KR102486060B1 - Method for the implementation of water-repellent and oil-repellent surfaces using crosslinking type PDMS - Google Patents
Method for the implementation of water-repellent and oil-repellent surfaces using crosslinking type PDMS Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
- B05D5/08—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05C3/00—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material
- B05C3/02—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material the work being immersed in the liquid or other fluent material
- B05C3/04—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material the work being immersed in the liquid or other fluent material with special provision for agitating the work or the liquid or other fluent material
- B05C3/08—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material the work being immersed in the liquid or other fluent material with special provision for agitating the work or the liquid or other fluent material the work and the liquid or other fluent material being agitated together in a container, e.g. tumbled
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05C9/00—Apparatus or plant for applying liquid or other fluent material to surfaces by means not covered by any preceding group, or in which the means of applying the liquid or other fluent material is not important
- B05C9/08—Apparatus or plant for applying liquid or other fluent material to surfaces by means not covered by any preceding group, or in which the means of applying the liquid or other fluent material is not important for applying liquid or other fluent material and performing an auxiliary operation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
- B05D3/0254—After-treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/14—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by electrical means
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/14—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by electrical means
- B05D3/141—Plasma treatment
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/16—Antifouling paints; Underwater paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/16—Antifouling paints; Underwater paints
- C09D5/1656—Antifouling paints; Underwater paints characterised by the film-forming substance
- C09D5/1662—Synthetic film-forming substance
- C09D5/1675—Polyorganosiloxane-containing compositions
Abstract
본 발명은 가교형 PDMS 유도체를 이용한 발수 및 발유 기재 표면 구현방법에 관한 것으로, 본 발명에 따른 기재 표면에 발유성 및 발수성을 부여하는 방법은, 기재 표면에 플라즈마 처리를 통해 수산화기를 형성한 다음, 실리콘에 치환되는 일부 치환기가 수소로 이루어져 있는 가교형 PDMS 유도체를 사용함에 따라서, 기재에 코팅제의 젖음성을 현저히 향상시키고, 다른 부가적인 성분의 사용 없이도 충분한 발수성 및 발유성을 부여할 수 있어, 유증기 회수 장치/설비, 파이프, 후드 등에 유용할 수 있다.The present invention relates to a method for realizing the surface of a water-repellent and oil-repellent substrate using a cross-linked PDMS derivative. By using a cross-linked PDMS derivative in which some substituents substituted for silicone are composed of hydrogen, the wettability of the coating agent on the substrate is significantly improved, and sufficient water and oil repellency can be imparted without using other additional components, so oil vapor recovery can be achieved. Can be useful for gizmos/equipment, pipes, hoods, etc.
Description
본 발명은 가교형 PDMS 유도체를 이용한 발수 및 발유 기재 표면 구현방법에 관한 것으로, 유증기 회수 장치/설비, 파이프, 후드, 후드의 부품, 관로, 노즐 등에 유용할 수 있다.The present invention relates to a method for realizing the surface of a water-repellent and oil-repellent substrate using a cross-linked PDMS derivative, and may be useful for oil vapor recovery devices/facility, pipes, hoods, parts of hoods, conduits, nozzles, and the like.
일반적으로 발수성과 발유성이란 각각 물과 기름에 젖기 어려운 성질을 뜻하는 것으로, 초발수성/초발유성이란 해당 분야에서 고체의 표면에 접촉한 물의 접촉각이 150°이상, 오일에 대한 접촉각이 150°이상인 경우로 일반적으로 정의된다.In general, water repellency and oil repellency mean properties that are difficult to get wet with water and oil, respectively. case is generally defined.
최근에 물에 대한 접촉각이 150°이상인 초발수성 표면은 기본적인 연구 및 실제적인 응용 모두에서의 중요성 때문에 상당한 관심을 끌어왔다. 초발수성(superhydrophobicity)과 초발유성(superoleophobicity)은 물체의 표면이 각각 물과 오일에 극히 젖기 어려운 물리적 특성을 말한다. 예를 들어, 식물의 잎, 곤충의 날개 또는 새의 날개는 외부의 어떠한 오염물질이 특별한 제거 작업 없이 제거되거나 처음부터 오염이 되지 않게 하는 특성을 지니고 있다. 이것은 식물의 잎, 곤충의 날개, 새의 날개 등이 초발수성을 지니고 있기 때문이다.Recently, superhydrophobic surfaces with water contact angles greater than 150° have attracted considerable attention due to their importance in both basic research and practical applications. Superhydrophobicity and superoleophobicity refer to physical properties in which the surface of an object is extremely difficult to get wet with water and oil, respectively. For example, the leaves of plants, the wings of insects, or the wings of birds have characteristics that prevent any external contaminants from being removed without special removal or from becoming contaminated in the first place. This is because plant leaves, insect wings, and bird wings have super-water repellent properties.
젖음성(wettability)은 고체 재료의 주요 표면 특성이고, 이것은 화학적 조성 및 기하학적 마이크로/나노 구조 둘 다에 의해 주로 지배된다. 젖음성 표면은 기름-물 분리, 반사 방지, 생체 유착 방지, 점착 방지, 오염 방지, 자기 세정 및 유체 난류 억제와 같은 다양한 분야에서 잠재적 응용성으로 인하여 많은 주의를 끌어왔다.Wettability is a key surface property of solid materials, and it is primarily governed by both the chemical composition and the geometrical micro/nanostructure. Wettable surfaces have attracted much attention due to their potential applications in various fields such as oil-water separation, anti-reflection, anti-bioadhesion, anti-adhesion, anti-fouling, self-cleaning and fluid turbulence suppression.
한편, 초발수성 알루미늄 제조에 대한 몇몇 보고가 있어 왔으나 금속 기재상의 초발수성/초발유성은 비교적 많은 주목을 받지 못하였다.On the other hand, there have been some reports on the production of superhydrophobic aluminum, but superhydrophobicity/superoil repellency on metal substrates has not received relatively much attention.
최근의 환경오염에 따른 대기 오염이 심각해지고, 황사나 미세먼지의 발생이 증가하면서, 창문을 열어 환기시키는 것보다 환풍 장치를 가동하여 실내의 공기를 정화시키는 경우가 많다. 또한, 가정, 작업장, 산업 현장, 식당, 사무실, 화장실이나 욕실 등과 같이 주거 시설, 업무용 시설, 상업용 시설 등에서 발생하는 생활 먼지, 음식 냄새, 담배 냄새, 작업시 발생하는 각종 유해 냄새, 일산화탄소와 같은 유해 공기 및 미세먼지, 유증기 등을 제거하기 위해서 상시적으로 환풍 장치를 가동하기도 한다.As air pollution due to recent environmental pollution has become serious and the occurrence of yellow dust and fine dust has increased, there are many cases in which a ventilation device is operated to purify indoor air rather than opening a window to ventilate. In addition, living dust, food odors, cigarette odors, various harmful odors generated during work, and harmful substances such as carbon monoxide generated from residential facilities, business facilities, and commercial facilities such as homes, workplaces, industrial sites, restaurants, offices, toilets, and bathrooms, etc. In order to remove air, fine dust, oil vapor, etc., a ventilation device is also operated at all times.
이러한 환풍 장치는, 일반적으로 특정 장소에 시스템화되어 설치되어, 실내 오염 정도에 따라 자동 가동되는 환풍 시스템과 같은 복잡한 설비에 의해 구현되거나, 외부와 인접한 벽에 설치되어 내외부의 공기를 단순히 순환시키는 창문형 환풍기에 의해 구현되고 있다.These ventilation devices are generally implemented by complex facilities such as a ventilation system that is systematized and installed in a specific place and automatically operated according to the degree of indoor contamination, or is a window type ventilator that is installed on a wall adjacent to the outside and simply circulates inside and outside air. is implemented by
그러나 이러한 환풍기는 일정시간 사용시에는 필연적으로 환풍기의 내외부에 먼지가 쌓이게 되는 문제점이 발생하고 있어, 비위생적이며, 먼지를 제거하기 위하여 환풍기를 분리하여 세척하는 번거로운 작업을 수행해야 하는 문제점이 있다.However, these ventilators have a problem that dust inevitably accumulates inside and outside the ventilator when used for a certain period of time, which is unsanitary and requires a cumbersome task of separating and washing the ventilator to remove dust.
특히, 식당이나 유증기가 발생하는 곳에 설치되는 환풍기에는 유분이나 미세먼지를 1차적으로 흡착하여 줄 어떠한 여과장치도 없어, 장기간 사용시에는 유분과 미세먼지가 결합되어 아래로 흐르는 경우가 발생하는 등, 위생에 심각한 우려를 줄 수가 있을 뿐만 아니라, 화재의 위험에도 노출이 될 여지가 있다.In particular, there is no filtering device to primarily adsorb oil or fine dust in ventilators installed in restaurants or places where oil vapor is generated. Not only can it pose a serious concern to fire, but it can also be exposed to the risk of fire.
본 발명의 목적은 기재 표면에 발유성 및 발수성을 부여하는 방법을 제공하는 것이다.An object of the present invention is to provide a method for imparting oil repellency and water repellency to the surface of a substrate.
본 발명의 다른 목적은 상기 방법으로 제조된 표면에 발유성 및 발수성이 부여된 기재를 제공하는 것이다.Another object of the present invention is to provide a substrate having oil repellency and water repellency imparted to the surface prepared by the above method.
본 발명의 또 다른 목적은 상기 기재를 포함하는 유증기 회수 장치, 유증기 회수 설비, 파이프, 후드, 후드의 부품, 관로 및 노즐을 제공하는 것이다.Another object of the present invention is to provide an oil vapor recovery device, an oil vapor recovery facility, a pipe, a hood, parts of the hood, a conduit, and a nozzle including the above substrate.
상기 목적을 달성하기 위하여,In order to achieve the above purpose,
본 발명은, The present invention,
(단계 1) 기재를 플라즈마 처리하여, 표면에 -OH 작용기를 생성함에 따른 젖음성을 향상시키는 단계;(Step 1) Plasma treatment of the substrate to improve wettability by generating -OH functional groups on the surface;
(단계 2) 열처리를 통한 기재 표면의 불순물을 제거하는 단계;(Step 2) removing impurities on the surface of the substrate through heat treatment;
(단계 3) 기재 표면에 하기 화학식 1로 표시되는 가교형 PDMS(Polydimethylsiloxane) 유도체를 코팅하는 단계; 및(Step 3) coating a cross-linked polydimethylsiloxane (PDMS) derivative represented by Chemical Formula 1 on the surface of the substrate; and
(단계 4) 열처리를 통해 경화시키는 단계;를 포함하는, (Step 4) curing through heat treatment; including,
기재 표면에 발유성 및 발수성을 부여하는 방법을 제공한다.A method for imparting oil repellency and water repellency to the surface of a substrate is provided.
[화학식 1][Formula 1]
(상기 화학식 1에서, x 및 y는 각각 1-10의 정수이다.)(In Formula 1, x and y are each an integer of 1-10.)
본 발명에 따른 방법은, 코팅제로서 화학식 1로 표시되는 가교형 PDMS 유도체를 단독으로 사용한다는 점, 그리고 처리 단계가 단조롭다는 점에서, 기재 표면에 발수성 및 발유성을 부여하는 처리비용이 절약되는 장점이 있다.The method according to the present invention is advantageous in that the treatment cost for imparting water and oil repellency to the surface of the substrate is saved in that the crosslinked PDMS derivative represented by Formula 1 is used alone as a coating agent and the treatment step is monotonous. there is
본 발명에 따른 방법에 있어서, 상기 단계 1은 기재를 플라즈마 처리하여, 표면에 -OH 작용기를 생성함에 따른 젖음성을 향상시키는 단계이다. 구체적으로, 상기 단계 1의 플라즈마 처리는 180-220W, 40-60kHz 및 40-60 sccm의 O2 조건으로 실시할 수 있다. 만약, 플라즈마 처리 조건이 상기 범위를 벗어날 경우 기재 표면의 젖음성이 충분하지 못한 문제가 있을 수 있다.In the method according to the present invention, step 1 is a step of plasma-treating the substrate to improve wettability by generating -OH functional groups on the surface. Specifically, the plasma treatment of step 1 may be performed under conditions of 180-220 W, 40-60 kHz, and 40-60 sccm O 2 . If the plasma treatment conditions are out of the above range, there may be a problem of insufficient wettability of the surface of the substrate.
본 발명에 따른 방법에 있어서, 상기 단계 2는 열처리를 통한 기재 표면의 불순물을 제거하는 단계이다. 구체적으로, 상기 단계 2의 열처리는 120-300 ℃에서 3-60분 동안 실시할 수 있다. 만약, 기재 표면 불순물 제거를 위한 단계 2의 열처리 조건이 상기 범위 미만일 경우 불순물의 제거율이 낮은 문제가 있을 수 있고, 상기 범위 초과일 경우 불순물 제거율의 증가없이 공정 비용이 증가되는 문제가 있을 수 있다.In the method according to the present invention, step 2 is a step of removing impurities from the surface of the substrate through heat treatment. Specifically, the heat treatment of step 2 may be performed at 120-300 °C for 3-60 minutes. If the heat treatment conditions of step 2 for removing impurities on the surface of the substrate are less than the above range, there may be a problem of low impurity removal rate, and if it exceeds the above range, there may be a problem of increasing process cost without increasing the impurity removal rate.
본 발명에 따른 방법에 있어서, 상기 단계 3은 기재 표면에 상기 화학식 1로 표시되는 가교형 PDMS(Polydimethylsiloxane) 유도체를 코팅하는 단계이다. 구체적으로, 상기 단계 3의 코팅은 스핀코팅, 딥코팅, 바코팅 등을 사용할 수 있고, 바람직하게는 스핀 코팅을 사용할 수 있다. In the method according to the present invention, step 3 is a step of coating a cross-linked polydimethylsiloxane (PDMS) derivative represented by Chemical Formula 1 on the surface of the substrate. Specifically, spin coating, dip coating, bar coating, etc. may be used for the coating in step 3, and spin coating may be preferably used.
상기 화학식 1의 가교형 PDMS 유도체의 분자량은 6000-8000 g/mol, 바람직하게는 6200-7800 g/mol, 더욱 바람직하게는 6500-7500 g/mol, 더욱 더 바람직하게는 6750-7250 g/mol일 수 있다. 만약, 분자량이 상기 범위 미만일 경우 발수성/발유성이 충분히 부여되지 못하여 내구성에 문제가 있을 수 있고, 상기 범위 초과일 경우 코팅면이 균일하게 형성되지 못하는 문제가 있을 수 있다.The molecular weight of the crosslinked PDMS derivative of Formula 1 is 6000-8000 g/mol, preferably 6200-7800 g/mol, more preferably 6500-7500 g/mol, still more preferably 6750-7250 g/mol can be If the molecular weight is less than the above range, water repellency/oil repellency may not be sufficiently imparted, resulting in a problem with durability, and if the molecular weight exceeds the above range, there may be a problem in that the coated surface is not uniformly formed.
상기 화학식 1의 가교형 PDMS 유도체는 실리콘에 치환되는 치환기로서 메틸과 수소가 존재하고, 이 중에서 수소는 플라즈마 처리를 통해 기재 표면에 형성된 수산화기와 서로 인력을 형성하여, 기재 표면에 화학식 1의 가교형 PDMS 유도체의 젖음성을 향상시키는 것을 특징으로 한다.The crosslinked PDMS derivative of Formula 1 has methyl and hydrogen as substituents substituted for silicon, and among them, hydrogen forms an attractive force with the hydroxyl formed on the surface of the substrate through plasma treatment, thereby forming a crosslinked PDMS derivative of Formula 1 on the surface of the substrate. It is characterized by improving the wettability of the PDMS derivative.
본 발명에 따른 방법에 있어서, 상기 단계 4는 열처리를 통해 경화시키는 단계이다. 구체적으로, 상기 단계 4의 열처리는 250-350℃에서 10-60분 동안 실시할 수 있다. 만약, 단계 4의 열처리 조건이 상기 범위 미만일 경우 경화 반응이 미완성되는 문제가 있을 수 있고, 상기 범위 초과일 경우 경화 완료 후에 공정 비용이 증가하는 문제와 물성이 저하되는 문제가 있을 수 있다.In the method according to the present invention, step 4 is a step of curing through heat treatment. Specifically, the heat treatment of step 4 may be performed at 250-350° C. for 10-60 minutes. If the heat treatment condition of step 4 is less than the above range, there may be a problem that the curing reaction is incomplete, and if it exceeds the above range, there may be a problem of increasing process cost and deterioration of physical properties after curing is completed.
상기 기재는 알루미늄, 알루미늄 합금, 타이타늄, 타이타늄 합금, 마그네슘, 마그네슘 합금, 스테인리스강, 철강, 귀금속, 희귀금속, 비결정성 금속, 알카리 금속, 알카리 토금속, 중금속, 합금, 초합금 등의 금속; 플라스틱; 유리 등을 사용할 수 있다.Metals such as aluminum, aluminum alloys, titanium, titanium alloys, magnesium, magnesium alloys, stainless steel, steel, noble metals, rare metals, amorphous metals, alkali metals, alkaline earth metals, heavy metals, alloys, and superalloys; plastic; glass etc. can be used.
또한, 본 발명은 상기 방법으로 제조된 표면에 발유성 및 발수성이 부여된 기재를 제공한다.In addition, the present invention provides a substrate having oil repellency and water repellency imparted to the surface prepared by the above method.
나아가, 본 발명은 상기 기재를 포함하는 유증기 회수 장치, 유증기 회수 설비, 파이프, 후드, 후드의 부품, 관로 및 노즐을 제공한다.Furthermore, the present invention provides an oil vapor recovery device, an oil vapor recovery facility, a pipe, a hood, parts of the hood, a conduit, and a nozzle including the substrate.
본 발명에 따른 기재 표면에 발유성 및 발수성을 부여하는 방법은, 기재 표면에 플라즈마 처리를 통해 수산화기를 형성한 다음, 실리콘에 치환되는 일부 치환기가 수소로 이루어져 있는 가교형 PDMS 유도체를 사용함에 따라서, 기재에 코팅제의 젖음성을 현저히 향상시키고, 다른 부가적인 성분의 사용 없이도 충분한 발수성 및 발유성을 부여할 수 있어, 유증기 회수 장치/설비, 파이프, 후드, 후드의 부품, 노즐, 관로 등에 유용할 수 있다.The method of imparting oil repellency and water repellency to the surface of a substrate according to the present invention uses a cross-linked PDMS derivative in which some substituents substituted for silicon are composed of hydrogen after forming hydroxyl groups on the surface of the substrate through plasma treatment, It can significantly improve the wettability of the coating agent on the substrate and impart sufficient water and oil repellency without using other additional components, so it can be useful for oil vapor recovery devices / facilities, pipes, hoods, hood parts, nozzles, pipelines, etc. .
도 1은 실시예 1에 따른 물/오일 접촉각 및 접촉이력각을 측정한 결과이다.
도 2는 실시예 2에 따른 물/오일 접촉각 및 접촉이력각을 측정한 결과이다.
도 3은 실시예 3에 따른 물/오일 접촉각 및 접촉이력각을 측정한 결과이다.
도 4는 실시예 4에 따른 물/오일 접촉각 및 접촉이력각을 측정한 결과이다.
도 5는 비교예 1(무처리군)에 따른 물/오일 접촉각 및 접촉이력각을 측정한 결과이다.1 is a result of measuring the water/oil contact angle and contact hysteresis angle according to Example 1.
Figure 2 is the result of measuring the water / oil contact angle and contact hysteresis angle according to Example 2.
Figure 3 is the result of measuring the water / oil contact angle and contact hysteresis angle according to Example 3.
Figure 4 is the result of measuring the water / oil contact angle and contact hysteresis angle according to Example 4.
Figure 5 is the result of measuring the water / oil contact angle and contact hysteresis angle according to Comparative Example 1 (untreated group).
이하, 본 발명을 하기의 실시예에 의하여 더욱 상세하게 설명한다. 단, 하기의 실시예는 본 발명을 예시하는 것일 뿐, 본 발명의 내용이 하기의 실시예에 의해 한정되는 것은 아니다.Hereinafter, the present invention will be described in more detail by the following examples. However, the following examples are merely illustrative of the present invention, and the contents of the present invention are not limited by the following examples.
<실시예> 발수성 및 발유성 부여 금속의 제조<Example> Preparation of metals imparting water and oil repellency
알루미늄 5052 합금을 코팅 대상 기재로 사용하였다.Aluminum 5052 alloy was used as the substrate to be coated.
단계 1: 플라즈마 처리Step 1: Plasma treatment
상기 기재를 200W, 50kHz, O2 : 50sccm 조건으로 15분 동안 플라즈마 처리하였다.The substrate was treated with plasma for 15 minutes under conditions of 200 W, 50 kHz, and O 2 : 50 sccm.
단계 2: 열처리를 통한 불순물 제거Step 2: Removal of impurities through heat treatment
상기 단계 1에서 플라즈마 처리가 끝난 기재를 150℃의 오븐에서 10분 동안 열처리하여 불순물을 제거하였다.The substrate subjected to plasma treatment in step 1 was heat treated in an oven at 150° C. for 10 minutes to remove impurities.
단계 3: 코팅제의 코팅Step 3: Coating of the coating agent
상기 단계 2에서 불순물이 제거된 기재에 코팅제로서 화학식 1로 표시되는 가교형 PDMS 유도체인 SYLGARD 184 Silicon Elastomer Curing Agent(제조사: Dow chemical company) 및/또는 화학식 2로 표시되는 PDMS 유도체인 SYLGARD 184 Silicon Elastomer Base(제조사: Dow chemical company)를 기재 면적 3cm×2cm 당 60μL 드롭한 다음, 스핀 코팅법으로 코팅하였다(실시예 2 및 4에 해당함). 스핀 코팅 조건은 1000rpm에서 30초간 실시하였다. 또한, 다른 코팅 방법으로 딥코팅을 실시하였다(실시예 1 및 3에 해당함).SYLGARD 184 Silicon Elastomer Curing Agent (manufacturer: Dow chemical company), a cross-linked PDMS derivative represented by Formula 1, and/or SYLGARD 184 Silicon Elastomer, a PDMS derivative represented by Formula 2, as a coating agent on the substrate from which impurities are removed in step 2 Base (manufacturer: Dow chemical company) was dropped in an amount of 60 μL per substrate area of 3 cm × 2 cm, and then coated by spin coating (corresponding to Examples 2 and 4). Spin coating was performed at 1000 rpm for 30 seconds. In addition, dip coating was performed by another coating method (corresponding to Examples 1 and 3).
실시예 1 및 2는 코팅제로 상기 Curing Agent(경화제, 화학식 1)를 단독으로 사용하였고, In Examples 1 and 2, the Curing Agent (curing agent, Chemical Formula 1) was used alone as a coating agent,
실시예 3 및 4는 코팅제로 상기 Base(주제, 화학식 2) 및 Curing Agent(경화제, 화학식 1)를 10:1 중량비로 혼합하여 사용하였다.In Examples 3 and 4, the base (subject, formula 2) and the curing agent (curing agent, formula 1) were mixed at 10:1 as a coating agent. They were mixed in a weight ratio and used.
단계 4: 열처리를 통한 경화Step 4: Hardening through heat treatment
상기 단계 3에서 코팅이 완료된 기재를 300℃의 오븐에서 30분 동안 열처리하여 경화를 완료하였다.The substrate coated in step 3 was heat treated in an oven at 300° C. for 30 minutes to complete curing.
(SYLGARD 184 Silicon Elastomer)coating agent
(SYLGARD 184 Silicon Elastomer)
[화학식 1: Curing agent][Formula 1: Curing agent]
x 및 y는 각각 1-10의 정수이다.x and y are each an integer from 1-10.
[화학식 2: Base][Formula 2: Base]
m은 1-60의 정수이다.m is an integer from 1 to 60;
<실험예 1> 코팅성(두께 및 갈라짐) 평가<Experimental Example 1> Evaluation of coating properties (thickness and cracking)
실시예 1 내지 4에서 제조한 샘플의 코팅성을 평가하기 위하여, 코팅 두께 및 코팅의 갈라짐을 평가하였다.In order to evaluate the coating properties of the samples prepared in Examples 1 to 4, coating thickness and cracking of the coating were evaluated.
(두꺼운 순으로 1>2>3>4점)coating thickness
(1>2>3>4 points in order of thickness)
(갈라짐 발생 순으로 1>2>3>4점)cracked coating
(1>2>3>4 points in order of crack occurrence)
표 2에 나타난 바와 같이, 코팅 두께가 가장 얇으면서, 갈라짐이 발생하지 않는 샘플의 코팅성이 가장 우수하다는 점에서, 실시예 2의 샘플이 가장 우수함을 확인할 수 있었다. 특히, As shown in Table 2, it was confirmed that the sample of Example 2 was the best in that the coating property of the sample with the thinnest coating thickness and no cracking was the best. Especially,
<실험예 2> 접촉각 및 접촉이력각 평가<Experimental Example 2> Evaluation of contact angle and contact hysteresis angle
물(정제수) 및 오일(식용유)을 시료로 하여, 접촉각 및 접촉이력각을 평가하였고, 그 결과를 도 1 내지 4에 나타내었으며, 도 1 내지 4의 결과를 요약하여 하기 표 3에 나타내었다. 비교예 1은 알루미늄 5052 합금에 아무런 처리를 하지 않음 샘플이다.Using water (purified water) and oil (edible oil) as samples, the contact angle and contact hysteresis angle were evaluated, and the results are shown in FIGS. 1 to 4, and the results of FIGS. 1 to 4 are summarized in Table 3 below. Comparative Example 1 is a sample of aluminum 5052 alloy without any treatment.
참조로, 발수성/발유성 평가에 있어서 접촉이력각이 낮을수록 발수성/발유성이 우수하다 할 수 있다.For reference, in water/oil repellency evaluation, it can be said that the lower the contact hysteresis angle, the better the water/oil repellency.
(Al 5052 합금)Comparative Example 1
(Al 5052 alloy)
표 3에 나타난 바와 같이, 실시예 2의 접촉이력각이 가장 낮게 나타남을 확인할 수 있었다. 특히, 실시예 2의 오일에 대한 접촉이력각이 유의미하게 낮게 나타났다.As shown in Table 3, it was confirmed that the contact hysteresis angle of Example 2 was the lowest. In particular, the contact hysteresis angle for the oil of Example 2 was significantly lower.
<실험예 3> 플라즈마 처리 여부에 따른 접촉이력각 평가<Experimental Example 3> Evaluation of contact hysteresis angle according to plasma treatment
실시예 2와 플라즈마 처리를 하지 않은 것을 제외하고는 동일한 샘플(비교예 2)의 접촉이력각을 평가하였다.The contact hysteresis angle of the same sample (Comparative Example 2) was evaluated except that Example 2 and plasma treatment were not performed.
표 4에 나타난 바와 같이, 플라즈마 전처리를 실시한 실시예 2가 비교예 2 대비 접촉이력각지 낮게 나타나 발유성 및 발수성이 우수함을 확인할 수 있었다.As shown in Table 4, Example 2, which was subjected to plasma pretreatment, showed a lower contact history than Comparative Example 2, confirming that oil repellency and water repellency were excellent.
이제까지 본 발명에 대하여 그 바람직한 실시예들을 중심으로 살펴보았다. 본 발명이 속하는 기술 분야에서 통상의 지식을 가진 자는 본 발명이 본 발명의 본질적인 특성에서 벗어나지 않는 범위에서 변형된 형태로 구현될 수 있음을 이해할 수 있을 것이다. 그러므로 개시된 실시예들은 한정적인 관점이 아니라 설명적인 관점에서 고려되어야 한다. 본 발명의 범위는 전술한 설명이 아니라 특히 청구범위에 나타나 있으며, 그와 동등한 범위 내에 있는 모든 차이점은 본 발명에 포함된 것으로 해석되어야 할 것이다.So far, the present invention has been looked at with respect to its preferred embodiments. Those of ordinary skill in the art to which the present invention pertains will understand that the present invention can be implemented in a modified form without departing from the essential characteristics of the present invention. Therefore, the disclosed embodiments should be considered from an illustrative rather than a limiting point of view. The scope of the present invention is particularly indicated in the claims rather than the foregoing description, and all differences within the equivalent range should be construed as being included in the present invention.
Claims (17)
(단계 2) 열처리를 통한 기재 표면의 불순물을 제거하는 단계;
(단계 3) 기재 표면에 하기 화학식 1로 표시되는 가교형 PDMS(Polydimethylsiloxane) 유도체를 코팅하는 단계; 및
(단계 4) 열처리를 통해 경화시키는 단계;를 포함하는,
기재 표면에 발유성 및 발수성을 부여하는 방법.
[화학식 1]
(상기 화학식 1에서, x 및 y는 각각 1-10의 정수이다.)
(Step 1) Plasma treatment of the substrate to improve wettability by generating -OH functional groups on the surface;
(Step 2) removing impurities on the surface of the substrate through heat treatment;
(Step 3) coating a cross-linked polydimethylsiloxane (PDMS) derivative represented by Chemical Formula 1 on the surface of the substrate; and
(Step 4) curing through heat treatment; including,
A method for imparting oil repellency and water repellency to the surface of a substrate.
[Formula 1]
(In Formula 1, x and y are each an integer of 1-10.)
상기 단계 1의 플라즈마 처리는 180-220W, 40-60kHz 및 40-60 sccm의 O2 조건으로 실시하는 것을 특징으로 하는, 기재 표면에 발유성 및 발수성을 부여하는 방법.
According to claim 1,
Plasma treatment in step 1 is performed under O 2 conditions of 180-220 W, 40-60 kHz and 40-60 sccm, characterized in that, a method for imparting oil and water repellency to the surface of the substrate.
상기 단계 2의 열처리는 120-300 ℃에서 3-60분 동안 실시하는 것을 특징으로 하는, 기재 표면에 발유성 및 발수성을 부여하는 방법.
According to claim 1,
The heat treatment in step 2 is performed at 120-300 ° C. for 3-60 minutes.
상기 단계 3의 코팅은 스핀코팅법을 사용하는 것을 특징으로 하는, 기재 표면에 발유성 및 발수성을 부여하는 방법.
According to claim 1,
The method of imparting oil repellency and water repellency to the surface of the substrate, characterized in that the coating in step 3 uses a spin coating method.
상기 단계 4의 열처리는 250-350℃에서 10-60분 동안 실시하는 것을 특징으로 하는, 기재 표면에 발유성 및 발수성을 부여하는 방법.
According to claim 1,
Characterized in that the heat treatment of step 4 is performed at 250-350 ° C. for 10-60 minutes, a method for imparting oil and water repellency to the surface of the substrate.
상기 기재는,
알루미늄, 알루미늄 합금, 타이타늄, 타이타늄 합금, 마그네슘, 마그네슘 합금, 스테인리스강, 철강, 귀금속, 희귀금속, 비결정성 금속, 알카리 금속, 알카리 토금속, 중금속, 합금 및 초합금 중 1종의 금속; 플라스틱; 또는 유리인 것을 특징으로 하는, 기재 표면에 발유성 및 발수성을 부여하는 방법.
According to claim 1,
The above description is
aluminum, aluminum alloys, titanium, titanium alloys, magnesium, magnesium alloys, stainless steel, steel, precious metals, rare metals, amorphous metals, alkali metals, alkaline earth metals, heavy metals, alloys, and superalloys; plastic; or a method for imparting oil repellency and water repellency to the surface of a substrate, characterized in that it is glass.
상기 기재는 알루미늄 합금인 것을 특징으로 하는, 기재 표면에 발유성 및 발수성을 부여하는 방법.
According to claim 6,
The method of imparting oil repellency and water repellency to the surface of the substrate, characterized in that the substrate is an aluminum alloy.
A substrate having oil repellency and water repellency imparted to the surface prepared by the method of claim 1.
An oil vapor recovery device comprising the substrate of claim 10.
An oil vapor recovery facility comprising the description of claim 10.
A pipe comprising the substrate of claim 10 .
A hood comprising the substrate of claim 10.
A part of a hood comprising the substrate of claim 10.
A conduit comprising the description of claim 10.
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| KR1020210012169A KR102486060B1 (en) | 2021-01-28 | 2021-01-28 | Method for the implementation of water-repellent and oil-repellent surfaces using crosslinking type PDMS |
| PCT/KR2022/001198 WO2022164147A1 (en) | 2021-01-28 | 2022-01-24 | Method for making hydrophobic and oleophobic surface by using crosslinking pdms |
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| JP2013514841A (en) * | 2009-12-21 | 2013-05-02 | イノベイティブ サーフェイス テクノロジーズ， インコーポレイテッド | Coating agents and coated articles |
| KR102127500B1 (en) * | 2019-07-10 | 2020-06-26 | 중앙대학교 산학협력단 | Master mold manufacturing method for polydimethylsiloxane double casting using plasma and alchol treatment and master mold for polydimethylsiloxane double casting using the same |
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| KR101786951B1 (en) * | 2010-04-23 | 2017-10-19 | 삼성전자주식회사 | Super-hydrorepellent composition, super-hydrorepellent coating layer including a cured product of the composition, and heat exchanger including the super-hydrorepellent coating layer |
| KR101317459B1 (en) * | 2011-12-23 | 2013-10-18 | 한국과학기술원 | Method for Optical Visualizing of Graphene Domains |
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| KR20150008633A (en) * | 2013-07-15 | 2015-01-23 | 한국생산기술연구원 | The method of surface modification for polymeric substance using atmospheric plasma and the surface modified articles |
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| JP2013514841A (en) * | 2009-12-21 | 2013-05-02 | イノベイティブ サーフェイス テクノロジーズ， インコーポレイテッド | Coating agents and coated articles |
| KR102127500B1 (en) * | 2019-07-10 | 2020-06-26 | 중앙대학교 산학협력단 | Master mold manufacturing method for polydimethylsiloxane double casting using plasma and alchol treatment and master mold for polydimethylsiloxane double casting using the same |
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