CN106711276A - 制造图案化导体的方法 - Google Patents
制造图案化导体的方法 Download PDFInfo
- Publication number
- CN106711276A CN106711276A CN201611034509.3A CN201611034509A CN106711276A CN 106711276 A CN106711276 A CN 106711276A CN 201611034509 A CN201611034509 A CN 201611034509A CN 106711276 A CN106711276 A CN 106711276A
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- Prior art keywords
- fiber
- patterning
- conductive layer
- substrate
- mask
- Prior art date
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- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 3
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Classifications
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- 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
- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
-
- 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
- H10K71/621—Providing a shape to conductive layers, e.g. patterning or selective deposition
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- 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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/02—Local etching
-
- 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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F4/00—Processes for removing metallic material from surfaces, not provided for in group C23F1/00 or C23F3/00
-
- 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
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
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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
- H01B13/0036—Details
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
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- H—ELECTRICITY
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- 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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Abstract
提供了一种制造图案化导体的方法,所述方法包含:提供衬底,所述衬底包含:上面沉积有导电层的基材;提供导电层蚀刻剂;提供纺纱材料,所述纺纱材料包含:载体;以及光敏掩模材料;提供显影剂;形成多个掩模纤维,并将它们沉积到所述导电层上,形成多个沉积的纤维;使所述多个沉积的纤维图案化,以提供处理的纤维部分和未处理的纤维部分;显影所述多个沉积的纤维,其中去除所述处理的纤维部分或所述未处理的纤维部分,留下图案化的纤维阵列;使所述导电层接触所述导电层蚀刻剂,其中去除未被所述图案化的纤维阵列覆盖的所述导电层,在所述衬底上留下图案化的导电网络。
Description
本发明总体涉及制造图案化的导体的领域。具体地,本发明涉及制造图案化的透明导体的领域。
呈现高度透明及高传导性的膜在广泛的电子应用中用作电极或涂层具有重要的价值,所述电子应用包括例如触屏显示器和光电池。当前用于这些应用的技术涉及使用通过物理气相沉积法沉积的含有掺杂锡的氧化铟(ITO)的膜。物理气相沉积法的高成本费用导致期望发现替代的透明导电材料和涂布方法。银纳米线分散为渗透网络的用途有希望成为含ITO膜的替代物。银纳米线的使用潜在地提供了可使用卷绕对位技术加工的优点。因此,银纳米线提供了如下优点:低制造成本,有潜力提供比常规含ITO的膜高的透明度和传导性。
在电容式触摸屏的应用中,需要导电图案。此类应用的一个关键挑战是人眼必须看不到(或者几乎看不到)形成的图案。
一种方法是Allemand等在美国专利No.8,018,568中公开的提供基于纳米线的图案化的透明导体。Allemand等公开了光学均匀的透明导体,包含:衬底;衬底上的导电膜,所述导电膜包括多个相互连接的纳米结构,其中导电膜上的图案限定了(1)具有第一电阻率、第一透射率和第一雾度的未蚀刻的区域以及(2)具有第二电阻率、第二透射率和第二雾度的蚀刻的区域;并且,其中,所述蚀刻的区域的传导性小于未蚀刻的区域,第一电阻率与第二电阻率的比为至少1000;第一透射率与第二透射率差异小于5%;并且第一雾度与第二雾度的差异小于0.5%。
Joo等在美国专利No.9,066,425中公开了生产图案化的透明导体的另一种方法。Joo等公开了提供制造图案化的导体的方法,包含:提供导电化衬底,其中所述导电化衬底包含衬底和导电层;提供导电层蚀刻剂;提供纺织材料;提供掩模纤维溶剂;形成多个掩模纤维,并且将多个掩模纤维沉积到导电层上;暴露所述导电层于导电层蚀刻剂,其中从所述衬底上去除未被所述多个掩模纤维覆盖的导电层,从而在多个掩模纤维覆盖的衬底上留下相互连接的导电网络;以及暴露多个掩模纤维于掩模纤维溶剂,其中去除多个掩模纤维,以在衬底上暴露互相连接的导电网络。
尽管如此,仍需要制造图案化的导体的替代方法。具体地,仍需要制造具有导电区和非导电区的图案化的透明导体的替代方法,其中,人眼基本上不能辨别导电区和非导电区,并且其中,使需要的工艺步骤的数目最少。
本发明提供了制造图案化的导体的方法,包含:提供衬底,其中,所述衬底包含:基材;以及导电层,其中所述导电层沉积在所述衬底上;提供导电层蚀刻剂;提供纺织材料,其中,所述纺织材料包含:载体;以及掩模材料,其中,所述掩模纤维为光敏材料;提供显影剂;通过选自由以下组成的群组中的工艺加工所述纺织材料而形成多个掩模纤维:电纺、喷气电纺、无针电纺和熔体电纺;在所述导电层上沉积所述多个掩模纤维,从而形成多个沉积的纤维;任选地,在所述导电层上压紧所述多个沉积的纤维;使所述多个沉积的纤维图案化,以改变所述多个沉积的纤维的选择部分的性质,从而提供处理的纤维部分和未处理的纤维部分;通过使所述多个沉积的纤维接触所述显影剂而显影所述多个沉积的纤维,其中,去除所述(i)处理的纤维部分或(ii)所述未处理的纤维部分;留下图案化的纤维阵列;使所述导电层接触所述导电层蚀刻剂,其中,从所述衬底上去除未被所述图案化的纤维阵列覆盖的所述导电层,在所述衬底上留下被所述图案化的纤维阵列覆盖的图案化的导电网络,以提供所述图案化的导体;任选地,提供剥离剂;以及,任选地,用所述剥离剂处理所述图案化纤维阵列,其中去除所述图案化的纤维阵列,以在所述衬底上暴露所述图案化的导电网络。
本发明提供了制造图案化的导体的方法,包含:提供衬底,其中所述衬底包含:基材;以及导电层,其中所述导电层沉积在所述衬底上;提供导电层蚀刻剂;提供纺织材料,其中所述纺织材料包含:载体;以及掩模材料,其中所述掩模纤维为光敏材料;提供显影剂;通过选自由以下组成的群组中的工艺加工所述纺织材料而形成多个掩模纤维:电纺、喷气电纺、无针电纺和熔体电纺;在所述导电层上沉积所述多个掩模纤维,从而形成多个沉积的纤维;任选地,在所述导电层上压紧所述多个沉积的纤维;使所述多个沉积的纤维图案化,以改变所述多个沉积的纤维的选择部分的性质,从而提供处理的纤维部分和未处理的纤维部分;通过使所述多个沉积的纤维接触所述显影剂而显影所述多个沉积的纤维,其中去除所述(i)处理的纤维部分或(ii)所述未处理的纤维部分;留下图案化的纤维阵列;使所述导电层接触所述导电层蚀刻剂,其中从所述衬底上去除未被所述图案化的纤维阵列覆盖的所述导电层,在所述衬底上留下被所述图案化的纤维阵列覆盖的图案化的导电网络,以提供所述图案化的导体;提供剥离剂;以及用所述剥离剂处理所述图案化的纤维阵列,其中去除所述图案化的纤维阵列,以在所述衬底上暴露所述图案化的导电网络。
本发明提供了制造图案化的导体的方法,包含:提供衬底,其中所述衬底包含:基材;以及导电层,其中所述导电层沉积在所述衬底上;提供导电层蚀刻剂;提供纺织材料,其中所述纺织材料包含:载体;以及掩模材料,其中所述掩模纤维为光敏材料;提供显影剂;通过选自由以下组成的群组中的工艺加工所述纺织材料而形成多个掩模纤维:电纺、喷气电纺、无针电纺和熔体电纺;在所述导电层上沉积所述多个掩模纤维,从而形成多个沉积的纤维;在所述导电层上压紧所述多个沉积的纤维;使所述多个沉积的纤维图案化,以改变所述多个沉积的纤维的选择部分的性质,从而提供处理的纤维部分和未处理的纤维部分;通过使所述多个沉积的纤维接触所述显影剂而显影所述多个沉积的纤维,其中去除所述(i)处理的纤维部分或(ii)所述未处理的纤维部分;留下图案化的纤维阵列;使所述导电层接触所述导电层蚀刻剂,其中从所述衬底上去除未被所述图案化的纤维阵列覆盖的所述导电层,在所述衬底上留下被所述图案化的纤维阵列覆盖的图案化的导电网络,以提供所述图案化的导体;提供剥离剂;以及用所述剥离剂处理所述图案化纤维阵列,其中去除所述图案化的纤维阵列,以在所述衬底上暴露所述图案化的导电网络。
本发明提供了根据本发明的方法制作的图案化的透明导体。
具体实施方式
本文中以及所附权利要求书中使用的术语“总透射率”是指根据ASTM D1003-11e1测量的本发明的图案化的透明导体呈现的光透射(按照%)。
本文中以及所附权利要求书中使用的术语“雾度”是指根据ASTM D1003-11e1测量的本发明的图案化的透明导体呈现的雾度(按照%)。
使用本发明的方法制作的图案化的导体用于各种应用,例如电磁屏蔽应用。使用本发明的方法制作的优选的图案化的透明导体特别用于电容触屏应用。为用于此类应用,需要提供具有导电区域和非导电区域的图案的透明导体。提供此类图案化的透明导体的一个重大挑战为使总透射率最大,并使雾度最小。另一个挑战为减少获得图案化的透明导体需要的工艺步骤的数目。本发明的方法能够使用比常规ITO工艺平板印刷方法所需的显著少的工艺步骤制备图案化的透明导体。
本发明制造图案化的导体(优选地,图案化的透明导体)的方法优选包含:提供基底(优选导电化的透明基底;更优选金属化的透明基底),其中所述基底包含:基材(优选地,其中所述基材为透明材料);以及导电层(优选导电金属层),其中所述导电层沉积在基材上;提供导电层蚀刻剂;提供纺织材料,其中所述纺织材料包含:载体;以及掩模材料,其中所述掩模材料为光敏材料(例如正向光阻材料或负向光阻材料);提供显影剂;通过选自由以下组成的群组中的工艺加工所述纺织材料而形成多个掩模纤维:电纺、喷气电纺、无针电纺和熔体电纺;在所述导电层上沉积所述多个掩模纤维,从而形成多个沉积的纤维;任选地,包含在所述导电层上压紧所述多个沉积的纤维;使所述多个沉积的纤维图案化,以改变所述多个沉积的纤维的选择部分的性质,从而提供处理的纤维部分和未处理的纤维部分;通过使所述多个沉积的纤维接触所述显影剂而显影所述多个沉积的纤维,其中去除(i)所述处理的纤维部分或(ii)所述未处理的纤维部分;留下图案化的纤维阵列;使所述导电层接触所述导电层蚀刻剂,其中从所述衬底上去除未被所述图案化纤维阵列覆盖的所述导电层,在所述衬底上留下被所述图案化的纤维阵列覆盖的图案化的导电网络,以提供所述图案化的导体;任选地,提供剥离剂;任选地,用所述剥离剂处理所述图案化纤维阵列,其中去除所述图案化的纤维阵列,以在所述衬底上暴露所述图案化的导电网络。
优选地,在本发明的方法中,提供的衬底包含选自任何已知基材的基材。优选地,所述基材为透明基材,包括透明导电基材和透明不导电基材两者。优选地,在本发明的方法中,提供的衬底包含基材,其中所述基材为选自由以下组成的群组的透明基材:聚对苯二甲酸乙二醇酯(PET)、聚碳酸酯(PC)、聚甲基丙烯酸甲酯(PMMA);聚萘二甲酸乙二醇酯(PEN)、聚醚砜(PES)、环烯烃聚合物(COP)、三乙酰纤维素(TAC)、聚乙烯醇(PVA)、聚酰亚胺(PI)、聚苯乙烯(PS)(例如,双向拉伸聚苯乙烯)、聚硫醇和聚芳醚酮(例如聚醚醚酮(PEEK))和玻璃(例如可从Dow Corning获得的玻璃和玻璃)。更优选地,在本发明的方法中,提供的衬底包含基材,其中,所述基材为选自由以下组成的群组的透明基材:玻璃、聚乙烯、聚对苯二甲酸乙二醇酯、聚碳酸酯和聚甲基丙烯酸甲酯。最优选地,在本发明的方法中,提供的衬底包含基材,其中所述基材为聚对苯二甲酸乙二醇酯。
优选地,在本发明的方法中,提供的衬底包含选自任何导电材料的导电层。优选地,在本发明的方法中,提供的衬底包含导电层,其中导电层包含导电金属或金属氧化物。优选地,在本发明的方法中,提供的衬底包含导电层,其中导电层为选自由以下组成的群组的导电金属层:银、铜、钯、铂、金、锌、硅、镉、锡、锂、镍、铟、铬、锑、镓、硼钼、锗、锆、铍、铝、镁、锰、钴、钛,它们的合金及氧化物。更优选地,在本发明的方法中,提供的衬底包括导电层,其中所述导电金属层选自由银以及银与选自由以下组成的群组中的至少一种元素的合金组成的组:铜、钯、铂、金、锌、硅、镉、锡、锂、镍、铟、铬、锑、镓、硼钼、锗、锆、铍、铝、镁、锰、钴和钛。最优选地,在本发明的方法中,提供的衬底包含导电层,其中所述导电金属层为银。
优选地,在本发明的方法中,提供的衬底包含基材和导电层,其中导电层沉积在衬底上。更优选地,在本发明的方法中,通过使用已知的技术连接而在基材上沉积导电层(优选地,其中基材为透明材料)。优选地,通过拿导电箔或片并使用粘合剂压到基材的表面上而在基材上沉积导电层(优选地,其中基材为透明材料)。优选地,在本发明的方法中,使用选自由以下组成的群组的方法通过在基材的表面上沉积图案化的导体而在基材上沉积导电层(优选地,其中基材为透明材料):溅射、等离子喷涂、热喷涂、电沉积、化学气相沉积(例如等离子体增强化学气相沉积、金属有机物化学气相沉积)、原子层沉积、物理气相沉积、脉冲激光沉积、阴极电弧沉积、电镀、无电镀和电流体沉积。优选地,在本发明的方法中,使用选自由以下组成的群组的方法通过在基材的表面上沉积图案化的导体而在基材上沉积导电层(优选地,其中基材为透明材料):化学液体沉积、喷漆、浸涂、旋涂、刮刀涂布、接触涂布、凹板式涂敷、丝网印刷、喷墨打印和移印。最优选地,在本发明的方法中,通过在基材的表面上溅射沉积图案化的导体而在基材上沉积导电层(优选地,其中基材为透明材料)。
优选地,在本发明的方法中,提供的衬底包含沉积在基材(优选地,其中所述基材为透明材料)上的导电层,其中导电层具有10-200nm(更优选50-150nm,最优选90-110nm)的平均厚度。
优选地,在本发明的方法中,进一步包含:提供粘合促进物质,并在沉积多个掩模纤维到图案化的导体上之前,施加粘合促进物质到导电层;其中粘合促进物质促进多个掩模纤维粘合到导电层。
用在本发明方法中的纺织材料优选包含掩模纤维。更优选,纺织材料包含掩模纤维和载体。本领域普通技术人员已知选择用作掩模纤维和载体的合适材料。优选的掩模纤维为光敏材料(例如正向光阻材料或负向光阻材料),适于通过选自由以下组成的群组的方法沉积:电纺、喷气电纺、无针电纺和熔体电纺;并且当暴露导电层(优选金属导电层)于导电层蚀刻剂(优选金属蚀刻剂)时适于作为抗蚀剂。优选地,掩模材料选自(a)重氮萘醌和酚醛树脂的混合物;以及(b)(烷基)丙烯酸烷基酯和烷基丙烯酸的混合物。更优选地,掩模材料为(烷基)丙烯酸烷基酯和烷基丙烯酸的混合物。进一步更优选地,掩模材料为(C1-4烷基)丙烯酸C1-5烷基酯和C1-5烷基丙烯酸的混合物。最优选地,掩模材料为甲基丙烯酸甲酯和甲基丙烯酸的共聚物。优选地,掩模材料为(烷基)丙烯酸烷基酯和烷基丙烯酸的共聚物,其中,共聚物包含5-15mol%(更优选5-10mol%,最优选6-9mol%)的烷基丙烯酸。更优选地,掩模材料为(C1-4烷基)丙烯酸C1-5烷基酯和C1-5烷基丙烯酸的共聚物,其中,所述共聚物含有5-10mol%(更优选5-10mol%,最优选6-9mol%)的C1-5烷基丙烯酸。最优选地,掩模材料为甲基丙烯酸甲酯和甲基丙烯酸的共聚物,其中,共聚物含有5-10mol%(更优选5-10mol%,最优选6-9mol%)的甲基丙烯酸。优选地,共聚物具有10,000-1,000,000g/mol(优选50,000-500,000g/mol,更优选75,000-300,000g/mol,最优选150,000-250,000g/mol)的数目平均分子量MN。优选地,载体选自氯仿、乳酸乙酯、甲基乙基酮、丙酮、丙醇、甲醇、异丙醇、四氢呋喃(THF)、二甲亚砜(DMSO)和丙烯腈(AN)的至少一种(优选地,载体是乙酸乙酯)。优选地,载体中,纺织材料含有5-25wt%(更优选7.5-20wt%,最优选8-15wt%)的掩模材料。
优选地,在本发明的方法中,通过选自由以下组成的群组的方法将纺织材料形成为纤维并沉积到导电层上:电纺、喷气电纺、无针电纺和熔体电纺。更优选地,在本发明的方法中,纺织材料通过电纺形成为纤维并沉积到导电层上。更优选地,在本发明的方法中,纺织材料通过电纺形成为纤维并沉积到导电层上,其中通过具有中央开口的喷嘴给料纺织材料,形成多个掩模纤维并沉积多个掩模纤维到透明衬底上的图案化的导体上。本领域普通技术人员知道选择合适的电纺工艺条件。优选地,在本发明的方法中,以0.1-100μL/min(更优选1-50μL/min,更优选10-40μL/min,最优选20-30μL/min)的流速通过喷嘴给料纺织材料。
优选地,在本发明的方法中,设定喷嘴为相对于衬底的电势的应用正差异。更优选地,应用电位差为5-50kV(优选5-30kV,更优选5-25kV,最优选5-10kV)。
优选地,在本发明的方法中,进一步包含:在导电层上压紧多个沉积的纤维,以确保多个沉积的纤维与导电层之间良好的接触。优选地,在压紧多个沉积的纤维前,通过在两个非粘合的片(例如两个聚四氟乙烯片)之间放置上面具有导电层和多个沉积的纤维的衬底,压紧导电层上的多个沉积的纤维。
优选地,在本发明的方法中,进一步包含:烘烤多个沉积的纤维,以确保多个沉积的纤维在导电层上的良好润湿。优选地,在Tg至Tg+20℃的温度烘烤多个沉积的纤维,其中Tg为多个沉积的纤维的玻璃化转变温度。更优选地,通过在设定为75-120℃(优选80-110℃,更具体地90-105℃)的炉中放置衬底10分钟至2小时(优选20分钟至1小时,更优选30-45分钟),而烘烤多个沉积的纤维。
优选地,在本发明的方法中,使多个沉积的纤维图案化,以改变多个沉积的纤维的选择部分的性质,以提供处理的纤维部分和未处理的纤维部分。优选地,所述多个沉积的纤维是光敏材料。更优选地,多个沉积的纤维为光成像。优选地,通过处理多个沉积的纤维的选择部分,而使多个沉积的纤维图案化,以形成放射(例如光化放射、紫外光、电子、x射线),以提供处理的纤维部分。更优选地,通过处理多个沉积的纤维的选择部分,而使多个沉积的纤维图案化,以用合适的波长光化照射。优选地,在本发明的方法中,多个沉积的纤维的图案化导致处理的纤维部分的显影剂的溶解度相对于未处理的纤维部分的变化。优选地,多个沉积的纤维具有被动抗蚀性质,其中处理的纤维部分在图案化过程中暴露于辐射时在显影剂中呈现不溶性,而未处理的纤维部分在显影剂中保持可溶。优选地,多个掩模纤维可具有主动抗蚀性质,其中处理的纤维部分在图案化过程中暴露于辐射时在显影剂中呈现可溶,而未处理的纤维部分在显影剂中保持不溶。
优选地,在本发明的方法中,基于处理的纤维部分和未处理的纤维部分的相对溶解度而选择显影剂。优选地,显影剂选自由以下组成的群组:氢氧化钠、氢氧化钾、四甲基氢氧化铵、异丙醇、丙酮及其混合物。更优选地,显影剂为异丙醇和丙酮的混合物。更优选地,显影剂为80-95wt%(更优选地85-95wt%;最优选88-92wt%)的异丙醇和20-5wt%(更优选15-5wt%;最优选12-8wt%)丙酮的混合物。
优选地,在本发明的方法中,在通过接触多个沉积的纤维与显影剂而图案化之后,显影多个掩模纤维,其中去除(i)处理的纤维部分或(ii)未处理的纤维部分;留下图案化纤维阵列。优选地,在图案化之后显影多个沉积的纤维,以通过暴露多个沉积的纤维于显影剂而去除处理的纤维部分,留下图案化纤维阵列。优选地,在图案化之后显影多个沉积的纤维,以通过暴露于显影剂而去除处理的纤维部分;留下图案化纤维阵列。优选地,在图案化之后,通过浸入显影剂而显影多个沉积的纤维,留下图案化纤维阵列。更优选地,在图案化之后,通过浸入搅拌的显影剂浴而显影多个沉积的纤维,留下图案化纤维阵列。
优选地,在本发明的方法中,其上沉积图案化纤维阵列的导电层与导电层蚀刻剂接触,其中,从衬底去除未被图案化纤维阵列覆盖的导电层(优选地蚀刻掉),在被图案化纤维阵列覆盖的衬底上留下至少一个相互连接导电网络。本领域中的普通技术人员已知选择合适的用在本发明的方法中的导电层中的导电层蚀刻剂。优选地,当所述导电层是银时,所述导电层蚀刻剂选自由以下组成的群组:氢氧化铵/过氧化氢在甲醇中的溶液(优选1:1:4摩尔比的NH4OH:H2O2:CH3OH混合物);九水合硝酸铁(III)的水溶液(优选1wt%Fe(NO3)3、0.2wt%硫脲以及任选的10wt%乙醇的水溶液);以及磷酸/硝酸/醋酸水溶液(优选3:3:23:1摩尔比的H3PO4:HNO3:CH3COOH:H2O的混合物)。当所述导电层是银时,所述导电层蚀刻剂更优选选自由以下组成的群组:九水合硝酸铁(III)的水溶液(优选1wt%Fe(NO3)3、0.2wt%硫脲以及任选的10wt%乙醇的水溶液);以及磷酸/硝酸/醋酸水溶液(优选3:3:23:1摩尔比的H3PO4:HNO3:CH3COOH:H2O的混合物)。当所述导电层是银时,导电层蚀刻剂最优选为九水合硝酸铁(III)的水溶液(优选1wt%Fe(NO3)3、0.2wt%硫脲以及任选的10wt%乙醇的水溶液)。
优选地,在本发明的方法进一步包含:提供脱模组合物;涂布所述脱模组合物到所述图案化的纤维阵列,以去除所述图案化的纤维阵列,并暴露衬底上的导电网络。优选地,提供的脱模组合物为用于图案化的纤维阵列的良好溶剂。优选地,提供的脱模组合物选自聚乙烯醇、氯仿、甲基乙基酮、丙酮、丙醇、甲醇、异丙醇和它们的混合物(更优选地丙酮和异丙醇的混合物;最优选丙酮)。
优选地,在本发明的方法中,提供的脱模组合物任选地进一步包括一种或多种其它组分,例如润湿剂或表面活性剂,防冻剂和粘度调节剂。优选的表面活性剂包括非离子型表面活性剂和阴离子型表面活性剂。更优选的表面活性剂包括非离子型表面活性剂。优选地,基于所述组合物的总重量,提供的脱模组合物含有0-5wt%(更优选0.2-5wt%,更优选0.5-3.5wt%)的表面活性剂。
优选地,在本发明的方法中,在衬底上以受控图案形成相互连接导电网络。优选地,受控图案为至少一种相互连接导电网络。更优选地,受控图案为多个分离的相互连接导电网络,其中,多个分离的相互连接导电网络中的每个相互连接导电网络与多个分离的相互连接导电网络中的其它相互连接导电网络电绝缘。更优选地,受控图案为被非导电区域多重分割的相互连接导电网络。最优选地,受控图案为多个分离的、相互连接导电线路的网格,其中所述导电线路的每个分离的相互连接的网格通过衬底上的一个或多个非导电区域彼此分离。优选地,每个相互连接网格具有网格图案。网格图案包括例如直边多边形(例如棱形、正方形、长方形、三角形、六边形等);圆形;多曲线形状;曲线和直线组合的形状(例如半圆形);以及它们的组合。
优选地,在本发明的方法中,形成的多个掩模纤维具有窄的直径。认为窄的纤维直径促进了具有窄的线宽度的相互连接导电网络的形成,使得光穿过图案化的透明导体的阻碍最小,以使得透射率最大,雾度最小,以及人眼对相互连接导电网络的可见度最小。优选地,形成多个掩模纤维中的掩模纤维,并沉积在导电层上,其中,所述沉积的掩模纤维具有≤200μm的平均直径。更优选地,形成多个掩模纤维中的掩模纤维,并沉积在导电层上,其中,所述沉积的掩模纤维具有≤100μm的平均直径。更优选地,形成多个掩模纤维中的掩模纤维,并沉积在导电层上,其中,所述沉积的掩模纤维具有≤20μm的平均直径。最优选地,形成多个掩模纤维中的掩模纤维,并沉积在导电层上,其中,所述沉积的掩模纤维具有≤2μm的平均直径。
使用本发明的方法制造的图案化的导体优选呈现≤100Ω/sq(更优选≤50Ω/sq,进一步优选≤10Ω/sq,最优选≤5Ω/sq)的薄层电阻Rs(如使用实例中描述的方法测量)。
使用本发明的方法制造的图案化的导体优选呈现≥80%(更优选≥90%;最优选≥95%)的总透射率。
使用本发明的方法制造的图案化的导体优选呈现≤5%的雾度(更优选≤4%;更优选≤3%)。
现将在下面的实例中详细地描述本发明的一些实施例。
使用BYK Instrument的Haze-gard plus透明度仪根据ASTM D1003-11e1测量实例中报告的数据总透射率TTrans。
使用BYK Instrument的Haze-gard plus透明度仪根据根据ASTM D1003-11e1测量实例中报告的雾度HHaze。
使用Delcom 717B非接触电导检测仪根据ASTM F1844以及使用来自JandelEngineering Limited的Jandel HM-20共线4点探针检测设备根据ASTM F390-11测量图案化的导体的薄层电阻。
用在实例中的衬底为镀银的聚对苯二甲酸乙二醇酯膜,具有150nm的平均银层厚度(可从Materion Corporation获得)。
所述纺织材料包括用于实例的掩模纤维和载体。所述使用的掩模纤维为甲基丙烯酸甲酯与8.2-8.5mol%的具有200,000g/mol的数目平均分子量MN的甲基丙烯酸的共聚物。然后用乳酸乙酯溶解掩模材料,以提供10wt%的溶液。然后,在氮气吹扫下通过蒸发从10wt%的溶液中去除83wt%的乳酸乙酯,然后加30wt%的丙酮到,以提供纺织材料。
实例:图案化的透明导体的制备
使用来自IME Technologies的装备单喷嘴纺丝头和旋转鼓基质载体的台式电纺舱(具有100mm直径和220mm长度的鼓的模块EM-RDC)电纺多个沉积的纤维到衬底上,以形成多个沉积的纤维。使用的喷嘴具有0.5mm的内径。当电纺时,使用ProSense ModelNo.NE1000注射泵供给纺丝原料到喷嘴,设定ProSense Model No.NE1000注射泵以表1中列出的流速输送纺丝原料。在来自IME Technologies的金属化面朝外的Module EM-RDC旋转鼓集线器周围包裹衬底。用于实例中纺丝操作的其它参数如下:设定旋转基质与针之间的距离为8.5cm;设定衬底下方的鼓为-4kV;以表1记录的rpm设定旋转鼓集线器(y轴)上的鼓旋转速度;以表1记录的电压设定喷嘴;以表1记录设定针扫描速度(x轴);并且,设定针扫描距离为120mm。让纺丝操作进行1分钟。然后,在旋转鼓上旋转衬底90度(使得衬底在旋转鼓上旋转的方向垂直于第一纺纱通道),重新开始纺纱操作,并让其进行另外1分钟。
表1
在每个实例中,然后将具有多个沉积的纤维的衬底放在炉中,并在表2中说明的条件下烘烤。
表2
根据实例T1制备衬底,然后通过用聚乙烯块覆盖所述多个沉积的纤维的一部分,并暴露所述多个沉积的纤维的未覆盖部分于紫外光而使多个沉积的纤维图案化,使用环境条件下设定为200nm的截止和1J/cm2的强度Xenon UVB灯的脉冲Xenon RC 800。多个沉积的纤维的未覆盖部分经100秒的总暴露时间,每个25秒的4个循环,以提供处理的纤维部分。然后,通过放置衬底于显影浴中而显影处理的纤维部分,轻微的搅拌30秒,其中,浴中的显影剂为异丙醇和丙酮90/10wt%的溶液。在显影后,在观察到未处理的纤维部分保持完整的同时,观察到已经从衬底的表面上去除了处理的纤维部分。
在每个实例中,然后将其上剩余多个掩模纤维的衬底浸入1wt%的硝酸九水合硝酸铁(III)、0.2wt%的硫脲和10wt%的乙醇的水溶液浴中以表3记录的时间。然后在常温在3个连续的去离子水浴中给予衬底5秒的浸泡。然后让衬底在室温下空气干燥,留下具有多个沉积的纤维覆盖的相互连接的银网络的图案化的导体。
在每个实例中,然后通过在丙酮浴中浸入衬底5分钟,不搅动而除去所述多个沉积的纤维。然后,从所述丙酮浴除去衬底,并让其在室温条件下于空气中干燥,留下在其上具有暴露的互相连接的银网络的衬底。
然后,在每个样本的多个点测量根据每个实例制备的衬底的总透射率、TTrans,雾度,HHaze,以及薄层电阻。在表3中报道了这些测量的平均值。
表3
实例 | 蚀刻时间(分钟) | TTrans(%) | HHaze(%) | 薄层电阻(Ω/sq) |
TC1 | 3.33 | 89.98 | 2.1 | -- |
TC2 | 3.33 | 89.94 | 2.3 | -- |
TC3 | 3.33 | 90.01 | 0.7 | -- |
T1 | 3 | 87.4 | 2.2 | 17到50 |
T2 | 5 | 88.4 | 1.1 | 38 |
T3 | 30 | 85.4 | 1.3 | 8 |
T4 | 41 | 87.6 | 1.3 | 15 |
Claims (10)
1.一种制造图案化的导体的方法,其包含:
提供衬底,其中所述衬底包含:
基材;以及
导电层,其中所述导电层沉积在所述衬底上;
提供导电层蚀刻剂;
提供纺织材料,其中所述纺织材料包含:
载体;以及
掩模材料,其中所述掩模材料为光敏材料;
提供显影剂;
通过选自由以下组成的群组的工艺加工所述纺织材料形成多个掩模纤维:电纺、喷气电纺、无针电纺和熔体电纺;
在所述导电层上沉积所述多个掩模纤维,从而形成多个沉积的纤维;
任选地,在所述导电层上压紧所述多个沉积的纤维;
使所述多个沉积的纤维图案化,以改变所述多个沉积的纤维的选择部分的性质,从而提供处理的纤维部分和未处理的纤维部分;
通过使所述多个沉积的纤维接触所述显影剂而显影所述多个沉积的纤维,其中去除(i)所述处理的纤维部分或(ii)所述未处理的纤维部分;留下图案化纤维阵列;
使所述导电层接触所述导电层蚀刻剂,其中从所述衬底上去除未被所述图案化的纤维阵列覆盖的所述导电层,从而在所述衬底上留下被所述图案化的纤维阵列覆盖的图案化的导电网络,以提供所述图案化的导体;
任选地,提供剥离剂;以及
任选地,用所述剥离剂处理所述图案化的纤维阵列,其中去除所述图案化的纤维阵列,以在所述衬底上暴露所述图案化的导电网络。
2.根据权利要求1所述的方法,其中所述图案化的导体是图案化的透明导体。
3.根据权利要求2所述的方法,其中所述导电层是选自由以下组成的群组的导电金属层:银、铜、钯、铂、金、锌、硅、镉、锡、锂、镍、铟、铬、锑、镓、硼钼、锗、锆、铍、铝、镁、锰、钴、钛,它们的合金或氧化物。
4.根据权利要求3所述的方法,其中所述多个掩模纤维使用电纺形成和沉积到所述导电层上。
5.根据权利要求4所述的方法,其中所述图案化的导电网络是所述衬底上的受控图案。
6.根据权利要求3所述的方法,其中所述导电层是银。
7.根据权利要求6所述的方法,其中所述图案化的透明导体具有≥80%的总透射率,≤5%的雾度以及≤5Ω/sq的薄层电阻。
8.一种图案化的透明导体,其根据权利要求7所述的方法制造。
9.根据权利要求4所述的方法,其中所述掩模材料为(烷基)丙烯酸烷基酯和烷基丙烯酸的共聚物。
10.根据权利要求9所述的方法,其中所述掩模材料为(C1-4烷基)丙烯酸C1-5烷基酯和C1-5烷基丙烯酸的共聚物,其中所述共聚物含有5-10mol%的所述C1-5烷基丙烯酸。
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