 있다. 종래 MAX 전구체의 제조 방법을 이용하여 MAX 전구체를 제조할 경우, 금속상태의 전이금속을 사용하기 때문에 생산비용이 고가인 문제가 있었다. 한편, 원재료로 금속산화물을 사용하였더라도 알루미나와 같은 MAX 성분이 아닌 다른 조성의 산화물이 동시에 제조되어 순도가 떨어지는 문제가 있었다.In addition, MXene is made from a MAX precursor, which has a chemical formula of M n+1 AX n , and consists of a compound of transition metal M, interlayer material A, and carbon or nitrogen. In the case of manufacturing the MAX precursor using the conventional MAX precursor manufacturing method, there is a problem that the production cost is high because a transition metal in a metallic state is used. there was. On the other hand, even when a metal oxide is used as a raw material, there is a problem in that the purity is deteriorated because oxides having a different composition than the MAX component such as alumina are simultaneously produced.
본 발명의 목적은 상기와 같은 문제를 해결하기 위한 것으로, 저급 금속 산화물을 이용한 맥스(MAX) 전구체 및 맥신(MXene) 나노 잉크를 제조하는 방법을 제공하는 것이다.An object of the present invention is to solve the above problems, and to provide a method for manufacturing a MAX precursor and MXene nano-ink using a lower metal oxide.
상기 목적을 달성하기 위하여 본 발명은 a) 저급 금속산화물을 탄소 또는 질소와 반응시켜 탄화물 또는 질화물을 제조하는 단계 및In order to achieve the above object, the present invention comprises the steps of: a) reacting a lower metal oxide with carbon or nitrogen to prepare a carbide or nitride;
b) 상기 a)단계에서 제조된 탄화물 또는 질화물을 알루미늄 또는 실리콘과 합성하는 단계를 포함하는 맥스(MAX) 전구체의 제조방법을 제공한다.b) provides a method for producing a MAX precursor comprising the step of synthesizing the carbide or nitride prepared in step a) with aluminum or silicon.
본 발명의 일 실시예에 있어서, 상기 금속은 Sc, Y, Lu, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo 및 W 중에서 선택되는 어느 하나 이상의 전이금속일 수 있다.In one embodiment of the present invention, the metal may be any one or more transition metals selected from Sc, Y, Lu, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, and W.
또한 본 발명은 1) 제 1항의 맥스(MAX) 전구체를 불소 원자를 함유하는 산 기반의 용액에 반응시켜 맥신(MXene) 나노 시트를 제조하는 단계; 및In addition, the present invention comprises the steps of 1) preparing a maxine (MXene) nanosheet by reacting the MAX precursor of claim 1 with an acid-based solution containing a fluorine atom; and
2) 상기 맥신(MXene) 나노 시트를 물(H2O) 및 유기용매 중에서 선택되는 어느 하나 이상에 분산시키는 단계를 포함하는 맥신(MXene) 나노 잉크의 제조방법을 제공한다.2) It provides a method for producing a maxine (MXene) nano ink comprising the step of dispersing the maxine (MXene) nanosheets in any one or more selected from water (H 2 O) and an organic solvent.
본 발명의 다른 일 실시예에 있어서, 상기 불소 원자를 함유하는 산 기반의 용액은 불산(HF), LiHF2, NaHF2, KHF2, 불소화리튬(LiF), 불화나트륨(NaF), 불화마그네슘(MgF2), 불화스트론튬(SrF2), 불화베릴륨(BeF2), 불화칼슘(CaF2), 불화암모늄(NH4F), 이불화암모늄(NH4HF2), 암모늄 헥사플루오로알루미네이트((NH4)3AlF6) 중에서 선택되는 어느 하나 이상을 포함할 수 있다.In another embodiment of the present invention, the acid-based solution containing a fluorine atom is hydrofluoric acid (HF), LiHF 2 , NaHF 2 , KHF 2 , lithium fluoride (LiF), sodium fluoride (NaF), magnesium fluoride ( MgF 2 ), strontium fluoride (SrF 2 ), beryllium fluoride (BeF 2 ) , calcium fluoride (CaF 2 ), ammonium fluoride (NH 4 F), ammonium difluoride (NH 4 HF 2 ), ammonium hexafluoroaluminate ( (NH 4 ) 3 AlF 6 ) It may include any one or more selected from.
본 발명의 다른 일 실시예에 있어서, 상기 유기용매는 메틸 아세테이트(methyl acetate), 에틸아세테이트(ethyl acetate), 아세톤(acetone), 에탄올(ethanol) 중에서 선택되는 어느 하나 이상일 수 있다.In another embodiment of the present invention, the organic solvent may be any one or more selected from methyl acetate, ethyl acetate, acetone, and ethanol.
본 발명은 상기 맥신(MXene) 나노 잉크로부터 제조된 투명 전극 또는 필름을 제공한다.The present invention provides a transparent electrode or film prepared from the MXene nano ink.
본 발명에 따른 맥스(MAX) 전구체 및 맥신(MXene) 나노 잉크의 제조방법은 전이금속 대신 금속 산화물을 사용함으로써 최종적으로 맥신(MXene) 나노 잉크의 생산 비용을 획기적으로 낮출 수 있으며, 고순도의 MAX 전구체를 얻을 수 있는 장점이 있다.The manufacturing method of the MAX precursor and the MXene nano ink according to the present invention can dramatically lower the production cost of the MXene nano ink by using a metal oxide instead of a transition metal, and a high-purity MAX precursor There are advantages to getting
또한, 본 발명에 따라 제조된 맥신(MXene) 나노 잉크를 이용하여 제조된 투명 전극 및 필름은 높은 전기적 특성을 나타낸다.In addition, the transparent electrode and the film prepared using the MXene nano ink prepared according to the present invention exhibit high electrical properties.
도 1은 본 발명에 따른 맥신(MXene) 나노 잉크의 제조방법을 예시한 흐름도이다.1 is a flowchart illustrating a method of manufacturing MXene nano ink according to the present invention.
도 2는 본 발명에 따라 제조된 맥신(MXene) 나노 잉크를 이용하여 고농도 필름을 제조할 때 사용되는 진공필터링 장치의 이미지(a), 상기 제조된 고농도 필름의 이미지(b) 및 상기 필름의 XRD(X-ray diffraction) 분석 결과(c)를 도시한 것이다.2 is an image (a) of a vacuum filtering device used when manufacturing a high-density film using the MXene nano-ink prepared according to the present invention, an image (b) of the manufactured high-density film, and XRD of the film (X-ray diffraction) The analysis result (c) is shown.
도 3은 본 발명에 따라 제조된 맥신(MXene) 나노 잉크를 이용하여 제조된 투명 전극의 이미지(a) 및 상기 투명 전극 표면의 SEM 이미지(b)를 도시한 것이다.3 shows an image (a) of a transparent electrode prepared using MXene nano ink prepared according to the present invention and an SEM image (b) of the surface of the transparent electrode.
이하, 본 발명을 상세히 설명한다.Hereinafter, the present invention will be described in detail.
본 발명은 a) 저급 금속산화물을 탄소 또는 질소와 반응시켜 탄화물 또는 질화물을 제조하는 단계; 및 b) 상기 a)단계에서 제조된 탄화물 또는 질화물을 알루미늄 또는 실리콘과 합성하는 단계를 포함하는 맥스(MAX) 전구체의 제조방법을 제공한다.The present invention comprises the steps of: a) reacting a lower metal oxide with carbon or nitrogen to prepare a carbide or nitride; and b) synthesizing the carbide or nitride prepared in step a) with aluminum or silicon.
본 발명의 일 실시예에 있어서, 상기 금속은 Sc, Y, Lu, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo 및 W 중에서 선택되는 어느 하나 이상의 전이금속일 수 있다.In one embodiment of the present invention, the metal may be any one or more transition metals selected from Sc, Y, Lu, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, and W.
상기 맥스(MAX) 전구체는 Mn+1AXn의 화학공식을 가지며, 상기 M은 전이금속이고, 상기 A는 중간층 물질로 알루미늄(Al), 규소(Si), P, S, Ga, Ge, As, Cd, In, Sn, Tl 및 Pb 중에서 선택되는 어느하나 일 수 있으며, 상기 X 탄소(C) 또는 질소(N)이고, 상기 n은 1 내지 3 중에서 선택되는 어느 하나이다. The MAX precursor has a chemical formula of M n+1 AX n , wherein M is a transition metal, and A is an intermediate layer material such as aluminum (Al), silicon (Si), P, S, Ga, Ge, It may be any one selected from As, Cd, In, Sn, Tl, and Pb, wherein X is carbon (C) or nitrogen (N), and n is any one selected from 1 to 3.
또한 상기 저급 금속 산화물에서 "저급"은 통상적으로 순도 99% 이하의 순도를 의미하며, 상기 저급 금속 산화물의 예로는 TiO2, V2O5, NbO2 등을 들 수 있으나, 이에 한정되지 않는다. In addition, in the lower metal oxide, "lower" generally means a purity of 99% or less, and examples of the lower metal oxide include TiO 2 , V 2 O 5 , NbO 2 and the like, but is not limited thereto.
상기 알루미늄은 순수 알루미늄 금속 분말 또는 Al2O3를 사용할 수 있으며, 상기 실리콘으로는 순수 실리콘 금속 분말 또는 SiO2사용할 수 있다.As the aluminum, pure aluminum metal powder or Al 2 O 3 may be used, and as the silicon, pure silicon metal powder or SiO 2 may be used.
또한 상기 맥스(MAX) 전구체의 예로는 Ti2CdC, Sc2InC, Ti2AlC, Ti2GaC, Ti2InC, Ti2TIC, V2AlC, V2GaC, Cr2GaC, Ti2AlN, Ti2GaN, Ti2InN, V2GaN, Cr2GaN, Ti2GeC, Ti2SnC, Ti2PbC, V2GeC, Cr2AlC, Cr2GeC, V2PC, V2AsC, Ti2SC, Zr2InC, Zr2TlC, Nb2AlC, Nb2GaC, Nb2InC, Mo2GaC, Zr2InN, Zr2TlN, Zr2SnC, Zr2PbC, Nb2SnC, Nb2PC, Nb2AsC, Zr2SC, Nb2SC, Hf2InC, Hf2TlC, Ta2AlC, Ta2GaC, Hf2SnC, Hf2PbC, Hf2SnN, Hf2SC, Ti3AlC2, V3AlC2, Ti3SiC2, Ti3GeC2, Ti3SnC2, Ta3AlC2, Ti4AlN3, V4AlC3, Ti4GaC3, Ti4SiC3, Ti4GeC3, Nb4AlC3, Ta4AlC3를 들 수 있으나, 이에 한정되는 것은 아니다.In addition, examples of the MAX precursor include Ti 2 CdC, Sc 2 InC, Ti 2 AlC, Ti 2 GaC, Ti 2 InC, Ti 2 TIC, V 2 AlC, V 2 GaC, Cr 2 GaC, Ti 2 AlN, Ti 2 GaN, Ti 2 InN, V 2 GaN, Cr 2 GaN, Ti 2 GeC, Ti 2 SnC, Ti 2 PbC, V 2 GeC, Cr 2 AlC, Cr 2 GeC, V 2 PC, V 2 AsC, Ti 2 SC, Zr 2 InC, Zr 2 TlC, Nb 2 AlC, Nb 2 GaC, Nb 2 InC, Mo 2 GaC, Zr 2 InN, Zr 2 TlN, Zr 2 SnC, Zr 2 PbC, Nb 2 SnC, Nb 2 PC, Nb 2 AsC, Zr 2 SC, Nb 2 SC, Hf 2 InC, Hf 2 TlC, Ta 2 AlC, Ta 2 GaC, Hf 2 SnC, Hf 2 PbC, Hf 2 SnN, Hf 2 SC, Ti 3 AlC 2 , V 3 AlC 2 , Ti 3 SiC 2 , Ti 3 GeC 2 , Ti 3 SnC 2 , Ta 3 AlC 2 , Ti 4 AlN 3 , V 4 AlC 3 , Ti 4 GaC 3 , Ti 4 SiC 3 , Ti 4 GeC 3 , Nb 4 AlC 3 , Ta 4 AlC 3 , but is not limited thereto.
상기 맥스(MAX) 전구체의 제조방법을 이용하여 맥스(MAX) 전구체를 제조할 경우, 전이금속 대신 금속 산화물을 사용함으로써 생산 비용을 최대 80%까지 낮출 수 있으며, 고순도의 MAX 전구체를 얻을 수 있는 효과가 있다.When the MAX precursor is prepared using the method for preparing the MAX precursor, the production cost can be reduced by up to 80% by using a metal oxide instead of a transition metal, and a high-purity MAX precursor can be obtained. there is
또한, 본 발명은 1) 제 1항의 맥스(MAX) 전구체를 불소 원자를 함유하는 산 기반의 용액에 반응시켜 맥신(MXene) 나노 시트를 제조하는 단계; 및 2) 상기 맥신(MXene) 나노 시트를 물(H2O) 및 유기용매 중에서 선택되는 어느 하나 이상에 분산시키는 단계를 포함하는 맥신(MXene) 나노 잉크의 제조 방법을 제공한다.In addition, the present invention comprises the steps of: 1) preparing a maxine nanosheet by reacting the MAX precursor of claim 1 with an acid-based solution containing a fluorine atom; and 2) dispersing the maxine (MXene) nanosheet in at least one selected from water (H 2 O) and an organic solvent.
맥스(MAX) 전구체를 상기 불소 원자를 함유하는 산 기반의 용액을 이용하여 중간층 물질이 제거함으로써 고순도의 맥신(MXene) 분말인 맥신(MXene) 나노 시트가 제조되며, 상기 맥신(MXene) 나노 시트를 물 또는 유기용매에 분산시켜 최종적으로 맥신(MXene) 나노 잉크를 얻을 수 있다.MXene nanosheets, which are high-purity MXene powders, are manufactured by removing the intermediate layer material from the MAX precursor using an acid-based solution containing the fluorine atom, and the MXene nanosheets Finally, MXene nano ink can be obtained by dispersing it in water or an organic solvent.
본 발명의 다른 일 실시예에 있어서, 상기 불소 원자를 함유하는 산 기반의 용액은 불산(HF), LiHF2, NaHF2, KHF2, 불소화리튬(LiF), 불화나트륨(NaF), 불화마그네슘(MgF2), 불화스트론튬(SrF2), 불화베릴륨(BeF2), 불화칼슘(CaF2), 불화암모늄(NH4F), 이불화암모늄(NH4HF2), 암모늄 헥사플루오로알루미네이트((NH4)3AlF6) 중에서 선택되는 어느 하나 이상을 포함할 수 있으나, 이에 한정되지 않는다.In another embodiment of the present invention, the acid-based solution containing a fluorine atom is hydrofluoric acid (HF), LiHF 2 , NaHF 2 , KHF 2 , lithium fluoride (LiF), sodium fluoride (NaF), magnesium fluoride ( MgF 2 ), strontium fluoride (SrF 2 ), beryllium fluoride (BeF 2 ) , calcium fluoride (CaF 2 ), ammonium fluoride (NH 4 F), ammonium difluoride (NH 4 HF 2 ), ammonium hexafluoroaluminate ( (NH 4 ) 3 AlF 6 ) It may include any one or more selected from, but is not limited thereto.
본 발명의 다른 일 실시예에 있어서, 상기 유기용매는 메틸 아세테이트(methyl acetate), 에틸아세테이트(ethyl acetate), 아세톤(acetone), 에탄올(ethanol) 중에서 선택되는 어느 하나 이상일 수 있으나, 이에 한정되지 않는다.In another embodiment of the present invention, the organic solvent may be any one or more selected from methyl acetate, ethyl acetate, acetone, and ethanol, but is not limited thereto. .
도 1은 본 발명에 따른 맥신(MXene) 나노 잉크의 제조방법을 예시한 흐름도로, 반응 조건, 반응물 등은 예시적으로 나타낸 것이며 이에 한정되지 않는다. 도 1을 이용하여 보다 상세히 설명하면 다음과 같다.1 is a flowchart illustrating a method of manufacturing MXene nano-ink according to the present invention, and reaction conditions, reactants, and the like are illustratively and not limited thereto. It will be described in more detail using FIG. 1 as follows.
저급 금속산화물과 탄소 분말을 혼합하여 1200℃에서 4시간 동안 반응시켜 탄화물을 제조한 후, 상기 탄화물과 알루미늄 분말을 혼합하여 1450℃에서 4시간 동안 반응시켜 맥스(MAX) 전구체를 제조한다. 상기 맥스(MAX) 전구체에 HF 기반의 산 용액에 반응시켜 맥신(MXene) 나노 시트를 제조한 후 물에 분산시켜 최종적으로 맥신(MXene) 나노잉크를 제조한다.A low-grade metal oxide and carbon powder are mixed and reacted at 1200° C. for 4 hours to prepare a carbide, and then the carbide and aluminum powder are mixed and reacted at 1450° C. for 4 hours to prepare a MAX precursor. MXene nanosheets are prepared by reacting the MAX precursor with an HF-based acid solution, and then dispersed in water to finally prepare MXene nanoinks.
본 발명은 상기 맥신(MXene) 나노 잉크로부터 제조된 투명 전극 또는 필름을 제공한다. 상기 투명 전극 및 필름은 유리 기판에 맥신(MXene) 나노 잉크를 코팅하여 형성된다.The present invention provides a transparent electrode or film prepared from the MXene nano ink. The transparent electrode and the film are formed by coating MXene nano ink on a glass substrate.
이하, 본 발명을 하기의 실시예에 의하여 더욱 상세하게 설명한다. 단, 하기의 실시예는 본 발명을 예시하는 것일 뿐, 본 발명의 내용이 하기의 실시예에 의해 한정되는 것은 아니다.Hereinafter, the present invention will be described in more detail with reference to the following examples. However, the following examples only illustrate the present invention, and the content of the present invention is not limited by the following examples.
제조예 1. 맥신(MXene) 나노 잉크의 제조Preparation Example 1. Preparation of MXene nano ink
TiO2 (Alfa Aesar, 99.5 %, 45 μm) 83.61g과 탄소 분말(Alfa Aesar, 99.9%, 3 μm) 37.62g을 1200℃ 에서 4시간 동안 반응시킨 후 알루미늄 분말(High Prity Chemical, 99.9%, 45 μm) 13.58g과 혼합하여 1450℃ 에서 4시간 동안 반응시켜 Ti3AlC2 분말 100 g을 제조하였다. 상기 Ti3AlC2 분말 10g을 HF 용액 100 ml과 10시간 동안 반응시켜 제조된 Ti3C2 나노 시트를 물에 0.5wt.% 농도로 분산시켜 Ti3C2 나노 잉크를 제조하였다.After reacting 83.61 g of TiO 2 (Alfa Aesar, 99.5 %, 45 μm) and 37.62 g of carbon powder (Alfa Aesar, 99.9%, 3 μm) at 1200° C. for 4 hours, aluminum powder (High Prity Chemical, 99.9%, 45 μm) 13.58 g and reacted at 1450° C. for 4 hours to prepare 100 g of Ti 3 AlC 2 powder. Ti 3 C 2 nano-ink was prepared by dispersing Ti 3 C 2 nanosheets prepared by reacting 10 g of the Ti 3 AlC 2 powder with 100 ml of an HF solution for 10 hours in water at a concentration of 0.5 wt.%.
실시예 1.Example 1. 맥신(MXene) 고농도 필름 제조Manufacture of MXene high-density film
상기 제조예 1에서 제조한 Ti3C2 나노 잉크를 진공 필터링(도 2, a)을 통해 고농도 필름을 제조하였다. 고농도 필름 제조 시 사용한 필터의 사이즈는 55 mm이며, 기공은 1 μm이다. 진공 필터링을 통해 고농도 필름이 제조되면 이를 진공 열처리 장치를 통해 45℃에서 1시간 동안 건조하였다. 이를 통해 제조된 고농도 필름의 두께는 10 μm이며, 도 2의(b)에 나타내었다.The Ti 3 C 2 nano ink prepared in Preparation Example 1 was subjected to vacuum filtering (FIG. 2, a) to prepare a high-concentration film. The size of the filter used to manufacture the high-concentration film was 55 mm, and the pores were 1 μm. When a high-concentration film was prepared through vacuum filtering, it was dried at 45° C. for 1 hour through a vacuum heat treatment apparatus. The thickness of the high-concentration film prepared through this was 10 μm, and is shown in FIG. 2(b).
실험예 1. XRD 분석Experimental Example 1. XRD analysis
상기 실시예 1에서 제조된 필름의 XRD(X-ray diffraction) 분석을 수행하였고, 그 결과를 도 2의 (c)에 나타내었다. XRD는 Cu-Kα 선을 사용하여 측정하였으며, XRD 측정 결과 Ti3C2 단일 상이 검출되었고 주요 피크는 (002) 면으로 형성되었으며, (002) 결정면 사이의 거리는 1.312 nm이다. XRD (X-ray diffraction) analysis of the film prepared in Example 1 was performed, and the results are shown in FIG. 2(c). XRD was measured using Cu-Kα ray, and as a result of XRD measurement, a Ti 3 C 2 single phase was detected, the main peak was formed as a (002) plane, and the distance between (002) crystal planes was 1.312 nm.
실험예 2. 전기적 특성 평가Experimental Example 2. Evaluation of electrical properties
상기 실시예 1 및 비교예 1인 상용 carbon-ukraine MXene(Carbon-Ukraine ltd., Ti3C2 aqueous solutions)의 필름에 대하여 하기와 같은 방법으로 저항, 면저항, 비저항 및 전기 전도도를 측정하여 그 결과를 표 1에 나타내었다. For the films of Example 1 and Comparative Example 1, commercially available carbon-ukraine MXene (Carbon-Ukraine ltd., Ti 3 C 2 aqueous solutions), resistance, sheet resistance, specific resistance and electrical conductivity were measured in the following manner. are shown in Table 1.
1) 저항: LCR (GWINSTEK, LCR-6002, Taiwan) 장비를 이용하여 측정하였다.1) Resistance: It was measured using LCR (GWINSTEK, LCR-6002, Taiwan) equipment.
2) 면저항: Four-point probe resistivity-meter (Mitsubishi, MCP-T370, Japan) 장비를 이용하여 측정하였다.2) Sheet resistance: It was measured using a four-point probe resistivity-meter (Mitsubishi, MCP-T370, Japan).
3) 비저항: Four-point probe resistivity-meter (Mitsubishi, MCP-T370, Japan) 장비를 이용하여 측정하였다.3) Resistivity: Measured using a four-point probe resistivity-meter (Mitsubishi, MCP-T370, Japan).
4) 전기 전도도: 상기 측정된 저항, 면저항, 비저항 및 필름 두께를 이용하여 전기 전도도를 계산하였다.4) Electrical Conductivity: Electrical conductivity was calculated using the measured resistance, sheet resistance, resistivity, and film thickness.
비교예 1Comparative Example 1 실시예 1Example 1
저항(Ω)Resistance (Ω) 0.14090.1409 0.07650.0765
면저항(Ω/sq)Sheet resistance (Ω/sq) 0.5730.573 0.39460.3946
비저항(Ω·cm)Specific resistance (Ω cm) 1.31×10-3 1.31×10 -3 6.14×10-4 6.14×10 -4
전기전도도electrical conductivity 763763 1,6281,628
상기 표 1에서 보이는 바와 같이, 실시예 1은 비교예 1에 비하여 전체적인 저항값이 낮고 전기전도도는 213.3% 증가하는 것을 확인하였다.As shown in Table 1, it was confirmed that Example 1 had a lower overall resistance value and increased electrical conductivity by 213.3% compared to Comparative Example 1.
실시예 2. 맥신(MXene) 투명 전극 제조Example 2. MXene transparent electrode manufacturing
상기 제조예 1에서 제조한 Ti3C2 나노 잉크를 유리 기판에 코팅하여 투명 전극을 제조하여, 도 3의 (a)에 도시된 바와 같이 투명 전극을 얻었다. 코팅은 스핀 코팅법을 사용하였으며, 이때 회전수는 3,000 rpm 이고 유지시간은 30 초 였으며, 1회 코팅에 약 5 ml 나노 잉크를 사용하였다.A transparent electrode was prepared by coating the Ti 3 C 2 nano ink prepared in Preparation Example 1 on a glass substrate, thereby obtaining a transparent electrode as shown in (a) of FIG. 3 . A spin coating method was used for coating, in which the rotation speed was 3,000 rpm and the holding time was 30 seconds, and about 5 ml of nano ink was used for one coating.
상기 투명 전극은 도 3의 (b)에 도시된 바와 같이 주사전자현미경((FE-SEM, SUPRA40VP, Carl Zeiss, Germany)을 통하여 빈 공간없이 완벽하게 코팅되었음을 확인하였다. As shown in (b) of FIG. 3, it was confirmed that the transparent electrode was completely coated without empty space through a scanning electron microscope ((FE-SEM, SUPRA40VP, Carl Zeiss, Germany).

Claims (7)

  1. a) 저급 금속산화물을 탄소 또는 질소와 반응시켜 탄화물 또는 질화물을 제조하는 단계; 및a) preparing a carbide or nitride by reacting a lower metal oxide with carbon or nitrogen; and
    b) 상기 a)단계에서 제조된 탄화물 또는 질화물을 알루미늄 또는 실리콘과 합성하는 단계를 포함하는 맥스(MAX) 전구체의 제조방법.b) A method of producing a MAX precursor comprising the step of synthesizing the carbide or nitride prepared in step a) with aluminum or silicon.
  2. 제 1항에 있어서,The method of claim 1,
    상기 금속은 Sc, Y, Lu, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo 및 W 중에서 선택되는 어느 하나 이상의 전이금속인 것을 특징으로 하는 맥스 전구체의 제조방법.The metal is Sc, Y, Lu, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, and a method for producing a max precursor, characterized in that any one or more transition metals selected from W.
  3. 1) 제 1항의 맥스(MAX) 전구체를 불소 원자를 함유하는 산 기반의 용액에 반응시켜 맥신(MXene) 나노 시트를 제조하는 단계; 및1) preparing MXene nanosheets by reacting the MAX precursor of claim 1 with an acid-based solution containing a fluorine atom; and
    2) 상기 맥신(MXene) 나노 시트를 물(H2O) 및 유기용매 중에서 선택되는 어느 하나 이상에 분산시키는 단계를 포함하는 맥신(MXene) 나노 잉크의 제조방법.2) A method of producing a maxine (MXene) nano-ink comprising dispersing the maxine (MXene) nanosheet in at least one selected from water (H 2 O) and an organic solvent.
  4. 제 3항에 있어서,4. The method of claim 3,
    상기 불소 원자를 함유하는 산 기반의 용액은 불산(HF), LiHF2, NaHF2, KHF2, 불소화리튬(LiF), 불화나트륨(NaF), 불화마그네슘(MgF2), 불화스트론튬(SrF2), 불화베릴륨(BeF2), 불화칼슘(CaF2), 불화암모늄(NH4F), 이불화암모늄(NH4HF2), 암모늄 헥사플루오로알루미네이트((NH4)3AlF6) 중에서 선택되는 어느 하나 이상을 포함하는 것을 특징으로 하는 맥신(MXene) 나노 잉크의 제조방법.The acid-based solution containing the fluorine atom is hydrofluoric acid (HF), LiHF 2 , NaHF 2 , KHF 2 , lithium fluoride (LiF), sodium fluoride (NaF), magnesium fluoride (MgF 2 ), strontium fluoride (SrF 2 ) , beryllium fluoride (BeF 2 ), calcium fluoride (CaF 2 ), ammonium fluoride (NH 4 F), ammonium difluoride (NH 4 HF 2 ), ammonium hexafluoroaluminate ((NH 4 ) 3 AlF 6 ) Maxine (MXene), characterized in that it comprises any one or more of the method for producing nano-ink.
  5. 제 3항에 있어서,4. The method of claim 3,
    상기 유기용매는 메틸 아세테이트(methyl acetate), 에틸아세테이트(ethyl acetate), 아세톤(acetone), 에탄올(ethanol) 중에서 선택되는 어느 하나 이상인 것을 특징으로 하는 맥신(MXene) 나노 잉크의 제조방법.The organic solvent is methyl acetate (methyl acetate), ethyl acetate (ethyl acetate), acetone (acetone), a method of manufacturing MXene nano ink, characterized in that at least one selected from the group consisting of ethanol (ethanol).
  6. 제 3항의 맥신(MXene) 나노 잉크로부터 제조된 투명 전극.A transparent electrode prepared from the MXene nano-ink of claim 3.
  7. 제 3항의 맥신(MXene) 나노 잉크로부터 제조된 필름.A film made from the MXene nano ink of claim 3.
PCT/KR2021/004705 2021-03-03 2021-04-14 Method for preparing max precursor and mxene nanoink WO2022186423A1 (en)

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