KR20110131533A - Method for preparing transparent conductor comprising nanowire - Google Patents
Method for preparing transparent conductor comprising nanowire Download PDFInfo
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- KR20110131533A KR20110131533A KR1020100051010A KR20100051010A KR20110131533A KR 20110131533 A KR20110131533 A KR 20110131533A KR 1020100051010 A KR1020100051010 A KR 1020100051010A KR 20100051010 A KR20100051010 A KR 20100051010A KR 20110131533 A KR20110131533 A KR 20110131533A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/02—Single bars, rods, wires, or strips
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/06—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions
- H01L29/0657—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions characterised by the shape of the body
- H01L29/0665—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions characterised by the shape of the body the shape of the body defining a nanostructure
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022408—Electrodes for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/022425—Electrodes for devices characterised by at least one potential jump barrier or surface barrier for solar cells
Abstract
Description
본 발명은 투명 도전체의 제조방법에 관한 것으로서, 보다 구체적으로 나노와이어를 포함함으로써 전기적, 광학적, 기계적 특성 등이 우수한 투명 도전체 및 이의 제조방법에 관한 것이다.The present invention relates to a method for manufacturing a transparent conductor, and more particularly, to a transparent conductor having excellent electrical, optical, mechanical properties, and the like by including nanowires, and a method for manufacturing the same.
투명 도전체는 고투과율 절연 표면 또는 기판 상에 코팅된 얇은 도전막을 말한다. 투명 도전체는 적절한 광학적 투명성을 유지하면서 표면 도전성을 갖도록 제조될 수 있다. 그러한 표면 도전 투명 도전체는 평판 액정 표시 장치(flat liquid crystal display), 터치 패널(touch panel), 전자 발광 장치(electroluminescent device), 박막 광전지(thin film photovoltaic cell) 등에서 투명 전극들로서 널리 사용되고, 대전 방치층 및 전자기파 차폐층으로 널리 사용되고 있다.Transparent conductor refers to a thin conductive film coated on a high transmittance insulating surface or substrate. The transparent conductor can be made to have surface conductivity while maintaining proper optical transparency. Such surface conducting transparent conductors are widely used as transparent electrodes in flat liquid crystal displays, touch panels, electroluminescent devices, thin film photovoltaic cells, etc. It is widely used as a layer and an electromagnetic shielding layer.
현재, 인듐 주석 산화물(indium tin oxide, ITO)과 같은 진공 증착 금속 산화물(vacuum deposited metal oxide)은 글래스(glass)와 중합체 막(polymeric film)과 같은 유전체 표면들에 대해 광학적 투명성 및 전기적 도전성을 제공하기 위한 산업 표준 물질이다. 그러나, 금속 산화막은 약하고 휨이나 다른 물리적인 스트레스들에 의해 손상되기 쉽다. 또한, 이들은 높은 도전성 수준들을 달성하기 위해 높은 증착온도 및/또는 높은 어닐링(annealing) 온도를 요한다. 플라스틱 및 유기 기판들, 예를 들어 폴리카보네이트와 같이 습기를 흡착하기 쉬운 기판들에게 급속 산화막의 접착력이 또한 문제될 수 있다. 따라서, 플렉서블(flexible) 기판 상에 금속 산화막을 적용하는 것은 매우 제한된다. 또한, 진공 증착은 비용이 많이 드는 공정이고 특수한 장비를 요구한다. 더구나, 진공 증착 공정은 패턴 및 회로를 형성하는데 있어서 도움이 되지 않으며, 이는 전형적으로 포토리소그래피와 같이 비용이 많이 드는 패터닝 공정들로 귀결된다.Currently, vacuum deposited metal oxides such as indium tin oxide (ITO) provide optical transparency and electrical conductivity to dielectric surfaces such as glass and polymeric films. Industry standard material. However, the metal oxide film is weak and easily damaged by warpage or other physical stresses. In addition, they require high deposition temperatures and / or high annealing temperatures to achieve high conductivity levels. The adhesion of the rapid oxide film can also be a problem for plastic and organic substrates, for example substrates that are susceptible to moisture, such as polycarbonate. Therefore, the application of the metal oxide film on the flexible substrate is very limited. In addition, vacuum deposition is an expensive process and requires special equipment. Moreover, vacuum deposition processes do not help in forming patterns and circuits, which typically results in costly patterning processes such as photolithography.
또한, 도전성 중합체는 광학적으로 투명한 전기적 도전체로서 사용되어 왔다. 그러나, 이들은 일반적으로 금속 산화막에 비해 낮은 전도율 값과 높은 광흡수성을 가지며, 화학적 및 장기적 안정성이 부족하다.In addition, conductive polymers have been used as optically transparent electrical conductors. However, they generally have lower conductivity values and higher light absorption than metal oxide films, and lack chemical and long term stability.
따라서, 저비용, 고처리율 공정으로 제조될 수 있고, 적절한 전기적, 광학적, 기계적 특성 등을 갖는 투명 도전체를 제조하는 연구가 필요하다.Therefore, there is a need for research to manufacture a transparent conductor that can be manufactured in a low cost, high throughput process, and has appropriate electrical, optical, and mechanical properties.
한편, 최근 나노 크기의 입자에 대한 관심이 증대되면서 나노 크기의 금속 물질에 대한 제조 및 응용 분야 연구가 활발히 진행되고 있다. 나노 입자는 같은 화학적 조성을 갖는 벌크상의 재료들과 비교하여 독특한 전기적, 자기적, 광학적, 기계적 성질들을 나타내기 때문에 전자재료, 센서, 흡착제, 크로마토그래피의 충진제, 촉매 담체 등 광범위한 분야에서 응용되고 있다. 특히, 그 중에서도 일차원적 구조(rods, wires, tubes, belts)를 가진 여러 금속 물질들은 나노 크기의 장치를 이루는데 중요한 역할을 할 것이라 기대되고 있다. 이러한 기대는 일차원적 구조를 지닌 물질들이 가지는 특별한 전기적, 기계적 물성에 기인하고, 일반적으로 나노 크기 금속 물질의 물성은 그것들의 크기와 구조에 따라 변화된다. 필요한 물성을 얻기 위한 방법은 나노 크기 물질의 형태를 어떻게 조절하는가에 따라 달라지며, 따라서 형태조절의 중요성이 부각되고 있는 상황이다. 나노와이어는 최근 일차원 구조를 가진 물질 중 그것들의 제조와 특성 평과에 관한 연구들이 활발히 수행되고 있다.Meanwhile, as interest in nano-sized particles has recently increased, research into manufacturing and application fields for nano-sized metal materials has been actively conducted. Nanoparticles have unique electrical, magnetic, optical, and mechanical properties compared to bulk materials with the same chemical composition, so they are used in a wide range of fields such as electronic materials, sensors, adsorbents, chromatography fillers, and catalyst carriers. In particular, many metal materials with one-dimensional structures (rods, wires, tubes, belts) are expected to play an important role in achieving nanoscale devices. This expectation is due to the special electrical and mechanical properties of materials with one-dimensional structures, and in general, the properties of nanoscale metal materials vary with their size and structure. The method of obtaining the required physical properties depends on how the shape of the nano-sized material is controlled, and thus the importance of shape control is emerging. In recent years, nanowires have been actively studied for their production and evaluation of properties among materials having a one-dimensional structure.
은(Ag)은 모든 금속 중에서 가장 높은 전기 및 열전도도를 가지는 특성으로 많은 관심과 연구가 진행되고 있다. 또한, 은은 상업적으로 응용분야가 넓고, 이러한 은의 일차원적 구조로의 변화는 높은 종횡비(aspect ratio)와 잘 정제된 결정면의 조절을 통해 여러 응용분야로의 확대가 기대되고 있는 바이다. 예를 들면, 은과 고분자의 혼합체에서 은 나노와이어가 혼재되었을 때 은 나노 입자가 혼재되어 있을 때보다 현저하게 낮은 전기적 부하가 발생된다.Silver (Ag) has the highest electrical and thermal conductivity among all metals, and much attention and research is being conducted. In addition, silver has a wide range of applications commercially, and the change of silver into one-dimensional structure is expected to be extended to various applications through high aspect ratio and control of well-refined crystal planes. For example, when silver nanowires are mixed in a mixture of silver and a polymer, a significantly lower electrical load is generated than when silver nanoparticles are mixed.
대부분의 연구에서는 반도체로서부터 유전체까지의 쓰임을 위해서 와이어를 제조하고 있다. 이러한 와이어들은 대부분 전기적 또는 전기화학적 방법을 포함한 주형(template)을 이용하여 제조하고 있고, 세공막(macroporous membranes), 메조포러스 물질(mesoporous materials), 탄소 나노튜브(carbon nanotubes), DNA 체인(DNA chain), 블록공중합체(block copolymer) 등이 와이어 성장을 위한 주형으로 이용되고 있다. 그러나, 이러한 주형을 이용한 방법은 최종 결과물인 와이어의 형상을 조절하기는 쉬우나, 주형의 이용은 주형의 제조와 와이어 형성, 주형의 제거 등 다단계 제조공정과 주형 이용의 제한성으로 대량생산에 적합하지 않아 상업적으로 의미 있는 생산성 확보를 위해서는 개선해야 할 과제가 많이 남아있다.Most studies produce wires for use from semiconductors to dielectrics. Most of these wires are manufactured using templates, including electrical or electrochemical methods, and include macroporous membranes, mesoporous materials, carbon nanotubes, and DNA chains. ), Block copolymers (block copolymer), etc. are used as a template for the growth of wire. However, the method using the mold is easy to control the shape of the final result wire, but the use of the mold is not suitable for mass production due to the multi-step manufacturing process such as the manufacture of the mold, the formation of the wire, and the removal of the mold. There are many challenges to improving to gain commercially meaningful productivity.
본 발명은, 저비용, 고처리율 공정으로 제조될 수 있고, 전기적, 광학적, 기계적 특성 등이 우수하고 부착력이 우수한 투명 도전체 및 이의 제조방법을 제공하고자 한다.The present invention, which can be produced in a low cost, high throughput process, is to provide a transparent conductor excellent in electrical, optical, mechanical properties and the like and excellent adhesion, and a method of manufacturing the same.
이에, 본 발명은Thus, the present invention
1) 표면처리된 기판을 준비하는 단계,1) preparing a surface-treated substrate,
2) 상기 기판 상에 산화형 중합 촉매 및 용매를 포함하는 조성물을 코팅하여 산화형 중합 촉매를 고정하는 단계,2) fixing the oxidative polymerization catalyst by coating a composition comprising an oxidative polymerization catalyst and a solvent on the substrate,
3) 금속 나노와이어 및 용매를 포함하는 조성물을 코팅한 후, 어닐링하는 단계, 및3) coating a composition comprising metal nanowires and a solvent, followed by annealing, and
4) 단량체를 투입하고 중합시키는 단계4) adding monomer and polymerizing
를 포함하는 투명 도전체의 제조방법을 제공한다.It provides a method of manufacturing a transparent conductor comprising a.
또한, 본 발명은 상기 투명 도전체의 제조방법으로 제조되는 투명 도전체를 제공한다.In addition, the present invention provides a transparent conductor manufactured by the method of manufacturing the transparent conductor.
또한, 본 발명은 상기 투명 도전체를 포함하는 전자 소자를 제공한다.In addition, the present invention provides an electronic device comprising the transparent conductor.
본 발명은, 저비용, 고처리율 공정으로 투명 도전체를 제조할 수 있다. 또한, 본 발명에 따라 제조되는 투명 도전체는 전기적, 광학적, 기계적 특성 등이 우수할 뿐만 아니라 부착력이 우수하여 전자 소자 등에 유용하게 적용할 수 있다.This invention can manufacture a transparent conductor in a low cost, high throughput process. In addition, the transparent conductor manufactured according to the present invention is not only excellent in electrical, optical, mechanical properties, etc., but also excellent in adhesion, and thus may be usefully applied to electronic devices.
도 1은 본 발명에 따른 투명 도전체의 제조방법의 일구체예를 개략적으로 나타낸 도이다.1 is a view schematically showing an embodiment of a method of manufacturing a transparent conductor according to the present invention.
이하, 본 발명을 보다 구체적으로 설명하기로 한다.Hereinafter, the present invention will be described in more detail.
금속 나노와이어를 기재 위에 코팅하는 경우에는 와이어간 계면에 전기저항이 발생하게 된다. 따라서, 와이어간 계면에 전기저항의 발생을 억제하기 위하여 어닐링 공정 등을 통하여 계면저항을 줄여주어야 한다. 한편, 코팅하고자 하는 기재, 즉 필름, 유리판 등의 기판에 금속 나노와이어만을 코팅하는 경우에는 코팅층과 기판과의 접착력이 약하여 이를 보강하는 바인더가 필요하게 된다. 또한, 코팅층의 평탄화를 위해서도 바인더 필요하다.When the metal nanowires are coated on the substrate, electrical resistance is generated at the interface between the wires. Therefore, in order to suppress the occurrence of electrical resistance at the interface between the wires, the interface resistance should be reduced through an annealing process or the like. On the other hand, in the case of coating only the metal nanowires on a substrate to be coated, that is, a film, such as a glass plate, the adhesion between the coating layer and the substrate is weak and a binder to reinforce it is required. In addition, a binder is also necessary for planarization of the coating layer.
종래에는 금속 나노와이어와 바인더를 혼합하여 기판에 코팅하는 방법을 이용하였는데, 이러한 방법은 금속 나노와이어와 금속 나노와이어 사이에 바인더가 존재할 가능성이 많게 되어 계면저항을 심화시킬 우려가 있다.Conventionally, a method of coating a substrate by mixing a metal nanowire and a binder has been used. In such a method, there is a possibility that a binder exists between the metal nanowire and the metal nanowire, thereby increasing the interfacial resistance.
그러나, 본 발명은 금속 나노와이어간 계면저항을 최소화할 수 있고, 바인더의 역할인 기판과의 접착력을 부여할 수 있으며, 코팅층을 평탄화시킬 수 있는 특징이 있다.However, the present invention may minimize the interfacial resistance between the metal nanowires, impart adhesion to the substrate, which serves as a binder, and planarize the coating layer.
본 발명에 따른 투명 도전체의 제조방법의 일구체예는 1) 표면처리된 기판을 준비하는 단계, 2) 상기 기판 상에 산화형 중합 촉매 및 용매를 포함하는 조성물을 코팅하여 산화형 중합 촉매를 고정하는 단계, 3) 금속 나노와이어 및 용매를 포함하는 조성물을 코팅한 후, 어닐링하는 단계, 및 4) 단량체를 투입하고 중합시키는 단계를 포함한다.One embodiment of the method for manufacturing a transparent conductor according to the present invention comprises the steps of 1) preparing a surface-treated substrate, 2) coating the composition comprising an oxidative polymerization catalyst and a solvent on the substrate to form an oxidative polymerization catalyst. Immobilizing, 3) coating the composition comprising the metal nanowires and a solvent, followed by annealing, and 4) adding and polymerizing the monomers.
본 발명에 따른 투명 도전체의 제조방법에 있어서, 상기 1) 단계의 기판은 당 기술분야에 알려진 유리판, 플라스틱 필름 등을 이용할 수 있다.In the method of manufacturing a transparent conductor according to the present invention, the substrate of step 1) may use a glass plate, a plastic film, or the like known in the art.
상기 1) 단계의 기판의 표면처리는 표면에서 정전기력(electrostatic force)으로 금속 또는 중합촉매를 고정(immobilization)시킬 수 있는 기능성(functionality)을 갖게 하기 위한 것이다.The surface treatment of the substrate of step 1) is intended to have a functionality capable of immobilizing a metal or a polymerization catalyst with an electrostatic force on the surface.
상기 1) 단계의 기판의 표면처리는 기판에 수산화기(-OH)를 도입한 후, 상기 수산화기(-OH)에 3-아미노프로필트리메톡시실란(3-aminopropyltrimethoxysilane) 등과 같은 아미노실란 화합물을 반응시킴으로써 수행될 수 있다. 상기 기판에 수산화기(-OH)를 도입하는 방법은 산 또는 염기 촉매 가수분해와 같은 화학적 처리방법과, 플라즈마 처리, 오존 처리와 같은 물리적 처리방법 등을 이용할 수 있다.Surface treatment of the substrate of step 1) by introducing a hydroxyl group (-OH) to the substrate, by reacting an aminosilane compound such as 3-aminopropyltrimethoxysilane to the hydroxyl group (-OH) Can be performed. As a method of introducing hydroxyl (-OH) to the substrate, a chemical treatment method such as acid or base catalytic hydrolysis, a physical treatment method such as plasma treatment, and ozone treatment may be used.
상기 1) 단계의 표면처리된 기판에서, 실란기는 수산화기에 커플링되고 아민기는 상기 2) 단계의 산화형 중합 촉매를 고정할 수 있다. 또한, 상기 아민기는 2) 단계에서 산화형 중합 촉매의 고정시 발생하는 산을 중화시킬 수 있다.In the surface-treated substrate of step 1), the silane group may be coupled to a hydroxyl group and the amine group may fix the oxidation type polymerization catalyst of step 2). In addition, the amine group may neutralize an acid generated when the oxidation type polymerization catalyst is fixed in step 2).
또한, 상기 1) 단계의 기판의 표면처리는 기판 상에 폴리(2-비닐피리딘)(poly(2-vinylpyridine)), 폴리(4-비닐피리딘)(poly(4-vinylpyridine), 폴리비닐피롤리돈(polyvinylpyrrolidone) 등과 같은 아민계 고분자; 설포네이티드 폴리스티렌(sulfonated polystyrene), 설포네이티드 폴리설폰(sulfonated polysulfone) 등과 같은 이온성 고분자를 코팅함으로써 수행될 수도 있다.In addition, the surface treatment of the substrate of step 1) is performed on poly (2-vinylpyridine), poly (4-vinylpyridine), and poly (4-vinylpyridine) on the substrate. Amine-based polymers such as polyvinylpyrrolidone, and the like; sulfonated polystyrene, sulfonated polysulfone, and the like may be performed by coating an ionic polymer.
본 발명에 따른 투명 도전체의 제조방법에 있어서, 상기 2) 단계는 표면처리된 기판 상에 산화형 중합 촉매 및 용매를 포함하는 조성물을 코팅하여 산화형 중합 촉매를 고정하는 단계이다.In the method of manufacturing a transparent conductor according to the present invention, step 2) is a step of fixing the oxidative polymerization catalyst by coating a composition comprising an oxidative polymerization catalyst and a solvent on a surface-treated substrate.
상기 2) 단계의 산화형 중합 촉매는 Cu, Fe, Mn, Ag, Pd 및 Co 복합체를 1종 이상 포함할 수 있고, 상기 2) 단계의 용매는 극성용매로서 알코올을 이용할 수 있다. 상기 2) 단계의 용매는 조성물의 코팅 후 제거될 수 있다.The oxidation type polymerization catalyst of step 2) may include one or more complexes of Cu, Fe, Mn, Ag, Pd, and Co, and the solvent of step 2) may use an alcohol as a polar solvent. The solvent of step 2) may be removed after coating of the composition.
본 발명에 따른 투명 도전체의 제조방법에 있어서, 상기 3) 단계는 금속 나노와이어 및 용매를 포함하는 조성물을 코팅한 후, 어닐링하는 단계이다.In the method of manufacturing a transparent conductor according to the present invention, step 3) is a step of coating an composition including a metal nanowire and a solvent, followed by annealing.
상기 3) 단계의 금속 나노와이어의 재료 및 제조방법은 당 기술분야에 알려진 재료 및 제조방법을 이용할 수 있다. 보다 구체적으로, 상기 3) 단계의 금속 나노와이어는 금 나노와이어, 은 나노와이어 등을 이용할 수 있으나, 이에만 한정되는 것은 아니다. 상기 3) 단계의 금속 나노와이어는 금, 백금, 은, 구리, 니켈, 철, 알루미늄, 팔라듐, 이리듐 등을 1종 이상 포함하는 금속 나노시드를 이용하고, 폴리올 공정에 의하여 제조될 수 있다.The material and manufacturing method of the metal nanowire of step 3) may use materials and manufacturing methods known in the art. More specifically, the metal nanowire of step 3) may use gold nanowires, silver nanowires, and the like, but is not limited thereto. The metal nanowire of step 3) may be prepared by a polyol process using metal nanoseeds including at least one of gold, platinum, silver, copper, nickel, iron, aluminum, palladium, and iridium.
또한, 상기 3) 단계의 용매는 극성용매로서 톨루엔, 헥산, 시클로헥산 등을 이용할 수 있다. 상기 3) 단계의 용매는 상기 2) 단계의 용매보다 극성이 낮은 용매를 이용하여 2) 단계의 고정된 산화형 중합 촉매를 분리되지 않게 하는 것이 바람직하다.In addition, toluene, hexane, cyclohexane, and the like may be used as the solvent of step 3) as a polar solvent. The solvent of step 3) is preferably a solvent having a lower polarity than the solvent of step 2) so as not to separate the fixed oxidation type polymerization catalyst of step 2).
상기 3) 단계의 어닐링의 온도는 90 ~ 150℃인 것이 바람직하나, 이에만 한정되는 것은 아니다. 상기 어닐링의 온도가 150℃를 초과하는 경우에는 미량의 산소가 존재하는 경우에도 쉽게 산화할 수 있고, 와이어의 형태를 완전히 잃어버리고 응집이 될 수 있는 문제점이 발생할 수 있고, 90℃ 미만인 경우에는 어닐링 효과가 미미하여 바람직하지 않다.The temperature of the annealing of step 3) is preferably 90 ~ 150 ℃, but is not limited thereto. If the temperature of the annealing exceeds 150 ℃ can be easily oxidized even when a small amount of oxygen is present, there may be a problem that can lose the form of the wire completely and become agglomerated, if less than 90 ℃ The effect is negligible and undesirable.
상기 3) 단계의 어닐링 공정시에는 바인더가 포함되어 있지 않고, 산화형 중합 촉매도 금속 나노와이어간에 있지 않으며 기판 표면에 고정화되어 있기 때문에 순수한 금속 나노와이어만 어닐링시키는 조건과 동일하여, 금속 나노와이어간 계면저항을 줄여줄 수 있다.In the annealing process of step 3), since the binder is not included and the oxidative polymerization catalyst is not between the metal nanowires and is immobilized on the surface of the substrate, the conditions are the same as those for annealing only pure metal nanowires. It can reduce the interface resistance.
본 발명에 따른 투명 도전체의 제조방법에 있어서, 상기 4) 단계는 단량체를 투입하고 기판 표면에 고정화되어 있는 산화형 중합 촉매를 이용하여 중합시키는 단계이다.In the method of manufacturing a transparent conductor according to the present invention, step 4) is a step of polymerizing the monomer using an oxidative polymerization catalyst immobilized on the surface of the substrate.
상기 4) 단계의 구체적인 방법으로서, 기체 또는 액체 상태의 단량체 챔버(chamber)에 1 내지 30분 정도 와이어까지 코팅된 기판을 담그면 기판 표면에 고정되어 있는 산화형 중합 촉매로 기판 표면에서만 중합반응이 진행되어 바인더로서의 형태로 표면에 코팅층이 형성된다. 상기 4) 단계로부터 제조되는 투명 도전체의 표면 거칠기(roughness)는 금속 나노와이어만 코팅한 경우보다 줄어들게 된다(바인더가 없는 경우: RMS roughness = 10 ~ 50nm, 바인더가 있는 경우: 5nm 미만).As a specific method of the step 4), when the substrate coated with a wire for about 1 to 30 minutes in a gaseous or liquid monomer chamber (chamber), the polymerization reaction proceeds only on the substrate surface with an oxidation type polymerization catalyst fixed to the substrate surface. Thus, a coating layer is formed on the surface in the form of a binder. The surface roughness of the transparent conductor manufactured from step 4) is reduced compared to the case of coating only the metal nanowires (when there is no binder: RMS roughness = 10 to 50 nm and with a binder: less than 5 nm).
상기 4) 단계의 단량체는 하기 구조식으로 이루어진 군으로부터 선택되는 1종 이상을 포함할 수 있다.The monomer of step 4) may include one or more selected from the group consisting of the following structural formulas.
또한, 본 발명은 상기 투명 도전체의 제조방법으로 제조되는 투명 도전체를 제공한다.In addition, the present invention provides a transparent conductor manufactured by the method of manufacturing the transparent conductor.
종래의 투명 도전체의 제조시 사용되는 바인더 수지는 나노와이어 간의 계면저항을 심화시키게 되어, 투명 도전체로서의 역할을 하지 못하는 문제점이 있었다. 특히, 은 나노와이어와 일반적인 고분자 간에는 표면에너지 차이가 매우 커서 기본적으로 계면이 불안정하게 되는 특성, 즉 은 나노와이어와 고분자가 쉽게 서로 혼합되지 않고, 분리되려는 경향을 보이게 된다. 또한, 상기 고분자의 대부분은 점도가 매우 높기 때문에 물리적으로 은 나오와이어와 고분자를 섞어놓은 경우에는 분리가 되지 않게 된다.Binder resins used in the manufacture of conventional transparent conductors have deepened the interfacial resistance between nanowires, and thus have a problem in that they do not function as transparent conductors. In particular, the surface energy difference between the silver nanowire and the general polymer is very large, so that the interface is basically unstable, that is, the silver nanowire and the polymer do not easily mix with each other, and tend to be separated. In addition, since most of the polymers are very high in viscosity, they are not separated when the silver nanowire and the polymer are physically mixed.
그러나, 본 발명에 따른 투명 도전체는 1) 표면처리된 기판을 준비하는 단계, 2) 상기 기판 상에 산화형 중합 촉매 및 용매를 포함하는 조성물을 코팅하여 산화형 중합 촉매를 고정하는 단계, 3) 금속 나노와이어 및 용매를 포함하는 조성물을 코팅한 후, 어닐링하는 단계, 및 4) 단량체를 투입하고 중합시키는 단계를 포함하는 방법으로 제조됨으로써, 금속 나노와이어간 계면저항을 최소화하여 전기전도도를 향상시킬 수 있고, 단량체의 중합으로부터 생성되는 바인더에 의하여 기판과의 접착력을 부여할 수 있으며, 금속 나노와이어를 포함하는 코팅층을 평탄화시킬 수 있다.However, the transparent conductor according to the present invention comprises the steps of 1) preparing a surface-treated substrate, 2) fixing a oxidative polymerization catalyst by coating a composition comprising an oxidative polymerization catalyst and a solvent on the substrate, 3 1) coating a composition comprising metal nanowires and a solvent, followed by annealing, and 4) adding and polymerizing monomers, thereby minimizing interfacial resistance between metal nanowires to improve electrical conductivity. It is possible to provide adhesion to the substrate by a binder produced from the polymerization of the monomer, and to flatten the coating layer containing the metal nanowires.
즉, 본 발명에 따른 투명 도전체는, 저비용, 고처리율 공정으로 제조할 수 있고, 전기적, 광학적, 기계적 특성 등이 우수할 뿐만 아니라 부착력이 우수하여 전자 소자 등에 유용하게 적용할 수 있다.That is, the transparent conductor according to the present invention can be manufactured in a low cost, high throughput process, and excellent in electrical, optical, mechanical properties, and the like, and can be usefully applied to electronic devices and the like.
상기 전자 소자로는 평판 액정 표시 장치(flat liquid crystal display), 터치 패널(touch panel), 전자 발광 장치(electroluminescent device), 박막 광전지(thin film photovoltaic cell) 등을 들 수 있다.The electronic device may be a flat liquid crystal display, a touch panel, an electroluminescent device, a thin film photovoltaic cell, or the like.
Claims (9)
2) 상기 기판 상에 산화형 중합 촉매 및 용매를 포함하는 조성물을 코팅하여 산화형 중합 촉매를 고정하는 단계,
3) 금속 나노와이어 및 용매를 포함하는 조성물을 코팅한 후, 어닐링하는 단계, 및
4) 단량체를 투입하고 중합시키는 단계
를 포함하는 투명 도전체의 제조방법.1) preparing a surface-treated substrate,
2) fixing the oxidative polymerization catalyst by coating a composition comprising an oxidative polymerization catalyst and a solvent on the substrate,
3) coating a composition comprising metal nanowires and a solvent, followed by annealing, and
4) adding monomer and polymerizing
Method for producing a transparent conductor comprising a.
상기 1) 단계의 기판의 표면처리는 기판에 수산화기(-OH)를 도입한 후, 상기 수산화기(-OH)에 아미노실란 화합물을 반응시킴으로써 수행되는 것을 특징으로 하는 투명 도전체의 제조방법.The method of claim 1,
The surface treatment of the substrate of step 1) is carried out by introducing a hydroxyl group (-OH) to the substrate, and then reacting the aminosilane compound with the hydroxyl group (-OH).
상기 1) 단계의 기판의 표면처리는 기판 상에 폴리(2-비닐피리딘)(poly(2-vinylpyridine)), 폴리(4-비닐피리딘)(poly(4-vinylpyridine) 및 폴리비닐피롤리돈(polyvinylpyrrolidone)으로 이루어진 군으로부터 선택되는 1종 이상의 아민계 고분자; 또는 설포네이티드 폴리스티렌(sulfonated polystyrene) 및 설포네이티드 폴리설폰(sulfonated polysulfone)으로 이루어진 군으로부터 선택되는 1종 이상의 이온성 고분자를 코팅함으로써 수행되는 것을 특징으로 하는 투명 도전체의 제조방법.The method of claim 1,
The surface treatment of the substrate of step 1) is performed on poly (2-vinylpyridine), poly (4-vinylpyridine) (poly (4-vinylpyridine) and polyvinylpyrrolidone ( by coating at least one amine polymer selected from the group consisting of polyvinylpyrrolidone or at least one ionic polymer selected from the group consisting of sulfonated polystyrene and sulfonated polysulfone Method for producing a transparent conductor, characterized in that.
상기 2) 단계의 산화형 중합 촉매는 Cu, Fe, Mn, Ag, Pd 및 Co 복합체로 이루어진 군으로부터 선택되는 1종 이상을 포함하는 것을 특징으로 하는 투명 도전체의 제조방법.The method of claim 1,
The oxidation type polymerization catalyst of step 2) is a method for producing a transparent conductor, characterized in that it comprises one or more selected from the group consisting of Cu, Fe, Mn, Ag, Pd and Co composite.
상기 3) 단계의 금속 나노와이어는 금, 백금, 은, 구리, 니켈, 철, 알루미늄, 팔라듐 및 이리듐으로 이루어진 군으로부터 선택되는 1종 이상을 포함하는 금속 나노시드를 이용하고, 폴리올 공정에 의하여 제조되는 것을 특징으로 하는 투명 도전체의 제조방법.The method of claim 1,
The metal nanowire of step 3) is prepared by a polyol process using a metal nanoseed containing at least one selected from the group consisting of gold, platinum, silver, copper, nickel, iron, aluminum, palladium and iridium. Method for producing a transparent conductor, characterized in that.
상기 3) 단계의 어닐링의 온도는 90 ~ 150℃인 것을 특징으로 하는 투명 도전체의 제조방법.The method of claim 1,
Method for producing a transparent conductor, characterized in that the temperature of the annealing of step 3) is 90 ~ 150 ℃.
상기 4) 단계의 단량체는 하기 구조식으로 이루어진 군으로부터 선택되는 1종 이상을 포함하는 것을 특징으로 하는 투명 도전체의 제조방법:
The method of claim 1,
The monomer of step 4) is a method for producing a transparent conductor, characterized in that it comprises one or more selected from the group consisting of the following structural formula:
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