CN106463199A - 导电糊剂、触控面板和导电图案的制造方法 - Google Patents
导电糊剂、触控面板和导电图案的制造方法 Download PDFInfo
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- CN106463199A CN106463199A CN201580024720.4A CN201580024720A CN106463199A CN 106463199 A CN106463199 A CN 106463199A CN 201580024720 A CN201580024720 A CN 201580024720A CN 106463199 A CN106463199 A CN 106463199A
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- Prior art keywords
- conductive paste
- conductive pattern
- pattern
- conductive
- compound
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1808—C8-(meth)acrylate, e.g. isooctyl (meth)acrylate or 2-ethylhexyl (meth)acrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F222/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
- C08F222/10—Esters
- C08F222/1006—Esters of polyhydric alcohols or polyhydric phenols
- C08F222/102—Esters of polyhydric alcohols or polyhydric phenols of dialcohols, e.g. ethylene glycol di(meth)acrylate or 1,4-butanediol dimethacrylate
- C08F222/1025—Esters of polyhydric alcohols or polyhydric phenols of dialcohols, e.g. ethylene glycol di(meth)acrylate or 1,4-butanediol dimethacrylate of aromatic dialcohols
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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Abstract
本发明的目的在于提供即使在高湿高热等环境下也能够稳定地维持接触电阻、并且可以制造与透明电极的连接可靠性高的微细的导电图案的导电糊剂。本发明提供的导电糊剂含有金属颗粒(A)、碳颗粒(B)、具有不饱和双键的化合物(C)、光聚合引发剂(D)、和溶剂(E)，上述金属颗粒(A)相对于上述碳颗粒(B)的质量比为20~1900。
Description
技术领域
本发明涉及导电糊剂和导电图案的制造方法。
背景技术
近年来，已开发了可以通过光刻法制造微细的导电图案的使导电填料分散在有机成分中而得到的导电糊剂(专利文献1及2)，其中，开发了特征在于与ITO等透明电极的连接可靠性高的导电糊剂(专利文献1)。
现有技术文献
专利文献
专利文献1 : 国际公开第2013/108696号
专利文献2 : 国际公开第2013/146107号。
发明内容
发明所要解决的课题
然而，对于使用以往的导电糊剂制造的如触控面板的周围布线那样的导电图案而言，被视为问题的是存在由于高温等热应力、湿度变化而导致在导电图案与ITO等透明电极的接触面处产生的电阻、即接触电阻变高的情况。
因此，本发明的目的在于提供即使经过高湿高热等环境变化也能够稳定地维持接触电阻、并且能够制造微细且电阻率低的导电图案的导电糊剂。
用于解决课题的手段
为了解决上述课题，本发明提供以下的(1)~(6)中记载的导电糊剂、触控面板和导电图案的制造方法。
(1) 导电糊剂，其含有：金属颗粒(A)、碳颗粒(B)、具有不饱和双键的化合物(C)、光聚合引发剂(D)、和溶剂(E)，上述金属颗粒(A)相对于上述碳颗粒(B)的质量比为20~1900。
(2) 上述(1)所述的导电糊剂，其中，作为上述光聚合引发剂(D)，含有肟酯系化合物。
(3) 上述(1)或(2)所述的导电糊剂，其中，上述金属颗粒(A)的体积平均粒径为0.1~10μm，并且，上述碳颗粒(B)的一次颗粒的体积平均粒径为0.005~0.5μm。
(4) 上述(1)~(3)中任一项所述的导电糊剂，其中，具有不饱和双键的化合物(C)的酸值为30~250mgKOH/g。
(5) 触控面板，其具有由上述(1)~(4)中任一项所述的导电糊剂形成的导电图案和由ITO形成的透明电极，上述透明电极与所述导电图案相连接。
(6) 导电图案的制造方法，其中，将上述(1)~(4)中任一项所述的导电糊剂涂布于基板上，进行干燥、曝光、显影，然后在100~300℃下进行固化。
发明的效果
根据本发明的导电糊剂，即使经过高湿高热等环境变化也能够抑制接触电阻的增加，并且能够制造微细且电阻率低的导电图案。
附图说明
图1：表示实施例的电阻率评价中使用的光掩模的透光图案的示意图。
图2：表示实施例的与ITO的连接可靠性评价中使用的光掩模的透光图案的示意图。
具体实施方式
本发明的导电糊剂的特征在于，其含有：金属颗粒(A)、碳颗粒(B)、具有不饱和双键的化合物(C)、光聚合引发剂(D)、和溶剂(E)，上述金属颗粒(A)相对于上述碳颗粒(B)的质量比为20~1900。
通过本发明的导电糊剂得到的导电图案成为有机成分与无机成分的复合物，金属颗粒(A)彼此通过固化时的固化收缩而相互接触，从而表现出导电性。
本发明的导电糊剂含有金属颗粒(A)。作为构成金属颗粒(A)的金属，可以举出银(以下称为“Ag”)、金(以下称为“Au”)、铜、铂、铅、锡、镍、铝、钨、钼、铬、钛或铟、或者这些金属的合金，从导电性的观点出发，优选Ag、Au或铜，从成本及稳定性的观点出发，更优选Ag。
本发明人等为了得到所期望的导电糊剂而反复进行深入研究。并且着眼于碳颗粒(B)。迄今为止，已知为了提高导电糊剂中的金属颗粒的分散性、或者调整导电性而添加碳颗粒。然而，为此必须添加大量的碳颗粒，从而导致导电性下降，即导致电阻率提高。
因此，本发明人等着眼于金属颗粒(A)相对于碳颗粒(B)的质量比。并且进一步反复进行研究，发现通过添加少量的碳颗粒，从而即使经过高湿高热等环境变化，也能够稳定地维持接触电阻。即，需要使金属颗粒(A)相对于碳颗粒(B)的质量比为20~1900，更优选为30~1000。
如果金属颗粒(A)的质量比为1900以下，则碳颗粒(B)与透明电极的接触概率提高，所制造的导电图案与透明电极的接触电阻即使经过高湿高热的环境变化也稳定地维持为低值。另一方面，如果金属颗粒(A)的质量比为20以上，则金属颗粒(A)彼此的接触概率提高，所制造的导电图案的电阻率充分降低。
金属颗粒(A)的体积平均粒径优选为0.1~10μm，更优选为0.5~6μm。如果体积平均粒径为0.1μm以上，则固化步骤中的金属颗粒(A)彼此的接触概率提高，所制造的导电图案的电阻率和断线概率变低。进一步，在曝光步骤中，曝光的光能够顺利地从涂布导电糊剂而得到的涂布膜中透过，变得容易进行微细的图案形成。另一方面，如果体积平均粒径为10μm以下，则所制造的导电图案的表面平滑度、图案精度及尺寸精度提高。应予说明，金属颗粒(A)的体积平均粒径可以通过库尔特计数法测定。
金属颗粒(A)的添加量相对于导电糊剂中的全部固体成分优选为60~95质量%。如果相对于全部固体成分的添加量为60质量%以上，则固化时的金属颗粒(A)彼此的接触概率提高，所制造的导电图案的电阻率和断线概率变低。另一方面，如果相对于全部固体成分的添加量为95质量%以下，则在曝光步骤中，曝光的光能够更顺利地从涂布导电糊剂而得到的涂布膜中透过，变得容易进行微细的图案形成。在此，全部固体成分是指将溶剂排除在外的导电糊剂的全部构成成分。
本发明的导电糊剂含有碳颗粒(B)。在此，碳颗粒是指碳在颗粒整体中所占的比例为50质量%以上的颗粒。导电糊剂中包含的碳颗粒由于特别是与透明电极当中的ITO的润湿性良好，所以碳颗粒在导电糊剂与ITO的界面处聚集，接触位点数增大，导电通路增加，因此下述效果得以增大：即使经过高湿高热等环境变化，也能够稳定地维持接触电阻。
作为碳颗粒(B)，可以举出例如MA77、7、8、11、100、100R、100S、230、14、220或600、或者#2650、2600、2350、2300、1000、1000N、980、970、960、950、900、850、750B、650B、52、47、45、45L、44、40、32、30、30L、25、20、10、5、95、85、260、4000B、3030B、3050B、3230B或3400B(以上均为三菱化学株式会社制)、トーカブラック#8500/F、8300/F、7550SB/F、7400、7360SB、7350/F、7270SB、7100F、7050、5500、4500、4400、4300、3855、3845或3800(以上均为東海カーボン株式会社制)、旭#78、80、70、70L、66、65、60HN、60H、60U、60、55、50HG、52、51、50U、50、35、15HS、15、8、或者旭F-200或AX-015、或者アサヒサーマル(以上均为旭カーボン株式会社制)。
碳颗粒(B)的一次颗粒的体积平均粒径优选为0.005~0.5μm。如果一次颗粒的体积平均粒径为0.005μm以上，则导电糊剂中的分散性及分散稳定性进一步变高，可以抑制凝集物产生。另一方面，如果一次颗粒的体积平均粒径超过0.5μm，则每一定质量的一次颗粒数减少，与ITO、银纳米线、氧化锌或氧化锡等透明电极的接触概率降低，从而存在所制造的导电图案与透明电极的接触电阻变高的情况。应予说明，碳颗粒(B)的一次颗粒的体积平均粒径可以通过以下方式计算：使用电子显微镜观察随机挑选的100个一次颗粒，测定各一次颗粒中的最大宽度，求出它们的平均值。
碳颗粒(B)的添加量相对于导电糊剂中的全部固体成分优选为0.05~3质量%，更优选为0.1~2质量%。如果相对于全部固体成分的添加量为0.05质量%以上，则碳颗粒(B)与透明电极的接触概率提高，所制造的导电图案与透明电极的接触电阻即使在高湿高热的环境下也稳定地变低。另一方面，如果相对于全部固体成分的添加量为3质量%以下，则在曝光步骤中，曝光的光能够顺利地从涂布导电糊剂而得到的涂布膜中透过，变得容易进行微细的图案形成。
本发明的导电糊剂含有具有不饱和双键的化合物(C)。作为具有不饱和双键的化合物(C)，可以举出例如苯乙烯、对甲基苯乙烯、邻甲基苯乙烯、间甲基苯乙烯、α-甲基苯乙烯、氯甲基苯乙烯或羟基甲基苯乙烯等苯乙烯类；丙烯酸系单体、1-乙烯基-2-吡咯烷酮、丙烯酸系共聚物或环氧羧酸酯化合物。
作为丙烯酸系单体，可以举出例如丙烯酸、丙烯酸甲酯、丙烯酸乙酯、丙烯酸2-乙基己酯、丙烯酸正丁酯、丙烯酸异丁酯、丙烯酸异丙酯、丙烯酸缩水甘油酯、丁氧基三乙二醇丙烯酸酯、丙烯酸二环戊基酯、丙烯酸二环戊烯基酯、丙烯酸2-羟基乙酯、丙烯酸异冰片基酯、丙烯酸2-羟基丙酯、丙烯酸异癸酯、丙烯酸异辛酯、丙烯酸月桂酯、丙烯酸2-甲氧基乙酯、甲氧基乙二醇丙烯酸酯、甲氧基二乙二醇丙烯酸酯、丙烯酸八氟戊酯、丙烯酸苯氧基乙酯、丙烯酸硬脂基酯、丙烯酸三氟乙酯、丙烯酸氨基乙酯、丙烯酸苯酯、丙烯酸苯氧基乙酯、丙烯酸1-萘基酯、丙烯酸2-萘基酯、苯硫酚丙烯酸酯或苯甲硫醇丙烯酸酯、烯丙基化环己基二丙烯酸酯、甲氧基化环己基二丙烯酸酯、1,4-丁二醇二丙烯酸酯、1,3-丁二醇二丙烯酸酯、乙二醇二丙烯酸酯、二乙二醇二丙烯酸酯、三乙二醇二丙烯酸酯、聚乙二醇二丙烯酸酯、新戊二醇二丙烯酸酯、丙二醇二丙烯酸酯、聚丙二醇二丙烯酸酯或三丙三醇二丙烯酸酯、三羟甲基丙烷三丙烯酸酯、二(三羟甲基丙烷)四丙烯酸酯、二季戊四醇单羟基五丙烯酸酯或二季戊四醇六丙烯酸酯、丙烯酰胺、N-甲氧基甲基丙烯酰胺、N-乙氧基甲基丙烯酰胺、N-正丁氧基甲基丙烯酰胺或N-异丁氧基甲基丙烯酰胺、用不饱和酸使环氧基开环而得到的具有羟基的乙二醇二缩水甘油醚的丙烯酸加成物、二乙二醇二缩水甘油醚的丙烯酸加成物、新戊二醇二缩水甘油醚的丙烯酸加成物、丙三醇二缩水甘油醚的丙烯酸加成物、双酚A二缩水甘油醚的丙烯酸加成物、双酚F的丙烯酸加成物或甲酚酚醛清漆(novolac)的丙烯酸加成物等环氧丙烯酸酯单体、或者γ-丙烯酰氧基丙基三甲氧基硅烷、或者将它们的丙烯酸基置换成甲基丙烯酸基而得到的化合物。
丙烯酸系共聚物是指使用的单体、即共聚成分中包含丙烯酸系单体的共聚物。
具有羧基的碱可溶性的丙烯酸系共聚物可以通过使用不饱和羧酸等不饱和酸作为单体而得到。作为不饱和酸，可以举出例如丙烯酸、甲基丙烯酸、衣康酸、巴豆酸、马来酸、富马酸或乙酸乙烯酯、或者它们的酸酐。可以通过所使用的不饱和酸的多少来调节所得到的丙烯酸系共聚物的酸值。
此外，通过使上述丙烯酸系共聚物所具有的羧基与(甲基)丙烯酸缩水甘油酯等具有不饱和双键的化合物反应，可以得到在侧链上具有反应性的不饱和双键的碱可溶性的丙烯酸系共聚物。
环氧羧酸酯化合物是指可以以环氧化合物和具有不饱和双键的羧基化合物为起始原料而合成的化合物。作为能够成为起始原料的环氧化合物，可以举出例如缩水甘油醚类、脂环式环氧树脂、缩水甘油酯类、缩水甘油基胺类或环氧树脂，更具体而言，可以举出甲基缩水甘油基醚、乙基缩水甘油基醚、丁基缩水甘油基醚、乙二醇二缩水甘油醚、二乙二醇二缩水甘油醚、丙二醇二缩水甘油醚、三丙二醇二缩水甘油醚、新戊二醇二缩水甘油醚、双酚A二缩水甘油醚、氢化双酚A二缩水甘油醚、双酚F二缩水甘油醚、双酚S二缩水甘油醚、双酚芴二缩水甘油醚、联苯二酚二缩水甘油醚、四甲基联苯二酚缩水甘油醚、三羟甲基丙烷三缩水甘油醚、3',4'-环氧环己基甲基-3,4-环氧环己烷甲酸酯或叔丁基缩水甘油基胺。此外，作为具有不饱和双键的羧基化合物，可以举出例如(甲基)丙烯酸、巴豆酸、肉桂酸或α-氰基肉桂酸。
也可以使环氧羧酸酯化合物与多元酸酐反应从而调节环氧羧酸酯化合物的酸值。作为多元酸酐，可以举出例如琥珀酸酐、邻苯二甲酸酐、四氢邻苯二甲酸酐、六氢邻苯二甲酸酐、衣康酸酐、3-甲基四氢邻苯二甲酸酐、4-甲基六氢邻苯二甲酸酐、偏苯三甲酸酐或马来酸酐。
也可以通过使上述与多元酸酐反应的环氧羧酸酯化合物所具有的羧基与(甲基)丙烯酸缩水甘油酯等具有不饱和双键的化合物反应，从而调节环氧羧酸酯化合物所具有的反应性的不饱和双键的量。
也可以通过使环氧羧酸酯化合物所具有的羟基与二异氰酸酯化合物反应从而进行氨基甲酸酯化。作为二异氰酸酯化合物，可以举出例如六亚甲基二异氰酸酯、四甲基亚二甲苯基二异氰酸酯、萘-1,5-二异氰酸酯、二甲基联苯二异氰酸酯(tolidenediisocyanate)、三甲基六亚甲基二异氰酸酯、异佛尔酮二异氰酸酯、烯丙基氰基二异氰酸酯或降冰片烷二异氰酸酯。
为了使碱可溶性为最合适，具有不饱和双键的化合物(C)的酸值优选为30~250mgKOH/g。如果酸值小于30mgKOH/g，则存在可溶部分的溶解性降低的情况。另一方面，如果酸值大于250mgKOH/g，则存在显影容许宽度变窄的情况。应予说明，具有不饱和双键的化合物(C)的酸值可以按照JIS K 0070(1992)测定。
本发明的导电糊剂含有光聚合引发剂(D)。作为光聚合引发剂(D)，可以举出例如1,2-辛二酮-1-[4-(苯硫基)-2-(O-苯甲酰基肟)]、2,4,6-三甲基苯甲酰基-二苯基-氧化膦、双(2,4,6-三甲基苯甲酰基)-苯基氧化膦、乙酮-1-[9-乙基-6-2(2-甲基苯甲酰基)-9H-咔唑-3-基]-1-(O-乙酰基肟)、二苯甲酮、邻苯甲酰基苯甲酸甲酯、4,4'-双(二甲基氨基)二苯甲酮、4,4'-双(二乙基氨基)二苯甲酮、4,4'-二氯二苯甲酮、4-苯甲酰基-4'-甲基二苯基甲酮、二苯甲基甲酮、芴酮、2,2'-二乙氧基苯乙酮、2,2-二甲氧基-2-苯基苯乙酮、2-羟基-2-甲基苯丙酮、对叔丁基二氯苯乙酮、噻吨酮、2-甲基噻吨酮、2-氯噻吨酮、2-异丙基噻吨酮、二乙基噻吨酮、苯偶酰、苯偶酰二甲基缩酮、苯偶酰-β-甲氧基乙基乙缩醛、苯偶姻、苯偶姻甲基醚、苯偶姻丁基醚、蒽醌、2-叔丁基蒽醌、2-戊基蒽醌、β-氯蒽醌、蒽酮、苯并蒽酮、二苯并环庚酮、亚甲基蒽酮(methyleneanthrone)、4-叠氮基苯甲叉基苯乙酮、2,6-双(对叠氮基苯甲叉基)环己酮、6-双(对叠氮苯甲叉基)-4-甲基环己酮、1-苯基-1,2-丁二酮-2-(O-甲氧基羰基)肟、1-苯基-丙二酮-2-(O-乙氧基羰基)肟、1-苯基-丙二酮-2-(O-苯甲酰基)肟、1,3-二苯基-丙三酮-2-(O-乙氧基羰基)肟、1-苯基-3-乙氧基-丙三酮-2-(O-苯甲酰基)肟、米蚩酮、2-甲基-[4-(甲硫基)苯基]-2-吗啉基-1-丙酮、萘磺酰氯、喹啉磺酰氯、N-苯基硫代吖啶酮、4,4'-偶氮双异丁腈、二苯基二硫醚、二硫化苯并噻唑、三苯基膦、樟脑醌、2,4-二乙基噻吨酮、异丙基噻吨酮、四溴化碳、三溴苯基砜、过氧化苯偶姻、曙红或亚甲基蓝等光还原性色素与抗坏血酸或三乙醇胺等还原剂的组合，优选光灵敏度高的肟酯系化合物。
光聚合引发剂(D)的添加量相对于100质量份的具有不饱和双键的化合物(C)优选为0.05~30质量份。如果相对于100质量份的具有不饱和双键的化合物(C)的添加量为0.05质量份以上，则曝光部的固化密度增加，可以提高显影后的残膜率。另一方面，如果相对于100质量份的具有不饱和双键的化合物(C)的添加量为30质量份以下，则在涂布导电糊剂而得到的涂布膜上部处的因光聚合引发剂(D)而导致的过量的光吸收受到抑制。其结果是，可以抑制因所制造的导电图案成为倒锥形状而导致的与基板的密合性降低。
本发明的导电糊剂可以在含有光聚合引发剂(D)的同时含有敏化剂。
作为敏化剂，可以举出例如2,4-二乙基噻吨酮、异丙基噻吨酮、2,3-双(4-二乙基氨基苯甲叉基)环戊酮、2,6-双(4-二甲基氨基苯甲叉基)环己酮、2,6-双(4-二甲基氨基苯甲叉基)-4-甲基环己酮、米蚩酮、4,4-双(二乙基氨基)二苯甲酮、4,4-双(二甲基氨基)查耳酮、4,4-双(二乙基氨基)查耳酮、对二甲基氨基肉桂叉基茚酮、对二甲基氨基苯甲叉基茚酮、2-(对二甲基氨基苯基亚乙烯基)异萘并噻唑、1,3-双(4-二甲基氨基苯基亚乙烯基)异萘并噻唑、1,3-双(4-二甲基氨基苯甲叉基)丙酮、1,3-羰基双(4-二乙基氨基苯甲叉基)丙酮、3,3-羰基双(7-二乙基氨基香豆素)、N-苯基-N-乙基乙醇胺、N-苯基乙醇胺、N-甲苯基二乙醇胺、二甲基氨基苯甲酸异戊酯、二乙基氨基苯甲酸异戊酯、3-苯基-5-苯甲酰基硫基四唑或1-苯基-5-乙氧基羰基硫基四唑。
敏化剂的添加量相对于100质量份的具有不饱和双键的化合物(C)优选为0.05~10质量份。如果相对于100质量份的具有不饱和双键的化合物(C)的添加量为0.05质量份以上，则光灵敏度提高。另一方面，如果相对于100质量份的具有不饱和双键的化合物(C)的添加量为10质量份以下，则在涂布导电糊剂而得到的涂布膜上部处的过量的光吸收受到抑制。其结果是，可以抑制因所制造的导电图案成为倒锥形状而导致的与基板的密合性降低。
本发明的导电糊剂含有溶剂(E)。作为溶剂(E)，可以举出例如N,N-二甲基乙酰胺、N,N-二甲基甲酰胺、N-甲基-2-吡咯烷酮、二甲基咪唑烷酮、二甲亚砜、γ-丁内酯、乳酸乙酯、1-甲氧基-2-丙醇、1-乙氧基-2-丙醇、乙二醇单正丙基醚、二丙酮醇、四氢糠醇、丙二醇单甲基醚乙酸酯、二乙二醇单乙基醚乙酸酯、二乙二醇单甲基醚、二乙二醇单乙基醚乙酸酯(以下称为“DMEA”)、二乙二醇单丁基醚、二乙二醇单丁基醚乙酸酯、三乙二醇二甲基醚或2,2,4-三甲基-1,3-戊二醇单异丁酸酯，优选沸点为150℃以上的溶剂。如果沸点为150℃以上，则溶剂(E)的挥发受到抑制，可以抑制导电糊剂的粘度增加。
本发明的导电糊剂只要在不损害其期望的的特性的范围内，则可以含有在分子内不具有不饱和双键的非感光性聚合物或增塑剂、流平剂、表面活性剂、硅烷偶联剂、消泡剂或颜料等添加剂。
作为上述非感光性聚合物，可以举出例如环氧树脂、酚醛清漆树脂、酚醛树脂、聚酰亚胺前体或已闭环的聚酰亚胺。
作为增塑剂，可以举出例如邻苯二甲酸二丁酯、邻苯二甲酸二辛酯、聚乙二醇或丙三醇。
作为流平剂，可以举出例如特殊乙烯基系聚合物或特殊丙烯酸系聚合物。
作为硅烷偶联剂，可以举出例如甲基三甲氧基硅烷、二甲基二乙氧基硅烷、苯基三乙氧基硅烷、六甲基二硅氮烷、3-甲基丙烯酰氧基丙基三甲氧基硅烷、3-环氧丙氧基丙基三甲氧基硅烷或乙烯基三甲氧基硅烷。
本发明的导电糊剂例如可以使用三辊磨、球磨机或行星式球磨机等分散机或混炼机制造。
本发明的导电图案的制造方法的特征在于，将本发明的导电糊剂涂布于基板上，进行干燥、曝光、显影，然后在100~300℃下进行固化。
通过将本发明的导电糊剂涂布于基板上从而得到涂布膜。
作为涂布本发明的导电糊剂的基板，可以举出例如聚对苯二甲酸乙二醇酯膜(以下称为“PET膜”)、聚酰亚胺膜、聚酯膜、芳族聚酰胺膜、环氧树脂基板、聚醚酰亚胺树脂基板、聚醚酮树脂基板、聚砜系树脂基板、玻璃基板、硅晶元、氧化铝基板、氮化铝基板、碳化硅基板、形成有装饰层的基板或形成有绝缘层的基板。
作为将本发明的导电糊剂涂布于基板上的方法，可以举出例如使用旋转器的旋涂、喷涂、辊涂、丝网印刷或使用刀涂机、模涂机、压延涂布机、弯月面涂布机或棒涂机的涂布。所得到的涂布膜的膜厚根据涂布的方法或导电糊剂的全部固体成分浓度或粘度等适当确定即可，优选使干燥后的膜厚达到0.1~50μm。应予说明，膜厚可以使用如サーフコム(注册商标)1400((株)东京精密制)那样的触针式台阶仪测定。更具体而言，用触针式台阶仪(测量长度：1mm，扫描速度：0.3mm/秒)分别测定随机选取的3个位置的膜厚，求出它们的平均值，由此算出。
将所得到的涂布膜干燥从而使溶剂挥发。作为将涂布膜干燥从而挥发除去溶剂的方法，可以举出例如通过烘箱、加热板或红外线等进行的加热干燥或真空干燥。加热温度优选为50~180℃，加热时间优选为1分钟~数小时。
对于干燥后的涂布膜，介由任意的图案形成用掩模，通过光刻法进行曝光。作为曝光的光源，优选为汞灯的i线(365nm)、h线(405nm)或g线(436nm)。
对于曝光后的涂布膜，使用显影液进行显影，将未曝光部溶解除去，得到所期望的图案。作为进行碱性显影时的显影液，可以举出例如四甲基氢氧化铵、二乙醇胺、二乙基氨基乙醇、氢氧化钠、氢氧化钾、碳酸钠、碳酸钾、三乙胺、二乙胺、甲胺、二甲胺、乙酸二甲基氨基乙酯、二甲基氨基乙醇、甲基丙烯酸二甲基氨基乙酯、环己胺、乙二胺或六亚甲基二胺的水溶液，也可在它们的水溶液中添加N-甲基-2-吡咯烷酮、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、二甲亚砜或γ-丁内酯等极性溶剂；甲醇、乙醇或异丙醇等醇类；乳酸乙酯或丙二醇单甲基醚乙酸酯等酯类；环戊酮、环己酮、异丁基酮或甲基异丁基酮等酮类；或者表面活性剂。
作为进行有机显影时的显影液，可以举出例如N-甲基-2-吡咯烷酮、N-乙酰基-2-吡咯烷酮、N,N-二甲基乙酰胺、N,N-二甲基甲酰胺、二甲亚砜或六甲基磷酰三胺等极性溶剂、或者这些极性溶剂与甲醇、乙醇、异丙醇、二甲苯、水、甲基卡必醇或乙基卡必醇的混合溶液。
作为显影的方法，可以举出例如在使基板静置或旋转的同时对涂布膜面喷洒显影液的方法、将基板浸渍于显影液中的方法、或在将基板浸渍于显影液中的同时施加超声波的方法。
对于通过显影而得到的图案，可以通过漂洗液实施漂洗处理。在此，作为漂洗液，可以举出例如水、或者在水中添加乙醇或异丙醇等醇类、或乳酸乙酯或丙二醇单甲基醚乙酸酯等酯类而得到的水溶液。
在100~300℃下固化所得到的图案。固化的温度优选为120~180℃。如果固化温度低于100℃，则树脂成分的体积收缩量不会变大，电阻率不会充分降低。另一方面，如果固化温度大于300℃，则无法在耐热性低的基板等材料上制造导电图案。
作为固化所得到的图案的方法，可以举出例如通过烘箱、惰性烘箱或加热板进行的加热干燥；通过紫外线灯、红外线加热器、卤素加热器或氙闪光灯等的电磁波、或微波进行的加热干燥；或者真空干燥。通过加热，所制造的层叠图案的硬度提高，可以抑制因与其他构件接触而导致的缺损、剥离等，进而可以提高与基板的密合性。
本发明的触控面板的特征在于，其具备由本发明的导电糊剂形成的导电图案和由ITO形成的透明电极，上述透明电极与上述导电图案相连接。
使用本发明的导电糊剂制造的导电图案适合用作具有由ITO形成的透明电极的触控面板用的周围布线。其原因在于，如上所述，导电糊剂中包含的碳颗粒特别是与透明电极当中的ITO的润湿性良好，因此碳颗粒在导电糊剂与ITO的界面处聚集，接触位点数增大，导电通路增大，因此下述效果得以增大：即使经过高湿高热等环境变化，也能够稳定地维持接触电阻。
作为触控面板的方式，可以举出例如电阻膜式、光学式、电磁感应式或静电容式。静电容式触控面板要求特别微细的布线，因此，更合适使用本发明的导电糊剂。
此外，对于静电容式触控面板而言，由于需要从透明电极向IC芯片传送电信号，因此周围布线的至少一部分需要形成于透明电极上。如上所述，使用本发明的导电糊剂制造的导电图案由于与ITO的连接可靠性优异，因此更合适使用。
在具有通过本发明的制造方法制造的导电图案作为其周围布线、并且该周围布线为50μm间距(布线宽度+布线间宽度)以下的触控面板中，可以使框部宽度变细，可以扩大可视区域。
实施例
以下，举出实施例及比较例进一步详细地说明本发明，但本发明不受它们的限制。
各实施例及比较例中使用的评价方法如下所述。
<图案形成性的评价方法>
在PET膜上以干燥后的膜厚达到7μm的方式涂布导电糊剂，将所得到的涂布膜在100℃的干燥烘箱内干燥5分钟。将以恒定的线宽/间距(line-and-space，以下称为“L/S”)排列的直线组、即透光图案作为1个单元，介由具有不同L/S值的9种单元中的每一种的光掩模，将干燥后的涂布膜曝光及显影，分别得到L/S的值不同的9种图案。然后，对所得到的9种图案均在140℃的干燥烘箱内固化30分钟，从而分别得到L/S的值不同的9种导电图案。对于光掩模所具有的各单元的L/S的值，线宽(μm)/间隔(μm)为500/500、250/250、100/100、50/50、40/40、30/30、25/25、20/20、15/15。用光学显微镜观察所得到的导电图案。确认在图案间不存在残渣且不存在图案剥离的L/S的值最小的导电图案。将该L/S的值作为能够显影的L/S的值。将达到过显影、图案消失的情况称为“图案流失”。
应予说明，曝光使用曝光装置(PEM-6M；ユニオン光学株式会社制)，以150mJ/cm2(波长365nm换算)的曝光量进行全射线曝光，对于显影，使基板浸渍于0.2质量%的Na2CO3溶液中30秒，然后通过超纯水实施漂洗处理来进行显影。
<电阻率的评价方法>
在PET膜上以干燥后的膜厚达到7μm的方式涂布导电糊剂，在100℃的干燥烘箱内干燥所得到的涂布膜5分钟。介由具有图1所示的透光图案A的光掩模，对干燥后的涂布膜进行曝光和显影，从而得到图案。然后，在140℃的干燥烘箱内固化所得到的图案30分钟，从而得到电阻率测定用的导电性图案。所得到的导电性图案的线宽为0.400mm，线长为80mm。
应予说明，曝光和显影的条件与上述图案形成性的评价方法相同。用电阻计连接所得到的电阻率测定用的导电图案的各端部，测定电阻值，基于下式(1)算出电阻率。将未观察到导通的情况作为“绝缘”。
电阻率 = 电阻值×膜厚×线宽/线长 …… (1)。
<与透明电极的连接可靠性评价方法>
在将透明电极整面形成于PET膜上而得到的透明导电膜上以干燥后的膜厚达到7μm的方式涂布导电糊剂，将所得到的涂布膜用100℃的干燥烘箱干燥5分钟。介由具有图2所示的透光图案A的光掩模，对干燥后的涂布膜进行曝光和显影，从而得到图案。然后，在140℃的干燥烘箱内固化所得到的图案30分钟，从而得到评价与透明电极的连接可靠性的样品。所得到的样品中的导电性图案的线宽为0.100mm，线间为5mm，端子部为直径2mm的圆形。
用万用表连接所得到的样品中的导电性图案的端子部，测定初始电阻值，然后在85℃、85%RH的恒温恒湿槽(LU-113；エスペック(株))内保管500小时。然后，用万用表连接取出的样品中的导电性图案的端子部，测定保管后电阻值，基于下式(2)算出电阻变化率。将算出的电阻变化率为1.30以下的情况判断为A，将大于1.30且为1.50以下的情况判断为B，将大于1.50的情况判断为C。
电阻变化率=保管后电阻值(500时间后)/初始电阻值 …… (2)。
应予说明，测定的初始电阻值和保管后电阻值严格而言是导电图案与透明电极的接触电阻的值加上导电图案的电阻值和透明电极的电阻值而得到的值。然而，导电图案的电阻值和透明电极的电阻值与接触电阻的值相比非常小，因此可以采用初始电阻值和保管后电阻值来评价接触电阻的变化率。
各实施例和比较例中使用的材料如下所述。
[金属颗粒(A)]
体积平均粒径为1.0μm的Ag颗粒
体积平均粒径为1.0μm的Au颗粒。
[碳颗粒(B)]
一次颗粒的体积平均粒径为0.05μm的碳颗粒(碳在颗粒整体中所占的比例：99质量%)。
[具有不饱和双键的化合物(C)]
(单体)
ライトアクリレートBP-4EA(以下称为“BP-4EA”；共荣社化学(株)制)。
(合成例1：化合物(C-1))
共聚比例(质量基准)：丙烯酸乙酯(以下称为“EA”)/甲基丙烯酸2-乙基己酯(以下、“2-EHMA”)/苯乙烯(以下、“St”)/甲基丙烯酸缩水甘油酯(以下称为“GMA”)/丙烯酸(以下称为“AA”)＝20/40/20/5/15
在氮气氛围的反应容器中，投入150g的DMEA，使用油浴升温至80℃。经1小时向其中滴加包含20g的EA、40g的2-EHMA、20g的St、15g的AA、0.8g的2,2'-偶氮双异丁腈及10g的DMEA的混合物。滴加结束后，进一步进行6小时聚合反应。然后，添加1g的氢醌单甲基醚，终止聚合反应。接着，经0.5小时滴加包含5g的GMA、1g的三乙基苯甲基氯化铵及10g的DMEA的混合物。滴加结束后，进一步进行2小时加成反应。用甲醇精制所得到的反应溶液从而除去未反应杂质，进一步进行24小时真空干燥，由此得到化合物(C-1)。所得到的化合物(C-1)的酸值为103mgKOH/g。
(合成例2：化合物(C-2))
共聚比例(质量基准)：环氧乙烷改性双酚A二丙烯酸酯(FA-324A；日立化成工业(株)制)/EA/GMA/AA＝60/25/10/5
在氮气氛围的反应容器中，投入150g的DMEA，使用油浴升温至80℃。经1小时滴加包含60g的环氧乙烷改性双酚A二丙烯酸酯、25g的EA、5g的AA、0.8g的2,2'-偶氮双异丁腈及10g的DMEA的混合物。滴加结束后，进一步进行6小时聚合反应。然后，添加1g的氢醌单甲基醚，终止聚合反应。接着，经0.5小时滴加包含10g的GMA、1g的三乙基苯甲基氯化铵及10g的DMEA的混合物。滴加结束后，进一步进行2小时加成反应。用甲醇精制得到的反应溶液从而除去未反应杂质，进一步进行24小时真空干燥，由此得到具有羧基和不饱和双键的化合物(C-2)。所得到的化合物(C-2)的酸值为1.4mgKOH/g。
(合成例3：化合物(C-3))
在氮气氛围的反应溶液中，投入123g的RE-310S(日本化药(株)制)、47g的AA、0.3g的氢醌单甲基醚及0.5g的三苯基膦，在98℃的温度下进行反应直至反应液的酸值达到0.5mgKOH/g以下，得到化合物(C-3)。所得到的化合物(C-3)的酸值为0.4mgKOH/g。
(合成例4：化合物(C-4))
在氮气氛围的反应溶液中投入164g的卡必醇乙酸酯、287g的EOCN-103S(日本化药(株)制)、96g的AA、2g的2,6-二叔丁基对甲酚及2g的三苯基膦，在98℃的温度下进行反应直至反应液的酸值达到0.5mgKOH/g以下，得到环氧羧酸酯化合物。接着，在该反应液中投入57g的卡必醇乙酸酯及67g的四氢邻苯二甲酸酐，在95℃下反应4小时，得到化合物(C-4)。所得到的化合物(C-4)的酸值为104mgKOH/g。
(合成例5：化合物(C-5))
在氮气氛围的反应容器中，投入123g的RE-310S(日本化药(株)制)、47g的AA、0.3g的氢醌单甲基醚及0.5g的三苯基膦，在98℃的温度下进行反应直至反应液的酸值达到0.5mgKOH/g以下，得到环氧羧酸酯化合物。然后，向该反应溶液中添加252g的卡必醇乙酸酯、89g的2,2-双(二羟甲基)-丙酸、0.4g的2-甲基氢醌及47g的螺二醇，升温至45℃。以反应温度不超过65℃的方式，向该溶液中缓缓滴加162g的三甲基六亚甲基二异氰酸酯。滴加结束后，将反应温度提升至80℃，反应6小时直至通过红外吸收光谱测定法得到的2250cm-1附近的吸收消失，得到化合物(C-5)。所得到的化合物(C-5)的酸值为80.0mgKOH/g。
(合成例6：化合物(C-6))
在氮气氛围的反应容器中，投入300g的デナコールEX-203(ナガセケムテックス(株)制)的丙烯酸加成物(分子量：368)、500g的DMEA、0.5g的2-甲基氢醌及200g的2,2-双(羟基甲基)丙酸，升温至45℃。以反应温度不超过50℃的方式，向该溶液中滴加201.3g的甲苯二异氰酸酯。滴加结束后，将反应温度提升至80℃，反应6小时直至通过红外吸收光谱测定法得到的2250cm-1附近的吸收消失。向该溶液中添加120g的甲基丙烯酸缩水甘油酯，升温至95℃，反应6时间，得到化合物(C-6)。所得到的化合物(C-6)的酸值为83mgKOH/g。
[光聚合引发剂(D)]
IRGACURE(注册商标)OXE-01(以下称为“OXE-01”；チバジャパン(株)制)
IRGACURE(注册商标)369(以下称为“IC-369”；チバジャパン(株)制)。
[溶剂(E)]
DMEA(东京化成工业(株)制)。
[透明电极]
ITO膜(日东电工(株)制)
银纳米线膜(日立化成(株)制)。
(实施例1)
向100mL洁净瓶中，投入10.0g的化合物(C-1)、0.50g的OXE-01、5.0g的DMEA及2.0g的BP-4EA，用自转-公转真空混合机 “あわとり錬太郎”ARE-310(注册商标；(株)シンキー制)进行混合，得到17.5g的树脂溶液(固体成分71.4质量%)。
将所得到的17.5g的树脂溶液、85.0g的Ag颗粒及2.5g的碳颗粒(B)进行混合，使用三辊磨(EXAKT M-50；EXAKT公司制)进行混炼，得到105.0g的导电糊剂。
使用所得到的导电糊剂，对导电图案的图案形成性、电阻率及与ITO的连接可靠性分别进行评价。作为图案形成性的评价指标的能够显影的L/S的值为15/15μm，确认到实现了良好的图案加工。导电图案的电阻率为5.5×10-5Ωcm。与ITO的连接可靠性评价中的电阻变化率为1.03，为良好。
(实施例2~14)
通过与实施例1同样的方法制造表1所示的组成的导电糊剂，进行与实施例1同样的评价，将结果示于表2。
(比较例1~4)
通过与实施例1同样的方法制造表1所示的组成的导电糊剂，进行与实施例1同样的评价，将结果示于表2。
对于实施例1~14的导电糊剂而言，均可以制造图案形成性、电阻率及与ITO的连接可靠性优异的导电图案。另一方面，对于比较例1的导电糊剂而言，在高温高湿度下与ITO的连接可靠性降低，对于比较例2及4的导电糊剂而言，在显影中图案流失从而不能制造微细的布线，此外，使用比较例3的导电糊剂制造的导电图案未显示导电性。
[表1]
。
[表2]
。
附图标记说明
A：透光图案。
工业实用性
本发明的导电糊剂可以合适地用于制造触控面板用的周围布线等的导电图案。
Claims (6)
1. 导电糊剂，其含有：
金属颗粒(A)、
碳颗粒(B)、
具有不饱和双键的化合物(C)、
光聚合引发剂(D)、和
溶剂(E)，
所述金属颗粒(A)相对于所述碳颗粒(B)的质量比为20~1900。
2.根据权利要求1所述的导电糊剂，其中，作为所述光聚合引发剂(D)，含有肟酯系化合物。
3.根据权利要求1或2所述的导电糊剂，其中，所述金属颗粒(A)的体积平均粒径为0.1~10μm，并且，
所述碳颗粒(B)的一次颗粒的体积平均粒径为0.005~0.5μm。
4.根据权利要求1~3中任一项所述的导电糊剂，其中，所述具有不饱和双键的化合物(C)的酸值为30~250mgKOH/g。
5.触控面板，其具有由权利要求1~4中任一项所述的导电糊剂形成的导电图案和由ITO形成的透明电极，所述透明电极与所述导电图案相连接。
6.导电图案的制造方法，将权利要求1~4中任一项所述的导电糊剂涂布于基板上，进行干燥、曝光、显影，然后在100~300℃下进行固化。
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| KR102308536B1 (ko) * | 2019-11-05 | 2021-10-05 | 덕산하이메탈(주) | 전도성 카본 페이스트 조성물 및 이를 이용한 전극 |
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| CN102365690A (zh) * | 2009-03-31 | 2012-02-29 | 太阳控股株式会社 | 感光性导电糊剂及电极图案 |
| CN102445846A (zh) * | 2010-09-30 | 2012-05-09 | 太阳控股株式会社 | 感光性导电糊剂 |
| WO2013108696A1 (ja) * | 2012-01-19 | 2013-07-25 | 東レ株式会社 | 導電ペーストおよび導電パターンの製造方法 |
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| JP2014085771A (ja) * | 2012-10-22 | 2014-05-12 | Toppan Printing Co Ltd | 静電容量式タッチパネルセンサー基板及びその製造方法並びに表示装置 |
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| US7608784B2 (en) * | 2006-07-13 | 2009-10-27 | E. I. Du Pont De Nemours And Company | Photosensitive conductive paste for electrode formation and electrode |
| JPWO2013038624A1 (ja) * | 2011-09-13 | 2015-03-23 | 凸版印刷株式会社 | 静電容量式タッチパネルセンサー基板の製造方法、静電容量式タッチパネルセンサー基板および表示装置 |
| WO2013146107A1 (ja) | 2012-03-28 | 2013-10-03 | 東レ株式会社 | 感光性導電ペーストおよび導電パターンの製造方法 |
| JPWO2014069436A1 (ja) * | 2012-10-31 | 2016-09-08 | 東レ株式会社 | 感光性導電ペースト及び導電パターンの製造方法 |
| JP6225708B2 (ja) * | 2012-11-13 | 2017-11-08 | 東レ株式会社 | 静電容量型タッチパネル |
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| CN102365690A (zh) * | 2009-03-31 | 2012-02-29 | 太阳控股株式会社 | 感光性导电糊剂及电极图案 |
| CN102445846A (zh) * | 2010-09-30 | 2012-05-09 | 太阳控股株式会社 | 感光性导电糊剂 |
| WO2013108696A1 (ja) * | 2012-01-19 | 2013-07-25 | 東レ株式会社 | 導電ペーストおよび導電パターンの製造方法 |
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| JP2014085771A (ja) * | 2012-10-22 | 2014-05-12 | Toppan Printing Co Ltd | 静電容量式タッチパネルセンサー基板及びその製造方法並びに表示装置 |
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| TWI658108B (zh) | 2019-05-01 |
| CN106463199B (zh) | 2018-07-13 |
| WO2015174348A1 (ja) | 2015-11-19 |
| JP6645186B2 (ja) | 2020-02-14 |
| JPWO2015174348A1 (ja) | 2017-04-20 |
| KR20170007733A (ko) | 2017-01-20 |
| KR102208100B1 (ko) | 2021-01-28 |
| TW201546212A (zh) | 2015-12-16 |
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