WO2021025206A1 - Method of storing mxene at low temperatures - Google Patents

Method of storing mxene at low temperatures Download PDF

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WO2021025206A1
WO2021025206A1 PCT/KR2019/009905 KR2019009905W WO2021025206A1 WO 2021025206 A1 WO2021025206 A1 WO 2021025206A1 KR 2019009905 W KR2019009905 W KR 2019009905W WO 2021025206 A1 WO2021025206 A1 WO 2021025206A1
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maxine
solution
maxine solution
stored
transition metal
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PCT/KR2019/009905
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French (fr)
Korean (ko)
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안치원
채윤정
이용희
이병주
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한국과학기술원
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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
    • C01B32/914—Carbides of single elements
    • C01B32/921—Titanium carbide
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • the present invention relates to a method of storing Maxine, and more particularly, to a method of storing Maxine at a low temperature capable of maintaining constant electrical characteristics through low temperature storage.
  • the MAX phase (where M is a transition metal, A is a group 13 or 14 element, X is a carbon and/or nitrogen) is a quasi-ceramic property MX and a metal element A different from M It has excellent physical properties such as electrical conductivity, oxidation resistance, and machinability due to the combined crystalline material. It is known that more than 60 types of MAX phases have been synthesized so far.
  • the MAX phase is a two-dimensional material, but unlike graphite or metal dichalcogenide materials, transition metal carbide is stacked with weak chemical bonds between the element A and the transition metal M between layers of each other. Therefore, it is difficult to transform into a two-dimensional structure using a general mechanical or chemical peeling method.
  • MXene has similar electrical conductivity and strength as graphene, and can be applied to various application technologies ranging from energy storage devices to biomedical applications and composites.
  • the technical problem to be achieved by the present invention is to provide a method for storing Maxine at a low temperature capable of maintaining constant electrical characteristics of Maxine by rapidly cooling Maxine and storing it in a low temperature state.
  • the method for storing Maxine at a low temperature includes the steps of: (a) preparing a Maxine solution consisting of a transition metal carbide and a transition metal carbonitride having a two-dimensional structure, and (b) a container containing the prepared Maxine solution. Putting in, (c) providing a step of rapidly cooling the Maxine solution contained in the container to maintain constant electrical properties.
  • the Maxine solution is Ti 2 C, Ti 3 C 2 , V 2 C, Nb 2 C, (Ti 0.5 , Nb 0.5 ) 2 CT x , Ti 3 CN, (V 0.5 , Cr 0.5 ) 3 C 2 , Ta 4 C 3 and Nb 4 C 3 It may be composed of any one of .
  • the Maxine solution in step (b), may be distributed and stored in small portions of 5 mL or less.
  • the Maxine solution may be formed of the formula of M n + 1 X n .
  • M may be a front transition metal.
  • X in the formula of M n + 1 X n may include at least one of carbon and nitrogen.
  • rapid cooling of the Maxine solution is performed through a freezer, and it is possible to maintain a low temperature by using helium or liquid nitrogen as a refrigerant.
  • step (c) it is also possible to store the Maxine solution in step (c) together with any one of inert gas, nitrogen gas, and air, or a mixed gas.
  • the rapid cooling temperature in step (c) may be set to -80°C or less.
  • the sheet resistance value of the Maxine solution may be maintained at 10 ⁇ /sq or less through low temperature storage.
  • the rapid cooling temperature in step (c) may be set to -18°C to -80°C or less.
  • the sheet resistance value of the Maxine solution may be maintained at 100000 ⁇ /sq or less through low temperature storage.
  • the Maxine device may be configured as an electrode material through the Maxine solution stored through the method of storing Maxine at a low temperature.
  • the Maxine solution stored through the low-temperature storage method of Maxine may be prepared in the form of a film through spin coating, drop cast, or vacuum filtration.
  • the method of storing Maxine at a low temperature is effective in maintaining constant electrical characteristics of Maxine by rapidly cooling Maxine and storing it in a low temperature state.
  • 1 is a flow chart of a method for storing Maxine at a low temperature according to the present invention.
  • 2 is a graph showing the concentration of Maxine solution according to the change of time and storage temperature and conditions of air or Ar atmosphere according to the present invention.
  • FIG. 4 is a photographic view of the changed Maxine solution when the Maxine solution is stored in air according to temperature and time in FIG. 3 according to the present invention.
  • FIG. 5 is a photographic view of the changed Maxine film in FIG. 3 according to the present invention when the Maxine film is stored in air according to temperature and time.
  • FIG. 6 is an imaging diagram and XRD graph of Maxine immediately after synthesis according to the present invention and Maxine stored in low temperature and air for 1 month.
  • the most preferred embodiment according to the present invention includes the steps of: (a) preparing a Maxine solution consisting of a transition metal carbide and a transition metal carbonitride of a two-dimensional structure; (b) putting the prepared Maxine solution in a container; (c) rapidly cooling the Maxine solution contained in the container so that the electrical properties are kept constant; It includes, and the rapid cooling temperature in the step (c) is characterized in that set to -80 °C or less.
  • 1 is a flow chart of a method for storing Maxine at a low temperature according to the present invention.
  • the low-temperature storage method of Maxine includes the steps of (a) preparing a Maxine solution consisting of a two-dimensional transition metal carbide and a transition metal carbonitride (S110), (b) putting the prepared Maxine solution in a container (S120). ), (c) providing a step (S130) of rapidly cooling the Maxine solution into a container so that the electrical properties of the Maxine solution are kept constant.
  • a method of storing Maxine at a low temperature may include preparing a Maxine solution composed of a transition metal carbide and a transition metal carbonitride having a two-dimensional structure.
  • Maxine is a two-dimensional layered structure, in which layers composed of atoms are stacked to form a multilayer structure.
  • the two-dimensional multi-layered structure, Maxine is light and has a low density, has excellent electrical conductivity, and can be easily separated from each other, so that it can be used as a radio wave absorber in various fields.
  • a Maxine solution composed of such two-dimensional transition metal carbide and transition metal carbonitride can be prepared for low temperature storage.
  • the Maxine solution is Ti 2 C, Ti 3 C 2 , V 2 C, Nb 2 C, (Ti 0.5 , Nb 0.5 ) 2 CT x , Ti 3 CN, (V 0.5 , Cr 0.5 ) 3 C 2 , Ta 4 C 3 and Nb 4 C 3 It may be composed of any one of .
  • the Maxine solution may be composed of a formula of M n + 1 X n, in the formula of M n + 1 X n , M is an early transition metal, and X is at least one of carbon and nitrogen. And, n may be an integer of 1 to 4.
  • the method of storing Maxine at a low temperature may include placing the prepared Maxine solution in a container.
  • the prepared Maxine solution In order to store the prepared Maxine solution at a low temperature, it is distributed and stored in 4 mL to 6 mL through the process of distributing and storing in a small amount in a container, preferably 5 mL and stored in the container. If the Maxine solution is distributed and stored in more than 7 mL, the efficiency of rapid cooling may be reduced because it is not uniformly cooled during rapid cooling. The efficiency of
  • the low-temperature storage method of Maxine may include the step of rapidly cooling the Maxine solution so as to maintain constant electrical characteristics of the Maxine solution in a container.
  • the Maxine solution may be rapidly cooled to a temperature of -80°C or less.
  • 2 is a graph showing the concentration of the Maxine solution according to the change of time during storage of the Maxine solution, the storage temperature (5°C, room temperature), and the conditions of the air or Ar (argon) atmosphere.
  • the sheet resistance value of the Maxine solution may be maintained at 10 ⁇ /sq or less through low temperature storage.
  • the Maxine solution is stored in a refrigerator (-80°C or less) and air, the electrical characteristics of the Maxine solution can be maintained constant.
  • FIG. 4 is an imaging diagram of the changed Maxine solution when the Maxine solution is stored in air according to temperature and time in FIG. 3.
  • the Maxine solution has a high temperature and is oxidized over time and gradually decreases in concentration, but there is relatively no change when stored in a refrigerator (-80°C or less). Therefore, if the Maxine solution is stored in a refrigerator (-80°C or less) and air, the electrical characteristics of the Maxine solution can be maintained constant.
  • 5 is a photographic view of the changed Maxine film when stored in air according to temperature and time by replacing the Maxine solution with Maxine film in FIG. 3.
  • the Maxine film has a high temperature and changes in color due to oxidation over time, but there is relatively no change when stored in a refrigerator (-80°C or less). Therefore, if the Maxine solution is stored in a refrigerator (-80°C or less) and air, the electrical characteristics of the Maxine solution can be maintained constant.
  • the lower the temperature, the lower the diffusion coefficient and reactivity of the air, and the air transmittance is very low in the Disordered ICE. Therefore, if Maxine solution is rapidly cooled in a freezer (-80°C or less), the disorder of ice becomes more severe compared to when stored in a freezer (-18°C), and as a result, the permeability of air penetration into Maxine decreases. . Therefore, if the Maxine solution is stored in a refrigerator (-80°C or less) and air, the electrical characteristics of the Maxine solution can be maintained constant.
  • Maxine device may be configured as an electrode material through the Maxine solution stored through the low-temperature storage method of Maxine.
  • the Maxine solution according to the present invention can maintain the temperature of the refrigerator at -18°C to -80°C and maintain an appropriate level of electrical characteristics through rapid cooling.
  • the Maxine solution can maintain almost constant electrical characteristics in a freezer (below -80°C), but it requires a lot of cost and additional equipment to maintain the temperature below -80°C.
  • the appropriate level of electrical characteristics is to be maintained at 10 ⁇ /sq or more to 100000 ⁇ /sq or less.
  • Maxine solution when stored in a refrigerator, it is selectively stored at -80°C or lower or -18°C to -80°C to maintain an appropriate level of electrical characteristics, and cost for storage may be reduced.
  • the Maxine solution when stored at a low temperature, it may be stored with any one of inert gas, nitrogen gas, and air, or a mixed gas.
  • the Maxine solution may be stored in an inert gas such as He, Ne, Ar, Kr, Xe, Rn, or any one of nitrogen gas or air, and the gas is mixed with a mixed gas or mixed gas. It is also possible to store in a mixture of air.
  • an inert gas such as He, Ne, Ar, Kr, Xe, Rn, or any one of nitrogen gas or air. It is also possible to store in a mixture of air.
  • contact with oxygen may be blocked by an inert gas or nitrogen gas, and electrical characteristics may be prevented from being changed due to the combination of the Maxine solution with oxygen.
  • the refrigerator for maintaining the Maxine solution at a low temperature may be driven using helium or liquid nitrogen as a refrigerant.
  • Maxine solution stored through the low-temperature storage method of Maxine may be a Maxine film manufactured in the form of a film through spin coating, drop cast, and vacuum filtration.
  • Maxine film by manufacturing a Maxine film through various methods such as spin coating, drop-casting and vacuum filtration as described above, it is possible to effectively produce a Maxine film according to manufacturing conditions or conditions.

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  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)

Abstract

The present invention relates to a method of storing MXene at low temperatures, and more specifically, the method comprises the steps of: (a) preparing a MXene solution consisting of a transition metal carbonitride and a transition metal carbide having a two-dimensional structure; (b) placing the prepared MXene solution in a container; and (c) quick-freezing the MXene solution placed in the container so as to maintain uniform electrical properties, wherein since MXene is quick-frozen and stored in a low-temperature state, electrical properties of MXene can be uniformly maintained. <Representative drawing> Figure 1

Description

맥신의 저온 보관방법How to store Maxine at low temperature
본 발명은 맥신의 보관방법에 관한 것으로, 더욱 상세하게는 저온 보관을 통해 전기적 특성을 일정하게 유지할 수 있는 맥신의 저온 보관방법에 관한 것이다.The present invention relates to a method of storing Maxine, and more particularly, to a method of storing Maxine at a low temperature capable of maintaining constant electrical characteristics through low temperature storage.
2차원 물질 중 하나로, MAX 상 (MAX phase, 여기서 M은 전이금속, A는 13 또는 14족 원소, X는 탄소 및/또는 질소)은 준 세라믹 특성의 MX와, M과는 다른 금속원소 A가 조합된 결정질로 전기전도성, 내산화성, 기계가공성 등의 물성이 우수하다. 현재까지 60 종류 이상의 MAX 상이 합성된 것으로 알려져 있다.As one of the two-dimensional materials, the MAX phase (where M is a transition metal, A is a group 13 or 14 element, X is a carbon and/or nitrogen) is a quasi-ceramic property MX and a metal element A different from M It has excellent physical properties such as electrical conductivity, oxidation resistance, and machinability due to the combined crystalline material. It is known that more than 60 types of MAX phases have been synthesized so far.
MAX 상은 이차원 물질이지만, 흑연이나 금속 디칼코게나이드 물질과 달리 전이금속 카바이드 서로의 층상 간에 A 원소와 전이금속 M 사이의 약한 화학적 결합으로 스택되어 있다. 따라서 일반적인 기계적인 박리법이나 화학적 박리법을 사용하여 2차원 구조로 변형시키기 어렵다.The MAX phase is a two-dimensional material, but unlike graphite or metal dichalcogenide materials, transition metal carbide is stacked with weak chemical bonds between the element A and the transition metal M between layers of each other. Therefore, it is difficult to transform into a two-dimensional structure using a general mechanical or chemical peeling method.
그러나, 최근 2011년도에 Drexel university의 Michel W. Barsoum 교수가 이끄는 연구진은 MAX 상인 3차원의 티타늄-알루미늄 카바이드에서 불산을 사용하여 알루미늄 층을 선택적으로 제거함으로써, 완전히 다른 특성을 갖는 2차원의 구조로 변형시키는데 성공하였다. 연구진은 MAX 상을 박리하여 얻어진 2차원의 물질을 "맥신(MXene)"이라 명명하였다. 맥신(MXene)은 그래핀과 같은 유사한 전기전도성과 강도를 가지며, 에너지 저장 장치에서부터 바이오메디컬 응용, 복합체에 이르는 다양한 응용 기술에 적용할 수 있다.However, recently, in 2011, a research team led by Professor Michel W. Barsoum of Drexel University developed a two-dimensional structure with completely different characteristics by selectively removing the aluminum layer using hydrofluoric acid from the three-dimensional titanium-aluminum carbide, a MAX merchant. It succeeded in transforming. The researchers named the two-dimensional material obtained by exfoliating the MAX phase as "MXene". MXene has similar electrical conductivity and strength as graphene, and can be applied to various application technologies ranging from energy storage devices to biomedical applications and composites.
하지만, 이러한 맥신을 물분산시켜 용액으로 보관 시 공기 및 물에 의해 산화되어 본래의 특성을 잃어버리기 쉽다.However, when the maxine is dispersed in water and stored as a solution, it is easy to lose its original properties due to oxidation by air and water.
*따라서, 본래의 특성을 유지하기 위해서 맥신용액의 보관 시 저온(5℃)에서 Ar 분위기를 형성하여 보관함으로써, 특성을 장기간 유지시킬 수 있었다.* Therefore, in order to maintain the original properties, by forming and storing an Ar atmosphere at a low temperature (5°C) when storing the Maxine solution, the properties could be maintained for a long time.
그러나, 이러한 보관방법은 Ar분위기를 유지시키기 위해서 진공장비 및 Ar 가스장치 등 추가적인 장비가 필요하므로 비용상승 및 불필요한 작업이 추가되었다.However, this storage method requires additional equipment such as vacuum equipment and Ar gas equipment in order to maintain the Ar atmosphere, thus increasing cost and adding unnecessary work.
따라서, 보다 간편하게 맥신용액의 특성을 유지시킬 수 있는 저장방법이 필요한 실정이다.Therefore, there is a need for a storage method that can more conveniently maintain the properties of Maxine solution.
<선행기술문헌> 공개특허공보 제 10-2017-0036507호(2017.04.03.<Prior technical literature> Unexamined Patent Publication No. 10-2017-0036507 (2017.04.03.
본 발명이 이루고자 하는 기술적 과제는 맥신을 급속냉각시켜 저온 상태로 저장함으로써, 맥신의 전기적 특성을 일정하게 유지시킬 수 있는 맥신의 저온 보관방법을 제공하는 것이다.The technical problem to be achieved by the present invention is to provide a method for storing Maxine at a low temperature capable of maintaining constant electrical characteristics of Maxine by rapidly cooling Maxine and storing it in a low temperature state.
본 발명이 이루고자 하는 기술적 과제는 이상에서 언급한 기술적 과제로 제한되지 않으며, 언급되지 않은 또 다른 기술적 과제들은 아래의 기재로부터 본 발명이 속하는 기술 분야에서 통상의 지식을 가진 자에게 명확하게 이해될 수 있을 것이다.The technical problem to be achieved by the present invention is not limited to the technical problems mentioned above, and other technical problems that are not mentioned can be clearly understood by those of ordinary skill in the technical field to which the present invention belongs from the following description. There will be.
상기 기술적 과제를 달성하기 위하여, 본 발명에 따른 맥신의 저온 보관방법은 (a)이차원구조의 전이금속 탄화물 및 전이금속 탄질화물로 구성된 맥신용액을 준비하는 단계, (b)상기 준비된 맥신용액을 용기에 담는 단계, (c) 상기 용기에 담긴 맥신용액을 전기적 특성이 일정하게 유지되도록 급속 냉각시키는 단계를 제공한다.In order to achieve the above technical problem, the method for storing Maxine at a low temperature according to the present invention includes the steps of: (a) preparing a Maxine solution consisting of a transition metal carbide and a transition metal carbonitride having a two-dimensional structure, and (b) a container containing the prepared Maxine solution. Putting in, (c) providing a step of rapidly cooling the Maxine solution contained in the container to maintain constant electrical properties.
본 발명의 실시예에 있어서, 상기 맥신용액은 Ti 2C, Ti 3C 2, V 2C, Nb 2C, (Ti 0.5, Nb 0.5) 2CT x, Ti 3CN, (V 0.5, Cr 0.5) 3C 2, Ta 4C 3 및 Nb 4C 3 중 어느 하나로 구성된 것일 수 있다.In an embodiment of the present invention, the Maxine solution is Ti 2 C, Ti 3 C 2 , V 2 C, Nb 2 C, (Ti 0.5 , Nb 0.5 ) 2 CT x , Ti 3 CN, (V 0.5 , Cr 0.5 ) 3 C 2 , Ta 4 C 3 and Nb 4 C 3 It may be composed of any one of .
본 발명의 실시예에 있어서, 상기 (b) 단계에서 상기 맥신용액은 5mL 이하로 소량씩 분배되어 저장된 것도 가능하다.In an embodiment of the present invention, in step (b), the Maxine solution may be distributed and stored in small portions of 5 mL or less.
본 발명의 실시예에 있어서, 상기 맥신용액은 M n+ 1X n의 화학식으로 이루진 것도 가능하다.In an embodiment of the present invention, the Maxine solution may be formed of the formula of M n + 1 X n .
본 발명의 실시예에 있어서, 상기 M n+ 1X n의 화학식에서 M은 앞전이금속인 것일 수 있다.In an embodiment of the present invention, in the formula of M n + 1 X n , M may be a front transition metal.
본 발명의 실시예에 있어서, 상기 M n+ 1X n의 화학식에서 X는 탄소 및 질소 중에서 적어도 하나를 포함하는 것도 가능하다.In an embodiment of the present invention, X in the formula of M n + 1 X n may include at least one of carbon and nitrogen.
*본 발명의 실시예에 있어서, 상기 맥신용액의 급속냉각은 냉동기를 통해서 이루어지고 헬륨 또는 액체질소를 냉매로 사용하여 저온이 유지되는 것도 가능하다.* In an embodiment of the present invention, rapid cooling of the Maxine solution is performed through a freezer, and it is possible to maintain a low temperature by using helium or liquid nitrogen as a refrigerant.
본 발명의 실시예에 있어서, 상기 (c) 단계에서 맥신용액을 불활성가스, 질소가스, 공기 중 어느 한가지 또는 혼합된 가스와 함께 보관되는 것도 가능하다.In an embodiment of the present invention, it is also possible to store the Maxine solution in step (c) together with any one of inert gas, nitrogen gas, and air, or a mixed gas.
본 발명의 실시예에 있어서, 상기 (c) 단계에서 급속냉각 온도는 -80℃ 이하로 설정된 것도 가능하다.In an embodiment of the present invention, the rapid cooling temperature in step (c) may be set to -80°C or less.
본 발명의 실시예에 있어서, 상기 맥신용액의 면저항값은 저온 보관을 통해 10Ω/sq 이하로 유지되는 것일 수 있다.In an embodiment of the present invention, the sheet resistance value of the Maxine solution may be maintained at 10 Ω/sq or less through low temperature storage.
본 발명의 실시예에 있어서, 상기 (c) 단계에서 급속냉각 온도는 -18℃ 내지 -80℃ 이하로 설정된 것도 가능하다.In an embodiment of the present invention, the rapid cooling temperature in step (c) may be set to -18°C to -80°C or less.
본 발명의 실시예에 있어서, 상기 맥신용액의 면저항값은 저온 보관을 통해 100000Ω/sq 이하로 유지되는 것일 수 있다.In an embodiment of the present invention, the sheet resistance value of the Maxine solution may be maintained at 100000Ω/sq or less through low temperature storage.
본 발명의 실시예에 있어서, 상기 맥신의 저온 보관방법을 통해 보관된 맥신용액을 통해 전극재료로 맥신소자가 구성될 수 있다.In an embodiment of the present invention, the Maxine device may be configured as an electrode material through the Maxine solution stored through the method of storing Maxine at a low temperature.
본 발명의 실시예에 있어서, 상기 맥신의 저온 보관방법을 통해 보관된 맥신용액이 스핀코팅, 드롭캐스트, 감압여과 방식을 통해 필름형태로 제조된 것일 수 있다.In an embodiment of the present invention, the Maxine solution stored through the low-temperature storage method of Maxine may be prepared in the form of a film through spin coating, drop cast, or vacuum filtration.
본 발명의 실시예에 따르면, 맥신의 저온 보관방법은 맥신을 급속냉각시켜 저온 상태로 저장함으로써, 맥신의 전기적 특성을 일정하게 유지시킬 수 있는 효과가 있다.According to an exemplary embodiment of the present invention, the method of storing Maxine at a low temperature is effective in maintaining constant electrical characteristics of Maxine by rapidly cooling Maxine and storing it in a low temperature state.
본 발명의 효과는 상기한 효과로 한정되는 것은 아니며, 본 발명의 상세한 설명 또는 특허청구범위에 기재된 발명의 구성으로부터 추론 가능한 모든 효과를 포함하는 것으로 이해되어야 한다.The effects of the present invention are not limited to the above effects, and should be understood to include all effects that can be inferred from the configuration of the invention described in the detailed description or claims of the present invention.
도 1은 본 발명에 따른 맥신의 저온 보관방법의 순서도이다.1 is a flow chart of a method for storing Maxine at a low temperature according to the present invention.
도 2는 본 발명에 따른 시간의 변화와 보관온도 및 공기 중 또는 Ar 분위기의 조건에 따른 맥신용액의 농도를 나타낸 그래프이다.2 is a graph showing the concentration of Maxine solution according to the change of time and storage temperature and conditions of air or Ar atmosphere according to the present invention.
도 3은 본 발명에 따른 아르곤 분위기 없이 공기 중에서 온도 및 시간의 변화에 따른 면저항값이 도시된다.3 shows sheet resistance values according to changes in temperature and time in air without an argon atmosphere according to the present invention.
도 4는 본 발명에 따른 도 3에서 맥신용액을 공기 중에서 온도 및 시간에 따라 보관하였을 때의 변화된 맥신용액의 촬상도이다.4 is a photographic view of the changed Maxine solution when the Maxine solution is stored in air according to temperature and time in FIG. 3 according to the present invention.
도 5는 본 발명에 따른 도 3에서 맥신필름을 공기 중에서 온도 및 시간에 따라 보관하였을 때의 변화된 맥신필름의 촬상도이다.5 is a photographic view of the changed Maxine film in FIG. 3 according to the present invention when the Maxine film is stored in air according to temperature and time.
도 6은 본 발명에 따른 합성 직후의 맥신 및 1개월간 저온 및 공기 중에서 보관된 맥신의 촬상도 및 XRD그래프이다.6 is an imaging diagram and XRD graph of Maxine immediately after synthesis according to the present invention and Maxine stored in low temperature and air for 1 month.
본 발명에 따른 가장 바람직한 일 실시예는, (a)이차원구조의 전이금속 탄화물 및 전이금속 탄질화물로 구성된 맥신용액을 준비하는 단계; (b)상기 준비된 맥신용액을 용기에 담는 단계; (c)상기 용기에 담긴 맥신용액을 전기적 특성이 일정하게 유지되도록 급속 냉각시키는 단계; 를 포함하며, 상기 (c) 단계에서 급속냉각 온도는 -80℃ 이하로 설정된 것을 특징으로 한다.The most preferred embodiment according to the present invention includes the steps of: (a) preparing a Maxine solution consisting of a transition metal carbide and a transition metal carbonitride of a two-dimensional structure; (b) putting the prepared Maxine solution in a container; (c) rapidly cooling the Maxine solution contained in the container so that the electrical properties are kept constant; It includes, and the rapid cooling temperature in the step (c) is characterized in that set to -80 ℃ or less.
이하에서는 첨부한 도면을 참조하여 본 발명을 설명하기로 한다. 그러나 본 발명은 여러 가지 상이한 형태로 구현될 수 있으며, 따라서 여기에서 설명하는 실시예로 한정되는 것은 아니다. 그리고 도면에서 본 발명을 명확하게 설명하기 위해서 설명과 관계없는 부분은 생략하였으며, 명세서 전체를 통하여 유사한 부분에 대해서는 유사한 도면 부호를 붙였다.Hereinafter, the present invention will be described with reference to the accompanying drawings. However, the present invention may be implemented in various different forms, and therefore is not limited to the embodiments described herein. In the drawings, parts irrelevant to the description are omitted in order to clearly describe the present invention, and similar reference numerals are assigned to similar parts throughout the specification.
명세서 전체에서, 어떤 부분이 다른 부분과 "연결(접속, 접촉, 결합)"되어 있다고 할 때, 이는 "직접적으로 연결"되어 있는 경우뿐 아니라, 그 중간에 다른 부재를 사이에 두고 "간접적으로 연결"되어 있는 경우도 포함한다. 또한 어떤 부분이 어떤 구성요소를 "포함"한다고 할 때, 이는 특별히 반대되는 기재가 없는 한 다른 구성요소를 제외하는 것이 아니라 다른 구성요소를 더 구비할 수 있다는 것을 의미한다.Throughout the specification, when a part is said to be "connected (connected, contacted, bonded)" with another part, it is not only "directly connected", but also "indirectly connected" with another member in the middle. "Including the case. In addition, when a part "includes" a certain component, it means that other components may be further provided, rather than excluding other components unless specifically stated to the contrary.
본 명세서에서 사용한 용어는 단지 특정한 실시예를 설명하기 위해 사용된 것으로, 본 발명을 한정하려는 의도가 아니다. 단수의 표현은 문맥상 명백하게 다르게 뜻하지 않는 한, 복수의 표현을 포함한다. 본 명세서에서, "포함하다" 또는 "가지다" 등의 용어는 명세서상에 기재된 특징, 숫자, 단계, 동작, 구성요소, 부품 또는 이들을 조합한 것이 존재함을 지정하려는 것이지, 하나 또는 그 이상의 다른 특징들이나 숫자, 단계, 동작, 구성요소, 부품 또는 이들을 조합한 것들의 존재 또는 부가 가능성을 미리 배제하지 않는 것으로 이해되어야 한다.The terms used in the present specification are only used to describe specific embodiments, and are not intended to limit the present invention. Singular expressions include plural expressions unless the context clearly indicates otherwise. In this specification, terms such as "comprise" or "have" are intended to designate the presence of features, numbers, steps, actions, components, parts, or a combination thereof described in the specification, but one or more other features. It is to be understood that the presence or addition of elements or numbers, steps, actions, components, parts, or combinations thereof, does not preclude in advance the possibility.
이하 첨부된 도면을 참고하여 본 발명의 실시예를 상세히 설명하기로 한다.Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
도 1은 본 발명에 따른 맥신의 저온 보관방법의 순서도이다.1 is a flow chart of a method for storing Maxine at a low temperature according to the present invention.
본 발명에 따른 맥신의 저온 보관방법은 (a)이차원구조의 전이금속 탄화물 및 전이금속 탄질화물로 구성된 맥신용액을 준비하는 단계(S110), (b)상기 준비된 맥신용액을 용기에 담는 단계(S120), (c)상기 맥신용액을 용기에 담고 상기 맥신용액의 전기적 특성이 일정하게 유지되도록 급속냉각 시키는 단계(S130)를 제공한다. The low-temperature storage method of Maxine according to the present invention includes the steps of (a) preparing a Maxine solution consisting of a two-dimensional transition metal carbide and a transition metal carbonitride (S110), (b) putting the prepared Maxine solution in a container (S120). ), (c) providing a step (S130) of rapidly cooling the Maxine solution into a container so that the electrical properties of the Maxine solution are kept constant.
본 발명의 실시예에 있어서, 맥신의 저온 보관방법은 이차원구조의 전이금속 탄화물 및 전이금속 탄질화물로 구성된 맥신용액을 준비하는 단계를 포함할 수 있다.In an embodiment of the present invention, a method of storing Maxine at a low temperature may include preparing a Maxine solution composed of a transition metal carbide and a transition metal carbonitride having a two-dimensional structure.
보다 상세하게는, 맥신은 2차원 층상 구조체로, 원자로 구성되는 층이 적층되어 다층 구조를 이루고 있다. 이와 같은 2차원 다층 구조체인 맥신은 가볍고 낮은 밀도를 가지며, 전기 전도도가 우수하고, 상호간에 쉽게 분리가 가능하여 다양한 분야에서 전파 흡수체로 사용될 수 있다.In more detail, Maxine is a two-dimensional layered structure, in which layers composed of atoms are stacked to form a multilayer structure. The two-dimensional multi-layered structure, Maxine, is light and has a low density, has excellent electrical conductivity, and can be easily separated from each other, so that it can be used as a radio wave absorber in various fields.
이러한 이차원구조의 전이금속 탄화물 및 전이금속 탄질화물로 구성된 맥신용액을 저온 보관을 위해 준비할 수 있다.A Maxine solution composed of such two-dimensional transition metal carbide and transition metal carbonitride can be prepared for low temperature storage.
이때, 상기 맥신용액은 Ti 2C, Ti 3C 2, V 2C, Nb 2C, (Ti 0.5, Nb 0.5) 2CT x, Ti 3CN, (V 0.5, Cr 0.5) 3C 2, Ta 4C 3 및 Nb 4C 3 중 어느 하나로 구성될 수 있다.At this time, the Maxine solution is Ti 2 C, Ti 3 C 2 , V 2 C, Nb 2 C, (Ti 0.5 , Nb 0.5 ) 2 CT x , Ti 3 CN, (V 0.5 , Cr 0.5 ) 3 C 2 , Ta 4 C 3 and Nb 4 C 3 It may be composed of any one of .
또한, 상기 맥신용액은 M n+ 1X n의 화학식으로 이루질 수 있고, 상기 M n+ 1X n의 화학식에서 M은 앞전이금속(early transition metal)이고, X는 탄소 및 질소 중에서 적어도 하나를 포함하며, n은 1 내지 4의 정수일 수 있다.In addition, the Maxine solution may be composed of a formula of M n + 1 X n, in the formula of M n + 1 X n , M is an early transition metal, and X is at least one of carbon and nitrogen. And, n may be an integer of 1 to 4.
또한, 맥신의 저온 보관방법은 준비된 맥신용액을 용기에 담는 단계를 포함할 수 있다.In addition, the method of storing Maxine at a low temperature may include placing the prepared Maxine solution in a container.
준비된 맥신용액을 저온 보관하기 위해서 용기에 소량으로 분배하여 담는 과정을 통해 4mL~6mL로 분배하여 저장하고, 바람직하게는 5mL로 분배하여 용기에 저장한다. 상기 맥신용액을 7mL이상으로 분배하여 저장하면 급속냉각 시 균일하게 냉각되지 않아 급속냉각의 효율이 감소될 수 있고, 상기 맥신용액을 3mL 이하로 분배하여 저장하면 소량분배로 인해 불필요한 작업량이 늘어나게 되어 업무의 효율이 떨어지게 된다.In order to store the prepared Maxine solution at a low temperature, it is distributed and stored in 4 mL to 6 mL through the process of distributing and storing in a small amount in a container, preferably 5 mL and stored in the container. If the Maxine solution is distributed and stored in more than 7 mL, the efficiency of rapid cooling may be reduced because it is not uniformly cooled during rapid cooling. The efficiency of
한편, 맥신의 저온 보관방법은 맥신용액을 용기에 담고 상기 맥신용액의 전기적 특성이 일정하게 유지되도록 급속 냉각시키는 단계를 포함할 수 있다.On the other hand, the low-temperature storage method of Maxine may include the step of rapidly cooling the Maxine solution so as to maintain constant electrical characteristics of the Maxine solution in a container.
맥신용액의 전기적 특성을 일정하게 유지하기 위해서, 상기 맥신용액을 -80℃ 이하의 온도로 급속 냉각시킬 수 있다.In order to keep the electrical properties of the Maxine solution constant, the Maxine solution may be rapidly cooled to a temperature of -80°C or less.
도 2는 맥신용액의 보관 시 시간의 변화와 보관온도 (5℃, 상온) 및 공기 중 또는 Ar(아르곤) 분위기의 조건에 따른 맥신용액의 농도를 나타낸 그래프이다.2 is a graph showing the concentration of the Maxine solution according to the change of time during storage of the Maxine solution, the storage temperature (5°C, room temperature), and the conditions of the air or Ar (argon) atmosphere.
도 2 를 참조하면, 도 2의 (a) 그래프를 살펴보면, 저온 및 아르곤 분위기에서의 맥신용액의 보관과 상온 및 공기 중의 맥신용액의 보관이 나타난다.Referring to FIG. 2, looking at the graph of FIG. 2 (a), storage of Maxine solution in a low temperature and argon atmosphere and storage of Maxine solution in room temperature and air are shown.
(a) 그래프에 따라 맥신용액은 저온 및 아르곤 분위기에서는 농도가 거의 일정하게 유지되지만 상온 및 공기 중에서 보관 시 맥신용액의 농도가 점차감소됨을 알 수 있다. (a) According to the graph, the concentration of Maxine solution is maintained almost constant in low temperature and argon atmosphere, but it can be seen that the concentration of Maxine solution gradually decreases when stored in room temperature and air.
또한, (b) 그래프를 살펴보면, 저온 및 아르곤 분위기, 상온 및 아르곤 분위기, 저온 및 공기 중, 상온 및 공기 중의 조건으로 맥신용액의 농도변화를 살펴보면, 저장온도 및 아르곤 분위기 모두 맥신용액의 농도변화에 영향을 미치는 것을 알 수 있다.In addition, looking at the graph (b), looking at the change in concentration of Maxine solution under the conditions of low temperature and argon atmosphere, room temperature and argon atmosphere, low temperature and air, room temperature and air, both storage temperature and argon atmosphere are You can see that it has an effect.
(a), (b)의 그래프를 종합했을 때, 맥신용액의 농도를 일정하게 유지하기 위해서는 저온 및 아르곤 분위기가 필요하다.When the graphs (a) and (b) are combined, a low temperature and argon atmosphere are required to keep the concentration of Maxine solution constant.
도 3은 아르곤 분위기 없이 공기 중에서 온도 및 시간의 변화에 따른 면저항값(전기전도도)이 도시된다.3 shows sheet resistance values (electrical conductivity) according to changes in temperature and time in air without an argon atmosphere.
도 3을 살펴보면, 아르곤 분위기없이 온도의 변화만으로 면저항값을 측정한 결과, 맥신용액을 저온(5℃) 및 공기 중에서 22일간 보관했을 때, 가장 큰 변화를 보이고, 저항값이 크게 증가된 것을 알 수 있다. 또한, 냉동기(-18℃) 및 공기 중에 22일간 보관했을 때는 저온(5℃) 및 공기 중에서 보관했을 때와 비교했을 때, 변화값이 비교적 적으며, 냉동기(-80℃ 이하) 및 공기 중에서 28일간 보관했을 때는 면저항값이 거의 일정하게 유지되었다.Referring to FIG. 3, as a result of measuring the sheet resistance value only with a change in temperature without an argon atmosphere, when the Maxine solution was stored for 22 days in low temperature (5°C) and air, it was found that the greatest change was observed and the resistance value was greatly increased. I can. In addition, when stored in a freezer (-18℃) and in air for 22 days, the change value is relatively small compared to when stored in a low temperature (5℃) and in air, and 28 in a freezer (below -80℃) and in air. When stored for a day, the sheet resistance value remained almost constant.
바람직하게는, 상기 맥신용액의 면저항값은 저온 보관을 통해 10Ω/sq 이하로 유지될 수 있다.Preferably, the sheet resistance value of the Maxine solution may be maintained at 10 Ω/sq or less through low temperature storage.
따라서, 맥신용액을 냉동기(-80℃ 이하) 및 공기 중에서 보관하면 상기 맥신용액의 전기적 특성을 일정하게 유지할 수 있다.Therefore, if the Maxine solution is stored in a refrigerator (-80°C or less) and air, the electrical characteristics of the Maxine solution can be maintained constant.
또한, 도 4는 도 3에서 맥신용액을 공기 중에서 온도 및 시간에 따라 보관하였을 때의 변화된 맥신용액의 촬상도이다.In addition, FIG. 4 is an imaging diagram of the changed Maxine solution when the Maxine solution is stored in air according to temperature and time in FIG. 3.
도 4를 참조하면, 맥신용액은 온도가 높고, 시간지날수록 산화되어 농도가 점차 감소되나, 냉동기(-80℃ 이하)에서 보관 시 비교적 변화가 없음을 도 4를 통해 식별가능하다. 따라서, 맥신용액을 냉동기(-80℃ 이하) 및 공기 중에서 보관하면 상기 맥신용액의 전기적 특성을 일정하게 유지할 수 있다.Referring to FIG. 4, it is possible to discern through FIG. 4 that the Maxine solution has a high temperature and is oxidized over time and gradually decreases in concentration, but there is relatively no change when stored in a refrigerator (-80°C or less). Therefore, if the Maxine solution is stored in a refrigerator (-80°C or less) and air, the electrical characteristics of the Maxine solution can be maintained constant.
도 5는 도 3에서 맥신용액 대신 맥신필름으로 대체하여 공기 중에서 온도 및 시간에 따라 보관하였을 때의 변화된 맥신필름의 촬상도이다.5 is a photographic view of the changed Maxine film when stored in air according to temperature and time by replacing the Maxine solution with Maxine film in FIG. 3.
도 5를 참조하면, 맥신필름은 온도가 높고, 시간지날수록 산화되어 색이 변화되나, 냉동기(-80℃ 이하)에서 보관 시 비교적 변화가 없음을 도 4를 통해 식별가능하다. 따라서, 맥신용액을 냉동기(-80℃ 이하) 및 공기 중에서 보관하면 상기 맥신용액의 전기적 특성을 일정하게 유지할 수 있다.Referring to FIG. 5, it is possible to discern through FIG. 4 that the Maxine film has a high temperature and changes in color due to oxidation over time, but there is relatively no change when stored in a refrigerator (-80°C or less). Therefore, if the Maxine solution is stored in a refrigerator (-80°C or less) and air, the electrical characteristics of the Maxine solution can be maintained constant.
도 6은 합성 직후의 맥신 및 1개월간 저온(5℃) 및 공기 중에서 보관된 맥신의 촬상도 및 XRD그래프이다.6 is an imaging diagram and XRD graph of Maxine immediately after synthesis and stored in low temperature (5°C) and air for 1 month.
도 6을 참조하면, 합성 직후의 맥신(왼쪽) 및 1개월간 저온(5℃) 및 공기 중에서 보관된 맥신(오른쪽)을 비교하면, 1개월간 저온(5℃) 및 공기 중에서 보관된 맥신은 합성 직후의 맥신에 비해 색의 변화가 심화되었고, XRD 분석을 통해 Ti의 산화가 진행되어 Ti 3C 2가 TiO 2로 변화된 것을 확인할 수 있다.6, when comparing Maxine immediately after synthesis (left) and Maxine stored in low temperature (5°C) and air for 1 month (right), Maxine stored in low temperature (5°C) and air for 1 month immediately after synthesis the color change compared to Maxine was deepening, the oxidation of Ti progress through XRD analysis, it can be confirmed that the Ti 3 C 2 is changed to TiO 2.
일반적으로, 온도가 낮을수록 공기의 확산계수(diffusion coefficient)와 반응성이 낮아지고, Disordered ICE에서 공기의 투과율이 매우 낮다. 따라서, 맥신용액을 냉동기(-80℃ 이하)에서 급속히 냉각시키면, 냉동기(-18℃)에서 보관할 때와 비교하여 ice의 disorder가 심해지고, 결과적으로 공기가 맥신 내부로 침투하는 투과도가 감소하게 된다. 따라서, 맥신용액을 냉동기(-80℃ 이하) 및 공기 중에서 보관하면 상기 맥신용액의 전기적 특성을 일정하게 유지할 수 있다.In general, the lower the temperature, the lower the diffusion coefficient and reactivity of the air, and the air transmittance is very low in the Disordered ICE. Therefore, if Maxine solution is rapidly cooled in a freezer (-80℃ or less), the disorder of ice becomes more severe compared to when stored in a freezer (-18℃), and as a result, the permeability of air penetration into Maxine decreases. . Therefore, if the Maxine solution is stored in a refrigerator (-80°C or less) and air, the electrical characteristics of the Maxine solution can be maintained constant.
또한, 상기 맥신의 저온 보관방법을 통해 보관된 맥신용액을 통해 전극재료로 맥신소자가 구성될 수 있다.In addition, the Maxine device may be configured as an electrode material through the Maxine solution stored through the low-temperature storage method of Maxine.
한편, 본 발명에 따른 맥신용액은 냉동기의 온도를 -18℃ 내지 -80℃로 유지하고 급속냉각을 통해 적정 수준의 전기적 특성을 유지할 수 있다.On the other hand, the Maxine solution according to the present invention can maintain the temperature of the refrigerator at -18°C to -80°C and maintain an appropriate level of electrical characteristics through rapid cooling.
보다 상세하게는, 상기 맥신용액은 냉동기(-80℃ 이하)에서 전기적 특성을 거의 일정하게 유지할 수 있지만 -80℃ 이하의 온도로 유지하는데 많은 비용과 추가적인 장비들이 필요하므로 냉동기의 온도를 -18℃ 내지 -80℃로 유지하여 적정 수준의 전기적 특성을 유지한다. 상기 적정 수준의 전기적 특성은 10Ω/sq 이상에서 100000Ω/sq 이하로 유지되도록 하는 것이다.More specifically, the Maxine solution can maintain almost constant electrical characteristics in a freezer (below -80°C), but it requires a lot of cost and additional equipment to maintain the temperature below -80°C. To -80 ℃ to maintain an appropriate level of electrical properties. The appropriate level of electrical characteristics is to be maintained at 10 Ω/sq or more to 100000 Ω/sq or less.
따라서, 제조 상황에 따라서 맥신용액을 냉동기에 보관 시 -80℃ 이하 또는 -18℃ 내지 -80℃로 선택적으로 보관하여 적정 수준의 전기적 특성을 유지할 수 있고, 보관을 위한 비용을 절감할 수 있다.Therefore, depending on the manufacturing situation, when the Maxine solution is stored in a refrigerator, it is selectively stored at -80°C or lower or -18°C to -80°C to maintain an appropriate level of electrical characteristics, and cost for storage may be reduced.
한편, 맥신용액을 저온에서 보관할 때, 불활성가스, 질소가스, 공기 중 어느 한가지 또는 혼합된 가스와 함께 보관될 수 있다.Meanwhile, when the Maxine solution is stored at a low temperature, it may be stored with any one of inert gas, nitrogen gas, and air, or a mixed gas.
보다 상세하게는, 맥신용액을 He, Ne, Ar, Kr, Xe, Rn 등 불활성 가스나, 질소가스 또는 공기 중 어느 한가지의 가스에서 보관될 수 있고, 상기 가스가 혼합된 혼합가스 또는 혼합가스와 공기가 혼합된 상태에서 보관되는 것도 가능하다.More specifically, the Maxine solution may be stored in an inert gas such as He, Ne, Ar, Kr, Xe, Rn, or any one of nitrogen gas or air, and the gas is mixed with a mixed gas or mixed gas. It is also possible to store in a mixture of air.
따라서, 불활성가스 또는 질소가스에 의해서 산소와의 접촉을 차단시킬 수 있고, 상기 맥신용액이 산소와 결합되어 전기적 특성이 변화되는 것을 방지할 수 있다.Accordingly, contact with oxygen may be blocked by an inert gas or nitrogen gas, and electrical characteristics may be prevented from being changed due to the combination of the Maxine solution with oxygen.
또한, 상기 맥신용액을 저온으로 유지시키기 위한 냉동기는 헬륨 또는 액체질소를 냉매로 사용하여 구동될 수 있다.In addition, the refrigerator for maintaining the Maxine solution at a low temperature may be driven using helium or liquid nitrogen as a refrigerant.
또한, 상기 맥신의 저온 보관방법을 통해 보관된 맥신용액이 스핀코팅(Spin coating), 드롭캐스트(Drop cast), 감압여과(Vacuum filtration) 방식을 통해 필름형태로 제조된 맥신필름일 수 있다.In addition, the Maxine solution stored through the low-temperature storage method of Maxine may be a Maxine film manufactured in the form of a film through spin coating, drop cast, and vacuum filtration.
따라서, 상기와 같은 스핀코팅, 드롭캐스트 및 감압여과 방식과 같이 다양한 방법을 통해 맥신필름을 제조함으로써, 제조여건이나 조건에 따라 효과적으로 맥신필름을 생산할 수 있다.Therefore, by manufacturing a Maxine film through various methods such as spin coating, drop-casting and vacuum filtration as described above, it is possible to effectively produce a Maxine film according to manufacturing conditions or conditions.
전술한 본 발명의 설명은 예시를 위한 것이며, 본 발명이 속하는 기술분야의 통상의 지식을 가진 자는 본 발명의 기술적 사상이나 필수적인 특징을 변경하지 않고서 다른 구체적인 형태로 쉽게 변형이 가능하다는 것을 이해할 수 있을 것이다. 그러므로 이상에서 기술한 실시예들은 모든 면에서 예시적인 것이며 한정적이 아닌 것으로 이해해야만 한다. 예를 들어, 단일형으로 설명되어 있는 각 구성 요소는 분산되어 실시될 수도 있으며, 마찬가지로 분산된 것으로 설명되어 있는 구성 요소들도 결합된 형태로 실시될 수 있다.The above description of the present invention is for illustrative purposes only, and those of ordinary skill in the art to which the present invention pertains will be able to understand that it can be easily modified into other specific forms without changing the technical spirit or essential features of the present invention. will be. Therefore, it should be understood that the embodiments described above are illustrative in all respects and not limiting. For example, each component described as a single type may be implemented in a distributed manner, and similarly, components described as being distributed may also be implemented in a combined form.
본 발명의 범위는 후술하는 특허청구범위에 의하여 나타내어지며, 특허청구범위의 의미 및 범위 그리고 그 균등 개념으로부터 도출되는 모든 변경 또는 변형된 형태가 본 발명의 범위에 포함되는 것으로 해석되어야 한다.The scope of the present invention is indicated by the claims to be described later, and all changes or modified forms derived from the meaning and scope of the claims and their equivalent concepts should be interpreted as being included in the scope of the present invention.

Claims (13)

  1. (a)이차원구조의 전이금속 탄화물 및 전이금속 탄질화물로 구성된 맥신용액을 준비하는 단계;(a) preparing a Maxine solution consisting of a two-dimensional transition metal carbide and a transition metal carbonitride;
    (b)상기 준비된 맥신용액을 용기에 담는 단계;(b) putting the prepared Maxine solution in a container;
    (c)상기 용기에 담긴 맥신용액을 전기적 특성이 일정하게 유지되도록 급속 냉각시키는 단계;(c) rapidly cooling the Maxine solution contained in the container so that the electrical properties are kept constant;
    를 포함하며,Including,
    상기 (c) 단계에서 급속냉각 온도는 -80℃ 이하로 설정된 것을 특징으로 하는 맥신의 저온 보관방법.In the step (c), the rapid cooling temperature is set to -80°C or less.
  2. 제 1 항에 있어서, 상기 맥신용액은 Ti 2C, Ti 3C 2, V 2C, Nb 2C, (Ti 0.5, Nb 0.5) 2CT x, Ti 3CN, (V 0.5, Cr 0.5) 3C 2, Ta 4C 3 및 Nb 4C 3 중 어느 하나로 구성된 것을 특징으로 하는 맥신의 저온 보관방법.The method of claim 1, wherein the Maxine solution is Ti 2 C, Ti 3 C 2 , V 2 C, Nb 2 C, (Ti 0.5 , Nb 0.5 ) 2 CT x , Ti 3 CN, (V 0.5 , Cr 0.5 ) 3 C 2 , Ta 4 C 3 and Nb 4 C 3 How to store Maxine at low temperatures.
  3. 제 2 항에 있어서, 상기 (b) 단계에서 상기 맥신용액은 급속냉각 시 냉각효율을 향상시키도록 5mL 이하로 소량씩 분배되어 저장된 것을 특징으로 하는 맥신의 저온 보관방법.The method of claim 2, wherein in step (b), the Maxine solution is distributed and stored in a small amount of 5 mL or less to improve cooling efficiency during rapid cooling.
  4. 제 3 항에 있어서, 상기 맥신용액은 M n+ 1X n의 화학식으로 이루진 것을 특징으로 하는 맥신의 저온 보관방법.The method of claim 3, wherein the Maxine solution is made of the formula of M n + 1 X n .
  5. 제 4 항에 있어서, 상기 M n+ 1X n의 화학식에서 M은 앞전이금속인 것을 특징으로 하는 맥신의 저온 보관방법.The method of claim 4, wherein M in the formula of M n + 1 X n is a front transition metal.
  6. 제 5 항에 있어서, 상기 M n+ 1X n의 화학식에서 X는 탄소 및 질소 중에서 적어도 하나를 포함하는 것을 특징으로 하는 맥신의 저온 보관방법.The method of claim 5, wherein X in the formula of M n + 1 X n includes at least one of carbon and nitrogen.
  7. 제 6 항에 있어서, 상기 맥신용액의 급속냉각은 냉동기를 통해서 이루어지고 헬륨 또는 액체질소를 냉매로 사용하여 저온이 유지되는 것을 특징으로 하는 맥신의 저온 보관방법.The method of claim 6, wherein the rapid cooling of the Maxine solution is performed through a freezer and the low temperature is maintained by using helium or liquid nitrogen as a refrigerant.
  8. 제 7 항에 있어서, 상기 (c) 단계에서 맥신용액을 불활성가스, 질소가스, 공기 중 어느 한가지 또는 혼합된 가스와 함께 보관되는 것을 특징으로 하는 맥신의 저온 보관방법.[8] The method of claim 7, wherein in the step (c), the Maxine solution is stored together with one of inert gas, nitrogen gas, and air, or a mixed gas.
  9. 제 1 항에 있어서, 상기 맥신용액의 면저항값은 저온 보관을 통해 10Ω/sq 이하로 유지되는 것을 특징으로 하는 맥신의 저온 보관방법.The method of claim 1, wherein the sheet resistance value of the Maxine solution is maintained at 10 Ω/sq or less through low temperature storage.
  10. (a)이차원구조의 전이금속 탄화물 및 전이금속 탄질화물로 구성된 맥신용액을 준비하는 단계;(a) preparing a Maxine solution consisting of a two-dimensional transition metal carbide and a transition metal carbonitride;
    (b)상기 준비된 맥신용액을 용기에 담는 단계;(b) putting the prepared Maxine solution in a container;
    (c)상기 용기에 담긴 맥신용액을 전기적 특성이 일정하게 유지되도록 급속 냉각시키는 단계;(c) rapidly cooling the Maxine solution contained in the container so that the electrical properties are kept constant;
    를 포함하며,Including,
    상기 (c) 단계에서 급속냉각 온도는 -18℃ 내지 -80℃ 로 설정된 것을 특징으로 하는 맥신의 저온 보관방법.In the step (c), the rapid cooling temperature is set to -18°C to -80°C.
  11. 제 10 항에 있어서, 상기 맥신용액의 면저항값은 저온 보관을 통해 10Ω/sq 이상에서 100000Ω/sq 이하로 유지되는 것을 특징으로 하는 맥신의 저온 보관방법.11. The method of claim 10, wherein the sheet resistance value of the Maxine solution is maintained from 10 Ω/sq to 100000 Ω/sq or less through low temperature storage.
  12. 제 1항에 따른, 상기 맥신의 저온 보관방법을 통해 보관된 맥신용액을 통해 전극재료로 구성된 것을 특징으로 하는 맥신소자.The Maxine device according to claim 1, wherein the electrode material is made of a Maxine solution stored through the method of storing Maxine at a low temperature.
  13. 제 1항에 따른, 상기 맥신의 저온 보관방법을 통해 보관된 맥신용액이 스핀코팅, 드롭캐스트, 감압여과 방식을 통해 필름형태로 제조된 것을 특징으로 하는 맥신필름.The Maxine film according to claim 1, wherein the Maxine solution stored through the low-temperature storage method of Maxine is manufactured in the form of a film through spin coating, drop cast, and vacuum filtration.
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