CN108137310A - 制备结构化表面的方法 - Google Patents
制备结构化表面的方法 Download PDFInfo
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- CN108137310A CN108137310A CN201680058653.2A CN201680058653A CN108137310A CN 108137310 A CN108137310 A CN 108137310A CN 201680058653 A CN201680058653 A CN 201680058653A CN 108137310 A CN108137310 A CN 108137310A
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Classifications
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- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
- B81C1/00444—Surface micromachining, i.e. structuring layers on the substrate
- B81C1/0046—Surface micromachining, i.e. structuring layers on the substrate using stamping, e.g. imprinting
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y40/00—Manufacture or treatment of nanostructures
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- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
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- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/0002—Lithographic processes using patterning methods other than those involving the exposure to radiation, e.g. by stamping
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- G06F3/01—Input arrangements or combined input and output arrangements for interaction between user and computer
- G06F3/03—Arrangements for converting the position or the displacement of a member into a coded form
- G06F3/041—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- 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
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- 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
- H01L31/0216—Coatings
- H01L31/02161—Coatings for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/02167—Coatings for devices characterised by at least one potential jump barrier or surface barrier for solar cells
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- 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
- H01L31/022466—Electrodes made of transparent conductive layers, e.g. TCO, ITO layers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01Q—ANTENNAS, i.e. RADIO AERIALS
- H01Q1/00—Details of, or arrangements associated with, antennas
- H01Q1/12—Supports; Mounting means
- H01Q1/22—Supports; Mounting means by structural association with other equipment or articles
- H01Q1/2208—Supports; Mounting means by structural association with other equipment or articles associated with components used in interrogation type services, i.e. in systems for information exchange between an interrogator/reader and a tag/transponder, e.g. in Radio Frequency Identification [RFID] systems
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/80—Constructional details
- H10K30/81—Electrodes
- H10K30/82—Transparent electrodes, e.g. indium tin oxide [ITO] electrodes
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/60—Forming conductive regions or layers, e.g. electrodes
- H10K71/611—Forming conductive regions or layers, e.g. electrodes using printing deposition, e.g. ink jet printing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/32—Processes for applying liquids or other fluent materials using means for protecting parts of a surface not to be coated, e.g. using stencils, resists
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/12—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by mechanical means
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
- B05D5/12—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain a coating with specific electrical properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
- B81B2203/00—Basic microelectromechanical structures
- B81B2203/04—Electrodes
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1262—Process of deposition of the inorganic material involving particles, e.g. carbon nanotubes [CNT], flakes
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/13338—Input devices, e.g. touch panels
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F2202/00—Materials and properties
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- G06F2203/00—Indexing scheme relating to G06F3/00 - G06F3/048
- G06F2203/041—Indexing scheme relating to G06F3/041 - G06F3/045
- G06F2203/04103—Manufacturing, i.e. details related to manufacturing processes specially suited for touch sensitive devices
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- G—PHYSICS
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- G06F2203/00—Indexing scheme relating to G06F3/00 - G06F3/048
- G06F2203/041—Indexing scheme relating to G06F3/041 - G06F3/045
- G06F2203/04112—Electrode mesh in capacitive digitiser: electrode for touch sensing is formed of a mesh of very fine, normally metallic, interconnected lines that are almost invisible to see. This provides a quite large but transparent electrode surface, without need for ITO or similar transparent conductive material
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/09—Use of materials for the conductive, e.g. metallic pattern
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/02—Apparatus or processes for manufacturing printed circuits in which the conductive material is applied to the surface of the insulating support and is thereafter removed from such areas of the surface which are not intended for current conducting or shielding
- H05K3/04—Apparatus or processes for manufacturing printed circuits in which the conductive material is applied to the surface of the insulating support and is thereafter removed from such areas of the surface which are not intended for current conducting or shielding the conductive material being removed mechanically, e.g. by punching
- H05K3/046—Apparatus or processes for manufacturing printed circuits in which the conductive material is applied to the surface of the insulating support and is thereafter removed from such areas of the surface which are not intended for current conducting or shielding the conductive material being removed mechanically, e.g. by punching by selective transfer or selective detachment of a conductive layer
- H05K3/048—Apparatus or processes for manufacturing printed circuits in which the conductive material is applied to the surface of the insulating support and is thereafter removed from such areas of the surface which are not intended for current conducting or shielding the conductive material being removed mechanically, e.g. by punching by selective transfer or selective detachment of a conductive layer using a lift-off resist pattern or a release layer pattern
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/12—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using thick film techniques, e.g. printing techniques to apply the conductive material or similar techniques for applying conductive paste or ink patterns
- H05K3/1208—Pretreatment of the circuit board, e.g. modifying wetting properties; Patterning by using affinity patterns
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/12—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using thick film techniques, e.g. printing techniques to apply the conductive material or similar techniques for applying conductive paste or ink patterns
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Abstract
本发明涉及一种制备结构化表面的方法,其中将包括纳米线的组合物施加到表面上并且将其结构化,特别地通过部分地移动组合物来结构化。当溶剂被去除时,纳米线聚集成结构体。这些结构体可以既是透明的又是导电的。
Description
发明领域
本发明涉及用于制备结构化的、尤其是导电的表面的方法,以及涉及在衬底上的这样的结构及其用途。
现有技术
透明导电电极(TCE)是诸如触摸屏、太阳能电池等的现代设备的重要组成部分。
正是在透明电极的情况下,所施加的结构必须被特别精细且均匀地结构化。
已知基于光刻或转印的制备工艺。这些工艺通常包括减压下的处理,特别地为了施加金属层。
从US 2003/0168639A1已知,纳米颗粒可以通过相应的印模来形成结构体。为了保持所述结构体的导电性,高含量的颗粒是必需的。因此,获得的结构体不透明。为了获得导电结构体,此外还需要热处理。
技术问题
本发明要解决的技术问题是,提供一种能够实现以简单的方式制备金属结构体、特别地导电结构体的方法。该方法也应当能够实现透明结构体的制备。
发明内容
该技术问题通过本发明采用独立权利要求的特征来得以解决。本发明的有利扩展方式在从属权利要求中表征。所有权利要求的原文由此通过引用并入本说明书的内容。本发明还涵盖独立和/或从属权利要求的所有合理的组合,尤其是所有提及的组合。
该技术问题通过用于制备金属结构体的方法解决,其中提供了包括纳米线和至少一种溶剂的组合物。使该组合物在衬底上结构化。
此后,至少部分地去除溶剂。由此导致纳米线与结构化相对应地加强聚集(积聚、沉积)在表面上。由此在表面上获得由纳米线组成的金属结构体。
优选将至少一种溶剂完全去除。
接下来详细描述了各个方法步骤。这些步骤不一定按照规定的顺序进行,并且待描述的方法还可以具有其它未列出的步骤。
组合物在表面上的结构化可以不同方式完成。例如可仅将组合物涂覆在特定区域上,尤其是线上,或者可以在那里聚集。这可例如通过在涂覆之前对表面进行相应的(适当的)处理来实现。
在本发明的另一个实施方式中,通过在组合物与表面接触之前或之后使结构模板与组合物接触来实现结构化。
在本发明的另一个实施方式中,通过将组合物涂覆到在所述涂覆之前施加在表面上的结构化掩模中来实现结构化。
在本发明的一个优选实施方式中,将组合物涂覆到衬底上,然后施加结构模板,同时部分地移动(排挤,)所述组合物(或使所述组合物部分地移位)。通过部分地移位而导致结构模板与衬底表面之间的接触。该方法具有以下优点:通过针对性地使所述组合物移位可以简单的方式实现结构化。这样的结构模板可以简单的方式制备。
在本发明的同样优选的实施方式中,将组合物施加到结构模板上,并将如此处理的结构模板施加到表面上。所述组合物可以例如处于结构模板的较深结构中。
在下一步骤中,至少部分去除溶剂。这可通过许多方式来完成。例如通过蒸发溶剂,其中可以通过加热来促进所述蒸发。由于通常较少的量,所述蒸发也可以在施加结构模板的情况下进行。加热的强度取决于所使用的材料和溶剂。例如可涉及最高达100℃的加热。
至少部分去除溶剂优选地与将结构模板施加到表面上一起进行。
组合物包括纳米线。在本发明的上下文中,通常将其理解为与球形纳米颗粒或纳米棒相比具有超过100的长径比的细长体。这样的纳米线例如能够借助两个参数来描述。一个是纳米线的平均直径,另一个是纳米线的长度。纳米线的特征特别在于它们具有低于100nm,优选低于50nm,优选低于20nm,更优选低于10nm,特别地低于5nm的直径。其长度在此大于300nm,优选大于500nm,更优选大于1μm。这些尺寸可以通过TEM确定。“长度”在此理解为表示组合物中存在的至少50重量%的纳米棒具有的长度,特别地至少60重量%,非常特别地至少80重量%,尤其是100重量%的纳米棒所具有的长度。纳米线在TEM中以较长的一侧搁置。所确定的直径因此是不同取向的纳米线的直径平均值。所述组合物中也可能出现纳米线聚集体(附聚物)。这些数据总是基于一条纳米线。
在本发明的一个实施方式中,组合物包括平均直径低于15nm,优选低于10nm,尤其低于5nm的纳米线。所述直径也可以低于3nm,优选低于2nm。特别优选的范围是0.5nm至5nm,特别地0.5nm至3nm或0.5nm至2nm。纳米线的长度在此大于1μm,优选大于1.5μm。与此无关地,长度可以最高达15μm,优选最高达10μm。长度可以例如是1μm至15μm,特别地2至15μm。
优选地,纳米线的长度与直径的长径比为大于500:1,特别地大于1000:1,非常特别地大于1500:1或大于2000:1。
优选地,组合物中至少50重量%,优选至少80重量%,尤其是100重量%的纳米线满足前文给定的尺寸数据。
由于纳米线直径小,它们具有高度的柔韧性。因此它们可以适配于结构体而不会断裂。由于它们特别大的表面积,它们也倾向于形成束。柔韧性还有利于形成束。
在去除溶剂时,这种高的长径比导致线彼此聚集形成少量的束。由于它们的柔韧性,它们在此也可以遵循结构模板的更复杂的结构。因此,能够毫无困难地制备弯曲的或交叉的结构体,例如网格。由于纳米线以错开(交错)的方式聚集,因此形成连续的结构体。由于平行取向,这样的束在金属相或半金属相之间具有显著更少的界面。因此,沿着该束的导电性比在可比较的纳米颗粒的排列的情况更好。渗透网络是可能的。在此,这些束与表面平行并沿纵向跟随结构模板的凹槽。
平行取向也可以获得各向异性的导电性。
高的长径比有利于纳米线聚集成束。与球形纳米颗粒相比,高的长径比还减少了沿特定距离的传导路径的接触位点的数量。
通过成束,所形成的结构体优选地比由结构模板中的凹槽预设的距离更薄。
对于制备纳米线可以考虑本领域技术人员已知的所有方法。这例如是还原相应的盐溶液。对于这样的方法,如何获得纳米线的条件是已知的。这样的方法的一个实例描述于:Feng等人,Simple and Rapid Synthesis of Ultrathin Gold Nanowires,theirSelf-assembly and Application in Surface-enhanced RamanScattering.Chem.Commun.2009,1984-1986。
在本发明的一个实施方式中,涉及的是无机纳米线。可涉及金属纳米线,所述金属纳米线包括一种金属、由两种或更多种金属构成的混合物或由两种或更多种金属构成的合金,例如FePt。所述金属优选地选自IUPAC第1-16族的金属以及镧系元素,优选地选自第4至16族的金属,尤其是Au,Ag,Cu,Pt,Pd,Ni,Ru,In,Rh,Al,Pb,Bi,Te。纳米线也可以包括导电或半导体氧化物。这样的氧化物(其也能够被掺杂)的实例是氧化铟锡(ITO)或氧化锑锡(ATO)。还可以使用第II-VI,III-V或IV族的半导体或这样的半导体的合金。对此的实例是CdS,CdSe,CdTe,InP,InAs,ZnS,ZnSe,ZnTe,HgTe,GaN,GaP,GaAs,GaSb,InSb,Si,Ge,AlAs,PbSe或PbTe。它们也可以是非金属纳米线,例如由前文列举的金属的氧化物,硫化物,硒化物构成。对此的实例是Cu2S、Bi2S3、Sb2S3、SmO3、PbS。
纳米线在组合物中的浓度优选低于30mg/ml,尤其低于15mg/ml,优选低于10mg/ml。可通过浓度来控制所得结构体的厚度。浓度优选大于0.1mg/ml,特别地大于0.5mg/ml,或大于1mg/ml,以及在上述边界值之间的范围内。
该组合物还可以包括至少一种稳定剂。所述稳定剂被理解为意指防止纳米线在组合物中存在的纳米线浓度下聚集的化合物。这通常是沉积在纳米线表面上的化合物。这通常是具有至少一个选自羟基、硫醚基(Sulfidgruppen)、醚基、羧酸酯基、酯基或氨基的官能团的有机化合物。这些化合物也可影响溶剂的选择。对于非极性溶剂,这些可以例如是烷基胺、醇、羧酸、硫醇,其具有含4至30个碳原子的脂族基团。
合适的溶剂是本领域技术人员已知的用于纳米线的溶剂。优选的是沸点低于150℃的溶剂。其可为极性或非极性溶剂。极性溶剂的实例可为去离子水,甲醇,乙醇,异丙醇,正丙醇或丁醇,酮例如丙酮,醚例如二***、甲基叔丁基醚,四氢呋喃,酯例如乙酸乙酯,卤代溶剂例如二氯甲烷、氯仿。非极性溶剂的实例为脂族或脂环族烃如正戊烷、异戊烷、正丁烷、正己烷、异己烷或环己烷、甲基环己烷、苯、甲苯、萘。
衬底可以是适用于此目的的任何材料。适合材料的实例是金属或金属合金,玻璃,陶瓷,包括氧化物陶瓷、玻璃陶瓷,或塑料,以及纸和其它含纤维素的材料。当然也可以使用具有由上述材料构成的表面层的衬底。表面层可以例如是金属化层、搪瓷层、玻璃层、陶瓷层或涂料层(涂漆)。
金属或金属合金的实例是钢,包括不锈钢、铬、铜、钛、锡、锌、黄铜和铝。玻璃的实例是钠钙玻璃、硼硅酸盐玻璃、铅晶体和石英玻璃。玻璃可以例如是平板玻璃,诸如容器玻璃的中空玻璃,或实验室设备玻璃。陶瓷可以例如是基于氧化物SiO2、Al2O3、ZrO2或MgO或相应的混合氧化物的陶瓷。塑料(其也可以像金属一样以膜的形式存在)的实例是聚乙烯(PET)例如HDPE或LDPE,聚丙烯,聚异丁烯,聚苯乙烯(PS),聚氯乙烯(PVC),聚偏二氯乙烯,聚乙烯醇缩丁醛,聚四氟乙烯,聚氯三氟乙烯,聚丙烯酸酯,聚甲基丙烯酸酯如聚甲基丙烯酸甲酯(PMMA),聚酰胺,聚对苯二甲酸乙二醇酯,聚碳酸酯,再生纤维素,硝酸纤维素,乙酸纤维素,三乙酸纤维素(TAC),乙酸丁酸纤维素或橡胶-盐酸盐。涂漆表面可由常规底漆或清漆形成。在优选的实施方式中,衬底为膜,特别地聚对苯二甲酸乙二醇酯膜或聚酰亚胺膜。
组合物可以使用常规方法施加,例如浸涂、辊涂、刮刀涂布、流涂(Fluten)、拉伸、喷涂、离心(Schleudern)或旋涂。也可包括另外的助剂如润湿助剂。
例如,组合物的涂覆可以通过放置在衬底上的框架来进行,并且将组合物引入到之后形成的由框架所界定的空间中。框架可由弹性材料构成。框架可具有任意形状。
在本发明的优选实施方式的另一步骤中,在所涂覆的组合物上施加结构模板,同时使所述组合物部分地移位。结构模板是任意成型的模板,它通过与衬底表面接触而在这些位置处使组合物移位。在此,衬底表面上的组合物必须是粘性的或流质的使得可造成移位。
结构模板可以例如是印模。结构模板可以由任意材料形成。结构模板的可能材料是本领域技术人员从微结构印模领域已知的。它们例如还可以通过光刻方法获得。实例是金属如镍,半金属如硅,或光刻胶。还可以使用硅酮(或称为聚硅氧烷),如PDMS(聚二甲基硅氧烷)。
结构模板优选地具有对应于线或网格的凹槽和凸起。各个凸起可具有方形、矩形、圆形和/或椭圆形的基面。它们优选以规则的方式排列,使得位于凸起之间的凹槽导致网格结构体的形成。
结构模板的凹槽的最小宽度优选地低于2μm。
可能需要处理结构模板的表面,例如通过用氟化硅烷处理。
结构模板的表面也可以通过其它处理如等离子体处理来改性。由此可使结构模板与组合物适配。
可能有必要使结构模板的设计适配于组合物层的厚度,例如以便为移位的前体化合物和可能夹带的空气提供足够的空间。这同样可受到结构模板的厚度或其表面上存在的凹槽的深度的影响。
关于由结构模板接触的区域,结构模板是所需结构体的负片(Negativ)。
还可能的是,首先将组合物施加到结构模板上并将两者一起施加到衬底上。
在至少部分去除溶剂之后,优选地将结构模板移除。
在本发明的另一个实施方式中,在形成结构体和必要时去除溶剂后,对衬底进行进一步处理。经涂覆的衬底可以例如通过在烘箱中加热,通过压缩空气和/或通过室温干燥来进行干燥。
还可以施加另外的层,例如用于保护经涂覆的表面免受氧化和水或UV辐射。
在一个优选的实施方式中,在结构化之后,特别地在移除结构模板之后,进行处理以至少部分地去除有机物质。这可以例如是在200℃以上或400℃以上的热处理。其还可以是等离子体处理。通过至少部分地去除有机成分来减少或去除在纳米线周围可能存在的有机壳。由此有助于纳米线之间的电子转移。这样可以大大提高所得结构的导电性。优选的是等离子体处理。
文献中经常描述在真空条件下获得等离子体的可能方式。电能可以通过电感或电容方式结合。其可为直流电或交流电;交流电的频率可达几kHz到MHz的范围。微波范围(GHz)内的能量供应也是可能的。
作为主要等离子体气体可以使用例如He、氩气、氙气、N2、O2、H2、蒸汽或空气,以及同样地这些化合物的混合物。优选由氢气和氩气构成的等离子体,例如氩气中1%至20体积%的氢气,特别地H2/Ar5%/95%。
在此,等离子体处理可以在低于50℃的温度下,特别地在室温下进行。这样,通过本发明的方法无需在超过100℃、特别地超过60℃的温度下的步骤就可以制备导电结构体。还能够实现整个方法均在室温下进行。
也不需要用于结构化的中间步骤,并且也可以省去化学再处理。
可能需要对衬底表面进行预处理。在本发明的一个优选扩展方式中,预处理包括等离子体处理、电晕处理、火焰处理和/或涂覆和硬化有机-无机涂层。特别地,对于膜衬底,尤其对于塑料膜,可以考虑等离子体处理、电晕处理和/或火焰处理。
本发明还包括该方法的另一个实施方式,其中该方法包括在结构化之前或之后将组合物施加到惰性表面上。
在此,该表面优选为包括至少一种含氟化合物的表面。
该表面可以例如是已经用包括单独地或与另外的可水解的硅烷结合的至少一种可水解的硅烷的组合物涂覆的表面,其中所述可水解的硅烷包含至少一个包括至少一个氟原子的不可水解的基团。这可以例如是具有含至少一个氟原子的不可水解的基团的硅烷。这种类型的硅烷例如描述于WO 92/21729 A1中。实例是以下通式的可水解的硅烷:
Rf(R)bSiX(3-b) (I)
其中X相同或不同并且是可水解的基团,R相同或不同并且是烷基取代基,b具有0、1或2的值。
上式的可水解分离的基团X的合适实例为氢,卤素(F、Cl、Br或I,特别地Cl或Br),烷氧基(例如C1-6-烷氧基,例如甲氧基、乙氧基、正丙氧基、异丙氧基和正丁氧基,异丁氧基,仲丁氧基或叔丁氧基),芳氧基(优选C6-10-芳氧基,例如苯氧基),烷芳氧基例如苯甲酰氧基,酰氧基(例如C1-6-酰氧基,优选C1-4-酰氧基,例如乙酰氧基或丙酰氧基)和烷基羰基(例如C2-7-烷基羰基如乙酰基)。同样合适的是NH2,用烷基、芳基和/或芳烷基单取代或双取代的氨基(其中烷基、芳基和/或芳烷基的实例是下面对R给定的那些),酰氨基如苯甲酰氨基或醛肟基或酮肟基。两个或三个基团X也可以彼此连接,例如在具有乙二醇、甘油或儿茶酚(Brenzcatechin)的Si-多元醇络合物的情况下。提及的基团可以任选地含有取代基,例如卤素、羟基、烷氧基、氨基或环氧基。优选的可水解分离的基团X是卤素、烷氧基和酰氧基。特别优选的可水解分离的基团是C1-4-烷氧基,特别地甲氧基和乙氧基。
式(I)中的不可水解分离的基团R例如为烷基(例如C1-20-烷基,特别地C1-4-烷基,例如甲基、乙基、正丙基、异丙基、正丁基、异丁基、仲丁基和叔丁基),链烯基(例如C2-20-链烯基,尤其是C2-4-链烯基,例如乙烯基、1-丙烯基、2-丙烯基和丁烯基),炔基(例如C2-20-炔基,尤其是C2-4-炔基,如乙炔基或炔丙基),芳基(尤其是C6-10-芳基,如苯基和萘基)和相应的芳烷基和烷芳基,如甲苯基和苄基,以及环状C3-12-烷基和-链烯基,如环丙基,环戊基和环己基。
基团R可以具有典型的取代基,所述取代基可以是如下的官能团:通过该官能团还能够按需地经由有机基团使缩合物交联。典型的取代基例如是卤素(例如氯或氟)、环氧化物(例如缩水甘油基或缩水甘油氧基)、羟基、醚、酯、氨基、单烷基氨基、二烷基氨基、任选取代的苯胺基、酰胺、羧基、烯基、炔基、丙烯酰基、丙烯酰氧基(Acryloxy)、甲基丙烯酰基、巯基、氰基、烷氧基、异氰酸基、醛、酮基、烷基羰基、酸酐和磷酸。这些取代基通过可被氧或-NH-基团中断的二价桥连基团、特别地亚烷基、亚烯基或亚芳基桥连基团与硅原子键合。桥连基团含有例如1至18、优选1至8、特别地1至6个碳原子。所提及的二价桥连基团例如衍生自上述一价烷基、烯基或芳基基团。当然,基团R也可具有一个以上的官能团。
Rf是具有1至30个与碳原子键合的氟原子的不可水解基团,其优选通过至少2个原子、优选亚乙基与Si隔开。基团Rf优选具有1至25个,特别地3至18个优选与脂族碳原子键合的氟原子。Rf优选为具有3至20个碳原子的氟化烷基。Rf的实例为CF3CH2CH2-、C2F5CH2CH2-、n-C6F13CH2CH2-、i-C3F7OCH2CH2CH2-、n-C8F17CH2CH2-和n-C10F21OCH2CH2-。
合适的氟化硅烷化合物的实例是CF3CH2CH2SiCl2(CH3)、CF3CH2CH2SiCl(CH3)2、CF3CH2CH2Si(CH3)(OCH3)2、C2F5-CH2CH2-SiZ3、n-C6F13-CH2CH2-SiZ3、n-C8F17-CH2CH2-SiZ3、n-C10F21-CH2CH2SiZ3(其中Z=OCH3、OC2H5或Cl)、i-C3F7O-CH2CH2CH2-SiCl2(CH3)、n-C6F13-CH2CH2-SiCl(OCH2CH3)2、C6F13-CH2CH2-SiCl(CH3)2和n-C6F13-CH2CH2-SiCl2(CH3)。
惰性表面影响表面的润湿特性。如果这时使包括纳米线的组合物与该表面接触,则会导致纳米线的在结构上真正的聚集(strukturtreuen Anlagerung)。
在本发明的该实施方式中,组合物优选包括平均直径低于50nm,特别地低于40nm的纳米线。平均直径优选地大于0.5nm,尤其地大于1nm,优选地3至30nm,尤其地5至20nm,最优选地15nm。在此,纳米线的长度大于1μm,尤其大于2μm,优选地3μm至200μm,更优选地4至130μm。
作为溶剂可以使用与本发明第一实施方式相同的溶剂。
惰性表面的使用改变了聚集的性质。在与表面相结合地去除溶剂时,导致沿结构化层由纳米线形成相互交织的结构体。取决于所使用的纳米线的浓度,可影响所述结构体的高度。
尤其是平均直径为3至30nm且长度为4μm至130μm的纳米线在此不太倾向于形成平行的聚集体,而是可能由于表面张力和惰性表面被组合物润湿的润湿性差而形成交织结构体。
在此,纳米线仅在很小的程度上与表面平行地布置,而是通过由交织的纳米线构成的结构体来填充结构空隙。为此目的,纳米线也需要一定的柔韧性。
为了能够形成交织结构,有利的可以是,所产生的结构化层具有0.2μm的最小横向维度。
在本发明的优选实施方式中,该结构化层包括具有小于1μm(通过AFM和SEM测量)的最小横向维度的结构体。这意味着在衬底上制备的结构体具有20μm的最小宽度,优选地具有小于10μm,特别地小于5μm的最小维度。
在优选实施方式中,结构化层包括线或网格。
本发明方法的一个特别的优点是,所用的组合物可以以简单的方式涂覆到衬底上。在此,纳米线的使用能够实现仅以几个步骤制备特别精细的、尤其是导电的结构体。所有已知的印刷方法都可用于此目的,例如喷墨印刷、凹版印刷、丝网印刷、胶版印刷或凸版和柔性版印刷。通常情况下,前述印刷方法的组合印刷也被用于电气功能的印刷。可能需要使所用的印刷板、印刷辊或印模与组合物的性质匹配,例如通过匹配它们的表面能。
对于通过结构化获得的结构体实际上没有限制,只要它们可以由纳米线形成即可。因此,优选地可以涂覆由分叉或未分叉的线组成的结构体,例如导体轨道或网格。由于良好的分辨率,通过该方法可涂覆肉眼不可见的导电结构体。这在触摸屏表面的制备中起着重要作用。
通过施加结构模板导致的结构化甚至可以集成到常规印刷方法中,方法是用结构模板取代印刷模板(Druckvorlage)。
本发明还涉及根据本发明的方法获得的经涂覆的衬底。
本发明还涉及结构化衬底,其在表面上包括由纳米线构成的结构体。
所述结构体优选为金属结构体,它们尤其包含金属铜、银、金、镍、锌、铝、钛、铬、锰、钨、铂或钯,优选银或金。
在本发明的特别有利的扩展方式中,经涂覆的衬底具有至少部分透明的金属结构体。这可以例如通过将分辨率低于20μm、优选低于10μm的结构体施加在透明的衬底上来实现。它们也可以是分辨率低于5μm或甚至1μm的结构体。在此,“分辨率”是指该结构体具有最小维度低于所述分辨率的结构体。这例如是具有所述分辨率的宽度的分叉或未分叉的线,其中这些线之间存在至少一个线宽的最大间距,特别地至少三倍线宽的间距。
通过本发明的方法获得的经涂覆的衬底可以用于许多应用。首先,该方法适用于将反射金属层施加到表面上。这些反射金属层可以例如用作全息图应用中的反射层。
本发明的一个特别的优点在于导电结构体的制备。这些导电结构体适合作为导体轨道在电子应用中,在触摸屏显示器、太阳能收集器、显示器中,作为RFID天线或在晶体管中使用。因此,它们适合作为目前基于ITO(氧化铟锡)制备的产品中的备件,例如在TCO涂层(TCO:透明导电氧化物)中的备件。
然而,该结构还可以用于晶体管领域。
由结合从属权利要求对优选的实施例的以下描述可获得进一步的细节和特征。在此,各个特征可以单独实现,或者两个或更多个特征可以彼此组合地实现。解决技术问题的手段不限于实施例。因此,范围数据例如总是包括所有未列出的中间值和所有可设想的子区间。
实施例在附图中被示意性地示出。在此,各附图中的相同的附图标记表示相同或具有相同功能或在其功能方面彼此对应的元件。具体地,示出了:
图1示出了a)金纳米线的TEM照片;b)金纳米线的TEM照片;c)所使用的印模的SEM照片。
图2示出了使用纳米线的本发明方法的示意性流程图;
图3示出了使用纳米线的本发明方法的一系列过程的示意图;
图4示出了使用纳米线的本发明方法的一系列过程的示意图;
图5示出了获得的两种结构化涂层的SEM照片;a)平均厚度为15纳米;b)平均厚度为45nm;小图显示了相应的SEM照片的放大片段;
图6示出了a)获得的结构化涂层的透射光谱(NM-15nm:来自图4a的结构体;NM-45nm:来自图4b的结构体);b)电导率测量(NM-15nm:来自图4a的结构体;NM-45nm:来自图4b的结构体);
图7示出了在使衬底弯曲时所测得的本发明的网格(AuNM)和市售可得的ITO网格(ITO在PET上)的电阻变化;
图8示出了弯曲的金纳米线的TEM照片;
图9示出了使用惰性表面的本发明方法的示意图;
图10示出了使用惰性表面的本发明方法的示意图;
图11示出了使用惰性表面的本发明方法的另一个实施方式的示意图;
图12示出了使用惰性表面的本发明方法的另一个实施方式的示意图;
图13示出了使用惰性表面的本发明方法的另一个实施方式的示意图;
图14示出了使用惰性表面的本发明方法的另一个实施方式的示意图;
图15示出了各种样品的透射率测量(1:网格结构体,变体1;2:网格结构体,变体2;3:纳米线,平面状;4:纳米线,平面状紧密堆积);
图16示出了按照变体1的获得的网格结构体的SEM照片(a)整体照片;b)更高分辨率下的结构体(结构体宽度18.68μm+/-0.98μm);
图17示出了按照变体2的获得的网格结构体的SEM照片(结构体宽度30.59μm+/-3.8μm);
图18平面状地示出了银纳米线的SEM照片;
图19示出了市售可得的银纳米线在结构化后的SEM照片(对照例)。
图20示出了市售可得的银纳米线在结构化后的SEM照片(对照例)。
I.通过聚集结构化
图1显示了金纳米线的TEM照片。纳米线在直径低于2nm的情况下具有远大于500nm的长度。在a)和b)中可明确辨认出,这些纳米线本身已经共同聚集成束。图1c)示出了所使用的印模之一。
图2示出了本发明方法的流程的示意图。在此,首先将组合物涂覆到表面上(200)。此后,使组合物中的纳米线结构化(210)。这优选通过施加结构模板同时使组合物部分地移位来完成。此后,至少部分地去除溶剂(220)。
图3示出了该方法的根据本发明的实施方式。如图3a)所示,在涂覆组合物之后,纳米线300随机排列在衬底310的表面上。此时它们仍然分散在溶剂中。之后,将优选地以印模320形式的结构模板施加到表面310上(图3b))。在该情况下,印模包括具有平面状端面的圆柱形凸起(类似于图1c))。这些平面状端面与衬底310的表面形成接触面。由此,组合物在这些区域中移位。由此将纳米线转移到凸起之间的空隙中。然后至少部分地去除溶剂。这可以例如通过使印模的凸起高于所涂覆的组合物的厚度来确保。由此可在组合物上方形成可用来蒸发溶剂的空腔。通过局部增加纳米线浓度而导致纳米线束330的形成。这些纳米线束优选聚集(沉积)在衬底310上的凸起320之间(图3c)。在去除结构模板之后,在衬底310的表面上剩下由纳米线形成的结构体340(图3d))。必要时,可能需要通过后处理去除所述结构的有机成分,这可例如通过等离子体处理来完成。
图4以垂直剖视图示出了图3中所示的方法的流程。图4a)中以垂直剖视图示出了图3b)的情况。涂覆的组合物布置在与衬底310的表面接触的两个凸起320之间。在该情况下,该组合物包括溶剂305和分散在其中的纳米线300,其在这里图示为圆形横截面。该图示并不意味着纳米线以完全分散的形式存在。很可能的是,它们已经在分散体中以部分相互聚集的方式存在,并因此已经形成了最初的束。在下一步中,去除溶剂305。凸起310之间的间隙中的纳米线330这时共同聚集在表面310上形成束。这也由纳米线非常长且柔韧的事实促成。
在去除印模后,仍然可以进行烧结步骤(图4c))。在此,例如通过等离子体处理去除纳米线的有机壳并且使纳米线束进一步紧密。由此可以增加纳米线束350的导电性。
图9、10、11、12、13和14显示了本发明的其它实施方式。
图9示出了衬底500,在衬底500的表面上已经施加了惰性层510。在所述惰性层上布置包括纳米线的组合物520。在该表面上施加以印模530形式的结构模板。在此,所述过程在图10中示出。结构模板530的凸起使组合物520移动到凸起之间的间隙中(该图的上部)。这由衬底500上的惰性表面510促进。当结构模板530的凸起与衬底500或与惰性表面510接触时,使整个组合物520布置在结构模板的凹槽中(图10的下部)。
图11至14显示了本发明的另一个实施方式。为此目的,将包括纳米线620的组合物提供到结构模板610上,所述结构模板可布置在载体600上(图11)。使用刮板630将组合物压入结构模板的凹槽中。在图12中示出由此获得的“已填充”的结构模板610,其中凹槽已被组合物620填充。结构模板可布置在载体600上。
如图13所示,这时可使在间隙中填充有组合物620的这种已填充的结构模板610与衬底650上的惰性表面640接触(该图的下部)。
为了在惰性表面上产生结构体,将结构模板与惰性表面一起旋转,使得惰性表面布置在下方。由此可使纳米线聚集在惰性表面上。
原则上获得了如图10下部所示的相同布置(组件)。
与组件的制备方式无关,现在至少部分地去除该组件中的组合物的溶剂。由此可以促进纳米线在惰性表面上的聚集。
之后,如图14所示,将结构模板610移除。由此获得了在惰性表面640上的金属结构体660。
1.1.实施例
TEM照片用JEM 2010(JEOL,德国)在200kV下拍摄。SEM照片用Quanta 400ESEM(FEI,德国)拍摄。用Cary 5000(Varian)记录光学测量值。采用玻璃衬底的光谱作为基线。电流/电压测量采用Keithley 2450型电流计进行。
金纳米线按照H.Feng,Y.Yang,Y.You,G.Li,J.Guo,T.Yu,Z.Shen,T.Wu,B.Xing,Chem.Commun.2009,1984和J.H.Μ.Maurer,L.González-García,B.Reiser,I.Kanelidis,T.Kraus,ACS Appl.Mater.Interfaces 2015,7,7838制备。
为此,将30mg HAuCl4xH2O溶解在5.8ml正己烷(99%,ABCR,德国)和1.7ml油胺((Z)-十八碳-9-烯胺,工业级,70%,Sigma-Aldrich,德国Steinheim)的混合物中。加入1.5ml三异丙基硅烷(98%,ABCR,德国)并将该溶液在室温下静置过夜。通过加入乙醇使纳米线沉淀。去除上清液并将纳米线重新分散在正己烷中。重复一次所述洗涤步骤,然后将纳米线重新分散在环己烷中,以获得金浓度为4mg/ml或8mg/ml的溶液。
将30μL分散在环己烷中的金纳米线组合物(4mg/ml,8mg/ml)提供到衬底上。之后,立即将由PDMS制成的结构化印模压到衬底上。由此将该组合物压入到印模的凹槽中。该印模包括直径为4μm的圆柱形凸起的六角形阵列和5μm的凸起间距(中心到中心)。凸起的高度为5μm。当溶剂蒸发时,在凹槽中形成金纳米线的束,这些束复制了凹槽的结构。移除印模后,将结构体在室温下用氢等离子体(由在氩气中的5%氢气构成的混合物)处理15分钟(RFPICO等离子体***(Diener electronic,Ebhausen,德国)0.3mbar,100W)。
取决于组合物中金纳米线的浓度,可控制所获得的结构体的厚度。当使用4mg/ml的浓度时,获得平均厚度为15nm的结构体。最小宽度为250nm(图5a))。当使用8mg/ml时,可以获得平均厚度为45nm和最小宽度为600nm的结构体(图5b))。在此,最小宽度对应于结构体的在SEM范围内找到的最小宽度。
图6a)示出了获得的网格的透射光谱。图5a)中的网格示出了在整个可见区域上的高透射率(上方的线)。图5b)中的网格也示出了最高达68%的高透射率(下方的线)。这些值与具有相同覆盖范围的网格的计算值高度一致。测得的雾度值为1.6%(图5a)和2.7%(图5b)。这低于显示器通常所需的值(<3%)。
图6b)示出了相应的电压/电流图。较薄的网格显示出227Ω/sq的电阻率,较厚的网格具有29Ω/sq的电阻率。这些值高于纯金的网格的计算值(当d=5μm,w=250nm,h=15nm时为32.5Ω/sq,并且当d=5μm,w=600nm,h=45nm时4.5Ω/sq,而金的电阻率为2.44×10-8Ωm)。然而,这可归因于网格中的不规则性,例如由烧结后的晶界以及未连接的网格接片造成的。
图7显示了弯曲试验的结果。在该图中,相对于弯曲循环的次数绘制电阻率相对于初始电阻率((R-R0)/R0)的变化。样品在弯曲半径为5mm的张力下弯曲。对于试验,使用10个在PET上的根据本发明的网格,所述网格的初始平均电阻率为100Ω/sq(AuNM)。对照试验所使用的是市售可得的在PET上的ITO网格,其电阻率为100Ω/sq(ITO在PET上,Sigma-Aldrich,R0=100Ω/sq)。几个周期后,对照样品的电阻率上升几个数量级。对于本发明的网格,在前50个周期内的上升低于一个数量级,随后是在450个周期后朝向(R-R0)R0=0.056的渐近线趋势。因此,本发明的网格也适用于柔性衬底。
图8显示了细的金纳米线的柔韧性的一个实例。R值表示与弯曲匹配的圆的半径。可以观察到最高达20nm的弯曲半径而不会导致纳米线断裂。
I.2.制备印模
PDMS印模是用有机硅模板制备的。将PDMS试剂盒(Sylgard 184,Dow Corning)的预聚物和交联剂以10:1(重量比)的比例混合并脱气。将该混合物填充到事先用三氯(十八烷基)硅烷(Sigma-Aldrich,St.Louis,MO,USA)硅烷化的模板中,并在70℃下硬化。之后,从模板上取下印模。
I.3.对照例
包括市售可得的银纳米线(Seashell Technology;直径130nm+/-10nm;长度35μm+/-15μm)的组合物以类似于实施例的方式制备并被施加至表面。已表明不产生聚集。纳米线也不可通过施加印模而移动,因此不会形成结构体。
图19示出了采用相同印模以类似的方式实施本发明方法。已表明不会导致结构化。
较大的印模(柱状凸起的直径为25μm,中心间隔为50μm)也不会导致结构化(图20)。
II.用惰性表面进行结构化
II.1.制备PDMS印模
接下来描述由PDMS(硅橡胶)制备压印印模作为镍母版铸件:
II.1.A.镍母版和铸模的描述
镍母版是电解制备的镍箔,例如尺寸为100mm×100mm的镍箔,其上施加了微结构体(直径大于1μm的规则排列的圆柱形柱)。该镍箔被粘接到由铝或类似材料制成的铸模的基座上,或者通过铁磁性粘接膜安装在所述基座上。这里应该注意的是,镍母版必须绝对以平面方式施加,因为任何不均匀性都会反映在后面的印模中。
此外,铸模必须放置在尽可能水平的位置,以使压印印模后来具有均匀的厚度。
II.1.B.硅橡胶和模具铸件的混合
将聚二甲基硅氧烷(PDMS)(例如Dow Corning的Sylgard 184)的基础材料和硬化剂以合适的比例(例如10:1)组合在一起,并通过搅拌混合两种组分。待混合的量由压印印模的所需厚度决定(典型的印模厚度:2至4毫米)。混合容器的容量应为混合物体积的3倍,以防止随后的脱气过程中的溢出。
为了去除在搅拌过程中混入的气泡,将混合物引入真空干燥箱(在室温下)并抽真空直到所有气泡已被去除。
这时将脱气的PDMS混合物倒入铸模中并使混合物硬化。在大多数情况下,合理的是通过对铸模进行热处理来加速硬化。通常,将铸模在70℃下加热一小时会导致PDMS完全硬化。
II.1.C.脱模过程
PDMS印模的脱模如下实现:使用手术刀或其它锋利的刀片将PDMS从铸模的垂直壁在整个圆周上切开,然后用扁平和钝的工具(例如,扁平的刮铲)将其从边缘提离,然后小心地从镍母版脱开。此时用锋利的刀片(例如地毯刀)切掉边缘处的不规则性。
II.2.衬底表面的官能化:
接下来描述(疏水的)防粘涂层材料的制备:
II.2.A.清漆制备
用量:
267.8克 甲基三乙氧基硅烷(MTEOS)
84.8克 四乙氧基硅烷(TEOS)
150.0克 Levasil 300/30
3.0克 浓(37%)盐酸
13.35克 全氟辛基三乙氧基硅烷(Dynasylan F 8261)
518.95克异丙醇
程序:
向具有内部温度计的2L反应器(具有连接上的冷却器的夹套容器)中加入所称取的量的MTEOS和TEOS。加入所称取的量的Levasil,并允许剧烈搅拌2-3分钟。然后加入所称取的量的浓盐酸并进一步搅拌。观察反应溶液和温度计上的内部温度,记录观察结果。此时反应器内的温度不应超过60℃。搅拌10-15分钟后,加入所称取的量的全氟辛基三乙氧基硅烷,并进一步搅拌30分钟。然后加入所称取的量的异丙醇并搅拌15分钟。将材料装填到2L玻璃瓶中,然后借助压滤(预滤器+0.45μm过滤器)进行过滤。完成的清漆被装填到2L Schott玻璃瓶中并储存在冰箱中直到进一步使用。
II.2.B.制备层
将所述清漆通过旋涂(1000rpm/分钟,30秒)进行涂覆并在烘箱中烘烤(空气气氛;在30分钟内加热至100℃;保持30分钟,在240分钟内加热至250℃,保持1小时,冷却)。
II.3.银纳米线溶液
接下来描述用于制备层的来自Cambrios的银纳米线溶液(溶剂:乙二醇)的制备:
II.3.A.通过错流过滤进行纯化和溶剂交换
将200ml在乙二醇中的银纳米线溶液用200ml纯H2O(Millipore)稀释并充入大玻璃烧杯中。借助蠕动泵(流速:1.2ml/秒),将溶液泵送通过滤筒(材料:PES;孔径:0.5μm;SpectrumLabs公司;型号:Microkros3x0.5μmPES 1.0mm MLL x FLL干燥(4/PK))。将分离的滤液收集在收集容器中。渗余物通过软管导入大玻璃烧杯。过滤这样长时间,直至分离出200毫升滤液。
该过程进行两次,以尽可能多地去除干扰性的银颗粒。纳米线溶液的纯度>90%。
II.3.B测定纯化的纳米线溶液在水中的银含量
称重前,手动搅动样品。称重在50ml玻璃烧瓶中进行,然后向样品中加入2ml HNO3(65%),并用超纯水填充。为了避免基质效应,标准样与样品的酸含量相匹配。为了验证可重复性,3次称量是并行进行的。
标准样:
元件 S0 S1 S2
Ag(mg/L) 0.0 5.0 8.0
仪器参数:
-ICP OES,Horiba Jobin Yvon Ultima 2
-银测定:Cinical雾化器:压力:2.00巴,流速:0.781/分钟
-Ag:λ=328.068nm
测定得到0.295重量%+/-0.002的银含量。
II.3.C.重新进行溶剂交换以获得具有与水基银纳米线溶液不同的流平性的涂覆溶液
将5ml纯化的银纳米线水溶液与2ml1-氨基-2-丁醇,5μlTODS(3,6,9-三氧杂癸酸)和10ml丙酮混合,并离心(速度:rcf=2000;持续时间:1分钟)。将所得上清液倾出,并将形成的沉淀物再分散在10ml1-氨基-2-丁醇中。
II.4.纳米压印1
接下来描述借助PDMS印模制备银纳米线的网格结构体(变体1),其中银纳米线按网格线排列:
II.4.A.在样品制备前不久准备银纳米线溶液的描述
在样品制备之前不久,借助涡旋器(Heidolph公司,型号:Reax control,速度:2500rpm)抖动其中存在纳米线溶液的样品容器,以便再分散沉淀物。
II.4.B.涂覆过程
将涂有抗粘附涂层材料(参见第II.2点)的玻璃衬底(尺寸:10cm×10cm×0.11cm)平放在实验室工作台上。中间施加一滴(体积:20μL)所准备的纳米线溶液。
手动按压结构化的PDMS印模(其制备在第1点中描述),使得溶液均匀分布在印模下并且排挤多余的材料。
为了蒸发掉多余的溶剂,将样品(衬底+印模)放置在加热板上并加热至50℃。在此过程中,将金属板(重量:800g)置于PDMS印模上以确保印模在衬底上的最佳的均匀粘合。15分钟后,将样品组件(衬底→印模→金属板)从电热板上取下并放在实验台上冷却。
一旦样品冷却,首先将金属板取下,一只手使衬底稳定在台面上,另一只手通过拉拔来去除PDMS印模。
II.4.C.涂覆过程变体2
将具有网格结构体(其制备描述于第1点中,线宽度15μm)的PDMS印模以其反面(未结构化)放置在未涂覆的玻璃衬底(尺寸:5cm×5cm×0.11cm)上。在PDMS印模的结构化侧,将所准备的纳米线溶液的液滴(体积:20μL)施加于边缘处。
借助一种刮板(在此为剃须刀片),将纳米线溶液的液滴均匀分布在PDMS印模的结构化表面上。
随后,用手将经涂覆的玻璃衬底(尺寸:5cm×5cm×0.11cm,涂覆有抗粘附涂层材料)以涂覆侧压到覆盖有纳米线的PDMS印模上。
将样品组件(未涂覆的玻璃衬底→PDMS印模→经涂覆的玻璃衬底)翻转并以在加热板上用金属板(重量:800g)加重的方式在50℃下干燥。1小时后,将样品组件从加热板上取下并放在实验台上冷却。一旦样品冷却,首先去除金属板,一只手使经涂覆的衬底稳定,另一只手通过拉拔来去除PDMS印模和未涂覆的玻璃衬底。
II.4.D.表征
1.透射率的测量:
借助光谱仪(仪器:Ocean Optics QEPro,灯:DH-2000-BAL)测定透射率。
2.电导率的测定:
借助两点测量仪(Keithley公司,仪器:2000万用表)在5mm×5mm的相应区域上测定电导率,其中在两个相对侧上用银导电漆形成触头。
II.5.纳米压印2
接下来描述借助PDMS印模由银纳米线制备网格结构体(变体2),其中银纳米线被布置在正方形网格区域中,并且这些区域分别通过网格状排列的线彼此分开:
II.5.A.经抗粘附涂覆的衬底的预处理
将具有网格结构体的PDMS印模(其制备描述于第1点中)放置在涂覆有抗粘附涂层材料(见第2点)的玻璃衬底(尺寸:10cm×10cm×0.11cm)上。然后,使衬底连同置于其上的印模在等离子室中经受等离子体处理(持续时间:30分钟,气体:氧气)。PDMS印模仅被放置并且未被按压,以便由此使印模的网格结构体的正方形区域亲水化。原本疏水的、经涂覆的衬底在等离子体处理之后也是亲水的。
II.5.B.在样品制备前不久准备银纳米线溶液的描述
在样品制备之前不久,借助涡旋器(Heidolph公司,型号:Reax control,速度:2500rpm)抖动其中存在纳米线溶液的样品容器,以便再分散沉淀物。
II.5.C.涂覆过程
将亲水化的衬底平放在实验室工作台上。在中间施加一滴(体积:20μL)所准备的纳米线溶液,并且用手按压亲水化的PDMS印模,使得溶液在印模下方均匀分布并且排挤出多余材料。为了蒸发掉多余的溶剂,将样品(衬底+印模)放置在加热板上并加热至50℃。在此过程期间,将金属板(重量:800克)放在PDMS印模上。15分钟后,将样品组件(衬底→印模→金属板)从加热板上取下并放在实验台上冷却。一旦样品冷却,首先将金属板取下,一只手使衬底稳定在台面上,另一只手通过拉拔来去除PDMS印模。
引用文献
H.Feng,Y.Yang,Y.You,G.Li,J.Guo,T.Yu,Z.Shen,T.Wu,B.Xing,Chem.Commun.2009,1984.
J.H.M.Maurer,L.González-García,B.Reiser,I.Kanelidis,T.Kraus,ACSAppl.Mater.Interfaces 2015,7,7838.
Claims (14)
1.一种制备金属结构体的方法,包括以下步骤:
(a)提供包括纳米线和至少一种溶剂的组合物;
(b)使组合物在衬底上结构化;
(c)至少部分地去除所述溶剂。
2.根据权利要求1所述的方法,其特征在于,通过将所述组合物涂覆在衬底上并且随后将结构模板施加到衬底上、同时使所述组合物部分地移位来实现涂覆和结构化。
3.根据权利要求1或2所述的方法,其特征在于,通过将所述组合物涂覆到结构化掩模中来实现涂覆和结构化。
4.根据权利要求1至3中任一项所述的方法,其特征在于,至少50重量%的纳米线具有超过1μm的长度。
5.根据权利要求1至4中任一项所述的方法,其特征在于,至少50重量%的纳米线具有至少500:1的长度对直径的长径比。
6.根据权利要求1至5中任一项所述的方法,其特征在于,纳米线是金属纳米线。
7.根据权利要求1至6中任一项所述的方法,其特征在于,纳米线具有低于15nm的平均直径。
8.根据权利要求1至7中任一项所述的方法,其特征在于,纳米线具有低于5nm的平均直径。
9.根据前述权利要求中任一项所述的方法,其特征在于,在进一步的步骤中对获得的结构体进行热处理或用等离子体进行处理。
10.根据权利要求1至6中任一项所述的方法,其特征在于,衬底具有包括至少一种含氟化合物的表面。
11.根据权利要求10所述的方法,其特征在于,纳米线具有低于100nm的平均直径。
12.经涂覆的衬底,其通过根据权利要求1至11中任一项所述的方法获得。
13.根据权利要求12所述的经涂覆的衬底,其特征在于,经涂覆的衬底和金属结构体看上去至少部分透明。
14.根据权利要求12或13中所述的衬底的用途,该衬底作为导体轨道在电子应用中,在触摸屏显示器、太阳能收集器、显示器中,作为RFID天线,或在晶体管中使用。
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AU2016320291A1 (en) | 2018-03-15 |
WO2017042094A1 (de) | 2017-03-16 |
CN116313235A (zh) | 2023-06-23 |
ES2891753T3 (es) | 2022-01-31 |
EP3347303A1 (de) | 2018-07-18 |
DE102015115004A1 (de) | 2017-03-09 |
US20180251370A1 (en) | 2018-09-06 |
KR20180049044A (ko) | 2018-05-10 |
EP3347303B1 (de) | 2021-07-28 |
CN108137310B (zh) | 2023-12-19 |
US10941035B2 (en) | 2021-03-09 |
JP2018536962A (ja) | 2018-12-13 |
AU2016320291B2 (en) | 2021-04-01 |
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