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전자빔 표면처리를 통한 Ti3C2Tx MXene의 유기물 흡착성능 향상

황윤재1, 임민혁2, 팽창웅2, 박형욱1, 김지수3,4,#orcid

Enhanced Adsorption Performance for Organic Materials by Electron Beam-Treated Ti₃C₂Tx MXene

Yun Jae Hwang1, Min Hyeok Lim2, Changung Paeng2, Hyung Wook Park1, Jisoo Kim3,4,#orcid
Journal of the Korean Society for Precision Engineering 2023;40(3):189-196.
Published online: March 1, 2023

1 울산과학기술원 기계공학과

2 경북대학교 에너지 신소재·화학공학부

3 경북대학교 정밀기계공학과

4 경북대학교 미래과학기술융합학과

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#E-mail: js.kim@knu.ac.kr, TEL: +82-53-950-1279
• Received: December 20, 2022   • Revised: January 10, 2023   • Accepted: January 17, 2023

Copyright © The Korean Society for Precision Engineering

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  • MXene is one of the most fascinating 2D materials owing to its great electrical properties and unique performance. Among various application areas, the performance of organic material adsorption has been highlighted with the growing interest in the biocompatible applications of MXene. Although previous research revealed that the huge surface area of this 2D nanomaterial could lead to superior organic material adsorption performance, surface functional groups were usually controlled by changing the pH, and the MXene was generally produced by HF etchant. In this study, a surface modification method of Ti3C2Tx MXene film was proposed to enhance organic material adsorption by irradiating the pulsed plasma electron beam (EB). Methylene blue (MB)-dispersed DI water was prepared, and pristine MXene was prepared at pH 7. The MB concentration was only reduced by 20% by pristine MXene. However, EB-treated MXene adsorbed about 75% of the MB within 20 min and over 90% within 80 min when the MXene film was ground to powder form. The results showed that the increased surface area and formation of hydrophilic functional groups successfully modified MB adsorption following EB irradiation under optimal processing conditions.
  • KEYWORDS: MXene, Ti3C2Tx, 2D nanomaterials, Organic materials adsorption, Electron beam
  • KEYWORDS: 맥신, 2차원 나노물질, 유기물 흡착, 전자빔
최근 세계적으로 산업과 경제의 발전에 따라 발생하는 환경오염에 대한 관심이 증가하는 추세이며 특히 수자원 오염에 관한 문제가 급격히 대두되고 있다[1,2]. 수자원 오염에는 다양한 원인이 있지만 가죽, 종이 등을 생산하는 과정 중 공장에서 발생하는 염료에 의한 오염이 높은 비중을 차지하고 있으며[3], 다양한 연구자 및 산업계 종사자들은 메틸렌 블루(Mythylene Blue, MB)와 같은 색상 변화를 유발하는 유기물의 제거를 위한 많은 노력을 기울여 왔다[4-6].
오수에서 유기물을 제거할 수 있는 방법은 광분해 방법을 활용한 유기물 분해[7], 필터를 활용한 유기물 제거[8], 화학 반응을 활용한 유기물 침전물 생성법[9], 생화학적 방법을 활용한 유기물 분해[10] 등 다양한 방법이 시도되어 왔다. 특히 유기물을 제거하는 방식 중 용매, 계면 활성제, 가스 등을 활용한 습식 제거 방식은 비용이 저렴하고 제거 효율이 높아[11-13] 활발히 연구된 분야 중 하나이다. 그러나 최근 이러한 유기물 제거에 활용되는 용매 및 계면 활성제가 2차적인 오염을 유발할 수 있다는 연구 결과들이 보고되면서 친환경적인 방법을 활용한 유기물 제거 방법에 관한 수요는 꾸준히 증가하는 추세이다[14].
이러한 수요에 맞추어 환경에 영향을 주지 않으며 높은 효율로 유기물을 제거할 수 있는 물질 중 하나로 최근 맥신(MXene)이 주목받고 있다[15,16]. MXene은 전이금속에 탄소(C) 또는 질소(N)가 결합된 2차원 판상구조의 물질로 알루미늄(Al)과 같이 중간 층을 형성하고 있는 MAX Phase에서 중간층만을 선택적으로 식각하는 방법을 통해 제작이 가능하다[17]. 특히 판상 구조의 특성을 활용해 높은 표면적과 전기전도도, 높은 화학적 안정성을 바탕으로 차세대 그래핀(Graphene)으로 불리며 배터리, 에너지 저장소재, 촉매 재료 등의 다양한 활용이 가능하다고 보고되고 있다[18,19]. 수처리 분야에서는 MXene을 활용한 해수의 담수화[20] 등의 연구가 수행되었고 최근에는 유기물 흡착 성능에 관한 보고가 증가하고 있는 추세이다[15,21].
하지만 기존의 MXene을 활용한 유기물 흡착 성능을 보고하는 논문의 대부분은 MXene을 용매에 분산한 상태에서 식각 과정 중 발생하는 플루오린(F) 이온과 관련된 작용기를 활용한 흡착 성능 향상을 목표로 하고 있다[15]. 특히 다른 이온으로 Termination된 특수한 작용기를 가지는 MXene을 활용한 유기물 흡착 성능 연구에서는 2차적인 화학물질 활용이 필수적이기 때문에 낮은 pH와 2차 오염 물질의 발생이 불가피하여 실제 수정화 공정에 적용이 어려운 실정이다[15].
본 연구에서는 전자빔 표면처리 공정을 MXene의 후처리 공정으로 도입하여 중성에서도 높은 유기물 흡착 성능을 가질 수 있는 MXene의 합성 방법을 소개하고자 한다. 가장 일반적으로 활용되는 Ti3C2Tx MXene을 MILD Etching Method를 활용해 제작하고 진공 여과를 통해 필름화하였으며, 제작된 필름에 대면적 펄스형 플라즈마 전자빔(Large-Area Pulsed Electron Beam, LPEB)을 조사하여 표면적의 향상 및 유기물 흡착 작용기 생성을 유도하였다. 유기물 흡착 성능을 대표적으로 분석하기 위해 MB 수용액에 MXene을 침지 혹은 혼합하여 농도변화를 분석하였다. 전자빔 조사를 통해 MXene의 표면적이 증가하는 것으로 분석되었으며 표면에서 생성되는 친수성 작용기 및 높은 표면에너지로 인해 유기물 흡착 성능이 향상되는 것으로 분석되었다. 본 연구를 통해 제안된 EB-Treated MXene은 2차 오염물의 발생이 없는 청정한 유기물 흡착재로의 산업적 활용이 가능할 것으로 생각되어 향후 수자원 오염 문제 해결에 적극 활용될 수 있을 것으로 기대된다.
2.1 Ti3C2Tx MXene의 합성
MXene은 일반적으로 플루오르화 수소산(Hydrofluoric Acid, HF)을 직접 활용하는 합성 방법과 간접적으로 HF 생성 반응을 유도하여 합성하는 방법으로 구분할 수 있다. 본 연구에서는 염산(Hydrochloric Acid, HCl, Sigma-Aldrich, 37%)과 플루오르화 리튬(Lithium Fluoride, LiF, Sigma-Aldrich, ~300 mesh)을 이용한 In-Situ MILD Etching 방법을 이용해 Ti3AlC2 MAX Phase 물질(MAX Powder, 99%, ~325 mesh)에서 알루미늄(Al)을 선택적으로 식각해 Ti3C2Tx MXene을 합성하였다. 식각 용액을 제조하기 위해 테플론 튜브에 탈이온수(Deionized (DI) Water) 5 ml와 37% HCl 15 ml를 투입한 후 플루오르화 리튬 1 g을 첨가했다. 테플론 튜브는 오일조에 고정시킨 뒤 35oC로 유지되는 가열 교반기 위에서 30분간 300 rpm의 속도로 교반을 유지했다. 그 다음 MAX 가루를 식각 용액에 30분에 걸쳐 조금씩 첨가한 후 24시간 동안 300 rpm을 유지하며 연속적으로 교반하여 Al 층을 식각했다. 식각 반응이 끝난 용액은 세척과 박리를 위해 50 ml 코니칼 튜브(Conical Tube)로 옮겨져 3,500 rpm에서 3분간 원심분리 했다. 이후 투명한 상등액을 제거하고 탈이온수를 추가해 재분산 시켰다. 상기 과정을 9,000 rpm까지 서서히 높여가며 pH가 6-7에 도달할 때까지 약 7회 반복했다. 모든 세척 과정에서 분산액을 5분 이상 충분히 흔들어 다층의 MXene을 단층의 MXene으로 박리시켰다. 마지막으로 세척이 완료된 분산액을 3,500 rpm에서 20분간 원심분리한 후 검은색 상등액만 사용했다. 이 검은색 상등액은 순수한 단층 Ti3C2Tx MXene을 포함하고 있다.
제작된 단층 Ti3C2Tx MXene은 진공 여과장치를 이용해 Free Standing Film으로 제조할 수 있다. 필터는 Anodic Aluminum Oxide (AAO) Membrane (WHATMAN, Pore size: 0.02 μm)을 사용했으며 150 ml의 DI Water에 7 mg의 MXene을 첨가해 진공 여과한 후 상온에서 12시간 동안 건조하였다. 마지막으로 필터에서 떼어낸 Free Standing Film을 실험에 사용했다. 이러한 과정은 Fig. 1에서 상세히 확인할 수 있다.
Fig. 1

Schematic diagram of the fabrication process of free standing Ti3C2Tx MXene film

KSPE_2023_v40n3_189_f001.jpg
2.2 전자빔 기반 표면처리 공정
본 연구에서는 기존에 금속의 표면처리에 활용되는 대면적 펄스형 전자빔을 활용한 표면처리 공정을 수행하였다[22]. 대면적 펄스형 전자빔은 약 60 mm의 직경을 가지는 플라즈마 전자빔을 활용한 표면처리 방식으로 2 μs의 매우 짧은 시간에 약 0-10 J/cm2의 에너지를 순간적으로 전달할 수 있는 표면처리 공정이다. 이 과정에서 발생한 폭발적인 에너지 전달을 활용해 소재의 용융 및 재결정화를 유도할 수 있으며, 금속의 경우 상 변화를 활용한 성능 향상을 기대할 수 있다. 금속 외의 폴리머, 세라믹 등의 소재는 표면에서 작용기(Functional Groups) 변화를 통해 표면에너지를 조정할 수 있으며 소재의 성분 변화를 통해 내식성 및 반응성 향상을 기대할 수 있다. 본 연구에서는 제작된 Ti3C2Tx 필름에 2-5 J/cm2의 에너지 밀도를 가지는 전자빔 표면처리를 적용하였으며, 사용된 Ti3C2Tx 필름의 두께가 매우 얇기 때문에 손상을 최소화하여 표면처리를 완료하기 위해서 1회의 조사 횟수만을 활용하였다. 1회를 초과하는 조사횟수를 적용할 경우, 필름이 손상되어 완전히 탄화되거나 찢어진 형태로 공정의 결과가 도출되었다. 전자빔 조사 공정에서의 진공 챔버는 10-6 Pa의 진공도를 유지하고 약 0.05 Pa까지 Ar을 플라즈마용 가스로 주입하여 조사가 진행되었으며, 양극 전압은 5 kV, 전자의 가속을 위한 솔레노이드 전압은 1.0-1.2 kV로 활용하였다. 전자빔의 에너지 밀도는 주로 가속전압인 음극 전압에 의해 결정되며, 2-5 J/cm2의 에너지 밀도를 형성하기 위해 전자빔의 가속전압은 10-12 kV로 활용하였다.
2.3 표면 및 구조분석
Ti3C2Tx MXene은 2차원의 판상구조를 가지고 있다. MXene의 합성 품질을 분석하기 위하여 표면과 단면에서 전계 방사형 주사 현미경(Field-Emission Scanning Electron Microscope; FE-SEM, HITACHI Regulus 8220, Japan)을 활용한 형상 분석을 수행하였다. 단면 분석을 위해 필름을 액화 질소에 넣어 급속냉각시킨 후 절단하는 전처리 과정을 거쳐 단면 분석이 수행되었다.
합성된 Ti3C2Tx의 성분 및 구조 분석을 위해 X-ray 회절 분석법(X-ray Diffraction Spectroscopy; XRD, RIGAKU SmartLab, Japan)이 활용되었다. 해당 분석을 통해 합성된 Ti3C2Tx 필름에 섞여 있는 불순물의 종류와 양에 대한 분석을 수행할 수 있어 합성된 필름의 품질을 분석할 수 있다. XRD 분석은 2θ의 범위를 5-65o 범위로 설정하고 0.05o의 Step Size로 Cu Kα Source를 이용해 진행되었다.
소재 표면에서의 작용기 변화에 따른 표면에너지 분석은 접촉각 측정(Contact Angle Measurement, FEMTOBIOMED Smart Drop, South Korea)을 통해 진행되었다. 본 연구에서는 Sessile Drop Method를 활용한 정접촉각 분석을 수행하였으며, 접촉각 분석은 3 μl의 DI Water를 사용해 진행되었다.
2.4 유기물 흡착성능 분석
Ti3C2Tx의 유기물 흡착성능 분석을 위해 메틸렌블루 수용액을 활용한 유기물 흡착성능 분석을 수행하였다. MB의 흡착성능 분석은 표면적 변화에 의한 영향 분석을 함께 수행하기 위해 필름 및 분말 형태의 분석을 함께 수행하였다. MB 수용액은 5 mg의 MB와 증류수 1 L를 교반하여 제작하였으며, 총 9 mg의 Ti3C2Tx를 필름과 분말형태로 제작하여 상온 및 암실 상태에서 흡착성능평가를 수행하였다. 국부적으로 변화하는 MB의 농도 변화에 의한 흡착성능의 변화를 균일하게 유지하기 위해 흡착 성능을 평가하는 동안 수용액은 자성 막대(Magnetic Bar)를 활용해 300 rpm의 균일한 속도로 교반하였다.
기존 논문에서 언급했다시피 MXene의 유기물 흡착 성능은 pH에 따라 급격히 변화한다[15]. 하지만 본 논문에서는 중성에서의 흡착성능 향상을 목표로 하고 있기 때문에 Ti3C2Tx가 침지 혹은 혼합된 MB 수용액의 pH를 중성(pH = 7)로 유지하는 것이 중요하다. 따라서 1PrJ›1pH의 측정은 pH 측정기(pH Meter, EcoTestr pH 1, Eutech, Singapore)를 사용하여 측정하였다. 정량적인 흡착도의 평가를 위해 흡착재와 교반 중인 MB 수용액에서 20분 간격으로 1 mL의 샘플을 채취하여 자외선-가시광선분광광도계(UV-vis Spectrophotometer, Flame VIS-NIR Miniature Spectrometer, Ocean Insight, United States)를 통해 UV Spectrum (500-800 nm)을 측정하였고, 664 nm 파장에서 메틸렌블루의 농도를 측정하여 교반 시간에 따른 흡착도를 분석하였다.
3.1 소재 특성 및 전자빔 조사에 따른 변화
Fig. 2는 합성된 Ti3C2Tx의 전자빔 표면처리 전후 단면의 SEM 사진을 보여준다. 사진에서 볼 수 있듯이, 합성과정을 통해 매우 균일한 판상구조의 MXene 형태가 합성된 것을 확인할 수 있으며, 표면에서의 형상을 통해 각 층이 매우 견고하게 흡착되어 있는 형태를 확인할 수 있다. 10 kV의 가속전압을 활용한 전자빔 조사 후에는 표면에서 약간의 층간 박리 현상을 볼 수 있으며 일부 표면이 손상을 거쳐 표면적이 약간 증가한 형태를 나타내는 것으로 확인되었다. 12 kV의 전자빔 가속전압을 이용한 조사 이후에는 Fig. 3(c)에서 볼 수 있듯이 표면이 매우 거칠게 꽃잎 모양의 표면을 형성한 것을 확인할 수 있으며, 기공이 다수 발생하는 다공성 구조를 형성한 것을 확인할 수 있다. 이러한 현상은 표면적을 증가시키는 매우 중요한 요인으로 작용하며 유기물 흡착성능의 향상에 영향을 주었을 것이라고 추측할 수 있다.
Fig. 2

Cross-sectional SEM images of Ti3C2Tx MXene films before and after the electron beam irradiations

KSPE_2023_v40n3_189_f002.jpg
Fig. 3

XRD spectra of Ti3C2Tx MXene before and after the electron beam irradiation in terms of the acceleration voltages

KSPE_2023_v40n3_189_f003.jpg
Fig. 3은 합성된 Ti3C2Tx 필름의 전자빔 표면처리 전후 XRD 분석 결과를 보여준다. 해당 그래프의 6.5o 부근에서 확인할 수 있는 (002) Main Peak를 통해 Ti3C2Tx MXene의 합성이 적절히 이루어진 것을 확인할 수 있으며, 전자빔 조사 후 해당 Peak의 증가를 통해 분순물이 제거된 것을 확인할 수 있다. 또한, (004), (006), (008) Plane의 고차원 Peak도 전자빔 조사 후 일괄적으로 증가한 것을 확인할 수 있다. 과도한 에너지가 조사되는 경우, TiCx 형태의 유기물 흡착과 관련이 없는 상이 부분적으로 형성된 것도 확인할 수 있어 5 Shots 이상의 높은 조사 횟수가 적용되는 경우, 과도한 에너지 전달로 인해 기존의 Ti3C2Tx MXene의 구조가 파괴되어 유기물 흡착 성능의 저하를 예상할 수 있다[23].
Fig. 4는 전자빔 조사 전후 MXene 필름 표면에서 접촉각의 변화를 보여준다. 그림에서 볼 수 있듯이 기본적으로 Pristine MXene의 경우, 필름 제작 후 건조 조건에 따라 표면에너지가 크게 변화하는 것으로 나타났다. Fig. 4(a)에서 볼 수 있듯이, 고온 및 진공환경에서 건조를 통해 제작된 MXene 필름의 경우 약 130o 내외의 접촉각을 보인 반면 상온 및 대기중 건조를 거친 MXene 필름의 경우, 대략적으로 약 66o 내외의 친수성을 나타내는 것으로 확인되었다. 진공 및 고온 건조의 경우 제조된 MXene 필름의 표면에서 친수성 작용기를 형성하기 위해 필수적으로 필요한 산소와 같은 원소가 접촉하기 어려운 환경이기 때문에 상대적으로 소수성 특성을 가지며, 대기 중에서 건조된 MXene 필름의 경우 건조 과정에서 산소와의 접촉이 다량 발생하기 때문에 산소를 포함하는 친수성 작용기가 다수 발생한 것으로 분석할 수 있다. 이러한 특성은 전자빔 조사 후 변화하는 표면 거칠기에 따라 표면에너지에 큰 영향을 미치는 것으로 분석되었다.
Fig. 4

Static contact angles of DI water on MXene films depending on the drying condition of the films before and after the EB irradiations

KSPE_2023_v40n3_189_f004.jpg
Fig. 2에서 볼 수 있듯이 전자빔 표면처리는 표면에 Flower-Like Defects 형성을 통해 표면 거칠기를 증대시키는 효과를 가진다.
(1)
cos θrCB=rfcos θe+f-1
(2)
cos θrW=rcos θe
이러한 표면적의 증가는 접촉각에 영향을 미친다. 식(1)과 식(2)는 표면 거칠기에 따라 변화하는 접촉각의 경향성을 설명하고 있다. 식에서 θe는 완전히 편평한 곳에서의 접촉각을, r은 표면 거칠기 상수(Roughness Factor)를, θr은 접촉 형태에 따른 접촉각을 나타낸다. 두 식에서 볼 수 있듯이, Cassie State와 Wenzel State 모두에서 친수성과 소수성이 구분되는 90o의 접촉각을 기준으로 표면이 거칠수로 친수성 물질의 표면은 더욱 친수성으로 변화하며, 소수성 물질의 표면은 더욱 소수성으로 변화한다. 따라서, 초기에 소수성 특성을 가지던 고온/진공 건조된 MXene 필름의 경우 전자빔 조사 후 더욱 소수성이 되는 것을 Fig. 4에서도 확인할 수 있다. 이와 반대로 상온/대기 중에서 건조된 MXene 필름의 경우 전자빔 조사를 거치면서 더욱 친수성이 되는 것을 확인할 수 있다. 이러한 접촉각은 결국 표면에너지를 대표하는 물성이기 때문에 낮은 표면에너지를 가지는 MXene의 경우 유기물 흡착성능이 낮을 것으로 예상할 수 있으며, 초친수성을 나타내는 MXene의 경우에는 전자빔 조사에 따라 유기물의 흡착 성능이 증대될 것으로 기대할 수 있다.
Fig. 5는 상온 및 대기 중에서 건조된 MXene의 전자빔 표면 처리 후 표면에서의 푸리에변환적외선분광(Fourier-Transform Infrared Spectroscopy; FT-IR, VARIAN 670, United States) 분석 결과를 보여준다. 그래프에서 확인할 수 있듯이 상온 및 대기 중 건조 과정에서 생성되는 Ti-OH (1,639 cm-1) 외에도 전자빔 조사 과정에서 높은 온도 및 표면 반응으로 인해 하이드록실(Hydroxyl Group) 작용기가 형성된 것을 확인할 수 있다. 해당 작용기는 친수성 작용기로서의 역할을 수행하기 때문에 전자빔 표면처리가 표면적을 넓히는 것 외에도 친수성 작용기를 추가로 생성하여 표면에너지를 높임으로써 유기물 흡착성능 향상에 영향을 줄 수 있는 것으로 예상할 수 있다.
Fig. 5

FT-IR Spectra of MXene films before and after the EB irradiations

KSPE_2023_v40n3_189_f005.jpg
3.2 유기물 흡착성능 분석 및 고찰
본 연구에서는 MXene의 제작에 활용되는 산에서 발생한 이온에 의한 흡착 성능을 배제하고 산업 적용이 불가능한 산성 MXene의 한계점을 극복하기 위해 중성(pH = 7)에서 MXene의 유기물 흡착 성능을 평가하였다. Fig. 6에서 확인할 수 있듯이 전자빔 표면처리 전후 모두 pH가 약 6.9–7 수준을 유지하여 MXene의 합성에 사용한 산이 충분히 씻겨 나간 것을 확인할 수 있었으며, 중성 흡착재로의 활용이 가능한 것으로 판단하였다.
Fig. 6

pH of MB-dispersed solutions mixed with (a) pristine and (b) EB-treated Ti3C2Tx MXene

KSPE_2023_v40n3_189_f006.jpg
Fig. 7은 전자빔 에너지 조건에 따른 유기물 흡착성능을 평가하기 위해 10 kV와 12 kV의 가속전압을 이용해 표면처리 공정을 적용하기 전후의 MXene 필름의 MB 흡착 성능을 분석한 결과를 보여준다. 필름 형태의 Pristine MXene의 경우, 약 10% 내외의 가장 낮은 흡착 성능을 보였다. 필름 형태를 직접 활용한 경우 MB 수용액과 접촉하는 면적이 상대적으로 적기 때문에 흡착 성능이 매우 낮은 것을 확인할 수 있다. 전자빔 표면처리를 거쳐 표면적을 증가시키고 표면에 친수성 작용기를 추가적으로 생성한 MXene의 경우 상대적으로 우수한 수준의 유기물 흡착 성능을 보여주었다. Fig. 7에서 확인할 수 있듯이 2시간 이내에 약 30% 내외의 흡착 성능을 보였으며 10 kV의 가속전압을 활용한 전자빔 표면처리가 가장 우수한 성능을 나타냈다. 그러나 12 kV의 가속전압을 활용한 경우에는 표면에서 흡착과 관련없는 물질인 TiCx 형성의 영향으로 흡착 성능이 다시 저하된 것을 확인할 수 있다. 따라서 본 연구에서는 10 kV의 가속전압을 최적화된 공정 조건으로 선정하고 접촉 면적을 극대화 시키기 위해 전자빔으로 표면처리된 MXene 필름을 가루 형태로 분쇄하여 MB의 흡착 성능을 평가하였다.
Fig. 7

Variations of relative concentration of MB adsorbed by Ti3C2Tx MXene films before and after the EB irradiations

KSPE_2023_v40n3_189_f007.jpg
Fig. 8에서 볼 수 있듯이, 가루 형태로 분쇄한 MXene의 경우 접촉 면적이 증가하면서 전자빔 표면처리를 하지 않은 경우에도 필름 형태보다 상대적으로 높은 흡착 성능을 보였지만, 2시간 동안 약 20-25% 내외의 최대 흡착 성능을 보여 유기물 흡착재로 활용이 어려운 수준의 흡착 성능을 나타냈다. 10 kV의 가속전압을 활용해 표면처리된 MXene을 가루로 분쇄한 경우에는 나노 물질의 높은 표면적과 표면에 형성된 친수성 작용기의 효과로 인해 월등히 향상된 흡착 성능을 보였다. Fig. 8에서 볼 수 있듯이, 10분 이내에 약 60%, 60분 이내에 약 95% 이상의 MB가 흡착된 것으로 나타났다. 이러한 흡착 성능은 색상 변화를 통해서도 뚜렷이 관찰할 수 있었다.
Fig. 8

Variations of relative concentration of MB adsorbed by Ti3C2Tx MXene powder before and after the EB irradiations

KSPE_2023_v40n3_189_f008.jpg
Fig. 9는 10 kV의 가속전압으로 표면처리 된 MXene을 가루로 분쇄하여 MB 수용액에 혼합한 뒤 경과한 시간에 따라 변화하는 색상을 보여주고 있다. 그림에서 보이듯 약 20분 이내에 명확한 색상 변화를 관찰할 수 있었으며, 60분이 경과한 후에는 투명에 가까운 색상을 나타내는 것을 확인할 수 있다. 따라서 플라즈마 전자빔을 이용한 MXene의 표면처리를 통해 표면적의 향상과 표면 작용기의 효과적인 조정을 통해 유기물 흡착성능을 극대화할 수 있다고 결론 내릴 수 있다.
Fig. 9

A color change of the MB solution mixed with Ti3C2Tx MXene powder irradiatied by the electron beam wi 10 kV of acceleration voltage

KSPE_2023_v40n3_189_f009.jpg
본 논문에서는 Ti3C2Tx MXene의 유기물 흡착성능 향상을 위해 대면적 플라즈마 기반의 전자빔 표면처리 공정을 소개하였다. 전자빔 가속전압에 따른 MXene 표면에서의 형상 및 물질 상태의 변화를 분석하였으며, 표면적의 변화 및 친수성 작용기의 형성 유무에 따른 유기물 흡착 성능을 MB를 이용해 평가하였다. MB 수용액을 이용한 MXene의 흡착 성능 평가를 통해 표면적이 넓은 가루 형태의 MXene에서 전자빔 표면처리 후 월등히 향상된 MB 흡착 성능을 확인할 수 있었으며, 10 kV의 가속전압을 활용한 최적화된 공정조건을 도출할 수 있었다. 본 연구를 통해 합성된 전자빔 표면처리 MXene은 산성을 가지고 있어 흡착 성능은 우수하지만 산업적 활용성이 떨어지던 기존 연구결과의 한계점을 극복할 수 있는 기술로 판단되며 향후 타 유기물의 흡착성능 평가결과를 추가로 분석하여 다양한 유기물 제거 관련 산업 활용 가능성이 매우 높을 것으로 기대된다.
이 논문은 2022년도 정부(교육부)의 재원으로 한국연구재단의 지원을 받아 수행된 기초연구사업이며(No. 2021R1I1A3045191), 2017년 과학기술정보통신부의 재원으로 한국연구재단의 지원을 받아 수행되었습니다(NRF-2017R1A5A1015311).
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Yun Jae Hwang
KSPE_2023_v40n3_189_bf001.jpg
Ph.D. candidate in the Department of Mechanical Engineering, Ulsan National Institute of Science and Technology. His research interest is hybrid manufacturing.
Min Hyeok Lim
KSPE_2023_v40n3_189_bf002.jpg
B.Sc. candidate in the Department of Department of Advanced Materials Science & Engineering, Kyungpook National University. His research interest is organic materials adsorption.
Changung Paeng
KSPE_2023_v40n3_189_bf003.jpg
B.Sc. candidate in the Department of Department of Advanced Materials Science & Engineering, Kyungpook National University. His research interest is materials fabrication
Hyung Wook Park
KSPE_2023_v40n3_189_bf004.jpg
Professor in the Department of Mechanical Engineering, Ulsan National Institute of Science and Technology. His research interest is manufacturing.
Jisoo Kim
KSPE_2023_v40n3_189_bf005.jpg
Assistant Professor in the Department of Precision Mechanical Engineering, Kyungpook National University. His research interest is energy beam manufacturing.

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Enhanced Adsorption Performance for Organic Materials by Electron Beam-Treated Ti₃C₂Tx MXene
J. Korean Soc. Precis. Eng.. 2023;40(3):189-196.   Published online March 1, 2023
DOI: https://doi.org/10.7736/JKSPE.022.147
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Enhanced Adsorption Performance for Organic Materials by Electron Beam-Treated Ti₃C₂Tx MXene
J. Korean Soc. Precis. Eng.. 2023;40(3):189-196.   Published online March 1, 2023
DOI: https://doi.org/10.7736/JKSPE.022.147
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Enhanced Adsorption Performance for Organic Materials by Electron Beam-Treated Ti₃C₂Tx MXene
Image Image Image Image Image Image Image Image Image
Fig. 1 Schematic diagram of the fabrication process of free standing Ti3C2Tx MXene film
Fig. 2 Cross-sectional SEM images of Ti3C2Tx MXene films before and after the electron beam irradiations
Fig. 3 XRD spectra of Ti3C2Tx MXene before and after the electron beam irradiation in terms of the acceleration voltages
Fig. 4 Static contact angles of DI water on MXene films depending on the drying condition of the films before and after the EB irradiations
Fig. 5 FT-IR Spectra of MXene films before and after the EB irradiations
Fig. 6 pH of MB-dispersed solutions mixed with (a) pristine and (b) EB-treated Ti3C2Tx MXene
Fig. 7 Variations of relative concentration of MB adsorbed by Ti3C2Tx MXene films before and after the EB irradiations
Fig. 8 Variations of relative concentration of MB adsorbed by Ti3C2Tx MXene powder before and after the EB irradiations
Fig. 9 A color change of the MB solution mixed with Ti3C2Tx MXene powder irradiatied by the electron beam wi 10 kV of acceleration voltage

Fig. 1

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Enhanced Adsorption Performance for Organic Materials by Electron Beam-Treated Ti₃C₂Tx MXene
JKSPE : Journal of the Korean Society for Precision Engineering

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