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1 한국정밀공학회지제 35 권제 4 호 pp April 2018 / 457 J. Korean Soc. Precis. Eng., Vol. 35, No. 4, pp ISSN (Print) / (Online) 티올코팅시간이구리나노와이어형상및젖음성에미치는영향 Effect of Thiol Coating Time on the Morphology and Wettability of Copper Nanowires 곽원식 1, 김기환 1, 조한동 1, 황운봉 1,# Wonshik Kwak 1, Kihwan Kim 1, Handong Cho 1, and Woonbong Hwang 1,# 1 포항공과대학교기계공학과 (Department of Mechanical Engineering, Pohang University of Science and Technology) # Corresponding Author / whwang@postech.ac.kr, TEL: ORCID: KEYWORDS: Thiol coating ( 티올코팅 ), Copper nanowire ( 구리나노와이어 ), Morphology ( 형상 ), Superhydrophobic surface ( 극소수성표면 ) A study of super-hydrophobic surface originated from the analysis of lotus leaf in the nature and fabrication method of super-hydrophobic surface on copper substrate has been researched for, showed functional surfaces with anti-corrosion. However, since copper nanowires decomposed during thiol coating, it is necessary to reseach on the relation with morphology of copper nanowires and thiol coating time. In this study, the research is all about the effect of thiol coating time on wettability of copper nanowires surface. Copper hydroxide nanowires were made up by oxidation using dipping method and a polymer layer was formed on nanowires using thiol coating. Surface characteristics were assessed using scanning electron microscopy and liquid contact angles. The conclusion showed relation for wettability of thiol coated copper hydroxide nanowires with thiol coating time and proposed method would be favorable for anti-corrosion functional surface. Manuscript received: December 8, 2017 / Revised: December 13, 2017 / Accepted: December 21, 2017 NOMENCLATURE WCA = Water contact angle ( o ) GCA = Glycerol contact angle ( o ) γ = Surface tension [mn/m] 1. 서론금속의표면개질연구에서흥미롭게연구되어지고있는극소수성표면 (Superhydrophobic Surface) 은물에대하여 150 o 이상의접촉각을가지는표면을말한다. 이표면은연잎 (Lotus Leaf) 의표면특성을자연모사하여구현한표면으로써, 표면에마이크로 / 나노스케일의구조생성과표면에너지를변화시키는화학 공정을통해연잎과동일표면의특성을모사한다. 1-5 이표면은높은접촉각으로인해물에젖지않는특성을가짐으로써, 항곰팡이 (Anti-Fungus), 6 자가세정 (Self Cleanig), 7 유수분리 (Oil/Water Separation), 8 방빙 (Anti-Icing) 9 등의수분과관련된응용분야에적용가능한성능을가지고있다. 최근에는, 금속표면의부식생성을억제하는방식 (Anti-Corrosion) 효과를얻기위해극소수성표면을제작하는연구가진행되고있다. Zhang et al. 은알루미늄금속표면에두겹의수산화물층 (Double Hydroxide Layer) 형성을통해극소수성표면을제작하여부식저항성을증가시켰으며, 9 Liu et al. 은아연 (Zinc) 금속표면에담금법을통해극소수성표면을구현하여부식방지능력을향상시켰다. 10 구리 (Copper) 역시부식에강한금속으로알려져있으며높은전기전도성등의강점을가지고있어산업전반에널리사용되고있어구리재질에젖음성표면을제작하기위한연구가진행되어왔다. Lyu et al. 는구리표면에 Cu(OH) 2 나노와이어 (Nanowire) 구조를 Copyright The Korean Society for Precision Engineering This is an Open-Access article distributed under the terms of the Creative Commons Attribution Non-Commercial License ( 3.0) which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original work is properly cited.

2 458 / April 2018 한국정밀공학회지제 35 권제 4 호 Fig. 1 (a) Schematic illustration of process to fabricate superhydrophobic surface with Cu(OH) 2 nanowire and (b) SEM and optical images of water contact angle for fabricated surface 제작한후 Heptadecafluoro-1,1,2,2-tetrahydrodecyl Trichlorosilane (HDFS) 로 Self-Assembled Monolayer (SAM) 방법으로코팅하여극소수성표면을제작하였다. 11 하지만, HDFS는단분자코팅임에따라코팅두께가얇아염소 (Cl) 성분에쉽게분해되어바닷가등과같은염소성분이농후한환경에서는표면의성질을잃게되어사용에어려움이있다. 염소성분에대한구리표면의부식을억제시키기위한연구로 Cho et al. 은구리메쉬 (Mesh) 에구리나노와이어를제작하여바닷물과기름을분리하는막을제작하였는데, 바닷물에대한부식을억제시키기위해티올코팅 (Thiol Coating) 을하여고분자층의두께를증가시켰다. 12 하지만티올코팅시간에따라고분자층의두께는증가하지만고분자층생성과정에서구리나노와이어가분해되어본연의나노와이어구조를잃게되어표면젖음성의변화를초래한다. 본논문에서는구리표면의부식발생의억제를위한극소수성표면을제작하였고담금법을이용하여구리나노와이어구조를표면에제작한후티올코팅을통해나노와이어구조위에고분자층을형성하여최종적으로극소수성표면을구현하였다. 고분자층이형성되는과정에서발생되는구리나노와이어구조의분해로인한표면형상 (Morphology) 의변화를코팅시간에따라분석하였으며, 그에따른젖음성의변화를분석하였다. 최종적으로, 티올코팅시간에따른접촉각변화를분석하여코팅시간과표면젖음성과의상관관계를규명하였다. 법을이용한구리나노와이어생성은 Wu et al. 의방법을이용하여제작하였다. 13 준비된구리시편의세척을위해 60% 의질산과물을 1:1 부피비로혼합한수용액에 1분간세척한후초음파세척기를이용하여에탄올환경에서 5분동안세척한다. 세척된구리시편을 2.5 M 농도의 NaOH와 0.1 M 농도의 (NH 4 ) 2 S 2 O 8 혼합액에 4 o C의온도에서 30분동안산화시킨다. 이후처리가끝난구리시편은물로세척후상온에서 1시간동안말린다. 2.2 티올코팅을이용한극소수성표면제작 0.01 M 농도의 1H,1H,2H,2H-perfluorodecanethiol을에탄올과혼합하여코팅요액을제조한다. Cu(OH) 2 나노와이어생성을완료한시편을코팅용액에상온에서담근후에일정시간이지나면꺼내어에탄올로세척후에 60 o C에서건조시킨다. 2.3 표면구조확인및젖음성 (Wettability) 평가 Cu(OH) 2 나노와이어구조형성후에티올코팅을이용하여제작된극소수성표면은 SEM (Scanning Electron Microscopy) 사진을촬영하여표면의구조변화를확인하였으며, 장비는 JEOL JSM7401F를사용하였다. 표면의젖음성을평가하기위해제작된표면의접촉각을측정하였으며, 장비는 FEMTOBIOMED 사의 SmartDrop 장비를사용하였다. 2. 시편제작및실험방법 3. 결과및토의 험에사용된시편은포일 (Foil) 형태의구리를 20 mm 20 mm mm 크기로가공하여사용하였다. 시편세척에질산 (Nitric Acid) 과에탄올을사용하였으며, 이는삼전화학 (Samchun Chemical) 에서구매하였다. 담금법에사용된용액은 NaOH와 (NH 4 ) 2 S 2 O 8 을혼합하여사용하였으며각각삼전화학과 Alfar Aesar에서구매하였다. 티올코팅에는 97% 농도의 1H,1H,2H,2H-perfluorodecanethiol을사용하였으며, 이는 Sigma-Aldrich에서구매하였다. 3.1 Cu(OH) 2 나노와이어구조생성구리표면은과황산암모늄 (NH 4 )S 2 O 8 과반응하여산화과정에서 Cu(OH) 2 의나노와이어구조를표면에생성하며반응식은다음과같다. 13 Cu + 4OH - + (NH 4 ) 2 S 2 O 8 (1) 2- Cu(OH) 2 + 2SO 4 + 2NH 3 + 2H 2 O 2.1 담금법을이용한 Cu(OH) 2 나노와이어생성 Fig. 1(a) 는구리나노와이어형성및티올코팅을이용하여구리표면에극소수성표면을제작하는과정을나타내고있다. 담금 구리표면에생성된 Cu(OH) 2 나노와이어구조는티올코팅과정에서 1H,1H,2H,2H-perfluorodecanethiol과반응하여분해가되어구리티올레이트Cu(SC 2 H 4 C 8 F 17 ) 2 로구성된고분자층을생성하며

3 한국정밀공학회지 제 35 권 제 4 호 April 2018 / 459 Fig. 2 (a) SEM images of Cu(OH)2 nanowire surface on copper substrate by thiol coating time during with (a) 5 min, (b) 10 min, (c) 20 min, (d) 30 min, (e) 45 min, (f) 60 min, (g) 90 min, (h) 2 h, (i) 4 h, (j) 6 h, (k) 12 h, (l) 24 h 화학식은 다음과 같다.14 Cu(OH)2 + 2(C2H4C8F17-SH) Cu(SC2H4C8F17)2 + 2H2O (2) Fig. 2는 산화반응을 통해 생성된 Cu(OH)2 나노와이어 구조에 티올 코팅시간에 따라 구조의 변화를 나타낸 SEM 사진이다. 전 체적으로 티올 코팅이 시간이 길어질수록 Cu(OH)2 나노와이어의 구조가 분해되어 구조가 붕괴되는 것을 확인할 수 있다. Figs. 2(a)-2(d)에서 보이는 바와 같이, 코팅 시간이 초기인 5-10분 정도 지났을 때는 아직 구조가 유지되는 것을 확인할 수 있다. 하지만 이는 상대적으로 Cu(SC2H4C8F17)2 층이 덜 생성되었다는 것을 말 한다. 티올 코팅 시간이 20분 소요되었을 때부터 사진상으로 Cu(OH)2 나노와이어 구조가 붕괴되는 것을 확인할 수 있으며, 30 분까지 나노와이어 구조의 형상을 관찰이 가능하지만 초기 존재 Fig. 3 SEM images and optical color of fabricated surface with thiol coating during (a) 5 min, (b) 20 min, (c) 60 min, (d) 24 h 했던 다발의 Cu(OH)2 나노와이어 구조 분포는 분해되어 붕괴된 것을 확인된다. Figs. 2(e)-2(h)에서 보이는 바와 같이, 티올 코팅 변화와 표면 색상을 나타낸 사진이다. 티올 코팅이 시간이 덜 진 시간이 45분-2시간 진행되었을 때 표면에 Cu(OH)2 나노와이어 행되었을 시에는 Cu(OH)2 나노와이어 구조 본연의 색상인 녹색 구조의 잔여물 만이 분포되어 있고 Cu(SC2H4C8F17)2 고분자층이 을 표면이 띄게 되지만 티올 코팅이 지속됨에 따라 나노와이어가 두꺼워지는 것을 확인할 수 있다. 티올 코팅 시간이 4시간 이상 분해되어 녹색의 색상이 옅어지게 되고 Cu(OH)2 나노와이어가 지속되었을 때는 표면에 나노와이어 구조가 모두 붕괴되어 고분 모두 분해되고 고분자층만이 존재했을 시에는 구리 본연의 색상 자 층만이 형성됐음을 Figs. 2(i)-2(l) 사진을 통해 확인이 된다. 인 갈색으로 변하게 된다. 티올 코팅 시간이 증가함에 따라 표면의 Cu(OH)2 나노와이어 구조가 분해되는 정도를 표면의 색상으로도 구별이 가능하다. Fig. 3은 티올 코팅시간에 따른 표면의 Cu(OH)2 나노와이어 구조의 3.2 젖음성 특성 평가 Cu(OH)2 나노와이어 구조 표면을 티올 코팅 시간에 따른 젖음

4 460 / April 2018 한국정밀공학회지제 35 권제 4 호 극소수성표면을제작하기위해서는최적의코팅시간이요구됨을확인하였으며, 티올코팅시간에따른표면의젖음성변화를규명하였다. 4. 결론 Fig. 4 Morphology transformation and graph of water and glycerol contact angles for fabricated surface by thiol coating time 금속의부식을억제하기위해구리금속에 Cu(OH) 2 나노와이어구조생성하고티올코팅을통한 Cl 성분에대해내식성이강한 Cu(SC 2 H 4 C 8 F 17 ) 2 고분자층형성을통해극소수성표면을제작하였다. 고분자층이형성되는과정에서구리나노와이어가분해됨에따라변화되는표면형상 (Morphology) 을티올코팅시간에따라분석하였으며, 그에따른젖음성의변화를물과글리세롤의접촉각을측정하여젖음성을분석하였다. 최종적으로, 티올코팅시간에따른접촉각변화를분석하여코팅시간과표면젖음성과의상관관계를규명하였다. 이러한연구결과는구리금속의젖음성연구분야에적용가능하며, 내식성향상을위한기능성표면이요구되는분야에응용이가능할것으로예상된다. 성을평가하기위해접촉각의변화를측정하였다. 젖음성평가에사용된용액의종류는 2가지이며, 물 (γ = 72.0) 과글리세롤 (γ = 60.3) 이다. 15 젖음성차이를확연히구분지어평가하기위해물보다표면장력이낮은글리세롤도같이젖음성평가에이용하였다. Fig. 4은티올코팅시간에따른표면에물과글리세롤에대한접촉각을나타낸그래프이다. 티올코팅을 5분했을때는물에대해서 ± 1.8 o 의접촉각을가지는것을확인하였다. 이는티올코팅시간이다소짧아 Cu(SC 2 H 4 C 8 F 17 ) 2 고분자층이충분히생성되지못하여극소수성의표면이나타나지않은것으로판단된다. 이후 10분이상티올코팅된표면에서는모두 150 o 이상의접촉각을가짐으로써극소수성의성질을만족하는것으로확인되었다. 이는 Cu(OH) 2 나노와이어구조가붕괴되더라도어느정도의표면거칠기를보유하기때문에극소수성표면의성질을보이는것으로판단된다. 이후티올코팅시간을늘려 24시간지속시킬경우물에대하여 150 o 미만의접촉각이나타나는것을확인하였다. 이는과도한티올코팅시간으로인해다량의고분자가생성되어필름 (Film) 형태의표면을구현함에따라표면거칠기마저상실되어극소수성의성질을잃는것으로판단된다. 물보다표면장력이낮은글리세롤을이용하여극소수성의성질을표면들간의젖음성특성을추가적으로평가하였다. 글리세롤이표면장력이물보다낮기때문에전체적으로접촉각이물보다낮게나왔다. 티올코팅시간에따른글리세롤접촉각의변화는물접촉각과유사한추세를보였으며 20분티올코팅한표면에서유일하게 150 o 도이상의글리세롤접촉각을가지는것을확인하였다. 이는 Cu(OH) 2 나노와이어구조와 Cu(SC 2 H 4 C 8 F 17 ) 2 고분자층이조화롭게형성되어젖음성이가장뛰어나게나타난것으로판단된다. 따라서, 구리나노와이어에티올코팅을통해고분자층을형성하여최적의 ACKNOWLEDGEMENT 이논문은 2012년도교육부와한국연구재단의지역혁신인력양성사업의지원을받아수행된연구임 (NRF-2012H1B8A ). REFERENCES 1. Extrand, C. W. and Moon, S. I., Repellency of the Lotus Leaf: Contact Angles, Drop Retention, and Sliding Angles, Langmuir, Vol. 30, No. 29, pp , Frankiewicz, C. and Attinger, D., Texture and Wettability of Metallic Lotus Leaves, Nanoscale, Vol. 8, No. 7, pp , Shi, X., Dou, R., Ma, T., Liu, W., Lu, X., et al., Bioinspired Lotus-Like Self-Illuminous Coating, ACS Applied Materials & Interfaces, Vol. 7, No. 33, pp , Lee, J. and Yong, K., Combining the Lotus Leaf Effect with Artificial Photosynthesis: Regeneration of Underwater Superhydrophobicity of Hierarchical ZnO/Si Surfaces by Solar Water Splitting, NPG Asia Materials, Vol. 7, No. 7, An, A. K., Guo, J., Lee, E.-J., Jeong, S., Zhao, Y., et al., PDMS/PVDF Hybrid Electrospun Membrane with Superhydrophobic Property and Drop Impact Dynamics for Dyeing Wastewater Treatment Using Membrane Distillation, Journal of Membrane Science, Vol. 525, pp , Kim, Y. and Hwang, W., Wettability Modified Aluminum Surface for a Potential Antifungal Surface, Materials Letters, Vol. 161, pp , 2015.

5 한국정밀공학회지제 35 권제 4 호 April 2018 / Cao, W.-T., Liu, Y.-J., Ma, M.-G., and Zhu, J.-F., Facile Preparation of Robust and Superhydrophobic Materials for Self- Cleaning and Oil/Water Separation, Colloids and Surfaces A: Physicochemical and Engineering Aspects, Vol. 529, pp , Zhang, Z., Ge, B., Men, X., and Li, Y., Mechanically Durable, Superhydrophobic Coatings Prepared by Dual-Layer Method for Anti-Corrosion and Self-Cleaning, Colloids and Surfaces A: Physicochemical and Engineering Aspects, Vol. 490, pp , Bengaluru Subramanyam, S., Kondrashov, V., Rühe, J. R., and Varanasi, K. K., Low Ice Adhesion on Nano-Textured Superhydrophobic Surfaces under Supersaturated Conditions, ACS Applied Materials & Interfaces, Vol. 8, No. 20, pp , Zhang, F., Zhao, L., Chen, H., Xu, S., Evans, D. G., et al., Corrosion Resistance of Superhydrophobic Layered Double Hydroxide films On Aluminum, Angewandte Chemie International Edition, Vol. 47, No. 13, pp , Liu, H., Szunerits, S., Xu, W., and Boukherroub, R., Preparation of Superhydrophobic Coatings on Zinc as Effective Corrosion Barriers, ACS Applied Materials & Interfaces, Vol. 1, No. 6, pp , Cho, H., Lee, J., Lee, S., and Hwang, W., Durable Superhydrophilic/Phobic Surfaces Based on Green Patina with Corrosion Resistance, Physical Chemistry Chemical Physics, Vol. 17, No. 10, pp , Wu, X. and Shi, G., Production and Characterization of Stable Superhydrophobic Surfaces Based on Copper Hydroxide Nanoneedles Mimicking the Legs of Water Striders, Journal of Physical Chemistry B, Vol. 110, No. 23, pp , Yao, X., Gao, J., Song, Y., and Jiang, L., Superoleophobic Surfaces with Controllable Oil Adhesion and their Application in Oil Transportation, Advanced Functional Materials, Vol. 21, No. 22, pp , Lide, D., Handbook of Chemistry and Physics, CRC Press, 86th Ed., 2005.

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