KR20170043350A - Preparing method of 2-dimensional nanosheet by exfoliation of materials with layered structure using shear force and liquefied high impact - Google Patents
Preparing method of 2-dimensional nanosheet by exfoliation of materials with layered structure using shear force and liquefied high impact Download PDFInfo
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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- 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
- C01B21/064—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 with boron
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Abstract
본 발명은 층상 구조 물질의 박리 방법에 관한 것으로, 구체적으로는 층상 구조를 갖는 물질에 평행하나 반대 방향으로 작용하는 힘(전단응력)을 인가하여 보다 단순화된 공정으로 얇은 두께 및 대면적을 가지는 고품질의 2차원 나노시트의 제조방법에 관한 것이다.More particularly, the present invention relates to a method of peeling a layered structure material by applying a force (shear stress) acting parallel to but opposite to a material having a layered structure, Dimensional nano-sheet of the present invention.
Description
본 발명은 층상 구조 물질의 박리 방법에 관한 것으로, 구체적으로는 유체충돌 방식을 이용하여 층상 구조를 갖는 물질에 평행하나 반대 방향으로 작용하는 힘(전단응력)을 인가하여 보다 단순화된 공정으로 얇은 두께 및 대면적을 가지는 고품질의 2차원 나노시트의 제조방법에 관한 것이다.More particularly, the present invention relates to a method of peeling a layered structure material by applying a force (shear stress) acting parallel to but opposite to a layered structure using a fluid collision method, And a method for producing a high-quality two-dimensional nanosheet having a large area.
최근 그라파이트(graphite), 보론 나이트라이드(BN), 이황화몰리브덴(MoS2), 포스포린(Phosphorene) 등 층상 구조를 가지고 있는 물질이 단층 또는 수층의 원자층을 갖는 2차원 나노시트일 때의 특성을 평가한 결과, 벌크 상태의 물질보다 우수한 특성을 나타낼 수 있음이 보고된 바 있다. 이러한 우수한 특성으로 인해, 2차원 나노 물질을 보다 효과적으로 양산할 수 있는 다양한 방법이 제안 또는 연구되어 왔다. 특히, 특성을 극대화하기 위하여 결함의 발생이 적으면서, 보다 얇은 두께 및 대면적을 갖도록 하는 단순화된 공정에 대한 방법에 관한 연구가 다양하게 이루어져 왔다.In recent years, the properties of layered structures such as graphite, boron nitride (BN), molybdenum disulfide (MoS 2 ), and phosphorane have been observed as a two-dimensional nanosheet having a single layer or an aqueous layer As a result of the evaluation, it has been reported that it can exhibit properties superior to those of the bulk state material. Due to these excellent properties, various methods have been proposed or studied to more efficiently produce two-dimensional nanomaterials. Particularly, there have been various studies on a method for a simplified process which has a thinner thickness and a larger area while generating less defects in order to maximize the characteristics.
먼저, 테이프를 사용하는 등의 물리적인 방법으로 그라파이트를 그래핀 나노시트로 박리하는 방법이 알려져 있지만, 이러한 방법은 대량 양산에 부적합하다.Firstly, a method of peeling a graphite into a graphene nanosheet by a physical method such as using a tape is known, but such a method is not suitable for mass production.
또한, 산, 염기 용액을 이용하여 화학적으로 2차원 나노시트 또는 산화물을 얻는 방법이 알려져 있다. 그러나 이러한 방법으로 얻어진 산화물을 다시 환원하여 나노시트를 얻는 과정에서 다수의 결함이 발생할 수 있다. 이는 최종 제조 물질의 특성에 큰 악영향을 미칠 수 있으며, 전체적인 공정이 복잡해진다.Also, a method of chemically obtaining two-dimensional nanosheets or oxides using an acid or a base solution is known. However, a number of defects may occur in the process of obtaining the nanosheet by reducing the oxide obtained by this method again. This can adversely affect the properties of the final product material and complicate the overall process.
최근에는 층상 구조 물질을 액상에 분산시킨 상태에서 초음파 조사 또는 볼밀링 등의 방법으로 층을 박리하여 다층의 나노시트를 제조하는 방법이 알려져 있다. 그러나 이러한 방법 역시 충분히 얇은 두께를 갖는 2차원 나노시트를 얻기 어렵고, 결함이 발생하는 등의 문제점이 있다.In recent years, there has been known a method for producing a multilayered nanosheet by separating a layer by a method such as ultrasonic irradiation or ball milling while dispersing a layered structure material in a liquid phase. However, this method also has a problem that it is difficult to obtain a two-dimensional nanosheet having a sufficiently thin thickness and defects occur.
이로 인해, 층상 구조를 갖는 물질을 보다 얇은 두께 및 대면적을 가지며, 결함이 적은 2차원 나노시트로 단순화된 공정을 통해 박리시킬 수 있는 공정 방법이 계속적으로 요구되고 있다. Accordingly, there is a continuing need for a process that can peel a material having a layered structure through a simplified process with a thinner and larger-sized two-dimensional nanosheet having few defects.
한편, 층상 구조 물질인 그라파이트를 박리하는 방법에 대해서는 대한민국등록특허 제10-1078734호에 개시된 바 있으나, 상기 대한민국등록특허 제10-1078734호는 고온고압을 이용하는 공정 상의 조건이 전제될 뿐만 아니라, 해압을 통한 충돌에 의한 박리만을 개시하고 있어, 단순화된 공정으로 전단응력 및 충돌에 의한 1, 2차 박리를 통해 보다 얇은 두께의 2차원 나노시트를 제조하는 것을 목적으로 하는 본 발명과는 차이가 있다.On the other hand, the method of peeling graphite as a layered structure material is disclosed in Korean Patent No. 10-1078734, but the above Korean Patent No. 10-1078734 is not only premised on a process condition using high temperature and high pressure, Dimensional nanosheet with a thinner thickness through first and second peeling due to shear stress and collision in a simplified process, which is different from the present invention .
본 발명은 상기 문제점을 해결하기 위하여, 층상 구조 물질을 단순화된 공정을 통해 보다 얇은 두께 및 대면적을 가지며, 결함 발생이 감소된 2차원 나노시트로 박리할 수 있는 방법을 제공하고자 한다.In order to solve the above problems, the present invention provides a method for peeling a layered structure material into a two-dimensional nanosheet having a thinner thickness and a larger area through a simplified process and having reduced defect occurrence.
본 발명은 층상 구조를 갖는 물질을 용매에 분산시켜 분산액을 형성하는 단계; 상기 분산액을 직경이 200 ㎛ 이하인 마이크로 노즐이 장착된 유체 충돌 방식 나노 미립화 장치에 투입하는 단계; 상기 투입된 분산액에 전단응력을 인가하고 상기 마이크로 노즐에 통과시켜 1차 박리하는 단계; 및 상기 1차 박리된 분산액 내 물질들을 고속으로 충돌시켜 2차 박리하는 단계를 포함하고 단층 또는 수층의 나노 스케일 두께를 갖는, 2차원 나노시트의 제조방법을 제공한다.The present invention relates to a method for manufacturing a semiconductor device, comprising: dispersing a material having a layered structure in a solvent to form a dispersion; Introducing the dispersion into a fluid-impingement nano-atomizer equipped with a micro-nozzle having a diameter of 200 μm or less; Applying a shear stress to the charged dispersion and passing the dispersion through the micro-nozzle to peel off first; And a second peeling step in which the materials in the primary peeled dispersion are collided at a high speed, and having a nanoscale thickness of a single layer or an aqueous layer.
본 발명에 따르면, 분산용매의 사용 및 유체 충돌 방식을 이용하여 적층 물질을 보다 균일하게 분산시킨 상태에서 이의 박리 방법을 최적화하여 2차원 나노시트를 제조할 수 있다.According to the present invention, a two-dimensional nanosheet can be manufactured by optimizing the peeling method in a state where the laminated material is more uniformly dispersed by using the dispersion solvent and the fluid collision method.
따라서, 본 발명에 따르면, 종래에 적용되었던 박리 공정의 전처리 공정 또는 후처리 공정을 생략할 수 있으며, 이는 공정 중에 발생할 수 있는 결함을 최소화 할 수 있다. 또한, 본 발명에 따르면 보다 얇은 두께 및 대면적을 갖는 2차원 나노시트를 높은 수율로 용이하게 제조될 수 있다.Therefore, according to the present invention, it is possible to omit the pre-treatment process or the post-treatment process of the conventional peeling process, which can minimize defects that may occur during the process. Further, according to the present invention, a two-dimensional nanosheet having a thinner thickness and a larger area can be easily produced at a high yield.
도 1은 본 발명에 따른 전단응력을 이용한 보론 나이트라이드(BN) 나노시트를 제조하는 방법을 나타낸 개략도이다
도 2는 도 1의 전단응력을 이용하여 보론 나이트라이드(BN) 분말이 나노시트로 박리되는 과정을 나타낸 세부 개략도이다
도 3은 실시예에 사용된 보론 나이트라이드(BN) 분말을 주사전자현미경(Scanning Electron Microscopy; SEM)으로 관찰한 이미지이다.
도 4는 도 1에 도시된 나노시트 제조방법을 이용하여 박리한 BN 나노시트를 투과전자현미경(Transmission Electron Microscopy; TEM)으로 관찰한 이미지이다.
도 5는 도 1에 도시된 나노시트 제조방법을 이용하여 박리한 보론 나이트라이드(BN) 나노시트를 고분해능 투과전자현미경(High-Resolution Transmission Electron Microscopy; HRTEM)으로 관찰한 이미지이다.FIG. 1 is a schematic view showing a method of manufacturing a boron nitride (BN) nanosheet using shear stress according to the present invention
FIG. 2 is a detailed schematic view showing a process in which a boron nitride (BN) powder is peeled off into a nanosheet using the shear stress of FIG. 1
3 is an image obtained by observing the boron nitride (BN) powder used in the examples by Scanning Electron Microscopy (SEM).
FIG. 4 is an image of a BN nanosheet peeled off using the nanosheet manufacturing method shown in FIG. 1 by transmission electron microscopy (TEM).
FIG. 5 is an image of a boron nitride (BN) nanosheet peeled off using the nanosheet manufacturing method shown in FIG. 1 by a high-resolution transmission electron microscopy (HRTEM).
이하에서는, 본 발명을 바람직한 실시예를 참조하여 더욱 구체적으로 설명한다. 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자가 용이하게 실시할 수 있도록 본 발명에 대해 상세히 설명한다.Hereinafter, the present invention will be described more specifically with reference to preferred embodiments. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.
본 발명은 층상 구조를 갖는 물질을 용매에 분산시켜 분산액을 형성하는 단계; 상기 분산액을 직경이 200 ㎛ 이하인 마이크로 노즐이 장착된 유체 충돌 방식 나노 미립화 장치에 투입하는 단계; 상기 투입된 분산액에 전단응력을 인가하고 상기 마이크로 노즐에 통과시켜 1차 박리하는 단계; 및 상기 1차 박리된 분산액 내 물질들을 고속으로 충돌시켜 2차 박리하는 단계를 포함하고 단층 또는 수층의 나노 스케일 두께를 갖는, 2차원 나노시트의 제조방법을 제공한다. The present invention relates to a method for manufacturing a semiconductor device, comprising: dispersing a material having a layered structure in a solvent to form a dispersion; Introducing the dispersion into a fluid-impingement nano-atomizer equipped with a micro-nozzle having a diameter of 200 μm or less; Applying a shear stress to the charged dispersion and passing the dispersion through the micro-nozzle to peel off first; And a second peeling step in which the materials in the primary peeled dispersion are collided at a high speed, and having a nanoscale thickness of a single layer or an aqueous layer.
본원의 일 구현예에 있어서, 상기 층상 구조를 갖는 물질은 그라파이트(graphite), 보론 나이트라이드(BN), MoS2, MoSe2 , WS2, WSe2 , NbS2, NbSe2, ZrS2, 포스포린(Phosphorene) 및 이들의 조합들로 이루어진 군에서 선택되는 1종 이상인 것을 특징으로 하나, 이에 제한되는 것은 아니다. 상기 물질들은 2차원 판상구조를 갖는 적층형 물질들로, 박리되어 단층 또는 수층의 나노 스케일 두께를 갖는 물질이면 제한없이 사용 가능하다.In one embodiment of the present application, the material having the layered structure is selected from the group consisting of graphite, boron nitride (BN), MoS 2 , MoSe 2 , WS 2 , WSe 2 , NbS 2 , NbSe 2 , ZrS 2 , (Phosphorene), and combinations thereof. However, the present invention is not limited thereto. These materials are stacked materials having a two-dimensional plate-like structure and can be used without limitation as long as they are peeled and have a single layer or a nanoscale thickness of an aqueous layer.
본원의 일 구현예에 있어서, 상기 용매는 물과 같은 수용매 또는 메탄올, 에탄올, 아세톤, 부탄올, 이소프로필알코올, N,N-디메틸포름아미드(N,N-dimethylformamide), 에틸렌글리콜, 디메틸아세트아미드, 포름산 에틸아세테이트, 아크릴로니트릴로 및 이들의 조합들로 이루어진 군에서 선택되는 1종 이상의 극성 유기용매인 것을 특징으로 하나, 이에 제한되는 것은 아니다. -OH, -COOH, -O-, -CN, -F 등의 극성 작용기를 가지고 있는 극성 유기용매에 층상 구조를 갖는 물질을 용해 또는 분산시켜 분산액을 제조할 수 있다.In one embodiment herein, the solvent is an aqueous solvent such as water or a solvent such as methanol, ethanol, acetone, butanol, isopropyl alcohol, N, N-dimethylformamide, ethylene glycol, dimethylacetamide , Formic acid ethyl acetate, acrylonitrile, and combinations thereof. However, the present invention is not limited thereto. A dispersion liquid can be prepared by dissolving or dispersing a material having a layered structure in a polar organic solvent having a polar functional group such as -OH, -COOH, -O-, -CN, -F.
본원의 일 구현예에 있어서, 상기 분산액이 마이크로 노즐을 통과하는 1차 박리 단계와 마이크로 노즐을 통과한 분산액 내 물질들이 충돌하는 2차 박리 단계가 연속적으로 이루어지는 것을 특징으로 한다. 상기 수용매 또는 유기용매에 층상 구조 물질을 혼합하여 제조한 분산액을 직경이 200 ㎛ 이하인 마이크로 노즐이 장착된 유체 충돌 방식 나노 미립화 장치로 통과시키면, 장치로부터 전단응력이 인가되어 다층 구조의 층상 물질이 단층 또는 수층을 갖는 나노시트로 1차 박리되고, 이어서 상기 1차 박리된 나노시트가 상기 마이크로 노즐을 포함하고 있는 챔버 내로 분사되어 낙하 및 이동되면서 입자간 고속 충돌이 발생하게 되는데, 이때 전단응력에 의해 추가로 2차 박리가 발생하게 된다. 이를 통해, 1차 박리로부터 수득된 나노시트보다 얇은 두께의 단층 또는 수층을 갖는 나노시트를 수득할 수 있다. In one embodiment of the present invention, the first separation step in which the dispersion passes through the micronozzles and the second separation step in which the materials in the dispersion liquid passing through the micronozzles collide are continuously performed. When a dispersion prepared by mixing a layered structure material in the water solvent or an organic solvent is passed through a fluid collision-type nano-atomizer equipped with a micro-nozzle having a diameter of 200 μm or less, shear stress is applied from the device, The nanosheets having a single layer or water layer are firstly peeled off, and then the primary peeled nanosheets are injected into the chamber containing the micro-nozzles to be dropped and moved so that high-speed collision between particles occurs. At this time, The second peeling occurs further. As a result, it is possible to obtain a nanosheet having a single layer or a water layer thinner than the nanosheet obtained from the first separation.
본원의 일 구현예에 있어서, 상기 용매의 종류 및 농도와 상기 분산액의 노즐 통과 및 충돌 횟수를 조절하여 단층 또는 수층의 나노 스케일 두께를 조절하는 것을 특징으로 한다. 상기 용매의 농도는 전체 용액의 중량을 기준으로 0.1중량% 내지 10중량%이며, 상기 분산액의 노즐 통과 및 충돌 횟수는 1차 및 2차 박리를 통칭하는 것을 1회(pass)로 하여 5회(pass) 내지 100회(pass)인 것을 특징으로 하나, 이에 제한되는 것은 아니다. 상기 용매의 농도는 예를 들어, 0.1% 내지 10%, 2% 내지 10%, 4% 내지 10%, 6% 내지 10%, 8% 내지 10%, 0.1% 내지 9%, 0.1% 내지 7%, 0.1% 내지 5%, 또는 0.1% 내지 3%일 수 있으나, 이에 제한되는 것은 아니다. 단, 노즐 통과 및 충돌 횟수가 5회(pass) 미만일 경우 층상 물질의 박리가 제대로 이뤄지지 않아 2차원 나노시트 제조가 어려울 수 있고, 60회(pass)를 초과할 경우 노즐 통과 및 충돌 시 발생하는 마찰력 및 열로 인해 생성된 2차원 나노시트에 결함이 발생할 수 있다.In one embodiment of the present invention, the nanoscale thickness of the single layer or the water layer is controlled by adjusting the type and concentration of the solvent and the number of times of passage and collision of the dispersion with the nozzle. The concentration of the solvent is 0.1% by weight to 10% by weight based on the weight of the total solution. The number of passes and the number of collisions of the dispersion is 5 times (pass) pass to 100 pass, but the present invention is not limited thereto. The concentration of the solvent may be, for example, from 0.1% to 10%, from 2% to 10%, from 4% to 10%, from 6% to 10% , 0.1% to 5%, or 0.1% to 3%, but is not limited thereto. However, when the number of passes and collisions of the nozzle is less than 5 passes, it is difficult to manufacture the two-dimensional nanosheet because the layered material does not peel off properly, and when the pass is more than 60 passes, And a defect may occur in the two-dimensional nanosheet generated by heat.
본원의 일 구현예에 있어서, 상기 용매 내에 산을 첨가하여 표면에 관능기를 부여할 수 있다. 상기 첨가되는 산은 염산, 황산, 질산, 브롬산, 요오드화수소산, 아세트산, 글리옥실산, 톨루엔산, 4-니트로벤조산, 말산, 말론산, 옥살산, 숙신산, 아스파트산, 크로토닉산, 카프릭산, 트리플루오로아세트산, 부티르산, 타타르산, 프탈산, 벤조산, 시트르산, 살리실산, 만델산, 및 이들의 조합들로 이루어진 군에서 선택되는 1종 이상인 것을 특징으로 하나, 이에 제한되는 것은 아니다.In one embodiment of the invention, an acid may be added to the solvent to impart functional groups to the surface. The acid added may be selected from the group consisting of hydrochloric acid, sulfuric acid, nitric acid, hydrobromic acid, hydroiodic acid, acetic acid, glyoxylic acid, toluenic acid, 4-nitrobenzoic acid, malic acid, malonic acid, oxalic acid, succinic acid, But are not limited to, at least one selected from the group consisting of hydrochloric acid, trifluoroacetic acid, butyric acid, tartaric acid, phthalic acid, benzoic acid, citric acid, salicylic acid, mandelic acid, and combinations thereof.
본원의 일 구현예에 있어서, 상기 나노시트 표면에 산 처리 등을 통해 카르복실기, 하이드록실기, 아미드기, 글리시딜기, 이소시아네이트기, 에폭사이드기, 고리형 에테르기, 설파이드기, 아세탈기, 락톤기 및 이들의 조합들로 이루어진 군에서 선택되는 1종 이상의 관능기를 도입할 수 있는 것을 특징으로 하나, 이에 제한되는 것은 아니다.In one embodiment of the present invention, the surface of the nanosheet is treated with an acid such as a carboxyl group, a hydroxyl group, an amide group, a glycidyl group, an isocyanate group, an epoxide group, a cyclic ether group, a sulfide group, Toners, and combinations thereof. However, the present invention is not limited thereto.
상술한 2차원 나노시트의 제조방법은 수회(pass)의 노즐 통과 및 충돌로 박리를 진행한 후에 상기 박리된 나노시트를 포함하고 있는 분산액으로부터 나노시트를 회수 및 건조하는 단계를 포함할 수 있다. 이때, 상기 2차원 나노시트의 회수는 원심 분리, 감압 여과 또는 가압 여과로 진행될 수 있고, 상기 건조는 약 30℃ 내지 약 100℃의 온도 하에서 진공 건조로 진행될 수 있다.The above-described method of manufacturing a two-dimensional nanosheet may include a step of passing through a nozzle of a pass and a step of removing the nanosheet from the dispersion containing the peeled nanosheet after the separation by the impact. At this time, the recovery of the two-dimensional nanosheets can be carried out by centrifugation, vacuum filtration or pressure filtration, and the drying can be performed by vacuum drying at a temperature of about 30 ° C to about 100 ° C.
이하, 본 발명을 구체적으로 설명하기 위해 실시예를 들어 상세하게 설명하기로 한다. 그러나 본 발명에 따른 실시예들은 여러 가지 다른 형태로 변형될 수 있으며, 본 발명의 범위가 아래에서 상술하는 실시예들에 한정되는 것으로 해석되어서는 안 된다. 본 발명의 실시예들은 당업계에서 평균적인 지식을 가진 자에게 본 발명을 보다 완전하게 설명하기 위해서 제공되는 것이다.BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in detail with reference to examples. However, the embodiments according to the present invention can be modified into various other forms, and the scope of the present invention should not be construed as being limited to the embodiments described below. Embodiments of the present invention are provided to more fully describe the present invention to those skilled in the art.
실시예Example
육방정 보론 나이트라이드(hexagonal boron nitride; h-BN) 분말(용매 중량 대비 1중량%)을 수용매인 물 100부피% 또는 물 50부피%와 극성 유기용매인 에탄올 50부피%의 혼합 용매에 분산시켜 분산액을 제조하였다. 상기 제조된 분산액을 200 ㎛ 직경의 마이크로 노즐이 장착된 유체 충돌 방식 나노 미립화 장치(Aqueous counter collision system, ㈜ CNNT Co.)에 투입하여, 마이크로 노즐을 통과시키는 1차 박리를 진행하였고, 이어서 1차 박리된 나노시트를 챔버내로 이동시켜 2차 박리를 진행하였다. 1차 및 2차 박리를 통칭하여 1회(pass)로 하였으며, 총 5 회(pass) 내지 60회(pass) (5, 10, 15, 20, 30, 40, 50, 60회(pass))의 박리를 진행하였고, 압력은 170 MPa로 하였다. 실시예의 자세한 조건은 하기 표 1에 상세히 나타내었다.(1 wt% based on the weight of the solvent) of hexagonal boron nitride (h-BN) powder was dispersed in a mixed solvent of 100 vol% of water or 50 vol% of water and 50 vol% of ethanol as a polar organic solvent To prepare a dispersion. The dispersion thus prepared was put into a fluid counter collision system (CNNT Co.) equipped with a micro-nozzle having a diameter of 200 mu m to carry out a first peeling through a micro-nozzle, The peeled nanosheets were moved into the chamber to carry out the second peeling. (5, 10, 15, 20, 30, 40, 50, 60 pass) in total from 5 pass to 60 pass And the pressure was set to 170 MPa. Detailed conditions of the examples are shown in Table 1 below.
상기 실시예의 h-BN 분말 입자가 2차원 나노시트로 박리되는 과정은 도 1 및 도 2의 개략도를 통해 용이하게 이해 가능하다. 도 1 및 도 2에 나타낸 바와 같이, 유체 충돌 방식 나노 미립화 장치의 분산액 공급부 말단에 마이크로 노즐이 장착되어 있고, 상기 마이크로 노즐은 분산액 공급부 일부를 포함하여, 박리 물질이 분사되는 챔버 내에 삽입되어 있다. 1차 박리를 위해 h-BN 분말 입자를 포함하는 분산액이 장치에 투입되고, 장치 공급부 말단으로부터 마이크로 노즐로 상기 분산액이 이동될 시에 전단응력을 인가받게 되는데, 이때 1차 박리가 이뤄지게 된다. 전단응력은 서로 나란하되 반대 방향으로 작용하는 힘으로, 도 2에 나타낸 바와 같이 3차원 구조의 h-BN 분말 입자가 마이크로 노즐을 통과할 시에 공급부와 마이크로 노즐 연결부의 직경 차이로 인해 장치로부터 전단응력을 인가받아 3차원 블록 형태의 h-BN 분말 입자가 2차원 판상구조를 갖는 나노시트로 박리된다.The process of peeling the h-BN powder particles of the above embodiment into two-dimensional nanosheets can be easily understood through the schematic diagrams of FIGS. 1 and 2. FIG. As shown in Figs. 1 and 2, a micro-nozzle is mounted at the end of the dispersion supply part of the fluid-impingement nano-atomization apparatus, and the micro-nozzle is inserted into the chamber including the part of the dispersion liquid supply part. The dispersion containing the h-BN powder particles is put into the apparatus for the first peeling, and the shear stress is applied when the dispersion liquid is moved from the end of the apparatus feeding section to the micronozzles. At this time, the first peeling is performed. As shown in Fig. 2, when the h-BN powder particles of the three-dimensional structure pass through the micro-nozzle, the shear stress acts in a direction parallel to each other but acts in the opposite direction. The h-BN powder particles in the form of a three-dimensional block are exfoliated into nanosheets having a two-dimensional plate-like structure by receiving a stress.
도 3은 상기 h-BN 분말 입자를 주사전자현미경으로 관찰한 이미지이다. 5 ㎛ 스케일바로 관찰하였으며, 박리 전 h-BN 분말 입자의 두께가 수백 나노미터의 크기에 달하는 것을 확인할 수 있었다.3 is an image of the h-BN powder particles observed by a scanning electron microscope. 5 μm scale, and it was confirmed that the thickness of the h-BN powder before peeling reached a size of several hundred nanometers.
도 4는 상술한 전단응력을 이용한 나노시트 제조방법을 이용하여 h-BN을 박리하여 얻은 BN 나노시트를 투과전자현미경으로 관찰한 이미지이다. 200 nm 및 5 nm의 스케일바로 관찰한 결과, 수 마이크로미터 크기와 수 나노미터의 두께를 갖는 BN 나노시트로 박리된 것을 확인할 수 있었다. 본원에 의해 박리되는 2차원 나노시트는 박리시에 결함이 최소화되는 것을 특징으로 한다. 표면에 큰 결함없이 박리된 BN 나노시트를 도 4를 통해 확인할 수 있다.FIG. 4 is an image of a BN nanosheet obtained by peeling h-BN by using the above-mentioned shear stress-induced nanosheet manufacturing method by a transmission electron microscope. As a result of observing the scale of 200 nm and 5 nm, it was confirmed that BN nanosheets having a thickness of several micrometers and a thickness of several nanometers were peeled off. The two-dimensional nanosheet to be peeled by the present invention is characterized in that defects are minimized during peeling. The BN nano-sheet peeled off without a large defect on the surface can be seen in Fig.
도 5는 상술한 전단응력을 이용한 나노시트 제조방법을 이용하여 h-BN을 박리하여 얻은 BN 나노시트를 고분해능 투과전자현미경으로 관찰한 이미지이다. 도 4에서 확인한 바와 마찬가지로 수 나노미터의 얇은 두께를 가지며 결함이 최소화된 BN 나노시트가 수득되었음을 확인하였다.FIG. 5 is an image of a BN nanosheet obtained by peeling h-BN using the above-described method for producing nanosheet using shear stress, with a high-resolution transmission electron microscope. As shown in FIG. 4, it was confirmed that a BN nanosheet having a thickness of several nanometers and a minimal defect was obtained.
Claims (7)
상기 분산액을 직경이 200 ㎛ 이하인 마이크로 노즐이 장착된 유체 충돌 방식 나노 미립화 장치에 투입하는 단계;
상기 투입된 분산액에 전단응력을 인가하고 상기 마이크로 노즐에 통과시켜 1차 박리하는 단계; 및
상기 1차 박리된 분산액 내 물질들을 고속으로 충돌시켜 2차 박리하는 단계
를 포함하고 단층 또는 수층의 나노 스케일 두께를 갖는, 2차원 나노시트의 제조방법.Dispersing a material having a layered structure in a solvent to form a dispersion;
Introducing the dispersion into a fluid-impingement nano-atomizer equipped with a micro-nozzle having a diameter of 200 μm or less;
Applying a shear stress to the charged dispersion and passing the dispersion through the micro-nozzle to peel off first; And
A step of subjecting the materials in the primary peeled dispersion to high-speed collision and secondary peeling
And having a nanoscale thickness of a single layer or an aqueous layer.
상기 층상 구조를 갖는 물질은 그라파이트(graphite), 보론 나이트라이드(BN), MoS2, MoSe2 , WS2, WSe2 , NbS2, NbSe2, ZrS2, 포스포린(Phosphorene) 및 이들의 조합들로 이루어진 군에서 선택되는 1종 이상인 것을 특징으로 하는 2차원 나노시트의 제조방법.The method according to claim 1,
Material having the layered structure of graphite (graphite), boron nitride (BN), the MoS 2, MoSe 2, WS 2 , WSe 2, NbS 2, NbSe 2, ZrS 2, phosphine tarpaulins (Phosphorene), and combinations thereof Wherein the nanoparticles are at least one selected from the group consisting of polyvinyl alcohol, polyvinyl alcohol, and polyvinyl alcohol.
상기 용매는 물, 메탄올, 에탄올, 아세톤, 부탄올, 이소프로필알코올, N,N-디메틸포름아미드(N,N-dimethylformamide), 에틸렌글리콜, 디메틸아세트아미드, 포름산 에틸아세테이트, 아크릴로니트릴로 및 이들의 조합들로 이루어진 군에서 선택되는 1종 이상인 것을 특징으로 하는 2차원 나노시트의 제조방법.The method according to claim 1,
The solvent is selected from the group consisting of water, methanol, ethanol, acetone, butanol, isopropyl alcohol, N, N-dimethylformamide, ethylene glycol, dimethylacetamide, ethyl acetate formate, acrylonitrile, Wherein the nanoparticles are at least one selected from the group consisting of nanoparticles and combinations thereof.
상기 분산액이 마이크로 노즐을 통과하는 1차 박리 단계와 마이크로 노즐을 통과한 분산액 내 물질들이 충돌하는 2차 박리 단계가 연속적으로 이루어지는 것을 특징으로 하는 2차원 나노시트의 제조방법.The method according to claim 1,
Wherein the first separation step in which the dispersion liquid passes through the micro-nozzle and the second separation step in which the materials in the dispersion liquid passing through the micro-nozzle collide with each other are continuously performed.
상기 용매의 농도는 0.1중량% 내지 10중량%이고, 상기 분산액의 노즐 통과 및 충돌 횟수는 5회(pass) 내지 60회(pass)이며, 상기 용매의 농도 및 상기 분산액의 노즐 통과 및 충돌 횟수에 따라 단층 또는 수층의 나노 스케일 두께를 조절하는 것을 특징으로 하는 2차원 나노시트의 제조방법.The method according to claim 1,
The concentration of the solvent is in the range of 0.1 wt% to 10 wt%, and the number of pass and collision of the dispersion in the nozzle is 5 pass to 60 pass. The concentration of the solvent, Wherein the nanoscale thickness of the single layer or the water layer is adjusted.
상기 용매 내에 산을 첨가하여 표면에 관능기를 부여할 수 있는 것을 특징으로 하는 2차원 나노시트의 제조방법.The method according to claim 1,
Wherein an acid is added to the solvent so that a functional group can be imparted to the surface of the two-dimensional nanosheet.
상기 나노시트 표면에 카르복실기, 하이드록실기, 아미드기, 글리시딜기, 이소시아네이트기, 에폭사이드기, 고리형 에테르기, 설파이드기, 아세탈기, 락톤기 및 이들의 조합들로 이루어진 군에서 선택되는 1종 이상의 관능기를 도입할 수 있는 것을 특징으로 하는 2차원 나노시트의 제조방법.The method according to claim 1,
Wherein the surface of the nanosheet is coated with a compound selected from the group consisting of a carboxyl group, a hydroxyl group, an amide group, a glycidyl group, an isocyanate group, an epoxide group, a cyclic ether group, a sulfide group, an acetal group, a lactone group, Wherein the functional group is capable of introducing at least two functional groups.
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| CN109205578A (en) * | 2018-08-09 | 2019-01-15 | 上海交通大学 | A kind of method of microwave-assisted liquid phase stripped laminar material preparation two-dimensional nano piece |
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| JP2019532001A (en) * | 2016-09-30 | 2019-11-07 | ザ リージェンツ オブ ザ ユニバーシティ オブ カリフォルニア | Continuous production of exfoliated 2D layered material by compressed flow |
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| US11472158B2 (en) | 2016-09-30 | 2022-10-18 | The Regents Of The University Of California | Continuous production of exfoliated 2D layered materials by compressive flow |
| CN110152587A (en) * | 2018-02-13 | 2019-08-23 | 华瑞墨石丹阳有限公司 | High-speed jet impingement device and method for preparing two-dimensional nanomaterials using the device |
| CN109205578A (en) * | 2018-08-09 | 2019-01-15 | 上海交通大学 | A kind of method of microwave-assisted liquid phase stripped laminar material preparation two-dimensional nano piece |
| CN109205578B (en) * | 2018-08-09 | 2021-07-13 | 上海交通大学 | A method for preparing two-dimensional nanosheets by microwave-assisted liquid phase exfoliation of layered materials |
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