KR101307332B1 - Carbon nanofiber with superhydrophobic, and the preparation method thereof - Google Patents
Carbon nanofiber with superhydrophobic, and the preparation method thereof Download PDFInfo
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- KR101307332B1 KR101307332B1 KR1020120083110A KR20120083110A KR101307332B1 KR 101307332 B1 KR101307332 B1 KR 101307332B1 KR 1020120083110 A KR1020120083110 A KR 1020120083110A KR 20120083110 A KR20120083110 A KR 20120083110A KR 101307332 B1 KR101307332 B1 KR 101307332B1
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 132
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 78
- 239000002134 carbon nanofiber Substances 0.000 title description 3
- 238000002360 preparation method Methods 0.000 title description 3
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 138
- 239000004917 carbon fiber Substances 0.000 claims abstract description 138
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 80
- 239000002086 nanomaterial Substances 0.000 claims abstract description 50
- 239000002717 carbon nanostructure Substances 0.000 claims abstract description 44
- 239000011787 zinc oxide Substances 0.000 claims abstract description 39
- 229920006254 polymer film Polymers 0.000 claims abstract description 34
- 229920000642 polymer Polymers 0.000 claims abstract description 12
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 31
- -1 polydimethylsiloxane Polymers 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 19
- 239000011248 coating agent Substances 0.000 claims description 18
- 238000000576 coating method Methods 0.000 claims description 18
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 18
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 18
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 230000015572 biosynthetic process Effects 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 7
- 229910052759 nickel Inorganic materials 0.000 claims description 7
- 239000010931 gold Substances 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 229920006136 organohydrogenpolysiloxane Polymers 0.000 claims description 5
- 238000005229 chemical vapour deposition Methods 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 3
- 239000000956 alloy Substances 0.000 claims description 3
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- 238000010891 electric arc Methods 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 238000000608 laser ablation Methods 0.000 claims description 3
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical group [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000126 substance Substances 0.000 abstract description 19
- 235000021355 Stearic acid Nutrition 0.000 abstract description 7
- 239000003637 basic solution Substances 0.000 abstract description 7
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 abstract description 7
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 abstract description 7
- 239000008117 stearic acid Substances 0.000 abstract description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 6
- 239000003929 acidic solution Substances 0.000 abstract description 6
- 239000010703 silicon Substances 0.000 abstract description 6
- 229910052710 silicon Inorganic materials 0.000 abstract description 6
- 230000005661 hydrophobic surface Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 13
- 240000002853 Nelumbo nucifera Species 0.000 description 12
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 12
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 9
- 239000010408 film Substances 0.000 description 8
- 230000002209 hydrophobic effect Effects 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 230000009977 dual effect Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000010409 thin film Substances 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 5
- 239000005871 repellent Substances 0.000 description 5
- 239000000758 substrate Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000012776 electronic material Substances 0.000 description 3
- 229920005597 polymer membrane Polymers 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 244000205754 Colocasia esculenta Species 0.000 description 2
- 235000006481 Colocasia esculenta Nutrition 0.000 description 2
- 241000238631 Hexapoda Species 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 239000002079 double walled nanotube Substances 0.000 description 2
- 230000001747 exhibiting effect Effects 0.000 description 2
- 239000002048 multi walled nanotube Substances 0.000 description 2
- 239000002073 nanorod Substances 0.000 description 2
- 239000002071 nanotube Substances 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000002940 repellent Effects 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002109 single walled nanotube Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000005660 hydrophilic surface Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000000206 photolithography Methods 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000004078 waterproofing Methods 0.000 description 1
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
- D02J3/00—Modifying the surface
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/44—Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic Table; Zincates; Cadmates
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/05—Lotus effect
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2401/00—Physical properties
- D10B2401/02—Moisture-responsive characteristics
- D10B2401/021—Moisture-responsive characteristics hydrophobic
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Abstract
Description
본 발명은 초소수성 탄소섬유 및 이의 제조방법에 관한 것이다.
The present invention relates to a superhydrophobic carbon fiber and a method for producing the same.
초소수성 표면은 물과의 접촉각이 150 °이상인 표면을 말하며, 이러한 초소수성 표면은 자가세정(self-cleaning), 김서림 방지(anti-fogging), 방수 기능 등을 가진다. 자연계에서는 연꽃잎이나 토란잎, 곤충의 날개와 다리 등에서 이러한 현상이 관찰되며, 이를 연꽃잎 효과 (lotus effect)라고 말한다. 이들의 표면 구조를 관찰해보면 마이크로-나노 크기의 이중구조로 이루어져 있다. 즉 마이크로 구조의 표면 위에 작은 크기의 나노구조를 가지게 돌기가 존재하여 물방울이 붙지 않고 굴러 떨어지는 초발수 현상이 나타나게 된다. 이러한 초소수성 표면은 화장품의 광촉매 억제 및 건축 내외장제, 유무기 재료의 산화 방지막, 방수 섬유 등 실생활에서도 다양하게 응용되며, 기초과학적으로도 많은 연구가 진행되고 있다.
A superhydrophobic surface refers to a surface having a contact angle of 150 ° or more, and the superhydrophobic surface has self-cleaning, anti-fogging, waterproofing, and the like. In nature, this phenomenon is observed in the lotus leaf, taro leaf, insect wings and legs, which is called the lotus effect. Observation of their surface structure consists of a micro-nano sized double structure. In other words, the projections have a small size nanostructure on the surface of the micro-structure, the super water-repellent phenomenon is falling without rolling water droplets. Such superhydrophobic surfaces are widely applied in real life, such as photocatalytic suppression of cosmetics and building interior and exterior agents, anti-oxidation film of organic and inorganic materials, waterproof fiber, and many researches are being conducted in basic science.
초소수성 표면과 같이 표면의 젖음성을 제어하기 위해서는 크게 2 가지 방법이 있으며, 첫째 화학적(chemical)으로 코팅층의 표면조성을 나노스케일로 제어하는 방법과, 둘째 물리적(physical)으로 코팅층의 표면구조를 제어하는 방법이 있다. 또한, 초소수성 표면을 제조하기 위한 종래의 기술로는 포토리소그래피(photolithography), 규소 및 폴리디메틸실록산 등을 이용한 플라즈마 에칭(plasma etching), 솔-겔(sol-gel), 필드 에이디드-임프린팅(field aided-imprinting), 전기수력학(electrohydrodynamics) 등의 공정이 있다. There are two ways to control the surface wettability, such as superhydrophobic surface. First, chemically control the surface composition of the coating layer in nanoscale, and secondly physically control the surface structure of the coating layer. There is a way. In addition, conventional techniques for producing superhydrophobic surfaces include plasma etching using photolithography, silicon and polydimethylsiloxane, sol-gel, field aided-imprinting, and the like. (field aided-imprinting), electrohydrodynamics and the like.
또한, 초소수성 표면을 제조하는 선행문헌으로, In addition, as a prior art for producing a superhydrophobic surface,
대한민국 공개특허 제10-2010-0008579호(공개일 2010.01.26)에서는 초소수성 및 초발수성 표면을 갖는 패턴 및 그 형성방법이 개시된 바 있으며, 소정의 지름과 깊이를 갖는 복수의 마이크로보울이 균일하게 배열된 마이크로보울어레이를 포함하는 패턴과 그의 형성방법을 제공하고 있다.Korean Patent Publication No. 10-2010-0008579 (published Jan. 26, 2010) discloses a pattern having a superhydrophobic and superhydrophobic surface and a method of forming the same, and a plurality of micro bowls having a predetermined diameter and depth are uniformly formed. A pattern comprising an arrayed micro bowl array and a method of forming the same are provided.
또한, 대한민국 공개특허 제10-2010-0003419호(공개일 2010.01.11)에서는 초발수 필름 및 이의 제조 방법이 개시된 바 있으며, (a)균일한 패턴 형상의 마스터 필름 기재를 준비하는 단계, (b)일정 크기의 다공성 입자를 수지액과 일정무게비로 혼합하여 도포용 혼합물을 제조하는 단계, (c)상기 도포용 혼합물을 상기 마스터 필름기재 상에 도포하여 돌기형 박막을 형성시키는 단계, (d)상기 돌기형 박막이 형성된 상기 마스터 필름을 실온 경화시키는 단계, 및 (e)상기 실온 경화시킨 마스터 필름 기재를 몰드(Mold) 기판으로 하여 상기 돌기형 박막 형상이 전사되도록 임프린팅(Imprinting)하는 단계를 포함하는 초발수 필름의 제조방법을 제공하고 있다.In addition, the Republic of Korea Patent Publication No. 10-2010-0003419 (published on Jan. 11, 2010) has disclosed a super water-repellent film and its manufacturing method, (a) preparing a master film substrate of a uniform pattern shape, (b A) mixing the porous particles of a certain size with a resin and a predetermined weight ratio to prepare a coating mixture, (c) applying the coating mixture on the master film substrate to form a projection-like thin film, (d) Curing the master film on which the projection thin film is formed at room temperature, and (e) imprinting the projection film to transfer the shape of the projection thin film using the master film substrate cured at room temperature as a mold substrate. It provides a method for producing a super water-repellent film comprising.
나아가, 대한민국 등록특허 제10-0686780호 (등록일 2007년 02월 16일)에서는 스테아린산(Stearic acid) 등의 유기물질로 형성된 소수성 박막을 포함하는 소수성 유기박막 구조체가 개시된 바 있다.
Furthermore, Korean Patent No. 10-0686780 (Registration Date February 16, 2007) discloses a hydrophobic organic thin film structure including a hydrophobic thin film formed of an organic material such as stearic acid.
이와 같이 소수성을 가지는 유기분자(스테아린 산)의 자기조립 현상을 이용하여 코팅하는 방식 등 초소수성 표면을 구현하기 위한 기술들이 많이 보고된 바 있으며, 특히 유기분자를 이용한 방법은 강한 소수성을 띄기 때문에 널리 사용되고 있다. 그러나, 유기분자를 통해 형성된 초소수성 표면은 빛 조사에 의해 쉽게 분해되거나 화학적 조성이 변하는 등 안정성이 현저히 떨어지는 문제가 있다.
As described above, many techniques for realizing superhydrophobic surfaces, such as coating by using self-assembly of hydrophobic organic molecules (stearic acid), have been reported. It is used. However, the superhydrophobic surface formed through the organic molecules has a problem that the stability is significantly degraded, such as easily decomposed by light irradiation or change in chemical composition.
한편, 탄소섬유는 높은 강도와 뛰어난 열 및 전기 전도율 등의 다양한 장점을 지니고 있어 미래의 첨단 소재로 주목받고 있으며, 특히 전자 소자 및 각종 센서, 트랜지스터 등의 분야에의 응용이 활발히 연구 중에 있다.On the other hand, carbon fiber has attracted attention as a high-tech material of the future because it has a variety of advantages, such as high strength and excellent thermal and electrical conductivity, and is being actively studied in the field of electronic devices, various sensors, transistors, and the like.
또한, 탄소섬유의 표면은 소수성을 나타냄에 따라 수처리 필터, 자정(self cleaning) 구조체 등으로 이용될 수 있어 탄소섬유 표면의 소수성을 향상시킴으로써 상기 필터 등으로의 적용을 더욱 원활하게 수행할 수 있을 것으로 기대되고 있다.
In addition, the surface of the carbon fiber may be used as a water treatment filter, a self-cleaning structure, etc., as the surface of the carbon fiber exhibits a hydrophobicity, thereby improving the hydrophobicity of the surface of the carbon fiber, and thus may be applied to the filter more smoothly. It is expected.
이에 본 발명자들은 초소수성 표면을 제조하는 공정을 연구하던 중, 탄소섬유의 표면에 탄소 나노구조체를 형성시키고, 상기 탄소 나노구조체의 표면 중 적어도 일부를 실리콘(Si)계 고분자 막으로 덮음으로써 탄소섬유의 표면이 초소수성을 나타낼 수 있음을 발견하고, 본 발명에 따른 탄소섬유를 완성하였다.
The inventors of the present invention, while studying a process for producing a superhydrophobic surface, by forming a carbon nanostructure on the surface of the carbon fiber, by covering at least a portion of the surface of the carbon nanostructure with a silicon (Si) -based polymer film It has been found that the surface of can exhibit superhydrophobicity, thus completing the carbon fiber according to the present invention.
본 발명의 목적은 초소수성 탄소섬유 및 이의 제조방법을 제공하는 데 있다.
It is an object of the present invention to provide a superhydrophobic carbon fiber and its manufacturing method.
상기 목적을 달성하기 위하여, 본 발명은 In order to achieve the above object,
탄소섬유를 지지체로 하여, 상기 탄소섬유의 표면에 구비되는 탄소 나노구조체; 및Carbon nano structure provided on the surface of the carbon fiber, the carbon fiber as a support; And
상기 탄소 나노구조체의 표면을 적어도 부분적으로 덮는 Si계 고분자 막;을 포함하는 초소수성 탄소섬유를 제공한다.
It provides a super hydrophobic carbon fiber comprising; Si-based polymer film at least partially covering the surface of the carbon nanostructure.
또한, 본 발명은In addition,
탄소섬유를 지지체로 하여, 상기 탄소섬유의 표면에 구비되는 산화아연 나노구조체; 및Zinc oxide nanostructures provided on the surface of the carbon fiber, the carbon fiber as a support; And
상기 산화아연 구조체를 적어도 부분적으로 덮는 Si계 고분자 막;을 포함하는 초소수성 탄소섬유를 제공한다.
It provides a super hydrophobic carbon fiber comprising; Si-based polymer film at least partially covering the zinc oxide structure.
나아가, 본 발명은Further,
탄소섬유 표면에 탄소 나노구조체 또는 산화아연 나노구조체를 형성시키는 단계(단계 1); 및Forming a carbon nanostructure or zinc oxide nanostructure on the surface of the carbon fiber (step 1); And
상기 단계 1에서 형성된 탄소 나노구조체 또는 산화아연 나노구조체로 Si계 고분자 막을 코팅하는 단계(단계 2)를 포함하는 초소수성 탄소섬유의 제조방법을 제공한다.
It provides a method of producing a super hydrophobic carbon fiber comprising the step (step 2) of coating a Si-based polymer film with a carbon nanostructure or zinc oxide nanostructure formed in step 1.
본 발명에 따른 초소수성 탄소섬유는 종래의 유기분자(스테아린 산)가 처리된 소수성 표면보다 더욱 높은 접촉각을 나타낼 수 있으며, Si계 고분자 막을 코팅함에 따라 화학적 안정성이 향상되어 염기성 및 산성 용액에 노출되더라도 초소수성 특성을 유지할 수 있는 효과가 있다. The superhydrophobic carbon fiber according to the present invention may exhibit a higher contact angle than the hydrophobic surface treated with conventional organic molecules (stearic acid), and even if exposed to basic and acidic solutions by improving the chemical stability by coating the Si-based polymer film It is effective to maintain superhydrophobic properties.
도 1은 실시예 1에서 제조된 초소수성 탄소섬유를 주사전자현미경으로 관찰한 사진이고;
도 2는 실시예 1 및 비교예 1에서 제조된 탄소섬유 표면의 물에 대한 접촉각을 측정한 사진이고;
도 3은 실시예 1에서 제조된 초소수성 탄소섬유 표면의 산성용액에 의한 접촉각 변화를 나타낸 사진이고;
도 4는 실시예 1에서 제조된 초소수성 탄소섬유 표면의 염기성용액에 의한 접촉각 변화를 나타낸 사진이고;
도 5는 비교예 2에서 제조된 탄소섬유 표면의 산성용액에 의한 접촉각 변화를 나타낸 사진이고;
도 6은 비교예 2에서 제조된 탄소섬유 표면의 염기성용액에 의한 접촉각 변화를 나타낸 사진이고;
도 7은 실시예 1에서 제조된 초소수성 탄소섬유 표면을 X-선 광전자 분광분석한 그래프들이다.1 is a photograph of a superhydrophobic carbon fiber prepared in Example 1 observed with a scanning electron microscope;
Figure 2 is a photograph measuring the contact angle with respect to the water of the carbon fiber surface prepared in Example 1 and Comparative Example 1;
3 is a photograph showing the change in contact angle by the acidic solution of the surface of the superhydrophobic carbon fiber prepared in Example 1;
Figure 4 is a photograph showing the change in contact angle by the basic solution of the surface of the superhydrophobic carbon fiber prepared in Example 1;
5 is a photograph showing a change in contact angle by the acid solution of the surface of the carbon fiber prepared in Comparative Example 2;
6 is a photograph showing a change in contact angle by a basic solution of the surface of the carbon fiber prepared in Comparative Example 2;
Figure 7 is a graph of the X-ray photoelectron spectroscopic analysis of the superhydrophobic carbon fiber surface prepared in Example 1.
본 발명은 The present invention
탄소섬유를 지지체로 하여, 상기 탄소섬유의 표면에 구비되는 탄소 나노구조체; 및Carbon nano structure provided on the surface of the carbon fiber, the carbon fiber as a support; And
상기 탄소 나노구조체의 표면을 적어도 부분적으로 덮는 Si계 고분자 막;을 포함하는 초소수성 탄소섬유를 제공한다.
It provides a super hydrophobic carbon fiber comprising; Si-based polymer film at least partially covering the surface of the carbon nanostructure.
전술한 바와 같이, 탄소섬유는 그 자체로도 표면에 소수성을 나타내는 물질이다. 그러나, 탄소섬유의 소수성을 분리필터 등에 이용하기 위해서는 탄소섬유의 소수성을 더욱 향상시키는 것이 요구된다. As mentioned above, carbon fiber is a material which shows hydrophobicity on its own surface. However, in order to use the hydrophobicity of carbon fiber for a separation filter or the like, it is required to further improve the hydrophobicity of the carbon fiber.
이에, 본 발명에 따른 상기 초소수성 탄소섬유는 탄소섬유의 표면에 구비되는 탄소 나노구조체를 포함한다. 이때, 상기 탄소 나노구조체로는 단일벽 탄소나노튜브, 이중벽 탄소나노튜브, 다중벽 탄소나노튜브, 다발형 탄소나노튜브, 탄소 나노섬유, 탄소나노로드, 카본 블랙 등을 이용할 수 있으며, 이들의 혼합물 또한 사용할 수 있다. Thus, the superhydrophobic carbon fiber according to the present invention includes a carbon nanostructure provided on the surface of the carbon fiber. In this case, as the carbon nanostructures, single-walled carbon nanotubes, double-walled carbon nanotubes, multi-walled carbon nanotubes, bundled carbon nanotubes, carbon nanofibers, carbon nanorods, carbon black, and the like may be used, and mixtures thereof. Can also be used.
전술한 바와 같이, 연꽃잎 효과(lotus effect)가 구현되는 표면 구조는 마이크로-나노 크기의 이중구조, 즉 마이크로 구조의 표면상에 형성된 나노구조로 인한 돌기가 존재하며, 이에 따라 표면에 물방울이 붙지 않고 굴러 떨어지는 초발수 현상이 나타난다. 본 발명에 따른 초소수성 탄소섬유는 이러한 마이크로-나노 크기의 이중구조를 탄소섬유에 적용한 것으로, 마이크로 스케일의 탄소섬유 표면에 탄소 나노구조체를 형성시킴에 따라, 이중구조로 인한 연꽃잎 효과로 인하여 더욱 소수성이 향상되게 된다.
As described above, the surface structure in which the lotus effect is realized has protrusions due to the micro-nano sized dual structure, that is, the nanostructure formed on the surface of the micro structure, and thus the water droplets do not adhere to the surface. The super water repellent phenomenon that falls without rolling appears. The superhydrophobic carbon fiber according to the present invention is to apply such a micro-nano sized dual structure to the carbon fiber, and as the carbon nanostructure is formed on the surface of the micro-scale carbon fiber, due to the lotus leaf effect due to the double structure Hydrophobicity is improved.
또한, 본 발명에 따른 초소수성 탄소섬유는 상기 탄소 나노구조체의 표면을 적어도 부분적으로 덮은 Si계 고분자 막을 포함한다. 상기 Si계 고분자 막은 탄소섬유의 소수성을 더욱 향상시키고, 나아가 탄소섬유의 내화학성을 향상시키기 위한 것으로, 상기 Si계 고분자로는 폴리디메틸실록산, 폴리디오가노실록산, 오가노하이드로겐폴리실록산, 오가노폴리실록산 등을 사용할 수 있으며, 바람직하게는 폴리디메틸실록산을 이용할 수 있으나, 탄소섬유의 소수성 및 내화학성을 향상시킬 수 있는 Si계 고분자라면 이에 제한되는 것은 아니다.
In addition, the superhydrophobic carbon fiber according to the present invention includes a Si-based polymer film at least partially covering the surface of the carbon nanostructure. The Si-based polymer membrane further improves the hydrophobicity of the carbon fibers, and further improves the chemical resistance of the carbon fibers. The Si-based polymers include polydimethylsiloxane, polydiorganosiloxane, organohydrogenpolysiloxane, and organopolysiloxane. And the like, and preferably, polydimethylsiloxane may be used, but is not limited thereto, as long as it is an Si-based polymer capable of improving hydrophobicity and chemical resistance of carbon fibers.
한편, 본 발명에 따른 초소수성 탄소섬유에 있어서, 지지체로 사용되는 상기 탄소섬유는 마이크로 스케일로써, 탄소 나노구조체와 이중구조(마이크로-나노)를 형성할 수 있다면 특별히 크기에 제한을 두지 않는다.
On the other hand, in the superhydrophobic carbon fiber according to the present invention, the carbon fiber used as a support is not particularly limited in size as long as it can form a carbon nanostructure and a double structure (micro-nano) with a micro scale.
또한, 탄소 나노구조체의 표면을 덮는 Si계 고분자 막의 두께는 1 내지 5 nm인 것이 바람직하다. 상기 Si 고분자 막의 두께가 1 nm 미만인 경우에는 Si계 고분자로 인한 내화학성 향상 및 소수성 향상 효과가 저하되는 문제가 있으며, 5 nm를 초과하는 경우에는 절연성을 나타내는 실리콘(Si)의 영향으로 인하여 지지체로 사용되는 탄소섬유의 우수한 전기적 특성이 저하되어, 본 발명에 따른 초소수성 탄소섬유의 전기전도성이 저하되는 문제가 있다. 즉, Si 고분자 막의 두께가 5 nm를 초과하는 경우에는 본 발명에 따른 초소수성 탄소섬유를 전자소재로 적용시키기 어려운 문제가 발생할 수 있다.
In addition, the thickness of the Si-based polymer film covering the surface of the carbon nanostructure is preferably 1 to 5 nm. When the thickness of the Si polymer film is less than 1 nm, there is a problem in that the chemical resistance and hydrophobicity improving effect due to the Si-based polymer is lowered. There is a problem that the excellent electrical properties of the carbon fiber used is reduced, the electrical conductivity of the superhydrophobic carbon fiber according to the present invention. That is, when the thickness of the Si polymer film exceeds 5 nm, it may be difficult to apply the superhydrophobic carbon fiber according to the present invention as an electronic material.
또한, 본 발명은In addition,
탄소섬유를 지지체로 하여, 상기 탄소섬유의 표면에 구비되는 산화아연 나노구조체; 및Zinc oxide nanostructures provided on the surface of the carbon fiber, the carbon fiber as a support; And
상기 산화아연 구조체를 적어도 부분적으로 덮는 Si계 고분자 막;을 포함하는 초소수성 탄소섬유를 제공한다.
It provides a super hydrophobic carbon fiber comprising; Si-based polymer film at least partially covering the zinc oxide structure.
본 발명에 따른 상기 초소수성 탄소섬유는 탄소섬유의 표면에 구비되는 산화아연 나노구조체를 포함한다. 이때, 상기 산화아연 나노구조체로는 산화아연 나노로드, 산화아연 나노와이어, 산화아연 나노튜브 등 산화아연으로 이루어지는 다양한 형태의 나노구조체들을 이용할 수 있으며, 이들의 혼합물 또한 사용할 수 있다. The superhydrophobic carbon fiber according to the present invention includes a zinc oxide nanostructure provided on the surface of the carbon fiber. In this case, as the zinc oxide nanostructures, nanostructures of various forms including zinc oxide such as zinc oxide nanorods, zinc oxide nanowires, and zinc oxide nanotubes may be used, and mixtures thereof may also be used.
상기 산화아연 나노구조체는 탄소섬유와 마이크로-나노 크기의 이중구조를 형성하여 이에 따른 초발수 현상이 구현되도록 하기 위함이다. 즉, 마이크로 스케일의 탄소섬유 표면에 산화아연 나노구조체를 형성시킴으로써, 이중구조로 인한 연꽃잎 효과에 따라 더욱 소수성이 향상되게 된다.
The zinc oxide nanostructures are intended to form a superstructure of carbon fiber and micro-nano so that a super water repellent phenomenon can be realized. That is, by forming a zinc oxide nanostructure on the surface of the carbon fiber of the micro-scale, the hydrophobicity is further improved according to the lotus leaf effect due to the double structure.
또한, 본 발명에 따른 초소수성 탄소섬유는 상기 산화아연 나노구조체의 표면을 적어도 부분적으로 덮은 Si계 고분자 막을 포함하며, 상기 Si계 고분자 막으로 인하여, 탄소섬유의 소수성 및 내화학성을 향상시킬 수 있다. 즉, 상기 Si계 고분자 막으로 인하여, 종래의 스테아린 산이 코팅되는 경우보다 산, 또는 염기 환경에서도 우수한 초소수성을 나타낼 수 있다. 이때, 상기 Si계 고분자로는 폴리디메틸실록산, 폴리디오가노실록산, 오가노하이드로겐폴리실록산, 오가노폴리실록산 등을 사용할 수 있으며, 바람직하게는 폴리디메틸실록산을 사용할 수 있으나, 탄소섬유의 소수성 및 내화학성을 향상시킬 수 있는 Si계 고분자라면 이에 제한되는 것은 아니다.
In addition, the superhydrophobic carbon fiber according to the present invention includes a Si-based polymer film at least partially covering the surface of the zinc oxide nanostructure, and due to the Si-based polymer film, it is possible to improve the hydrophobicity and chemical resistance of the carbon fiber. . That is, due to the Si-based polymer film, it is possible to exhibit excellent superhydrophobicity even in an acid or base environment than when the conventional stearic acid is coated. In this case, as the Si-based polymer, polydimethylsiloxane, polydiorganosiloxane, organohydrogenpolysiloxane, organopolysiloxane, etc. may be used. Preferably, polydimethylsiloxane may be used, but the hydrophobicity and chemical resistance of carbon fibers may be used. If the Si-based polymer that can improve the is not limited thereto.
한편, 본 발명에 따른 초소수성 탄소섬유에 있어서, 지지체로 사용되는 상기 탄소섬유는 마이크로 스케일로써, 탄소 나노구조체와 이중구조(마이크로-나노)를 형성할 수 있다면 특별히 크기에 제한을 두지 않는다.
On the other hand, in the superhydrophobic carbon fiber according to the present invention, the carbon fiber used as a support is not particularly limited in size as long as it can form a carbon nanostructure and a double structure (micro-nano) with a micro scale.
또한, 탄소 나노구조체의 표면을 덮는 Si계 고분자 막의 두께는 1 내지 5 nm인 것이 바람직하다. 상기 Si 고분자 막의 두께가 1 nm 미만인 경우에는 Si계 고분자로 인한 내화학성 향상 및 소수성 향상 효과가 저하되는 문제가 있으며, 5 nm를 초과하는 경우에는 절연성을 나타내는 실리콘(Si)의 영향으로 인하여 지지체로 사용되는 탄소섬유의 우수한 전기적 특성이 저하되어, 본 발명에 따른 초소수성 탄소섬유의 전기전도성이 저하되는 문제가 있다. 즉, Si 고분자 막의 두께가 5 nm를 초과하는 경우에는 본 발명에 따른 초소수성 탄소섬유를 전자소재로 적용시키기 어려운 문제가 발생할 수 있다.
In addition, the thickness of the Si-based polymer film covering the surface of the carbon nanostructure is preferably 1 to 5 nm. When the thickness of the Si polymer film is less than 1 nm, there is a problem in that the chemical resistance and hydrophobicity improving effect due to the Si-based polymer is lowered. When the thickness of the Si polymer film is greater than 5 nm, the support is due to the influence of silicon (Si), which exhibits insulation properties. There is a problem that the excellent electrical properties of the carbon fiber used is reduced, the electrical conductivity of the superhydrophobic carbon fiber according to the present invention. That is, when the thickness of the Si polymer film exceeds 5 nm, it may be difficult to apply the superhydrophobic carbon fiber according to the present invention as an electronic material.
본 발명에 따른 상기 초소수성 탄소섬유들은 물에 대하여 160 °이상의 접촉각을 나타낸다. 이는 초소수성(superhydrophobic)의 기준인 150 °를 상회하는 것으로, 본 발명에 따른 초소수성 탄소섬유들이 매우 강한 소수성을 나타냄을 의미한다. 이와 같이, 본 발명에 초소수성 탄소섬유들이 높은 접촉각을 나타내는 것은 나노구조체와 탄소섬유 간의 이중구조(마이크로-나노)로 인한 것이나, 탄소 나노구조체와 산화아연 나노구조체 스스로 소수성을 나타낼 수 있는 물질들이며, 나아가 Si계 고분자 막 또한 소수성을 나타낼 수 있는 물질이기에, 이들이 탄소섬유 상에 형성됨에 따라 본 발명의 초소수성 탄소섬유가 물에 대하여 매우 높은 접촉각을 나타낼 수 있다.
The superhydrophobic carbon fibers according to the present invention exhibit a contact angle of 160 ° or more with respect to water. This is higher than the superhydrophobic standard of 150 °, which means that the superhydrophobic carbon fibers according to the present invention exhibit very strong hydrophobicity. As such, the superhydrophobic carbon fibers exhibiting a high contact angle in the present invention are due to the dual structure (micro-nano) between the nanostructure and the carbon fiber, but the carbon nanostructure and the zinc oxide nanostructure are materials that can exhibit hydrophobic properties themselves. Furthermore, since the Si-based polymer film is also a material capable of exhibiting hydrophobicity, the superhydrophobic carbon fiber of the present invention may exhibit a very high contact angle with respect to water as they are formed on the carbon fiber.
나아가, 본 발명은 Further,
탄소섬유 표면에 탄소 나노구조체 또는 산화아연 나노구조체를 형성시키는 단계(단계 1); 및Forming a carbon nanostructure or zinc oxide nanostructure on the surface of the carbon fiber (step 1); And
상기 단계 1에서 형성된 탄소 나노구조체 또는 산화아연 나노구조체로 Si계 고분자 막을 코팅하는 단계(단계 2)를 포함하는 초소수성 탄소섬유의 제조방법을 제공한다.
It provides a method of producing a super hydrophobic carbon fiber comprising the step (step 2) of coating a Si-based polymer film with a carbon nanostructure or zinc oxide nanostructure formed in step 1.
이하, 본 발명에 따른 초소수성 탄소섬유의 제조방법을 각 단계별로 상세히 설명한다.
Hereinafter, the manufacturing method of the superhydrophobic carbon fiber according to the present invention will be described in detail for each step.
본 발명에 따른 초소수성 탄소섬유의 제조방법에 있어서, 단계 1은 탄소섬유 표면에 탄소 나노구조체 또는 산화아연 나노구조체를 형성시키는 단계이다. In the method for producing a superhydrophobic carbon fiber according to the present invention, step 1 is a step of forming a carbon nanostructure or zinc oxide nanostructure on the surface of the carbon fiber.
상기 단계 1의 탄소 나노구조체 또는 산화아연 나노구조체의 형성은 탄소섬유와 이중구조(마이크로-나노)를 형성함으로써 연꽃잎 효과(lotus effect)가 구현되도록 하기 위함이다. 상기 탄소 나노구조체로는 단일벽 탄소나노튜브, 이중벽 탄소나노튜브, 다중벽 탄소나노튜브, 다발형 탄소나노튜브, 탄소 나노섬유, 탄소나노로드, 카본 블랙 등을 이용할 수 있으며, 상기 산화아연 나노구조체로는 산화아연 나노로드, 산화아연 나노와이어, 산화아연 나노튜브 등 산화아연으로 이루어지는 다양한 형태의 나노구조체들을 이용할 수 있으나, 상기 나노구조체들의 형태가 이에 제한되는 것은 아니다.
The formation of the carbon nanostructure or zinc oxide nanostructure of step 1 is to form a lotus effect by forming a double structure (micro-nano) with carbon fiber. The carbon nanostructures may include single-walled carbon nanotubes, double-walled carbon nanotubes, multi-walled carbon nanotubes, bundled carbon nanotubes, carbon nanofibers, carbon nanorods, carbon black, and the like. As the furnace, various types of nanostructures including zinc oxide, such as zinc oxide nanorods, zinc oxide nanowires, and zinc oxide nanotubes, may be used, but the shape of the nanostructures is not limited thereto.
한편, 상기 단계 1의 나노구조체 형성은 On the other hand, the nanostructure formation of step 1
금(Au), 니켈(Ni), 코발트(Co), 철(Fe), 및 이들의 합금으로 이루어지는 군으로 선택되는 1종의 촉매금속을 이용하여 탄소섬유 표면에 씨드(seed)를 형성시키는 단계(단계 a); 및Forming a seed on the surface of the carbon fiber by using one catalyst metal selected from the group consisting of gold (Au), nickel (Ni), cobalt (Co), iron (Fe), and alloys thereof. (Step a); And
상기 단계 a에서 형성된 씨드 상으로 탄소 나노구조체 또는 산화아연 나노구조체를 성장시키는 단계(단계 b);를 포함하는 공정을 통해 수행될 수 있다.
Growing a carbon nanostructure or zinc oxide nanostructures on the seed formed in step a (step b); can be carried out through a process comprising a.
상기 단계 a의 씨드는 탄소 나노 구조체 또는 산화아연 나노구조체가 성장할 수 있는 씨드로써, 금(Au), 니켈(Ni), 코발트(Co), 철(Fe) 등의 촉매금속을 이용하여 상기 씨드를 형성시킬 수 있으며, 상기 촉매금속들의 합금 또한 씨드 형성을 위해 사용할 수 있다. 그러나, 단계 a의 씨드가 상기 촉매금속에 의해서만 형성되는 것은 아니며, 탄소 나노구조체 또는 산화아연 나노구조체를 형성시키기 적합한 촉매물질을 적절히 선택하여 씨드를 형성시킬 수 있다. The seed of step a is a seed from which carbon nanostructures or zinc oxide nanostructures can be grown, and the seed is formed using a catalyst metal such as gold (Au), nickel (Ni), cobalt (Co), iron (Fe), or the like. And an alloy of the catalytic metals can also be used for seed formation. However, the seed of step a is not formed only by the catalyst metal, and the seed may be formed by appropriately selecting a catalyst material suitable for forming the carbon nanostructure or zinc oxide nanostructure.
단계 b에서는 상기 단계 a에서 형성된 씨드 상으로 탄소 나노구조체 또는 산화아연 나노구조체가 성장하며, 이러한 나노구조체의 성장을 화학기상성장, 아크방전, 레이저 어블레이션(laser ablation) 등의 공정을 통해 수행될 수 있으나, 씨드 상에 나노구조체를 성장시킬 수 있는 공정이라면 이에 제한되는 것은 아니다.
In step b, carbon nanostructures or zinc oxide nanostructures are grown on the seed formed in step a, and the growth of the nanostructures is performed through a process such as chemical vapor growth, arc discharge, laser ablation, and the like. However, the process of growing the nanostructures on the seed is not limited thereto.
이때, 본 발명에 따른 초소수성 탄소섬유 제조방법 중 단계 1에서 탄소섬유상에 나노구조체를 형성시키는 것을 상기한 바와 같이 예를 들어 설명하였으나, 단계 1의 나노구조체 형성이 상기 공정으로 제한되는 것은 아니며, 탄소섬유 상에 탄소 나노구조체 또는 산화아연 나노구조체를 형성시킬 수 있는 공정들을 적절히 선택하여 수행할 수 있다.
In this case, the formation of the nanostructure on the carbon fiber in step 1 of the superhydrophobic carbon fiber manufacturing method according to the present invention, for example, as described above, for example, but the formation of the nanostructure of step 1 is not limited to the above process, Processes capable of forming carbon nanostructures or zinc oxide nanostructures on carbon fibers may be appropriately selected.
본 발명에 따른 초소수성 탄소섬유의 제조방법에 있어서, 단계 1은 상기 단계 1에서 형성된 탄소 나노구조체 또는 산화아연 나노구조체로 Si계 고분자 막을 코팅하는 단계이다. In the method of manufacturing a superhydrophobic carbon fiber according to the present invention, step 1 is a step of coating the Si-based polymer film with a carbon nanostructure or zinc oxide nanostructures formed in step 1.
상기 Si계 고분자 막은 탄소섬유의 소수성 향상 및 내화학성 향상을 위한 것으로, 상기 Si계 고분자로는 폴리디메틸실록산, 폴리디오가노실록산, 오가노하이드로겐폴리실록산, 오가노폴리실록산 등을 이용할 수 있으며, 바람직하게는 폴리디메틸실록산을 이용할 수 있으나, 탄소섬유의 소수성 및 내화학성을 향상시킬 수 있는 Si계 고분자라면 이에 제한되는 것은 아니다. The Si-based polymer membrane is to improve the hydrophobicity and chemical resistance of the carbon fiber, the Si-based polymer may be used, such as polydimethylsiloxane, polydiorganosiloxane, organohydrogenpolysiloxane, organopolysiloxane, and the like. The polydimethylsiloxane may be used, but is not limited thereto as long as it is a Si-based polymer capable of improving hydrophobicity and chemical resistance of carbon fibers.
이때, 상기 단계 2의 Si계 고분자 막은 1 내지 5 nm 두께로 코팅되는 것이 바람직하다. 상기 Si 고분자 막의 두께가 1 nm 미만인 경우에는 Si계 고분자로 인한 내화학성 향상 및 소수성 향상 효과가 저하되는 문제가 있으며, 5 nm를 초과하는 경우에는 절연성을 나타내는 실리콘(Si)의 영향으로 인하여 지지체로 사용되는 탄소섬유의 우수한 전기적 특성이 저하되어, 본 발명에 따라 제조되는 초소수성 탄소섬유의 전기전도성이 저하되는 문제가 있다. 즉, Si 고분자 막의 두께가 5 nm를 초과하는 경우에는 제조된 초소수성 탄소섬유를 전자소재로 적용시키기 어려운 문제가 발생할 수 있다. At this time, the Si-based polymer film of step 2 is preferably coated with a thickness of 1 to 5 nm. When the thickness of the Si polymer film is less than 1 nm, there is a problem in that the chemical resistance and hydrophobicity improving effect due to the Si-based polymer is lowered. There is a problem that the excellent electrical properties of the carbon fiber used is lowered, and the electrical conductivity of the superhydrophobic carbon fiber produced according to the present invention is lowered. That is, when the thickness of the Si polymer film exceeds 5 nm, it may be difficult to apply the prepared superhydrophobic carbon fiber as an electronic material.
또한, 상기 단계 2의 코팅은 화학기상성장, 아크방전, 레이저 어블레이션(laser ablation) 등의 공정을 통해 수행될 수 있다. 상기 공정들은 Si계 고분자 막을 건식으로 코팅할 수 있는 공정들로 용매를 이용하는 습식공정보다 더욱 환경친화적인 공정이며, 나노스케일의 미세 구조까지 균일하게 코팅하기 어려운 습식공정과 비교하여 상기 건식공정들은 나노스케일의 미세 구조까지 코팅이 가능한 장점이 있다. 그러나, 상기 단계 2의 코팅을 수행하는 것이 상기 공정들로 제한되는 것은 아니며, 나노구조체 상에 Si계 고분자 막을 나노스케일로 성장시킬 수 있는 공정을 적절히 선택하여 수행될 수 있다.
In addition, the coating of step 2 may be performed through a process such as chemical vapor growth, arc discharge, laser ablation, and the like. The processes are more environmentally friendly than wet processes that use solvents to dry coat Si-based polymer membranes, and the dry processes are nano compared to wet processes that are difficult to uniformly coat nanoscale microstructures. There is an advantage that can be coated up to the fine structure of the scale. However, the coating of step 2 is not limited to the above processes, and may be performed by appropriately selecting a process capable of growing a Si-based polymer film on a nanostructure at a nanoscale.
나아가, 본 발명은Further,
탄소섬유 표면에 탄소 나노구조체 또는 산화아연 나노구조체를 형성시킨 후, 상기 탄소 나노구조체 또는 산화아연 나노구조체를 Si계 고분자 막으로 코팅하는 것을 특징으로 하는 탄소섬유 표면의 초소수성 처리방법을 제공한다.
After forming a carbon nanostructure or zinc oxide nanostructures on the surface of the carbon fiber, it provides a super hydrophobic treatment method of the carbon fiber surface, characterized in that the coating of the carbon nanostructure or zinc oxide nanostructures with a Si-based polymer film.
본 발명에 따른 초소수성 처리방법은 마이크로 스케일의 탄소섬유 표면에 나노구조체를 형성시킴으로써 마이크로-나노 크기의 이중구조를 형성시킨 후, 상기 나노구조체의 표면으로 Si계 고분자 막을 더욱 코팅하여 소수성 및 내화학성을 향상시킨다. In the superhydrophobic treatment method according to the present invention, after forming a nano-structure on the surface of the carbon fiber of the micro-scale to form a micro-nano sized dual structure, and further coating the Si-based polymer film on the surface of the nano-structure hydrophobic and chemical resistance To improve.
이때, 상기 마이크로-나노 크기의 이중구조는 전술한 바와 같이, 연꽃잎이나 토란잎, 곤충의 날개와 다리 등에서 관찰되는 연꽃잎 효과(lotus effect)를 구현하기 위한 것으로, 이에 따라 소수성이 향상되게 된다. At this time, the dual structure of the micro-nano size is to implement the lotus effect (lotus effect) observed in the lotus leaf, taro leaf, insect wings and legs, as described above, thereby improving hydrophobicity. .
나아가, Si계 고분자막을 추가 코팅함으로써 소수성이 더욱 향상되어 물에 대하여 160 °이상의 접촉각을 나타낼 수 있으며, 내화학성이 향상되어 탄소섬유가 염기 또는 산성 물질에 노출되더라도 소수성 특성을 유지할 수 있다.
Furthermore, by further coating the Si-based polymer film, the hydrophobicity is further improved to show a contact angle of 160 ° or more with respect to water, and the chemical resistance is improved to maintain the hydrophobic property even when the carbon fiber is exposed to a base or an acidic material.
또한, 본 발명은In addition,
상기 초소수성 탄소섬유를 포함하는 자정(Self cleaning) 구조체를 제공하며,It provides a self-cleaning structure containing the superhydrophobic carbon fiber,
나아가, 본 발명은 상기 초소수성 탄소섬유를 포함하는 필터를 제공한다.
Furthermore, the present invention provides a filter comprising the superhydrophobic carbon fiber.
상기 초소수성 탄소섬유는 전술한 바와 같이, 물에 대하여 매우 높은 접촉각을 나타내며, 본 발명에서는 이러한 초소수성 탄소섬유의 특성을 이용하여 자정 구조체를 제공한다.As described above, the superhydrophobic carbon fiber has a very high contact angle with respect to water, and the present invention provides a self-cleaning structure by using the characteristics of the superhydrophobic carbon fiber.
자정(Self cleaning) 기술은 크게 친수성(hydrophilic)과 소수성(hydrophobic)을 이용한 방법으로 나눌 수 있다. 이때, 친수성 표면의 경우 액상(liquid)의 표면과 고상(solid) 표면이 90 도 미만인 접촉각을 나타내며, 액상이 고상의 표면에 판모양으로 넓게 퍼짐으로써 표면의 오염물을 끌어들여 제거하게 되며, 소수성 표면의 경우 물방울이 표면을 굴러 가면서 오염물을 흡착하여 제거하게 된다. 특히, 접촉각이 극대화 또는 극소화되어 초소수성 또는 초친수성을 나타내는 표면에서 자정 현상이 두드러지게 나타나게 된다. Self cleaning techniques can be largely divided into hydrophilic and hydrophobic methods. At this time, in the case of the hydrophilic surface, the liquid surface and the solid surface have a contact angle of less than 90 degrees, and the liquid phase spreads in a plate shape on the surface of the solid phase to attract and remove contaminants on the surface. In the case of water droplets roll the surface to adsorb contaminants and remove them. In particular, the contact angle is maximized or minimized so that the phenomenon of midnight is prominent on the surface showing superhydrophobicity or superhydrophilicity.
따라서, 본 발명에 따른 초소수성 탄소섬유를 포함하는 자정 구조체는 초소수성으로 인한 자정현상이 두드러지게 발현될 수 있다.
Therefore, the self-cleaning structure including the superhydrophobic carbon fiber according to the present invention can be markedly expressed in the self-crystallization phenomenon due to the superhydrophobic.
한편, 상기 초소수성 탄소섬유를 포함하는 필터는 초소수성 특성을 이용하여물/기름과 같은 혼합물 분리 등 다양한 기능성 필터로 이용될 수 있으며, 바람직하게는 수처리용 필터로 이용될 수 있으나, 상기 필터의 적용분야가 이에 제한되는 것은 아니다.
Meanwhile, the filter including the superhydrophobic carbon fiber may be used as various functional filters such as mixture separation such as water / oil by using superhydrophobic characteristics, and may be preferably used as a filter for water treatment. The field of application is not limited thereto.
이하, 본 발명을 실시예를 통해 보다 구체적으로 설명한다. 그러나, 하기 실시예는 본 발명을 설명하기 위한 것일 뿐, 하기 실시예에 의하여 본 발명의 권리범위가 한정되는 것은 아니다.
Hereinafter, the present invention will be described more specifically by way of examples. However, the following examples are intended to illustrate the present invention, but the scope of the present invention is not limited by the following examples.
<실시예 1> 초소수성 탄소섬유의 제조 1Example 1 Preparation of Superhydrophobic Carbon Fiber 1
단계 1 : 직경이 약 6-7 ㎛인 탄소섬유 표면에 평균 20 nm 크기의 니켈(Ni) 씨드를 스퍼터링 공정을 통해 증착시켰다. 이후, 화학기상증착법을 통해 상기 니켈 씨드에서 탄소 나노구조체를 형성시켰다. Step 1: An average 20 nm nickel (Ni) seed was deposited on a surface of a carbon fiber having a diameter of about 6-7 μm through a sputtering process. Thereafter, carbon nanostructures were formed from the nickel seeds through chemical vapor deposition.
이때, 상기 화학기상증착은 200 sccm의 유량으로 수소가 흐르는 상압하에서 500 ℃ 온도로 20분간 전처리를 수행하는 단계;At this time, the chemical vapor deposition is a step of performing a pre-treatment at 500 ℃ temperature for 20 minutes under the normal pressure flowing hydrogen at a flow rate of 200 sccm;
550 ℃ 온도에서 8 sccm C2H2 및 100 sccm NH3을 3분간 공급하여 탄소 나노구조체를 성장시키는 단계; 및Growing carbon nanostructures by supplying 8 sccm C 2 H 2 and 100 sccm NH 3 at 550 ° C. for 3 minutes; And
50 sccm 아르곤(Ar) 및 450 sccm 질소(N2)가 흐르는 불활성 분위기 하에서 냉각시키는 단계;를 통해 수행되었다.
Cooling under an inert atmosphere in which 50 sccm argon (Ar) and 450 sccm nitrogen (N 2 ) flow.
단계 2 : 상기 단계 1에서 형성된 탄소 나노구조체의 표면에 폴리디메틸실록산을 3 nm의 두께로 코팅하였다. Step 2: Polydimethylsiloxane was coated on the surface of the carbon nanostructure formed in Step 1 to a thickness of 3 nm.
이때, 상기 코팅은 200 ℃ 온도의 챔버내에서 폴리디메틸실록산 및 경화제를 기화시킨 후, 탄소 나노구조체의 표면에 증착함으로써 수행되었다.
At this time, the coating was carried out by vaporizing the polydimethylsiloxane and the curing agent in a chamber at a temperature of 200 ℃, and then deposited on the surface of the carbon nanostructures.
<실시예 2> 초소수성 탄소섬유의 제조 2Example 2 Preparation of Superhydrophobic Carbon Fiber 2
단계 1 : 직경이 약 6-7 ㎛인 탄소섬유 표면에 평균 20 nm 크기의 니켈(Ni) 씨드를 스퍼터링 공정을 통해 증착시켰다. 이후, 전기화학증착을 통해 상기 니켈 씨드에서 산화아연 나노구조체를 형성시켰다.
Step 1: An average 20 nm nickel (Ni) seed was deposited on a surface of a carbon fiber having a diameter of about 6-7 μm through a sputtering process. Thereafter, zinc oxide nanostructures were formed from the nickel seeds through electrochemical deposition.
단계 2 : 상기 단계 1에서 형성된 산화아연 나노구조체의 표면에 폴리디메틸실록산을 3 nm의 두께로 코팅하였다. Step 2: The surface of the zinc oxide nanostructures formed in step 1 was coated with a polydimethylsiloxane to a thickness of 3 nm.
이때, 상기 코팅은 200 ℃ 온도의 챔버내에서 폴리디메틸실록산 및 경화제를 기화시킨 후, 산화아연 나노구조체의 표면에 증착함으로써 수행되었다.
At this time, the coating was carried out by vaporizing the polydimethylsiloxane and the curing agent in a chamber at a temperature of 200 ℃, and then deposited on the surface of the zinc oxide nanostructures.
<비교예 1>≪ Comparative Example 1 &
나노구조체의 형성없이 탄소섬유의 표면에 폴리디메틸실록산만을 3 nm 두께로 코팅하였다.
Only polydimethylsiloxane was coated to a thickness of 3 nm on the surface of the carbon fiber without the formation of nanostructures.
<비교예 2>Comparative Example 2
상기 실시예 1의 단계 2에서 폴리디메틸실록산 대신 스테아린 산을 코팅한 것을 제외하고는 상기 실시예 1과 동일하게 수행하였다.
Except for coating stearic acid instead of polydimethylsiloxane in step 2 of Example 1 was carried out in the same manner as in Example 1.
<실험예 1> 주사전자현미경을 통한 미세구조 분석Experimental Example 1 Analysis of Microstructure Using Scanning Electron Microscope
상기 실시예 1에서 제조된 초소수성 탄소섬유의 표면을 주사전자현미경을 이용하여 미세구조를 분석하였고, 그 결과를 도 1에 나타내었다. The microstructure of the superhydrophobic carbon fiber prepared in Example 1 was analyzed using a scanning electron microscope, and the results are shown in FIG. 1.
도 1에 나타낸 바와 같이, 본 발명에 따른 초소수성 탄소섬유 표면에는 나노구조체들이 형성되어 있는 것을 알 수 있다. 즉, 마이크로 스케일의 탄소섬유 표면에 나노구조체가 형성되어 이중구조를 이루고 있음을 알 수 있으며, 이에 따라 연꽃잎 효과(lotus effect)가 구현될 수 있음을 확인하였다.
As shown in Figure 1, it can be seen that the nanostructures are formed on the surface of the superhydrophobic carbon fiber according to the present invention. That is, it can be seen that the nanostructure is formed on the surface of the carbon fiber of the micro-scale to form a double structure, thereby confirming that the lotus effect (lotus effect) can be implemented.
<실험예 2> 물에 대한 접촉각 분석Experimental Example 2 Analysis of Contact Angle for Water
상기 실시예 1 및 비교예 1에서 제조된 탄소섬유의 물에 대한 접촉각을 분석하였고, 그 결과를 도 2에 나타내었다. The contact angles of the carbon fibers prepared in Example 1 and Comparative Example 1 with respect to water were analyzed, and the results are shown in FIG. 2.
도 2에 나타낸 바와 같이, 대조군으로 표기된 순수 탄소섬유는 물에 대한 접촉각이 133 °를 나타내었으며, 비교예 1에서 제조된 탄소섬유는 물에 대한 접촉각이 144 °를 나타내었다. 반면, 실시예 1에서 제조된 탄소섬유는 물에 대한 접촉각이 167 °를 나타내었으며, 이는 실시예 1의 탄소섬유 표면에 마이크로-나노 크기의 이중구조가 형성됨에 따라 연꽃잎 효과(lotus effect)가 구현되어 소수성이 더욱 향상되었기 때문임을 알 수 있다.
As shown in FIG. 2, the pure carbon fiber designated as the control group exhibited a contact angle of 133 ° for water, and the carbon fiber prepared in Comparative Example 1 exhibited a contact angle of 144 ° for water. On the other hand, the carbon fiber prepared in Example 1 exhibited a contact angle of 167 ° with respect to water, which showed a lotus leaf effect as a micro-nano sized dual structure was formed on the surface of the carbon fiber of Example 1 It can be seen that the implementation is further improved hydrophobicity.
<실험예 3> 내화학성 분석Experimental Example 3 Chemical Resistance Analysis
상기 실시예 1 및 비교예 2에서 제조된 탄소섬유의 내화학성을 분석하기 위하여, 상기 탄소섬유들의 표면으로 염기성용액(pH 13인 NaOH 용액) 또는 산성용액(pH 1인 염산용액)을 떨어뜨려 접촉각의 변화를 관찰하였으며, 그 결과를 도 3 내지 6에 나타내었다. In order to analyze the chemical resistance of the carbon fibers prepared in Example 1 and Comparative Example 2, the contact angle by dropping the basic solution (NaOH solution pH 13) or acidic solution (pH 1 hydrochloric acid solution) to the surface of the carbon fibers The change of was observed, and the results are shown in FIGS.
도 3 및 도 4에 나타낸 바와 같이, 상기 실시예 1에서 제조된 탄소섬유는 산성용액 또는 염기성용액을 떨어뜨려도 접촉각의 큰 변화가 없음을 알 수 있다. 3 and 4, it can be seen that the carbon fiber prepared in Example 1 has no large change in contact angle even when the acidic solution or the basic solution is dropped.
반면 도 5 및 도 6에 나타낸 바와 같이, 비교예 2에서 스테아린 산이 코팅된 탄소섬유는 산성용액 또는 염기성용액을 떨어뜨린 후, 점차 접촉각이 낮아지는 것을 알 수 있으며, 30 분 후에는 접촉각을 측정할 수 없을 만큼 낮아진 것을 알 수 있다. On the other hand, as shown in Figure 5 and 6, in the comparative example 2 stearic acid-coated carbon fiber after dropping the acidic solution or basic solution, it can be seen that the contact angle gradually decreases, after 30 minutes to measure the contact angle You can see that it is too low.
이를 통해, 본 발명에 따른 초소수성 탄소섬유는 초소수성뿐만 아니라, 우수한 내화학성을 또한 나타낼 수 있음을 확인하였다.
Through this, it was confirmed that the superhydrophobic carbon fiber according to the present invention may exhibit not only superhydrophobicity but also excellent chemical resistance.
<실험예 4> X-선 광전자 분광분석(x-ray photoelectron spectroscopy)Experimental Example 4 X-ray Photoelectron Spectroscopy
상기 실시예 1에서 제조된 탄소섬유의 표면을 X-선 광전자 분광분석 하였고, 그 결과를 도 7에 나타내었다. The surface of the carbon fiber prepared in Example 1 was subjected to X-ray photoelectron spectroscopy, and the results are shown in FIG. 7.
도 7에 나타낸 바와 같이, 대조군으로 표기된 순수 탄소섬유는 실리콘(Si 2p)에 해당하는 피크 및 산소(O 1s)에 해당하는 피크(~)가 나타나지 않거나 매우 낮은 수준으로 나타났으나, 실시예 1에서 제조된 탄소섬유 표면에서는 실리콘에 해당하는 피크 및 산소에 해당하는 피크가 강하게 나타나는 것을 알 수 있다. As shown in FIG. 7, the pure carbon fibers designated as the control group showed no peaks (~) corresponding to silicon (
이는 실시예 1에서 제조된 탄소섬유의 표면에 폴리디메틸실록산이 코팅된 것을 나타내는 것으로, 이를 통해 폴리디메틸실록산의 코팅이 원활하게 진행되었음을 알 수 있다.This indicates that the polydimethylsiloxane is coated on the surface of the carbon fiber prepared in Example 1, it can be seen that the coating of the polydimethylsiloxane proceeded smoothly.
또한, 탄소(C 1s)에 해당하는 피크는 실시예 1의 탄소섬유의 경우 피크의 강도가 일부 감소되었지만, 폴리디메틸실록산이 매우 얇은 박막으로 형성됨에 따라 그 감소정도가 크지않음을 알 수 있다.
In addition, the peak corresponding to the carbon (C 1s), but the intensity of the peak in the carbon fiber of Example 1 is partially reduced, it can be seen that the degree of reduction is not large as the polydimethylsiloxane is formed into a very thin film.
Claims (12)
상기 탄소 나노구조체의 표면을 적어도 부분적으로 덮는 Si계 고분자 막;을 포함하는 초소수성 탄소섬유.
Carbon nano structure provided on the surface of the carbon fiber, the carbon fiber as a support; And
Superhydrophobic carbon fiber comprising; Si-based polymer film at least partially covering the surface of the carbon nanostructure.
상기 산화아연 구조체를 적어도 부분적으로 덮는 Si계 고분자 막;을 포함하는 초소수성 탄소섬유.
Zinc oxide nanostructures provided on the surface of the carbon fiber, the carbon fiber as a support; And
And a Si-based polymer film at least partially covering the zinc oxide structure.
The superhydrophobic carbon fiber according to claim 1 or 2, wherein the Si-based polymer is at least one member selected from the group consisting of polydimethylsiloxane, polydiorganosiloxane, organohydrogenpolysiloxane, and organopolysiloxane. .
The superhydrophobic carbon fiber according to claim 1 or 2, wherein the superhydrophobic carbon fiber has a contact angle with water of 160 ° or more.
상기 단계 1에서 형성된 탄소 나노구조체 또는 산화아연 나노구조체로 Si계 고분자 막을 코팅하는 단계(단계 2)를 포함하는 초소수성 탄소섬유의 제조방법.
Forming a carbon nanostructure or zinc oxide nanostructure on the surface of the carbon fiber (step 1); And
Method of producing a super hydrophobic carbon fiber comprising the step (step 2) of coating the Si-based polymer film with the carbon nanostructure or zinc oxide nanostructures formed in step 1.
금(Au), 니켈(Ni), 코발트(Co), 철(Fe), 및 이들의 합금으로 이루어지는 군으로 선택되는 1종의 촉매금속을 이용하여 탄소섬유 표면에 씨드(seed)를 형성시키는 단계(단계 a); 및
상기 단계 a에서 형성된 씨드 상으로 탄소 나노구조체 또는 산화아연 나노구조체를 성장시키는 단계(단계 b);를 포함하는 공정으로 수행되는 것을 특징으로 하는 초소수성 탄소섬유의 제조방법.
The method of claim 5, wherein the formation of the carbon nanostructure or zinc oxide nanostructures of step 1
Forming a seed on the surface of the carbon fiber by using one catalyst metal selected from the group consisting of gold (Au), nickel (Ni), cobalt (Co), iron (Fe), and alloys thereof. (Step a); And
Growing carbon nanostructures or zinc oxide nanostructures on the seed formed in step a (step b); a method of producing a superhydrophobic carbon fiber, characterized in that carried out in a process comprising a.
The method of claim 6, wherein the growth of step b is performed by one process selected from the group consisting of chemical vapor deposition (CVD), arc discharge, and laser ablation. Method for producing superhydrophobic carbon fiber.
The superhydrophobic carbon fiber of claim 5, wherein the Si-based polymer of step 2 is at least one selected from the group consisting of polydimethylsiloxane, polydiorganosiloxane, organohydrogenpolysiloxane, and organopolysiloxane. Manufacturing method.
And forming a carbon nanostructure or zinc oxide nanostructure on the surface of the carbon fiber, and then coating the carbon nanostructure or zinc oxide nanostructure with a Si-based polymer film.
10. The superhydrophobic treatment method of claim 9, wherein the superhydrophobic surface of the carbon fiber treated by the treatment method exhibits a contact angle of 160 ° or more with respect to water.
A self cleaning structure comprising the superhydrophobic carbon fiber of claim 1.
A filter comprising the superhydrophobic carbon fiber of claim 1.
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| KR20180042255A (en) * | 2015-08-27 | 2018-04-25 | 서레이 나노시스템즈 리미티드 | Low reflectivity coating, and method and system for coating substrate |
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| CN115726216A (en) * | 2022-11-29 | 2023-03-03 | 中国民用航空飞行学院 | Super-hydrophobic paper mulching film and preparation method and application thereof |
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