KR101817679B1 - Fabrics with super water-repellent function including fluorocarbon thin film and Method of Manufacturing The Same - Google Patents
Fabrics with super water-repellent function including fluorocarbon thin film and Method of Manufacturing The Same Download PDFInfo
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- KR101817679B1 KR101817679B1 KR1020150182969A KR20150182969A KR101817679B1 KR 101817679 B1 KR101817679 B1 KR 101817679B1 KR 1020150182969 A KR1020150182969 A KR 1020150182969A KR 20150182969 A KR20150182969 A KR 20150182969A KR 101817679 B1 KR101817679 B1 KR 101817679B1
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- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
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- D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
- D06M15/277—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof containing fluorine
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- D06B1/10—Applying liquids, gases or vapours onto textile materials to effect treatment, e.g. washing, dyeing, bleaching, sizing or impregnating by contact with a member carrying the treating material
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Abstract
The present invention relates to a super-water-repellent coating fiber comprising a fluorocarbon thin film excellent in water repellency against moisture and a method of manufacturing the same. More specifically, the present invention relates to a super- To a super-water-repellent coating fiber coated with a sputtering method regardless of an output voltage so as to have a super water-repellent property on the surface of the fabric, and a method for producing the same.
Description
The present invention relates to a super-water-repellent coating fiber comprising a fluorocarbon thin film improved in water resistance to moisture and a method for producing the same.
Recently, considerable attention has been focused on processes for treating textile materials to obtain environmentally sustainable functional products. These functional fiber materials are new materials with various advanced technologies such as IT, BT and NT. They can be applied not only to clothing but also to industries such as automobile, electronics, aerospace, medical and military industries. In many applications, in particular, textile materials used for clothing and packaging materials are required to have hydrophobic and self-cleaning properties, and in order to meet the needs of the consumer, a high- Research on the development of textile materials has been actively conducted.
Such a super-water-repellent fiber material can be realized by a method such as coating a fluorine-based resin or a silicone resin on the surface of a fiber through a wet or dry process to repel the fiber or laminating a membrane having a super water-repellent property on the fiber have. However, the water-repellent processing of the fiber surface through the wet or dry process causes various environmental problems due to a large amount of water and chemicals used in the process, and the polymer resin is coated on the surface of the fabric in a thickness of several tens of micrometers The inherent tactile sensation and color of the fibers are lowered, and the adhesion of the coated polymer resin and the fibers is limited, so that the water repellency during washing is lowered. In addition, in order to realize ultra-hydrophobic surface, various chemical companies have developed a super water-repellent agent applied to fibers, but they have limitations in the durability or super-hydrophobic properties in treatment of fibers.
Specifically, Patent Document 1 discloses a porous polytetrafluoroethylene membrane having waterproofness and moisture permeability. This is because the raw material particles of the raw raw material form a three-dimensional matrix or a lattice structure in which a fibrous fibril is connected. In this case, there are many fine voids, and water permeability and water vapor permeability It also has a moisture permeability as much as possible. Similarly, Patent Document 2 also discloses a porous polyurethane film as a thin film having both waterproof property and moisture permeability. However, such porous polytetrafluoroethylene membranes and porous polyurethane membranes tend to be deformed by an external force, and once they are deformed, they do not return to their original positions. When the size of the pore of the membrane becomes large due to such deformation, or when the pore breaks, the waterproof property remarkably decreases.
In order to solve the problems of the prior art as described above, the present applicant has conducted in-depth research in order to meet the need in the art, and as a result, it has been found that sputtering with a nano-sized thickness Supercooled coated fiber containing a fluorocarbon thin film was devised. In addition, it is possible to deposit at a high deposition rate by DC or MF sputtering in addition to solving the problems of conventional fluorocarbon thin film deposition, which had to be applied with high energy, and to make a super large water repellent coated fiber using a continuous roll to roll deposition system By developing a new technique, the present invention has been completed.
It is an object of the present invention to provide a super water-repellent coated fiber which can remarkably improve not only an external contaminant but also water resistance to moisture by including a fluorocarbon thin film having super water repellency and high insulation. The super-water-repellent coating fiber according to the present invention can exhibit excellent transparency and flexibility, and can impart excellent flame retardancy, self-cleaning properties and mechanical properties.
Still another object of the present invention is to provide a method for producing a super-water-repellent coated fiber comprising a fluorocarbon thin film deposited at a high deposition rate using MF or a DC power source method at a lower voltage by using a fluorine-based polymer composite target having conductivity will be.
The present invention can be modified into a super water repellent surface regardless of the kind of the fabric by a single process and remarkably improves the adhesion between the fluorocarbon thin film and the fiber fabric to reduce deterioration of the super water- . In addition, the present invention is capable of easily controlling the thickness of a thin film having a super water-repellent property on a textile fabric through sputtering using a more industrially useful power supply system such as MF or DC, It is possible to provide various types of textile fabrics by being able to realize conductivity, heat radiation, thermal insulation, antifouling, flame retardance, antibacterial, electromagnetic shielding and improved appearance characteristics.
The present invention provides a method for producing an ultra water-repellent coated fiber comprising a step of sputtering and depositing a water repellent agent layer containing a fluorinated polymer and a functionalizing agent having conductivity on a fiber fabric. At this time, the functionalizing agent may be one or more selected from the group consisting of conductive particles, conductive polymers and metal components, but is not limited thereto.
The water repellent layer according to an exemplary embodiment of the present invention may be formed by sputtering using RF, MF, or DC power. Since the water-repellent layer uses a fluorine-based polymer composite target containing a functionalizing agent, damage to the deposition target due to deterioration phenomenon, which is a problem caused by application of high energy when the fluorine-based polymer is deposited, It is possible to effectively improve the deposition rate due to the generation of plasma with a lower efficiency than the applied voltage due to the generation of an arc or the like between the conductive particles and the conductive particles, , It can be effectively deposited on the textile fabric with a high deposition rate even with commercially useful MF or DC sputtering.
The water repellent layer according to an embodiment of the present invention is not limited as long as it can suppress the permeation of water, but it does not deteriorate adhesion to the fabric, and can improve heat resistance, flame resistance, antibacterial property, It may further include a metal compound in the water repellent agent layer having conductivity. At this time, the metal compound includes at least one selected from the group consisting of silicon oxide, aluminum oxide, and silicon nitride as a main component, and at least one selected from the group consisting of Ti, Zr, Hf, Nb, Ta, And at least one oxide or nitride selected from vanadium (V), tungsten (W), aluminum (Al), gallium (Ga), indium (In), zinc (Zn) and germanium (Ge)
The present invention also relates to a method for producing an ultra-water-repellent coating fiber, comprising the step of forming a water repellent agent layer using a fluoropolymer composite target comprising a conductive particle, a conductive polymer and at least one functional agent selected from metal components on a fiber fabric .
Forming an inorganic layer using a metal target, a metal oxide target or a metal nitride target prior to the step of forming the water repellent layer; And forming an organic layer using a fluorine-based polymer composite target comprising a fluorine-based polymer and at least one conductive material selected from conductive particles, conductive polymers, and metal components; and at least one step selected from the group consisting of And a manufacturing method thereof. The inorganic layer and the organic layer may be formed by MF or DC sputtering, which is a power supply type having a frequency of a frequency of several tens of KHz or less, which is lower than RF, and they can be applied to a continuous roll-to-roll type sputtering deposition system So that the super water-repellent coated fiber can be economically large-sized.
The inorganic layer according to an embodiment of the present invention can be formed at a high deposition rate using a metal target, a metal oxide target, or a metal nitride target, and can improve the adhesion to a fabric. The metal target may be at least one selected from the group consisting of titanium, zirconium, hafnium, niobium, tantalum, vanadium, tungsten, aluminum, gallium ), Indium (In), zinc (Zn), silicon (Si), germanium (Ge), and the like, and is oxidized by a reaction gas to be deposited as a metal oxide or a metal nitride thin film.
At this time, the reactant gas is nitrous oxide (N 2 0), nitrogen dioxide (N0 2), nitrogen monoxide (NO) and can have one or more selected from oxygen (O 2), preferably nitrogen dioxide (N0 2), oxygen ( O 2 ) or a mixed reaction gas thereof.
The organic layer according to an embodiment of the present invention includes a fluorine-based polymer and a conductive material capable of imparting conductivity. The conductive material may be a conductive particle, a conductive polymer, a metal component, or the like, and is not limited as long as it is a material capable of imparting conductivity. The conductive particles may be at least one selected from the group consisting of carbon nanotubes, carbon nanofibers, carbon black, graphene, graphite, and carbon fibers. Non-limiting examples of the conductive polymer Examples include polyaniline, polyacetylene, polythiophene, polypyrrole, polyfluorene, polypyrene, polyazulene, polynaphthalene, Polyphenylene, polyphenylene vinylene, polycarbazole, polyindole, polyazaphine, polyethylene, polyethylene vinylene, and the like. , Polyphenylene sulfide, polyfuran, polyselenophene, polytellurophene, and the like. The term " polyphenylene sulfide " And at least one metal selected from the group consisting of Cu, Al, Ag, Si, Au, W, Mg, Ni, Mo, V, Nb, Ti, Pt, have.
The fluorinated polymer composite target according to an embodiment of the present invention may further include at least one metal compound selected from metal organic compounds, metal oxides, metal carbon materials, metal hydroxides, metal carbonates, metal bicarbonates, metal nitrides and metal fluorides The metal compound may be, for example, SiO 2 , Al 2 O 3 , ITO, IGZO, ZnO, In 2 O 3 , SnO 2 , TiO 2 , AZO, ATO, SrTiO 3 , CeO 2 , MgO, NiO, CaO, ZrO 2 , Y 2 O 3 , Al 2 O 3 , MgF 2 , CuF 2, Si 3 N 4 , CuN, Nb 2 O 5 , V 2 O 5 , AlN, and the like, but is not limited thereto.
In the method for producing super-water-repellent coated fiber according to an embodiment of the present invention, the water-repellent layer may be repeatedly deposited one or more times. In order to remarkably improve the adhesion to the fabric, Or a water repellent agent layer may be formed after the inorganic layer and the organic layer are sequentially formed.
In the method of manufacturing the super-water-repellent coated fiber according to an embodiment of the present invention, the fiber fabric may be made of polyvinyl alcohol, polyacrylonitrile, nylon, polyester, polyurethane, polyvinyl chloride, polystyrene, , One made of one or more yarns selected from silk, cotton yarn, polylactic acid, polylactic-co-glycolic acid, polyglycolic acid polycaprolactone, collagen, polypyrrole, polyaniline and poly (styrene-co-maleic anhydride) . Also, natural parasites; Synthetic pigments synthesized by adding a resin such as PU or PVC to a fiber bubble having a relatively simple structure such as woven fabric, knitted fabric and nonwoven fabric; (Detergent, lactose, disinfectant, etc.), maximizing the water repellency and anti-fouling properties, and can be applied to polyimide multifilaments, glass fibers or the like High-strength fabrics made of high-strength yarns such as carbon fibers can be used to improve water repellency after friction as well as early water repellency and effectively prevent the wrinkles of the fiber fabric generated during the water repellent treatment.
Also, the present invention provides an super-water-repellent coating fiber produced by the above-described method. The water-repellent coating fiber according to the present invention imparts super water-repellency to the surface of the fiber fabric using the fluoropolymer composite target and further imparts special functions such as antibacterial, anti-fouling, flame retardant and electromagnetic shielding, .
The present invention provides a high-performance super-water-repellent coating fiber imparted with special functions such as excellent hydrophobic properties, flame retardancy, flame retardancy, self-cleaning properties, water repellency, mechanical properties, antibacterial properties and electromagnetic shielding properties on the surface of fiber fabric .
The method of manufacturing the super-water-repellent coated fiber according to the present invention is a method of maximizing productivity by directly coating a water repellent agent layer (fluorocarbon thin film) on the surface of a textile fabric in a single process without using harmful chemicals such as organic solvents And can minimize the generation of contaminants that can occur in the process. Further, the super-water-repellent coating fiber according to the present invention maximizes the adhesion between the fiber fabric and the water-repellent layer by introducing an inorganic layer using a metal target, a metal oxide target or a metal nitride target, .
The present invention relates to a fluorine-based polymer composite target that can be sputtered in MF or DC, which is lower in voltage than RF, by using a conductive fluorine-based polymer composite target, to prevent dielectric breakdown, Water-repellent coating fiber including a water-repellent layer of a water-repellent agent can be provided. In addition, adhesion of the water-repellent coating layer to the fabric can be remarkably improved.
In addition, the method of producing super-water-repellent coated fiber according to the present invention can be applied to a conventional roll-to-roll method capable of producing a large area without any additional modification cost, Multilayer super water-repellent coating fiber including a layer, an organic layer, and the like can be simultaneously produced in-line, thereby optimizing the process efficiency.
Fig. 1 shows XPS analysis results of the water-repellent layer of the super-water-repellent coating fiber prepared by the method of Example 5. Fig.
The super-water-repellent coated fiber including the fluorocarbon thin film according to the present invention and the method of manufacturing the same are described below. However, unless otherwise defined in the technical terms and scientific terms used herein, the ordinary knowledge in the technical field A description of known functions and configurations that may unnecessarily obscure the gist of the present invention will be omitted in the following description.
The term " water repellent agent layer " of the present invention means a fluorocarbon thin film containing a fluorinated polymer and at least one functionalizing agent, and can be interpreted to have the same meaning as the fluorocarbon thin film unless otherwise specified.
The term " waterproof " of the present invention means a property that water does not permeate, and can be interpreted in the same sense as water repellency. In general, when the contact angle is 110 ° or more, the fabric is evaluated as a water-repellent fiber fabric, and when the contact angle is 140 °, the fabric is evaluated as a water-repellent fabric.
In recent years, interest in cool biz or cool clothing has increased as a result of global efforts to reduce energy consumption. As functional apparel used mainly in sports outdoor activities has become popular, consumers are expected to use functional materials Is increasing. Such comfort and functionality include breathability, moisture fastness, lightweight, antifouling, antibacterial and deodorizing properties. Among these functions, functions related to sweat and moisture have recently attracted particular attention.
Therefore, the present applicant has found that a fluorocarbon thin film excellent in transparency and excellent in adhesion to a fabric can be applied to a fiber fabric by a sputtering method so that the surface of the fabric can be super-water-repellent without adversely affecting the hygroscopicity, Water-repellent coated fiber which can effectively give a water-repellent coating fiber.
The super-water-repellent coating fiber according to the present invention can be produced by sputtering a water repellent layer containing a fluorine-based polymer and a functionalizing agent having conductivity on a fiber fabric. At this time, the water-repellent layer may be sputtered by RF or a DC or DC power source, which is an applied voltage lower than RF.
The water repellent layer according to an exemplary embodiment of the present invention is sputtered using a fluoropolymer composite target comprising a fluoropolymer and at least one functionalizing agent selected from conductive particles, conductive polymers, metal components, etc., and the fluoropolymer composite target is sputtered using a voltage The fluorine-based polymer composite target has a remarkable effect that the fluorine-based polymer composite target does not undergo deformation even when high energy is applied. In addition, the power source such as MF (mid-range frequency) and DC (direct current) can easily deposit by the role of the functionalizing agent and also remarkably increase the deposition efficiency.
The fluorine-based polymer composite target according to an exemplary embodiment of the present invention includes a functionalizing agent having conductivity, so that sputtering is possible not only in MF or DC which are lower in voltage than RF, but also in a high deposition rate have. Also, the water repellent agent layer includes a functionalizing agent having conductivity, so that it is possible to realize excellent adhesion to a backing plate of a target and a fiber fabric as an adherend.
Such a conductive functionalizing agent may be at least one selected from conductive particles, conductive polymers, metal components, and the like. Here, the conductive particles include, but are not limited to, carbon nanotubes (carbon nanotubes), carbon nanofibers, And may be at least one selected from carbon black, graphene, graphite, carbon fiber, and the like, and may include other organic conductive particles. At this time, when the organic conductive particles, which are an example of the conductive particles, are used, the conductivity can be imparted while maintaining the fluorocarbon component. Non-limiting examples of the conductive polymer include polyaniline, polyacetylene, polythiophene, polypyrrole, polyfluorene, polypyrene, polyazulene, polyazulene, polynaphthalene, polyphenylene, polyphenylene vinylene, polycarbazole, polyindole, polyazepine, polyethylene, and the like. Polyethylene vinylene, polyphenylene sulfide, polyfuran, polyselenophene, polytellurophene, polytetrafluoroethylene, polyphenylene sulfide, And the like, but the present invention is not limited thereto. The non-limiting examples of the metal component include copper (Cu), aluminum (Al), silver (Ag), silicon (Si), gold (Au), tungsten (W), magnesium (Mg) ), Molybdenum (Mo), vanadium (V), niobium (Nb), titanium (Ti), platinum (Pt), chromium (Cr), tantalum (Al), silver (Ag), silicon (Si), gold (Au), tungsten (W), magnesium (Mg), and the like are preferably used in view of good adhesion with the metal electrode. Nickel (Ni) or a mixture thereof, more preferably copper (Cu), aluminum (Al), silver (Ag), silicon (Si), gold (Au) or a mixture thereof.
The fluoropolymer contained in the fluoropolymer composite target according to an embodiment of the present invention is not particularly limited as long as it is a fluorine-containing resin, but it is preferably a fluorine-containing olefin polymerized with polytetrafluoroethylene (PTFE, polytetrafluoroethylene), polychlorotrifluoroethylene (PCTFE), polyvinylidenedifluoride (PVDF), fluorinated ethylene propylene copolymer (FEP), polyethylene-tetrafluoroethylene (Ethylene-co-tetrafluoroethylene), ethylene-co-chloro trifluoroethylene (ECTFE), polytetrafluoroethylene-fluoroalkyl vinyl ether (PFA, poly tetra fluoro ethylene-co-fluoro alkyl vinyl ether), and the like; At least one fluorine rubber selected from vinyl fluoride homopolymer rubber, vinyl fluoride copolymer rubber, vinylidene fluoride homopolymer rubber and vinylidene fluoride copolymer rubber, and the like; , And more preferably polytetrafluoroethylene (PTFE), but is not limited thereto.
The super-water-repellent coating fiber according to an embodiment of the present invention is excellent in durability including a water-repellent layer deposited with excellent bonding strength. Particularly, such super-water-repellent characteristics do not deteriorate water repellency even after washing several times, It is good to be able to maintain water repellency for a long time regardless.
Also, since the water repellent layer has high transparency, it can be applied not only to fiber fabrics of various colors, but also to various functionalizing agents because it does not impair the inherent characteristics such as the feel and color of the textile fabric. .
The super-water-repellent coating fiber according to an exemplary embodiment of the present invention may be made of polyvinyl alcohol, polyacrylonitrile, nylon, polyester, polyurethane, polyvinyl chloride, polystyrene, cellulose, chitosan, silk, cotton yarn, polylactic acid, And may be one made of one or more yarns selected from polylactic-co-glycolic acid, polyglycolic acid polycaprolactone, collagen, polypyrrole, polyaniline and poly (styrene-co-maleic anhydride) , Polyacrylonitrile, nylon, polyester, polyurethane, polyvinyl chloride, and the like, and more preferably one made of one or more yarns selected from nylon, polyester, polyurethane and the like It is good.
Further, the present invention relates to a natural parasite; Synthetic pigments synthesized by adding a resin such as PU or PVC to a fiber bubble having a relatively simple structure such as woven fabric, knitted fabric and nonwoven fabric; (Detergent, lactose, disinfectant, etc.), maximizing the water repellency and anti-fouling properties, and can be applied to polyimide multifilaments, glass fibers or the like High-strength fabrics made of high-strength yarns such as carbon fibers can be used to improve water repellency after friction as well as early water repellency and effectively prevent the wrinkles of the fiber fabric generated during the water repellent treatment.
At this time, there is no particular limitation on the diameter and length of the yarn, but the diameter may be between 1 and 100 mu m, preferably between 5 and 20 mu m, and the length is usually 500 mu m to 10 cm, Mu] m to 5 cm.
The present invention can uniformly sputter a water repellent layer containing a fluorinated polymer on a fiber surface in a nano-sized thickness and modify the surface of the fabric to have super-water repellency regardless of the kind of the fabric by a single process , The adhesion of the water repellent layer to the fabric is remarkably improved, and the super water repellency can be maintained for a long time regardless of whether or not the fabric is washed.
In addition, the present invention can provide a highly functional coated fiber having special functions such as antifouling property, antimicrobial property, deodorizing property, flame retardancy, electromagnetic shielding property as well as super water repellent property by further including various metals or ceramics in the water repellent agent layer.
The ceramic may be ceramic fine particles such as pegmatite, bentonite and the like which emit far-infrared rays. The fine particles may have an average diameter of 0.01 to 10 μm, And preferably 0.01 to 3 mu m. The pegmatite is generally composed of quartz, quartz and alumite, which are composed of quartz, silicate, puddite, albaite and the like. Bentonite is a clay mainly containing montmorillonite, which is a mineral belonging to monoclinic having a crystal structure such as mica, and is composed of quartz, feldspar, zeolite, etc. emitting far-infrared rays. It may be included.
The present invention also includes a step of forming a water repellent layer using a fluorinated polymer composite target comprising at least one functionalizing agent selected from conductive particles, conductive polymers and metal components on a textile fabric, DC sputtering to form a super-water-repellent coating fiber.
The fluorine-based polymer composite target according to the present invention includes at least one conductive material selected from conductive particles, conductive polymers, and metal components capable of imparting conductivity, and is capable of stably forming a plasma, A high deposition rate can be realized even by using the power supply method. At this time, the fluorine-based polymer composite target may further include a metal compound in at least one conductive material selected from the conductive material to realize improved durability (particularly, washability).
The metal compound may be at least one selected from metal organic compounds, metal oxides, metal carbon materials, metal hydroxides, metal carbonates, metal bicarbonates, metal nitrides and metal fluorides, For example, SiO 2 , Al 2 O 3 , ITO, IGZO, ZnO, In 2 O 3 , SnO 2 , TiO 2 , AZO, ATO, SrTiO 3 , CeO 2 , MgO, NiO, CaO, ZrO 2 , Y 2 O 3 , Al 2 O 3 , MgF 2 , CuF 2 , Si 3 N 4 , CuN, Nb 2 O 5 , V 2 O 5 , AlN, and the like, but is not limited thereto.
The fluorocarbon polymer composite target according to the present invention may contain 0.01 to 2000 parts by weight of the functionalizing agent per 100 parts by weight of the fluoropolymer, although it is not limited, and a higher deposition rate and insulation breakage are prevented, Preferably from 0.5 to 1500 parts by weight, more preferably from 1 to 1000 parts by weight, from the viewpoint of the ability to deposit a fluoride thin film (fluorocarbon thin film).
In addition, the super-water-repellent coating fiber according to an embodiment of the present invention may be formed by forming a water repellent layer using a fluoropolymer composite target comprising a fiber fabric and at least one functionalizing agent selected from conductive particles, conductive polymers, metal components, Wherein the water repellent layer may be formed by depositing by MF or DC sputtering.
Forming an inorganic layer using a metal target, a metal oxide target or a metal nitride target prior to the step of forming the water repellent layer; Forming an organic layer using a fluorine-based polymer composite target comprising a fluorine-based polymer and at least one conductive material selected from conductive particles, conductive polymers, and metal components; Wherein the water-repellent coated fiber further comprises at least one selected from the following. The inorganic layer and the organic layer may be formed by MF or DC sputtering, which is a power supply type having a frequency of a frequency of several tens of KHz or less, which is lower than RF, and they can be applied to a continuous roll-to-roll type sputtering deposition system Water-repellent coating fiber can be economically large-sized, and additionally an organic layer, an inorganic layer and the like can be additionally provided, so that the adhesion of the fiber fabric and the water repellent layer can be remarkably improved.
The manufacturing method according to an embodiment of the present invention is capable of sputtering the water repellent layer, the inorganic layer, and the organic layer at a lower energy band than RF, and is applicable to a continuous roll-to-roll type sputtering deposition system, It is possible to produce super-water-repellent coated fiber of the area, and the production speed can be shortened, thereby further improving the work efficiency.
The fiber fabric according to an embodiment of the present invention is not limited when applied to a roll-to-roll type sputtering deposition system, but is transported at a speed of 0.1 m / min to 20 m / min, preferably 0.5 m / min to 5 m / min. < / RTI >
In addition, the method of producing super-water-repellent coated fiber according to the present invention can realize an excellent deposition rate even at a low energy band such as commercially available MF or DC, and can be applied directly without supplementing the existing roll-to-roll type sputter deposition system Water repellent layer, an organic layer, an inorganic layer and the like can be formed at the same time quickly without defects, and thus the super water-repellent coating fiber can be economically provided.
At this time, the inorganic layer may be formed of at least one selected from the group consisting of Ti, Zr, Hf, Nb, Ta, V, W, ), Indium (In), zinc (Zn), silicon (Si) and germanium (Ge), or an oxide or nitride of the above metal. At this time, when the metal is used as a target, the metal may be oxidized by a reaction gas to form an inorganic layer containing a metal oxide or a metal nitride.
Reaction gas in accordance with one embodiment of the present invention are selected from but are not limited so long as it can oxidize the metal nitrous oxide (N 2 0), nitrogen dioxide (N0 2), nitrogen monoxide (NO) and oxygen (O 2) (NO 2 ), oxygen (O 2 ), or a mixed reaction gas thereof, from the viewpoint of economical efficiency.
The water repellent layer, the inorganic layer, and the organic layer of the super-water-repellent coating fiber according to an exemplary embodiment of the present invention may be deposited to a thickness of 5 nm to 1 탆, though not limited thereto. In view of lower permeability to water , It can be deposited to a thickness of 10 nm to 200 nm, and the adhesion to the fabric can be improved as compared with the case where the inorganic layer, the organic layer and the water-repellent layer have a multi-layer structure in this order.
The super-water-repellent coating fiber according to an embodiment of the present invention is formed by repeating the step of forming an inorganic layer and the step of forming an organic layer two or more times in order, whereby the water repellent agent layer is removed from the fabric by deterioration, impact, Can be remarkably reduced.
The present invention provides a multifunctional super-water-repellent coated fiber produced by the above-described method. Preferably, the water repellent coating fiber according to the present invention may contain 0.01 to 50% by weight of the atomic weight of the metal atom based on 100% by weight of the total amount of the water-repellent layer.
In addition, the water-repellent layer of the super-water-repellent coating fiber according to an embodiment of the present invention further includes a metal compound in addition to the functionalizing agent having conductivity, thereby improving the electrical conductivity, heat radiation, Appearance, and the like, so that various types of textile fabrics can be provided. As a non-limiting example, the water repellent layer may be formed of Al 2 O 3 And metal components such as Ag may be included in order to impart excellent antibacterial properties, but the present invention is not limited thereto.
The super-water-repellent coating fiber according to the present invention may have a lower surface energy by introducing a super-hydrophobic water repellent layer (fluorocarbon thin film) at the outermost layer, and the contact angle with water may be in the range of 90 to 150 °, And preferably has a contact angle of 110 to 150 degrees, more preferably 140 degrees or more.
Hereinafter, the present invention will be described in more detail with reference to the following examples. However, these embodiments are provided to aid understanding of the present invention, and the scope of the present invention is not limited thereto in any sense.
(Example 1)
A cluster sputtering system was used to deposit the water repellent layer on a polyester (100 mm wide, 100 mm long, 0.1 mm thick) substrate by mid-range frequency (MF) sputtering. In the cluster sputtering apparatus, the substrate is composed of a loader section, a transporting module section for transporting the substrate, and a sputtering chamber section for depositing the thin film, and the sputtering chamber section is composed of a MF dual sputtering cathode.
(4 inches in diameter, 6 mm in thickness) made of a round PTFE (polytetrafluoroethylene, DuPont 7AJ) 85 wt% and graphite (Timcal, 40um) And attached to the electrode surface. This was installed in the MF dual sputtering cathode of the sputtering chamber part.
A polyester fiber cloth (100 mm in width and 100 mm in thickness, 0.1 mm in thickness) was attached to the substrate and the inside of the chamber was evacuated to a vacuum of 50 mtorr by a rotary pump, and then a cryo pump Thereby forming a high vacuum (5 x 10 < -5 > Torr). At this time, pre-sputtering was performed at an MF power of 100 W while injecting argon gas as a process gas at a flow rate of 50 sccm to remove contaminants. Thereafter, the water repellent layer was deposited for 30 minutes at MF power of 300 W, and the deposited polyester fiber fabric was taken out from the loader part to complete the fabrication of the super water repellent coating fiber.
In order to confirm the physical properties of the super-water-repellent coating fiber prepared by the above method, the contact angle and the film thickness were measured by the following methods, and the results are shown in Table 1.
1. Contact angle measurement
The water contact angle of the resulting super-water-repellent coating film was measured using a contact angle meter (
2. Thin film thickness measurement
In order to measure the thickness of the finished super-water-repellent coating film, the fiber substrate was cut and its cross-section was measured using a FE-SEM (Field Effect-Scanning Electron Microscope, Philips XL30S FEG) apparatus.
(Example 2)
A SPW-060 roll-to-roll sputter apparatus was used to deposit a water repellent layer (fluorocarbon thin film) on a nylon fiber fabric substrate by roll to roll sputtering. The SPW-060 roll-to-roll sputtering apparatus comprises an unwinder portion for loading a textile fabric, a process chamber portion for depositing a thin film on the textile fabric, and a winder portion for recharging the formed textile fabric And the process chamber portion is composed of three MF dual sputtering cathodes (cathodes 1 to 3) and one DC sputtering cathode (cathode 4) independently.
A fluoropolymer composite target (length 950 mm, width 127 mm, thickness 6 mm) made of a rectangular plate containing 90 wt% of powder PTFE (polytetrafluoroethylene, DuPont 7AJ) and 10 wt% of carbon nanotubes was placed on a copper backing plate plate electrode surface. This was installed in MF dual sputtering cathode 1 (cathode 1). Thereafter, a nylon fiber fabric (600 mm wide, 0.1 mm thick, 30 m long rolls) was loaded into the unwinder chamber and the inside of the roll-to-roll sputter device was vacuumed to 50 mtorr using a rotary pump and a booster pump vacuum was evacuated to a low vacuum state and then a high vacuum (2 × 10 -4 Pa) was formed using a turbo molecular pump. When the internal vacuum degree of the roll-to-roll sputtering apparatus was 2 × 10 -4 Pa or less, argon (Ar) gas was injected into the cathode at a flow rate of 400 sccm, and pre-sputtering was performed with MF power of 1 kW. Thereafter, while the temperature of the main roll was lowered to 10 ° C and the nylon fiber fabric was conveyed at a speed of 1 m / min, the MF power was set to 3 kW by using the MF dual sputtering cathode 1, And the deposited nylon fiber fabric was taken out from the winder part to complete the fabrication of the super water repellent coating fiber.
In order to confirm the physical properties of the super-water-repellent coating fiber prepared as described above, the contact angle and the thickness of the super-water-repellent coating film were measured in the same manner as in Example 1, and the results are shown in Table 1.
(Example 3)
A high purity Si (99.9%, Mitsui) Target (square plate, length 950 mm, width 127 mm, thickness 6 mm) was attached to the Cu backing plate electrode surface and this was attached to MF dual sputtering cathode 1 Respectively. A fluoropolymer composite target (length 950 mm, width 127 mm, thickness 6 mm) made of a rectangular plate containing 90 wt% of powder PTFE (polytetrafluoroethylene, DuPont 7AJ) and 10 wt% of carbon nanotubes was placed on a copper backing plate plate electrode surface. This was installed in MF dual sputtering cathode 2 (cathode 2). Thereafter, a nylon fiber fabric (600 mm wide, 0.1 mm thick, 30 m long rolls) was loaded into the unwinder chamber and the inside of the roll-to-roll sputter device was vacuumed to 50 mtorr using a rotary pump and a booster pump vacuum was evacuated to a low vacuum state and then a high vacuum (2 × 10 -4 Pa) was formed using a turbo molecular pump. When the internal vacuum degree of the roll-to-roll sputtering apparatus was 2 × 10 -4 Pa or lower, argon (Ar) gas was injected into each cathode at a flow rate of 400 sccm, and pre-sputtering was performed at MF power of 1 kW. Thereafter, while the temperature of the main roll was lowered to 10 캜 and the nylon fiber fabric was conveyed at a speed of 1 m / min, the MF power was set to 10 kW by the MF dual sputtering cathode 1, A silicon oxide (SiO 2 ) inorganic coating layer was deposited while the gas was injected in a PID controlled manner to maintain a sputtering voltage of 80%. Then, the water repellent agent layer was continuously deposited on the cathode 2 at an MF power of 3 kW, and the deposited nylon fiber fabric was taken out from the winder part to complete the fabrication of the super water repellent coating fiber.
In order to confirm the physical properties of the super-water-repellent coating fiber prepared by the above method, the contact angle and the thickness of the super-water-repellent coating film were measured in the same manner as in Example 1, and the results are shown in Table 1.
(Example 4)
A fluoropolymer composite target (length 950 mm, width 127 mm, thickness 6 mm) made of a rectangular plate containing 85 wt% of PTFE (polytetrafluoroethylene, DuPont 7AJ) and 15 wt% of carbon nanotubes was placed on a copper backing plate plate electrode surface. This was installed in a DC (direct current) single sputtering cathode 4 (cathode 4). Thereafter, a nylon fiber fabric (600 mm wide, 0.1 mm thick, 30 m long rolls) was loaded into the unwinder chamber and the inside of the roll-to-roll sputter device was vacuumed to 50 mtorr using a rotary pump and a booster pump vacuum was evacuated to a low vacuum state and then a high vacuum (2 × 10 -4 Pa) was formed using a turbo molecular pump. When the internal vacuum degree of the roll-to-roll sputtering apparatus was 2 × 10 -4 Pa or lower, argon (Ar) gas was injected into the cathode at a flow rate of 400 sccm, and DC power was pre-sputtered at 1 kW. Thereafter, the temperature of the main roll was lowered to 10 ° C, and the nylon fiber fabric was transported at a rate of 1 m / min while the dc power was set to 1 kW by the DC sputtering cathode 4 (cathode 4) And the deposited nylon fiber fabric was taken out from the winder part to complete the fabrication of the super water repellent coating fiber.
In order to confirm the physical properties of the super-water-repellent coating fiber prepared as described above, the contact angle and the thickness of the super-water-repellent coating film were measured in the same manner as in Example 1, and the results are shown in Table 1.
(Example 5)
A cluster sputtering system was used to deposit the water repellent layer on a polyester (100 mm wide, 100 mm long, 0.1 mm thick) substrate by mid-range frequency (MF) sputtering. In the cluster sputtering apparatus, the substrate is composed of a loader section, a transporting module section for transporting the substrate, and a sputtering chamber section for depositing the thin film, and the sputtering chamber section is composed of a MF dual sputtering cathode.
(4 inches in diameter, 6 mm in thickness) fabricated in a circular shape containing 65 wt% of PTFE (polytetrafluoroethylene, DuPont 7AJ), 5 wt% of carbon nanotubes and 30 wt% of Al 2 O 3 was coated on a copper backing plate Cu backing plate. This was installed in the MF dual sputtering cathode of the sputtering chamber part.
A polyester fiber cloth (100 mm in width and 100 mm in thickness, 0.1 mm in thickness) was attached to the substrate and the inside of the chamber was evacuated to a vacuum of 50 mtorr by a rotary pump, and then a cryo pump Thereby forming a high vacuum (5 x 10 < -5 > Torr). At this time, pre-sputtering was performed at an MF power of 100 W while injecting argon gas as a process gas at a flow rate of 50 sccm to remove contaminants. Thereafter, the water repellent layer was deposited for 30 minutes at MF power of 300 W, and the deposited polyester fiber fabric was taken out from the loader part to complete the fabrication of the super water repellent coating fiber.
In order to quantify the chemical bonding state and the chemical composition in the water-repellent layer of the super-water-repellent coating fiber prepared by the above-mentioned method, X-ray photoelectron spectroscopy (XPS) was performed using monochromatic Al- 800 [mu] m, small spot size: 10 [mu] m). An Al-Kα light source was used, and an accelerating voltage of 15 kV and an emission current of 10 mA were set to confirm the chemical bonding state and chemical composition in the water-repellent layer.
As a result, as shown in FIG. 1, as a result of the C1s spectrum of the water repellent agent layer, carbon-fluorine bonds and CC carbon-carbon bonds such as CF, CF 2 , CF 3 and CCF were observed. At this time, it was found that the carbon atoms (C) was 29.57 wt%, the fluorine atoms (F) were 59.02 wt%, and the aluminum atoms (Al) were 6.64 wt% based on 100 wt% of the total atoms in the water repellent layer.
The contact angle and the thickness of the coating film were measured in the same manner as in Example 1 to confirm the physical properties of the coated fiber produced by the above method, and the results are shown in Table 1.
(Comparative Example 1)
A roll-to-roll sputter (ULVAC, SPW-060) apparatus was used for the nylon fiber fabric, and a 100% PTFE target was used instead of the fluorinated polymer composite target in Example 2. At this time, in order to form the fluorocarbon thin film, the MF power was applied through the cathode 1 at 3 kW, but the plasma was not formed and deposition of the water repellent layer was impossible.
(Comparative Example 2)
A fluoropolymer composite target containing 90 wt% PTFE and 10 wt% SiO 2 was used instead of the fluoropolymer composite target in Example 2 using a roll-to-roll sputter (ULVAC, SPW-060) apparatus in a nylon fiber fabric. At this time, in order to form the fluorocarbon thin film, the MF power was applied through the cathode 1 at 3 kW, but the plasma was not formed and deposition of the water repellent layer was impossible.
(Comparative Example 3)
A nylon fiber fabric was intended to form only the inorganic layer according to Example 3 using a roll-to-roll sputter (ULVAC, SPW-060) device. At this time, coated fibers deposited under the atmosphere of oxygen (O 2 ) at an MF power of 10 kW through the cathode 2 were formed to form the inorganic layer.
The contact angle and the thickness of the coating film were measured in the same manner as in Example 1 to confirm the physical properties of the coated fiber produced by the above method. The results are shown in Table 1.
The present invention includes a fluorocarbon thin film (water repellent agent layer) uniformly deposited at a high deposition rate even with an MF or DC power source, which is different from a conventional fluorocarbon thin film in that it can be implemented regardless of an output voltage, Water-repellent coating fiber. Also, it can be seen that the super-water-repellent coating fiber has a high contact angle of 140 ° or more and has a relatively high deposition rate (see Table 1).
In addition, the method for producing super-water-repellent coated fiber according to the present invention is applicable not only to a conventional roll-to-roll equipment but also to a large-area thin film in a short time, It can contribute to the mass production of high functional fiber with high quality with simplified manufacturing process and reduced manufacturing cost by continuous process for fabric production.
That is, the present invention can provide a continuous process of imparting various functions to a textile fabric in a single machine, which can dramatically improve productivity and can replace existing processes using a large amount of water and chemicals, Minimizes problems, and has an advantage in energy saving.
Claims (12)
Wherein the conductive functionalizing agent is at least one selected from conductive particles, conductive polymers and metal components.
Wherein the water repellent agent layer further comprises a metal compound.
Wherein the conductive particles are at least one selected from carbon nanotubes, carbon nanofibers, carbon black, graphene, graphite, and carbon fibers.
The conductive polymer may be at least one selected from the group consisting of polyaniline, polyacetylene, polythiophene, polypyrrole, polyfluorene, polypyrene, polyazulene, polynaphthalene, polyphenylene, polyphenylene vinylene, polycarbazole, polyindole, polyazepine, Wherein at least one selected from the group consisting of polyethylene terephthalate, polyethylene terephthalate, polyethylene terephthalate, polyethylene terephthalate, polyethylene terephthalate, polyethylene vinylene, polyphenylene sulfide, polyfuran, polyselenophen,
Wherein the metal component is at least one selected from copper, aluminum, silver, gold, tungsten, magnesium, nickel, molybdenum, vanadium, niobium, titanium, platinum, chromium and tantalum.
Wherein the metal compound is at least one selected from metal organic materials, metal oxides, metal carbon materials, metal hydroxides, metal carbonates, metal bicarbonates, metal nitrides and metal fluorides.
The textile fabric may be selected from the group consisting of polyvinyl alcohol, polyacrylonitrile, nylon, polyester, polyurethane, polyvinyl chloride, polystyrene, cellulose, chitosan, silk, cotton yarn, polylactic acid, polylactic- Wherein the fabric is made of at least one yarn selected from polylactic acid, glycolic acid polycaprolactone, collagen, polypyrrole, polyaniline and poly (styrene-co-maleic anhydride).
Wherein the fiber fabric is transferred in a roll-to-roll fashion to deposit a water repellent layer.
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