KR101701967B1 - Method for preparing transparent conductor comprising nanowire - Google Patents
Method for preparing transparent conductor comprising nanowire Download PDFInfo
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- KR101701967B1 KR101701967B1 KR1020100051010A KR20100051010A KR101701967B1 KR 101701967 B1 KR101701967 B1 KR 101701967B1 KR 1020100051010 A KR1020100051010 A KR 1020100051010A KR 20100051010 A KR20100051010 A KR 20100051010A KR 101701967 B1 KR101701967 B1 KR 101701967B1
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- 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
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Abstract
본 발명은 투명 도전체의 제조방법에 관한 것으로서, 보다 구체적으로 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. 본 발명에 따라 제조되는 투명 도전체는 전기적, 광학적, 기계적 특성 등이 우수할 뿐만 아니라, 부착력이 우수하여 전자 소자 등에 유용하게 적용할 수 있다.The present invention relates to a method for producing a transparent conductor, more specifically, 1) preparing a surface-treated substrate, 2) 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) charging and polymerizing the monomer. The transparent conductor produced according to the present invention has excellent electrical, optical and mechanical properties, and is excellent in adhesion and can be applied to electronic devices and the like.
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.TECHNICAL FIELD The present invention relates to a method of manufacturing a transparent conductor, and more specifically, to a transparent conductor having excellent electrical, optical, and mechanical characteristics by including a nanowire and a method of 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.The 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 a surface conductive transparent conductor is widely used as transparent electrodes in a flat liquid crystal display, a touch panel, an electroluminescent device, a thin film photovoltaic cell and the like, Layer and an electromagnetic wave 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.Presently, vacuum deposited metal oxides such as indium tin oxide (ITO) provide optical transparency and electrical conductivity for dielectric surfaces such as glass and polymeric films. Is an industry standard material for However, the metal oxide film is weak and prone to damage by warping or other physical stresses. In addition, they require high deposition temperatures and / or high annealing temperatures to achieve high conductivity levels. Adhesion of the rapid oxide film to substrates that are susceptible to moisture, such as plastic and organic substrates, such as polycarbonate, may also be a problem. Therefore, application of a metal oxide film on a flexible substrate is very limited. In addition, vacuum deposition is a costly process and requires specialized equipment. Moreover, vacuum deposition processes are not helpful 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.Thus, there is a need for research to produce transparent conductors that can be fabricated with low cost, high throughput processes and have appropriate electrical, optical, mechanical properties, and the like.
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.Recently, as interest in nano-sized particles has increased, studies on manufacturing and application of nano-sized metal materials have been actively conducted. Nanoparticles have been used in a wide range of fields including electronic materials, sensors, adsorbents, chromatography fillers, and catalyst carriers because they exhibit unique electrical, magnetic, optical, and mechanical properties compared to bulk phase materials with the same chemical composition. In particular, many metallic materials with one-dimensional structures (rods, wires, tubes, belts) are expected to play an important role in forming nanoscale devices. These expectations are due to the particular electrical and mechanical properties of materials with one-dimensional structures, and in general, the properties of nano-sized metal materials vary with their size and structure. The way to obtain the necessary properties depends on how the shape of the nanoscale material is controlled, and therefore the importance of shape control is becoming more important. Recently, nanowires have been actively studied for their manufacture and characterization 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 are underway. In addition, silver has a wide range of applications in commerce, and the change to silver one-dimensional structure is expected to expand to various application fields through control of high aspect ratio and well-refined crystal plane. For example, when silver nanowires are mixed in a mixture of silver and a polymer, a significantly lower electrical load is generated than when 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.In most studies, wires are manufactured for use from semiconductors to dielectrics. Most of these wires are fabricated using templates containing electrical or electrochemical methods, and they are used in the production of macroporous membranes, mesoporous materials, carbon nanotubes, DNA chains ), Block copolymers and the like are used as molds for wire growth. However, the method using such a mold is easy to control the shape of the final resultant wire, but the use of the mold is not suitable for mass production due to the limitation of the multistage manufacturing process and mold use such as the production of a mold, wire formation, There are still many challenges to be gained in order to achieve 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 is to provide a transparent conductor which can be manufactured by a low-cost, high-throughput process, excellent in electrical, optical, mechanical characteristics, and excellent in adhesion, and a method of manufacturing the transparent conductor.
이에, 본 발명은Therefore,
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) coating the substrate with a composition comprising an oxidizing polymerization catalyst and a solvent to fix the oxidizing polymerization catalyst,
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) Step of adding monomer and polymerizing
를 포함하는 투명 도전체의 제조방법을 제공한다.And a transparent conductive material.
또한, 본 발명은 상기 투명 도전체의 제조방법으로 제조되는 투명 도전체를 제공한다.Further, the present invention provides a transparent conductor produced by the above-mentioned method for producing a transparent conductor.
또한, 본 발명은 상기 투명 도전체를 포함하는 전자 소자를 제공한다.The present invention also 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.The present invention can produce a transparent conductor with a low-cost, high-throughput process. In addition, the transparent conductor produced according to the present invention has excellent electrical, optical, and mechanical properties, and is also excellent in adhesion so that it can be applied to electronic devices and the like.
도 1은 본 발명에 따른 투명 도전체의 제조방법의 일구체예를 개략적으로 나타낸 도이다.BRIEF DESCRIPTION OF DRAWINGS FIG. 1 is a schematic view showing one embodiment of a method for producing a transparent conductor according to the present invention. FIG.
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 metal nanowires are coated on a substrate, electrical resistance is generated at the interface between the wires. Therefore, the interfacial resistance must be reduced through an annealing process or the like in order to suppress the occurrence of electrical resistance at the interface between the wires. On the other hand, in the case of coating only a metal nanowire on a substrate to be coated, that is, a film, a glass plate, or the like, a binder is required to reinforce the adhesive strength between the coating layer and the substrate. Further, a binder is also required 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 mixing a metal nanowire with a binder and coating the metal nanowire on a substrate has been used. In such a method, there is a high possibility that a binder is present between the metal nanowire and the metal nanowire, which may increase 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 is capable of minimizing the interfacial resistance between metal nano-wires and wafers, imparting adhesive strength to a substrate, which serves as a binder, and flattening 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 producing a transparent conductor according to the present invention comprises the steps of 1) preparing a surface-treated substrate, 2) coating a composition comprising an oxidative polymerization catalyst and a solvent on the substrate, , 3) coating a composition comprising metal nanowires and a solvent, and then annealing, and 4) injecting and polymerizing the monomer.
본 발명에 따른 투명 도전체의 제조방법에 있어서, 상기 1) 단계의 기판은 당 기술분야에 알려진 유리판, 플라스틱 필름 등을 이용할 수 있다.In the method for manufacturing a transparent conductor according to the present invention, a glass plate, a plastic film, and the like known in the art can be used as the substrate in the step 1).
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 in the step 1) is intended to have the functionality to immobilize the metal or polymerization catalyst by an electrostatic force at 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.The surface treatment of the substrate in the step 1) may be carried out by introducing a hydroxyl group (-OH) to the substrate and then reacting the hydroxyl group (-OH) with an aminosilane compound such as 3-aminopropyltrimethoxysilane . As a method of introducing hydroxyl group (-OH) into the substrate, a chemical treatment method such as acid or base catalyst hydrolysis and a physical treatment method such as plasma treatment and ozone treatment can 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 in the step 1), the silane group is coupled to the hydroxyl group and the amine group can fix the oxidized polymerization catalyst in the step 2). In addition, the amine group may neutralize the acid generated upon fixing the oxidation type polymerization catalyst 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 in the above step 1) may be carried out by using a solution of poly (2-vinylpyridine), poly (4-vinylpyridine), polyvinylpyrrolidine An ionic polymer such as an amine-based polymer such as polyvinylpyrrolidone, sulfonated polystyrene, sulfonated polysulfone, or the like.
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 for manufacturing a transparent conductor according to the present invention, the step 2) is a step of fixing an oxidizing polymerization catalyst by coating a surface-treated substrate with a composition comprising an oxidizing polymerization catalyst and a solvent.
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 oxidizing polymerization catalyst in the step 2) may include one or more of Cu, Fe, Mn, Ag, Pd and Co complexes, and the solvent in the step 2) may be an alcohol as a polar solvent. The solvent of step 2) may be removed after coating 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 for manufacturing a transparent conductor according to the present invention, the step 3) is a step of coating a 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 the manufacturing method of the metal nanowire in the step 3) can use materials and manufacturing methods known in the art. More specifically, the metal nanowires in the step 3) may be gold nanowires, silver nanowires, or the like, but are not limited thereto. The metal nanowire in the step 3) may be prepared by a polyol process using a metal nano-seed containing 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.The solvent in step 3) may be toluene, hexane, cyclohexane or the like as a polar solvent. It is preferable that the solvent of the step 3) is not separated from the fixed oxidative polymerization catalyst of the step 2) by using a solvent having a lower polarity than the solvent of the 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 annealing temperature in step 3) is preferably 90 to 150 ° C, but is not limited thereto. If the temperature of the annealing is higher than 150 ° C, it can be easily oxidized even in the presence of a trace amount of oxygen, thereby completely losing the shape of the wire and causing coagulation. If the annealing temperature is lower than 90 ° C, The effect is insignificant.
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.Since the binder is not included in the annealing step in the step 3) and the oxidized polymerization catalyst is also immobilized on the surface of the substrate instead of the metal nanowires, the conditions for annealing pure metal nanowires are the same, The interface resistance can be reduced.
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 for producing a transparent conductor according to the present invention, the step 4) is a step of introducing a monomer and carrying out polymerization using an oxidative polymerization catalyst immobilized on the substrate surface.
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 concrete method of step 4), when a substrate coated with a wire is immersed in a monomer chamber in a gas or liquid state for 1 to 30 minutes, the polymerization reaction proceeds only on the substrate surface And a coating layer is formed on the surface in the form of a binder. The surface roughness of the transparent conductor prepared in the step 4) is reduced as compared with the case where only the metal nanowire is coated (in the case of no binder: RMS roughness = 10 to 50 nm, in the case of binder: less than 5 nm).
상기 4) 단계의 단량체는 하기 구조식으로 이루어진 군으로부터 선택되는 1종 이상을 포함할 수 있다.The monomer of the step 4) may include at least one monomer selected from the group consisting of the following structural formulas.
또한, 본 발명은 상기 투명 도전체의 제조방법으로 제조되는 투명 도전체를 제공한다.Further, the present invention provides a transparent conductor produced by the above-mentioned method for producing a 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.The binder resin used in the production of the conventional transparent conductor deepens the interface resistance between the nanowires and has a problem that it can not serve as a transparent conductor. In particular, the difference in surface energy between silver nanowires and general polymers is so large that basically the interface becomes unstable, that is, silver nanowires and polymers tend to be separated without being easily mixed with each other. In addition, since most of the polymers have a very high viscosity, they are not physically separated from each other when a wire and a polymer are 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 can be manufactured by the steps of 1) preparing a surface-treated substrate, 2) coating a composition comprising an oxidizing polymerization catalyst and a solvent on the substrate to fix the oxidizing polymerization catalyst, 3 ) Coating a composition comprising a metal nanowire and a solvent, and then annealing, and 4) introducing and polymerizing the monomer to thereby improve the electrical conductivity by minimizing the metal nano-wire-to-wire interface resistance And can be imparted with an adhesive force to the substrate by the binder produced from polymerization of the monomer, and the coating layer including the metal nanowires can be planarized.
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 by a low-cost, high-throughput process, and is excellent in electrical, optical, and mechanical properties, and is excellent in adhesion so that it can be 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.Examples of the electronic device include a flat liquid crystal display, a touch panel, an electroluminescent device, and a thin film photovoltaic cell.
Claims (9)
2) 상기 기판 상에 산화형 중합 촉매 및 제1 용매를 포함하는 조성물을 코팅하여 산화형 중합 촉매를 고정하는 단계,
3) 금속 나노와이어 및 제2 용매를 포함하는 조성물을 코팅한 후, 어닐링하는 단계, 및
4) 단량체를 투입하고 중합시키는 단계를 포함하고,
상기 제1 용매 및 제2 용매는 극성 용매이며;
상기 제2 용매는 상기 제1 용매보다 극성이 낮으며;
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.1) preparing a surface-treated substrate,
2) coating the substrate with a composition comprising an oxidizing polymerization catalyst and a first solvent to fix the oxidizing polymerization catalyst,
3) coating a composition comprising a metal nanowire and a second solvent, followed by annealing, and
4) introducing and polymerizing the monomer,
Wherein the first solvent and the second solvent are polar solvents;
The second solvent has a lower polarity than the first solvent;
Wherein the surface treatment of the substrate in the step 1) is performed by introducing a hydroxyl group (-OH) into the substrate, and then reacting the hydroxyl group (-OH) with the aminosilane compound.
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 according to claim 1,
Wherein the oxidizing polymerization catalyst in step 2) comprises at least one selected from the group consisting of Cu, Fe, Mn, Ag, Pd and Co complexes.
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 according to claim 1,
The metal nanowire in the step 3) may be prepared by using a metal nano-seed containing at least one selected from the group consisting of gold, platinum, silver, copper, nickel, iron, aluminum, palladium and iridium, Wherein the transparent conductive material is a transparent conductive material.
상기 3) 단계의 어닐링의 온도는 90 ~ 150℃인 것을 특징으로 하는 투명 도전체의 제조방법.The method according to claim 1,
Wherein the annealing temperature in the step 3) is 90 to 150 ° C.
상기 4) 단계의 단량체는 하기 구조식으로 이루어진 군으로부터 선택되는 1종 이상을 포함하는 것을 특징으로 하는 투명 도전체의 제조방법:
The method according to claim 1,
Wherein the monomer in step 4) comprises at least one monomer selected from the group consisting of the following structural formulas:
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