TWI658108B - 導電糊、觸控面板及導電圖案的製造方法 - Google Patents
導電糊、觸控面板及導電圖案的製造方法 Download PDFInfo
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- TWI658108B TWI658108B TW104115138A TW104115138A TWI658108B TW I658108 B TWI658108 B TW I658108B TW 104115138 A TW104115138 A TW 104115138A TW 104115138 A TW104115138 A TW 104115138A TW I658108 B TWI658108 B TW I658108B
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- conductive paste
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- XUCHXOAWJMEFLF-UHFFFAOYSA-N bisphenol F diglycidyl ether Chemical compound C1OC1COC(C=C1)=CC=C1CC(C=C1)=CC=C1OCC1CO1 XUCHXOAWJMEFLF-UHFFFAOYSA-N 0.000 description 1
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- 125000002147 dimethylamino group Chemical group [H]C([H])([H])N(*)C([H])([H])[H] 0.000 description 1
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- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical compound C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 description 1
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
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- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 description 1
- YFNKIDBQEZZDLK-UHFFFAOYSA-N triglyme Chemical compound COCCOCCOCCOC YFNKIDBQEZZDLK-UHFFFAOYSA-N 0.000 description 1
- SRPWOOOHEPICQU-UHFFFAOYSA-N trimellitic anhydride Chemical compound OC(=O)C1=CC=C2C(=O)OC(=O)C2=C1 SRPWOOOHEPICQU-UHFFFAOYSA-N 0.000 description 1
- JPMBLOQPQSYOMC-UHFFFAOYSA-N trimethoxy(3-methoxypropyl)silane Chemical compound COCCC[Si](OC)(OC)OC JPMBLOQPQSYOMC-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- 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
-
- 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
- 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
-
- 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
-
- 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
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Abstract
本發明的目的在於提供一種能夠製造即便於高濕高熱等環境下亦能夠穩定地維持接觸電阻、且與透明電極的連接可靠性高的微細導電圖案的導電糊。本發明提供一種導電糊,其含有金屬粒子(A)、碳粒子(B)、具有不飽和雙鍵的化合物(C)、光聚合起始劑(D)、以及溶劑(E),且上述金屬粒子(A)相對於上述碳粒子(B)的質量比為20~1900。
Description
本發明是有關於一種導電糊及導電圖案的製造方法。
近年來,一直開發能夠藉由光微影(photolitho)法來製造微細導電圖案的、使導電填料分散於有機成分而得的導電糊(專利文獻1及專利文獻2),其中正在開發以與氧化銦錫(indium tin oxide,ITO)等透明電極的連接可靠性高為特徵的導電糊(專利文獻1)。
[現有技術文獻]
[專利文獻]
[專利文獻1]國際公開第2013/108696號
[專利文獻2]國際公開第2013/146107號
然而,於使用現有的導電糊而製造的如觸控面板的周邊配線那樣的導電圖案中,有時由於高溫等熱應力或濕度變化,於導電圖案與ITO等透明電極的接觸面產生的電阻即接觸電阻變高已被視為問題。
因此,本發明的目的在於提供一種能夠製造即便經過高
濕高熱等環境變化亦能夠穩定地維持接觸電阻,且微細、比電阻低的導電圖案的導電糊。
為了解決上述課題,本發明提供一種以下的(1)~(6)中記載的導電糊、觸控面板及導電圖案的製造方法。
(1)一種導電糊,其含有金屬粒子(A)、碳粒子(B)、具有不飽和雙鍵的化合物(C)、光聚合起始劑(D)、以及溶劑(E),且上述金屬粒子(A)相對於上述碳粒子(B)的質量比為20~1900。
(2)如上述(1)所述的導電糊,其含有肟酯系化合物作為上述光聚合起始劑(D)。
(3)如上述(1)或(2)所述的導電糊,其中上述金屬粒子(A)的體積平均粒徑為0.1μm~10μm,且上述碳粒子(B)的一次粒子的體積平均粒徑為0.005μm~0.5μm。
(4)如上述(1)至(3)中任一項所述的導電糊,其中具有不飽和雙鍵的化合物(C)的酸價為30mgKOH/g~250mgKOH/g。
(5)一種觸控面板,其具備由如上述(1)至(4)中任一項所述的導電糊所形成的導電圖案、與包含ITO的透明電極,且上述透明電極與上述導電圖案相連接。
(6)一種導電圖案的製造方法,其是將如上述(1)至(4)中任一項所述的導電糊塗佈於基板上並加以乾燥,於進行曝光、
顯影後,以100℃~300℃加以固化(cure)。
根據本發明的導電糊,可製造即便經過高濕高熱等環境變化亦能夠抑制接觸電阻的增加,且微細、比電阻低的導電圖案。
A‧‧‧透光圖案
圖1是表示實施例的比電阻評價中使用的光罩的透光圖案的示意圖。
圖2是表示實施例的與ITO的連接可靠性評價中使用的光罩的透光圖案的示意圖。
本發明的導電糊的特徵在於:含有金屬粒子(A)、碳粒子(B)、具有不飽和雙鍵的化合物(C)、光聚合起始劑(D)、以及溶劑(E),且上述金屬粒子(A)相對於上述碳粒子(B)的質量比為20~1900。
藉由本發明的導電糊而獲得的導電圖案成為有機成分與無機成分的複合物(composite),且是藉由金屬粒子(A)彼此因固化時的硬化收縮而相互接觸,從而顯現出導電性者。
本發明的導電糊含有金屬粒子(A)。作為構成金屬粒子(A)的金屬,可列舉銀(以下為「Ag」)、金(以下為「Au」)、銅、鉑、鉛、錫、鎳、鋁、鎢、鉬、鉻、鈦或銦或者該些金屬的合金,就導電性的觀點而言,較佳為Ag、Au或者銅,就成本及
穩定性的觀點而言,更佳為Ag。
本發明者等人為了獲得所期望的導電糊而反覆進行努力研究。而且,著眼於碳粒子(B)。迄今為止,已知為了提高導電糊中的金屬粒子的分散性、或調整導電性而添加碳粒子。然而,為此必須添加大量的碳粒子,而導致導電性下降、即比電阻提高。
因此,本發明者等人著眼於金屬粒子(A)相對於碳粒子(B)的質量比。而且,進一步反覆研究而發現:藉由添加少量的碳粒子,而可即便經過高濕高熱等環境變化亦能夠穩定地維持接觸電阻。即,金屬粒子(A)相對於碳粒子(B)的質量比需為20~1900,更佳為30~1000。
若金屬粒子(A)的質量比為1900以下,則碳粒子(B)與透明電極的接觸幾率提高,即便經過高濕高熱的環境變化,所製造的導電圖案與透明電極的接觸電阻亦穩定地保持為低。另一方面,若金屬粒子(A)的質量比為20以上,則金屬粒子(A)彼此的接觸幾率提高,所製造的導電圖案的比電阻充分變低。
金屬粒子(A)的體積平均粒徑較佳為0.1μm~10μm,更佳為0.5μm~6μm。若體積平均粒徑為0.1μm以上,則固化步驟中的金屬粒子(A)彼此的接觸幾率提高,所製造的導電圖案的比電阻及斷線幾率變低。進而,於曝光步驟中,曝光光可於塗佈導電糊而獲得的塗佈膜中順利地透過,微細圖案成形變得容易。另一方面,若體積平均粒徑為10μm以下,則所製造的導電圖案的表面平滑度、圖案精度及尺寸精度提高。再者,金屬粒子(A)
的體積平均粒徑可藉由庫爾特計數器法(Coulter counter method)而測定。
金屬粒子(A)的添加量較佳為相對於導電糊中的總固體成分為60質量%~95質量%。若相對於總固體成分的添加量為60質量%以上,則固化時的金屬粒子(A)彼此的接觸幾率提高,所製造的導電圖案的比電阻及斷線幾率變低。另一方面,若相對於總固體成分的添加量為95質量%以下,則於曝光步驟中,曝光光可於塗佈導電糊而獲得的塗佈膜中更順利地透過,微細的圖案成形變得容易。此處,所謂總固體成分,是指除溶劑外的導電糊的總構成成分。
本發明的導電糊含有碳粒子(B)。此處,所謂碳粒子,是指碳於粒子總體中所佔的比例為50質量%以上的粒子。由於導電糊中所含的碳粒子於透明電極中尤其是與ITO的潤濕性良好,因此碳粒子聚集於導電糊與ITO的界面,接觸點數增大,導電路徑增加,故使即便經過高濕高熱等環境變化亦能夠穩定地維持接觸電阻的效果增大。
作為碳粒子(B),例如可列舉: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(以上均為三菱化學股份有限公司製造),東海黑(TOKABLACK)#8500/F、
8300/F、7550SB/F、7400、7360SB、7350/F、7270SB、7100F、7050、5500、4500、4400、4300、3855、3845或3800(以上均為東海碳素(Tokai Carbon)股份有限公司製造),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或者旭薩摩(Asahithermal)(以上均為旭碳(Asahi Carbon)股份有限公司製造)。
碳粒子(B)的一次粒子的體積平均粒徑較佳為0.005μm~0.5μm。若一次粒子的體積平均粒徑為0.005μm以上,則導電糊中的分散性及分散穩定性進一步提高,可抑制凝聚物的產生。另一方面,若一次粒子的體積平均粒徑超過0.5μm,則每固定質量的一次粒子數減少,與ITO、銀奈米線(nanowire)、氧化鋅或者氧化錫等透明電極的接觸幾率降低,而存在所製造的導電圖案與透明電極的接觸電阻變高的情況。再者,碳粒子(B)的一次粒子的體積平均粒徑可藉由以下方式而算出:使用電子顯微鏡對隨機選擇的100個一次粒子進行觀察,測定各一次粒子中的最大寬度並求出該些的平均值。
碳粒子(B)的添加量較佳為相對於導電糊中的總固體成分為0.05質量%~3質量%,更佳為0.1質量%~2質量%。若相對於總固體成分的添加量為0.05質量%以上,則碳粒子(B)與透明電極的接觸幾率提高,所製造的導電圖案與透明電極的接觸電阻即便於高濕高熱的環境下亦穩定地變低。另一方面,若相對於總固體成分的添加量為3質量%以下,則於曝光步驟中,曝光光可於
塗佈導電糊而獲得的塗佈膜中順利地透過,微細的圖案成形變得容易。
本發明的導電糊含有具有不飽和雙鍵的化合物(C)。作為具有不飽和雙鍵的化合物(C),例如可列舉:苯乙烯、對甲基苯乙烯、鄰甲基苯乙烯、間甲基苯乙烯、α-甲基苯乙烯、氯甲基苯乙烯或羥基甲基苯乙烯等苯乙烯類,丙烯酸系單體,1-乙烯基-2-吡咯啶酮,丙烯酸系共聚物或者環氧基羧酸酯化合物。
作為丙烯酸系單體,例如可列舉: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、丙烯酸異丁酯、異丙烷丙烯酸酯(isopropane acrylate)、丙烯酸縮水甘油酯、丁氧基三乙二醇丙烯酸酯、丙烯酸二環戊基酯、丙烯酸二環戊烯酯、丙烯酸2-羥基乙酯、丙烯酸異冰片酯、丙烯酸2-羥基丙酯、丙烯酸異癸酯、丙烯酸異辛酯、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、丙烯酸硬脂酯、丙烯酸三氟乙酯、丙烯酸胺基乙酯、丙烯酸苯酯、丙烯酸苯氧基乙酯、丙烯酸1-萘酯、丙烯酸2-萘酯、丙烯酸苯硫酚酯(thiophenol acrylate)或丙烯酸苄硫醇酯(benzyl mercaptan acrylate)、烯丙基化環己基二丙烯酸酯、甲氧基化環己基二丙烯酸酯、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甘油二丙烯酸酯、
三羥甲基丙烷三丙烯酸酯、二-三羥甲基丙烷四丙烯酸酯、二季戊四醇單羥基五丙烯酸酯或二季戊四醇六丙烯酸酯、丙烯醯胺、N-甲氧基甲基丙烯醯胺、N-乙氧基甲基丙烯醯胺、N-正丁氧基甲基丙烯醯胺或N-異丁氧基甲基丙烯醯胺、具有藉由不飽和酸使環氧基開環的羥基的乙二醇二縮水甘油醚的丙烯酸加成物、二乙二醇二縮水甘油醚的丙烯酸加成物、新戊二醇二縮水甘油醚的丙烯酸加成物、丙三醇二縮水甘油醚(glycerine diglycidyl ether)的丙烯酸加成物、雙酚A二縮水甘油醚的丙烯酸加成物、雙酚F的丙烯酸加成物或甲酚酚醛清漆的丙烯酸加成物等環氧丙烯酸酯單體或γ-丙烯醯氧基丙基三甲氧基矽烷、或者將該些的丙烯酸基取代為甲基丙烯酸基而成的化合物。
所謂丙烯酸系共聚物,是指於所使用的單體即共聚合成分中包含丙烯酸系單體的共聚物。
具有羧基的鹼可溶性的丙烯酸系共聚物可藉由使用不飽和羧酸等不飽和酸作為單體而獲得。作為不飽和酸,例如可列舉:丙烯酸、甲基丙烯酸、衣康酸、丁烯酸、馬來酸、富馬酸或乙酸乙烯酯或者該些的酸酐。可藉由所使用的不飽和酸的多寡來調整所得的丙烯酸系共聚物的酸價。
另外,藉由使上述丙烯酸系共聚物所具有的羧基、與(甲基)丙烯酸縮水甘油酯等具有不飽和雙鍵的化合物反應,可獲得於側鏈具有反應性不飽和雙鍵的鹼可溶性的丙烯酸系共聚物。
所謂環氧基羧酸酯化合物,是指可將環氧化合物、與具
有不飽和雙鍵的羧基化合物作為起始原料進行合成的化合物。作為可成為起始原料的環氧化合物,例如可列舉縮水甘油醚類、脂環式環氧樹脂、縮水甘油酯類、縮水甘油胺類或者環氧樹脂,更具體而言,可列舉:甲基縮水甘油醚、乙基縮水甘油醚、丁基縮水甘油醚、乙二醇二縮水甘油醚、二乙二醇二縮水甘油醚、丙二醇二縮水甘油醚、三丙二醇二縮水甘油醚、新戊二醇二縮水甘油醚、雙酚A二縮水甘油醚、氫化雙酚A二縮水甘油醚、雙酚F二縮水甘油醚、雙酚S二縮水甘油醚、雙酚茀二縮水甘油醚、聯苯酚二縮水甘油醚、四甲基聯苯酚縮水甘油醚、三羥甲基丙烷三縮水甘油醚、3',4'-環氧環己基甲基-3,4-環氧環己烷羧酸酯或者第三丁基縮水甘油胺。另外,作為具有不飽和雙鍵的羧基化合物,例如可列舉(甲基)丙烯酸、丁烯酸、桂皮酸或者α-氰基桂皮酸。
亦可使環氧羧酸酯化合物與多元酸酐反應來調整環氧羧酸酯化合物的酸價。作為多元酸酐,例如可列舉:丁二酸酐、鄰苯二甲酸酐、四氫鄰苯二甲酸酐、六氫鄰苯二甲酸酐、衣康酸酐、3-甲基四氫鄰苯二甲酸酐、4-甲基-六氫鄰苯二甲酸酐、偏苯三甲酸酐或者馬來酸酐。
亦可藉由使與上述多元酸酐反應而得的環氧羧酸酯化合物所具有的羧基、與(甲基)丙烯酸縮水甘油酯等具有不飽和雙鍵的化合物反應,來調整環氧羧酸酯化合物所具有的反應性不飽和雙鍵的量。
亦可藉由使環氧羧酸酯化合物所具有的羥基與二異氰酸
酯化合物反應而進行胺基甲酸酯化。作為二異氰酸酯化合物,例如可列舉:六亞甲基二異氰酸酯、四甲基二甲苯二異氰酸酯、萘-1,5-二異氰酸酯、甲伸苯基二異氰酸酯(tolylene diisocyanate)、三甲基六亞甲基二異氰酸酯、異佛爾酮二異氰酸酯、烯丙基氰基二異氰酸酯或者降冰片烷二異氰酸酯。
為使鹼可溶性極為合適,具有不飽和雙鍵的化合物(C)的酸價較佳為30mgKOH/g~250mgKOH/g。若酸價未滿30mgKOH/g,則有時可溶部分的溶解性降低。另一方面,若酸價超過250mgKOH/g,則有時顯影容許範圍變窄。再者,具有不飽和雙鍵的化合物(C)的酸價可以JIS K 0070(1992)為基準進行測定。
本發明的導電糊含有光聚合起始劑(D)。作為光聚合起始劑(D),例如可列舉:1,2-辛二酮-1-[4-(苯硫基)-2-(O-苯甲醯肟)]、2,4,6-三甲基苯甲醯基-二苯基-氧化膦、雙(2,4,6-三甲基苯甲醯基)-苯基氧化膦、乙酮-1-[9-乙基-6-2-(2-甲基苯甲醯基)-9H-咔唑-3-基]-1-(O-乙醯肟)、二苯甲酮、鄰苯甲醯基苯甲酸甲酯、4,4'-雙(二甲胺基)二苯甲酮、4,4'-雙(二乙胺基)二苯甲酮、4,4'-二氯二苯甲酮、4-苯甲醯基-4'-甲基二苯基酮、二苄基酮、茀酮、2,2'-二乙氧基苯乙酮、2,2-二甲氧基-2-苯基苯乙酮、2-羥基-2-甲基苯丙酮、對第三丁基二氯苯乙酮、噻噸酮、2-甲基噻噸酮、2-氯噻噸酮、2-異丙基噻噸酮、二乙基噻噸酮、苯偶醯、苯偶醯二甲基縮酮、苄基-β-甲氧基乙基縮醛、安息香、安息香甲醚、安息香丁醚、蒽醌、
2-第三丁基蒽醌、2-戊基蒽醌、β-氯蒽醌、蒽酮、苯并蒽酮、二苯并環庚酮(dibenzosuberone)、亞甲基蒽酮、4-疊氮亞苄基苯乙酮(4-azidobenzal acetophenone)、2,6-雙(對疊氮苯亞甲基)環己酮、6-雙(對疊氮苯亞甲基)-4-甲基環己酮、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-苯甲醯基)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-苯甲醯基)肟、米氏酮(Michler's ketone)、2-甲基-[4-(甲硫基)苯基]-2-嗎啉基-1-丙酮、萘磺醯氯(naphthalene sulfonyl chloride)、喹啉磺醯氯(quinoline sulfonyl chloride)、N-苯基硫代吖啶酮(N-phenylthioacridone)、4,4'-偶氮雙異丁腈、二硫化二苯(diphenyl disulfide)、二硫化苯并噻唑、三苯基膦、樟腦醌(camphorquinone)、2,4-二乙基噻噸酮、異丙基噻噸酮、四溴化碳、三溴苯碸(tribromophenyl sulfone)、過氧化苯甲醯、曙紅(eosin)或者亞甲基藍等光還原性色素與抗壞血酸或三乙醇胺等還原劑的組合,較佳為光感度高的肟酯系化合物。
光聚合起始劑(D)的添加量較佳為相對於具有不飽和雙鍵的化合物(C)100質量份為0.05質量份~30質量份。若相對於具有不飽和雙鍵的化合物(C)100質量份的添加量為0.05質量份以上,則曝光部的硬化密度增加,可提高顯影後的殘膜率。另一方面,若相對於具有不飽和雙鍵的化合物(C)100質量份的添加量為30質量份以下,則會抑制塗佈導電糊而獲得的塗佈膜上部的因光聚合起始劑(D)所致的過剩的光吸收。結果會抑制因所製
造的導電圖案成為倒錐形狀所致的與基板的密接性降低。
關於本發明的導電糊,亦可與光聚合起始劑(D)一併而含有增感劑。
作為增感劑,例如可列舉:2,4-二乙基噻噸酮、異丙基噻噸酮、2,3-雙(4-二乙胺基亞苄基)環戊酮、2,6-雙(4-二甲胺基亞苄基)環己酮、2,6-雙(4-二甲胺基亞苄基)-4-甲基環己酮、米氏酮、4,4-雙(二乙胺基)二苯甲酮、4,4-雙(二甲胺基)查耳酮、4,4-雙(二乙胺基)查耳酮、對二甲胺基苯亞烯丙基二氫茚酮(p-dimethylamino cinnamylidene indanone)、對二甲胺基苯亞甲基二氫茚酮(p-dimethylamino benzylidene indanone)、2-(對二甲胺基苯基亞乙烯基)異萘并噻唑、1,3-雙(4-二甲胺基苯基亞乙烯基)異萘并噻唑、1,3-雙(4-二甲胺基亞苄基)丙酮、1,3-羰基雙(4-二乙胺基亞苄基)丙酮、3,3-羰基雙(7-二乙胺基香豆素)、N-苯基-N-乙基乙醇胺、N-苯基乙醇胺、N-甲苯二乙醇胺(N-tolyldiethanolamine)、二甲胺基苯甲酸異戊酯、二乙胺基苯甲酸異戊酯、3-苯基-5-苯甲醯基硫代四唑或者1-苯基-5-乙氧基羰基硫代四唑。
增感劑的添加量較佳為相對於具有不飽和雙鍵的化合物(C)100質量份為0.05質量份~10質量份。若相對於具有不飽和雙鍵的化合物(C)100質量份的添加量為0.05質量份以上,則光感度提高。另一方面,若相對於具有不飽和雙鍵的化合物(C)100質量份的添加量為10質量份以下,則會抑制塗佈導電糊而獲得的塗佈膜上部的過剩的光吸收。結果會抑制因所製造的導電圖
案成為倒錐形狀所致的與基板的密接性降低。
本發明的導電糊含有溶劑(E)。作為溶劑(E),例如可列舉:N,N-二甲基乙醯胺、N,N-二甲基甲醯胺、N-甲基-2-吡咯啶酮、二甲基咪唑啶酮、二甲基亞碸、γ-丁內酯、乳酸乙酯、1-甲氧基-2-丙醇、1-乙氧基-2-丙醇、乙二醇單正丙醚、二丙酮醇、四氫糠醇、丙二醇單甲醚乙酸酯、二乙二醇單甲醚、二乙二醇單乙醚乙酸酯(diethyleneglycol monoethyl ether acetate)(以下為「DMEA」)、二乙二醇單丁醚、二乙二醇單丁醚乙酸酯、三乙二醇二甲醚或者2,2,4-三甲基-1,3-戊二醇單異丁酸酯,較佳為沸點為150℃以上的溶媒。若沸點為150℃以上,則溶劑(E)的揮發得到抑制,可抑制導電糊的增稠。
關於本發明的導電糊,只要為不損及其所期望的特性的範圍,則亦可含有分子內不具有不飽和雙鍵的非感光性聚合物或者塑化劑、調平劑、界面活性劑、矽烷偶合劑、消泡劑或顏料等添加劑。
作為上述非感光性聚合物,例如可列舉:環氧樹脂、酚醛清漆樹脂、苯酚樹脂、聚醯亞胺前驅物或者已閉環的聚醯亞胺。
作為塑化劑,例如可列舉:鄰苯二甲酸二丁酯、鄰苯二甲酸二辛酯、聚乙二醇或者甘油。
作為調平劑,例如可列舉:特殊乙烯系聚合物或者特殊丙烯酸系聚合物。
作為矽烷偶合劑,例如可列舉:甲基三甲氧基矽烷、二
甲基二乙氧基矽烷、苯基三乙氧基矽烷、六甲基二矽氮烷、3-甲基丙烯醯氧基丙基三甲氧基矽烷、3-縮水甘油氧基丙基三甲氧基矽烷或者乙烯基三甲氧基矽烷。
本發明的導電糊是使用例如三輥、球磨機或行星式球磨機等分散機或者混煉機而製造。
本發明的導電圖案的製造方法的特徵在於:將本發明的導電糊塗佈於基板上並加以乾燥,於進行曝光、顯影後,以100℃~300℃加以固化。
藉由將本發明的導電糊塗佈於基板上而獲得塗佈膜。
作為塗佈本發明的導電糊的基板,例如可列舉:聚對苯二甲酸乙二酯膜(polyethylene terephthalate film)(以下為「PET膜」)、聚醯亞胺膜、聚酯膜、聚芳醯胺膜(aramid film)、環氧樹脂基板、聚醚醯亞胺樹脂基板、聚醚酮樹脂基板、聚碸系樹脂基板、玻璃基板、矽晶圓、氧化鋁基板、氮化鋁基板、碳化矽基板、裝飾層形成基板或者絕緣層形成基板。
作為將本發明的導電糊塗佈於基板的方法,例如可列舉:使用旋轉器(spinner)的旋轉塗佈、噴霧(spray)塗佈、輥塗(roll coating)、網版印刷或者使用刮刀塗佈機、模塗機、砑光塗佈機(calender coater)、凹凸塗佈機(meniscus coater)或棒塗機的塗佈。所得的塗佈膜的膜厚只要根據塗佈的方法或者導電糊的總固體成分濃度或黏度等而適宜決定即可,較佳為乾燥後的膜厚成為0.1μm~50μm。再者,膜厚可使用薩弗科姆(SURFCOM)
(注冊商標)1400(東京精密(股)製造)般的觸針式階差計進行測定。更具體而言,可藉由利用觸針式階差計(關鍵尺寸:1mm、掃描速度:0.3mm/sec)分別測定隨機選擇的三個位置的膜厚並求出該些的平均值而算出。
對所得的塗佈膜加以乾燥而使溶劑揮發。作為對塗佈膜加以乾燥而使溶劑揮發去除的方法,例如可列舉藉由烘箱、加熱板或紅外線等的加熱乾燥或者真空乾燥。加熱溫度較佳為50℃~180℃,加熱時間較佳為1分鐘~幾小時。
對於乾燥後的塗佈膜,介隔任意的圖案形成用遮罩,藉由光微影(photolithography)法進行曝光。作為曝光的光源,較佳為水銀燈的i射線(365nm)、h射線(405nm)或者g射線(436nm)。
對於曝光後的塗佈膜,使用顯影液進行顯影,將未曝光部溶解去除而獲得所期望的圖案。作為進行鹼顯影時的顯影液,例如可列舉:氫氧化四甲基銨、二乙醇胺、二乙胺基乙醇、氫氧化鈉、氫氧化鉀、碳酸鈉、碳酸鉀、三乙胺、二乙胺、甲胺、二甲胺、乙酸二甲胺基乙酯、二甲胺基乙醇、甲基丙烯酸二甲胺基乙酯、環己胺、乙二胺或者六亞甲基二胺的水溶液,亦可於該些水溶液中添加N-甲基-2-吡咯啶酮、N,N-二甲基甲醯胺、N,N-二甲基乙醯胺、二甲基亞碸或γ-丁內酯等極性溶媒,甲醇、乙醇或異丙醇等醇類,乳酸乙酯或丙二醇單甲醚乙酸酯等酯類,環戊酮、環己酮、異丁酮或甲基異丁酮等酮類或者界面活性劑。
作為進行有機顯影時的顯影液,例如可列舉:N-甲基-2-吡咯啶酮、N-乙醯基-2-吡咯啶酮、N,N-二甲基乙醯胺、N,N-二甲基甲醯胺、二甲基亞碸或六甲基磷醯三胺(hexamethylphosphortriamide)等極性溶媒或者該些極性溶媒與甲醇、乙醇、異丙醇、二甲苯、水、甲基卡必醇或乙基卡必醇的混合溶液。
作為顯影方法,例如可列舉:將基板靜置或者使其旋轉,同時對塗佈膜面噴霧(spray)顯影液的方法;將基板浸漬於顯影液中的方法;或者將基板浸漬於顯影液中,同時施加超音波的方法。
對於藉由顯影而獲得的圖案,亦可藉由淋洗液而實施淋洗處理。此處,作為淋洗液,例如可列舉水、或者於水中加入乙醇或異丙醇等醇類或者乳酸乙酯或丙二醇單甲醚乙酸酯等酯類而得的水溶液。
對於所得的圖案,以100℃~300℃加以固化。固化的溫度較佳為120℃~180℃。若固化溫度未滿100℃,則樹脂成分的體積收縮量不會變大,比電阻不會充分降低。另一方面,若固化溫度超過300℃,則無法在耐熱性低的基板等材料上製造導電圖案。
作為對所得的圖案加以固化的方法,例如可列舉:藉由烘箱、惰性烘箱(Inert Oven)或者加熱板而進行的加熱乾燥,藉由紫外線燈、紅外線加熱器、鹵化加熱器或氙閃光燈
(xenon flash lamp)等的電磁波或者微波進行的加熱乾燥,或者真空乾燥。藉由加熱,所製造的積層圖案的硬度提高,可抑制因與其他構件接觸所致的缺陷或剝落等,進而可提高與基板的密接性。
本發明的觸控面板的特徵在於:具備由本發明的導電糊所形成的導電圖案、與包含ITO的透明電極,且上述透明電極與上述導電圖案相連接。
使用本發明的導電糊所製造的導電圖案可適宜地用作具備包含ITO的透明電極的觸控面板用的周邊配線。如上所述,原因在於:由於導電糊中所含的碳粒子於透明電極中尤其是與ITO的潤濕性良好,因此碳粒子聚集於導電糊與ITO的界面,接觸點數增大,導電路徑增加,故使即便經過高濕高熱等環境變化亦能夠穩定地維持接觸電阻的效果增大。
作為觸控面板的方式,例如可列舉電阻膜式、光學式、電磁感應式或者靜電電容式。靜電電容式觸控面板尤其要求微細的配線,因此更適宜使用本發明的導電糊。
另外,於靜電電容式觸控面板中,由於需自透明電極向積體電路(integrated circuit,IC)晶片傳送電信號,因此周邊配線的至少一部分需形成於透明電極上。如上所述,使用本發明的導電糊所製造的導電圖案與ITO的連接可靠性優異,因此可更適宜地使用。
於具備藉由本發明的製造方法所製造的導電圖案作為其
周邊配線、且該周邊配線為50μm間距(配線寬度+配線間寬度)以下的觸控面板中,可將邊框寬度變窄,且可將可視區域(view area)擴大。
[實施例]
以下,列舉實施例及比較例來更詳細地對本發明進行說明,但本發明並不限定於該些。
各實施例及比較例中使用的評價方法如下所述。
<圖案成形性的評價方法>
於PET膜上,以乾燥後的膜厚成為7μm的方式塗佈導電糊,將所得的塗佈膜於100℃的乾燥烘箱內乾燥5分鐘。將以一定的線與間隙(Line and Space)(以下為「L/S」)排列的直線群組即透光圖案設為一個單元,介隔分別具有L/S值不同的9種單元的光罩,對乾燥後的塗佈膜進行曝光及顯影,而分別獲得L/S值不同的9種圖案。其後,將所得的9個圖案於140℃的乾燥烘箱內均固化30分鐘,而分別獲得L/S值不同的9種導電圖案。光罩所具有的各單元的L/S值為線寬(μm)/間隔(μm)為500/500、250/250、100/100、50/50、40/40、30/30、25/25、20/20、15/15。藉由光學顯微鏡對所得的導電圖案進行觀察。確認圖案間無殘渣且無圖案剝落、L/S值最小的導電圖案。將該L/S值設為能夠顯影的L/S值。將過顯影而圖案消失者設為「圖案殘缺」。
再者,曝光是使用曝光裝置(PEM-6M;聯合光學(Union Optical)股份有限公司製造)以曝光量150mJ/cm2(波長365nm
換算)來進行全線曝光,顯影是將基板於0.2質量%的Na2CO3溶液中浸漬30秒後,藉由超純水實施淋洗處理來進行。
<比電阻的評價方法>
於PET膜上,以乾燥後的膜厚成為7μm的方式塗佈導電糊,將所得的塗佈膜於100℃的乾燥烘箱內乾燥5分鐘。介隔具有圖1所示的透光圖案A的光罩,對乾燥後的塗佈膜進行曝光及顯影而獲得圖案。其後,將所得的圖案於140℃的乾燥烘箱內固化30分鐘,而獲得比電阻測定用的導電圖案。所得的導電圖案的線寬為0.400mm,線長為80mm。
再者,曝光及顯影的條件與上述圖案成形性的評價方法相同。藉由電阻計將所得的比電阻測定用的導電圖案的各個端部連結並測定電阻值,基於以下的式(1)來算出比電阻。將未能見到導通者設為「絕緣」。
比電阻=電阻值×膜厚×線寬/線長…(1)。
<與透明電極的連接可靠性評價方法>
於PET膜的整面形成有透明電極的透明導電膜上,以乾燥後的膜厚成為7μm的方式塗佈導電糊,藉由100℃的乾燥烘箱將所得的塗佈膜乾燥5分鐘。介隔具有圖2所示的透光圖案A的光罩,對乾燥後的塗佈膜進行曝光及顯影而獲得圖案。其後,將所得的圖案於140℃的乾燥烘箱內固化30分鐘,而獲得與透明電極的連
接可靠性評價樣品。所得的樣品中導電圖案的線寬為0.100mm,線間為5mm,端部為直徑2mm的圓形。
藉由試驗器(tester)將所得的樣品中導電圖案的端部連結,測定初始電阻值後,於85℃、85%RH的恒溫恒濕槽(LU-113;愛斯佩克(Espec)(股))內保管500小時。其後,藉由試驗器將取出的樣品中導電圖案的端部連結,測定保管後電阻值,基於以下的式(2)算出電阻變化率。將所算出的電阻變化率為1.30以下者判定為A,將大於1.30且為1.50以下者判定為B,將大於1.50者判定為C。
電阻變化率=保管後電阻值(500小時後)/初始電阻值…(2)。
再者,所測定的初始電阻值及保管後電阻值是嚴格地將導電圖案與透明電極的接觸電阻的值與導電圖案的電阻值及透明電極的電阻值相加而算出的值。然而,導電圖案的電阻值及透明電極的電阻值與接觸電阻的值相比極小,因此能夠以初始電阻值及保管後電阻值來評價接觸電阻的變化率。
各實施例及比較例中使用的材料如下所述。
[金屬粒子(A)]
體積平均粒徑為1.0μm的Ag粒子;體積平均粒徑為1.0μm的Au粒子。
[碳粒子(B)]
一次粒子的體積平均粒徑為0.05μm的碳粒子(碳於粒子總體中所佔的比例:99質量%)。
[具有不飽和雙鍵的化合物(C)]
(單體)
萊特丙烯酸酯(Light Acrylate)BP-4EA(以下為「BP-4EA」;共榮社化學(股)製造)
(合成例1:化合物(C-1))
共聚合比率(質量基準):丙烯酸乙酯(以下為「EA」)/甲基丙烯酸2-乙基己酯(以下為「2-EHMA」)/苯乙烯(以下為「St」)/甲基丙烯酸縮水甘油酯(以下為「GMA」)/丙烯酸(以下為「AA」)=20/40/20/5/15
向氮氣環境的反應容器中裝入150g的DMEA,使用油浴(oil bath)升溫至80℃。於其中,用1小時滴加包含20g的EA、40g的2-EHMA、20g的St、15g的AA、0.8g的2,2'-偶氮雙異丁腈及10g的DMEA的混合物。滴加結束後,進而進行6小時聚合反應。其後,添加1g的對苯二酚單甲醚,停止聚合反應。繼而,用0.5小時滴加包含5g的GMA、1g的三乙基苄基氯化銨(triethylbenzylammonium chloride)及10g的DMEA的混合物。滴加結束後,進而進行2小時加成反應。藉由利用甲醇對所得的反應溶液進行純化而將未反應雜質去除,進而進行24小時真空乾燥,藉此獲得化合物(C-1)。所得的化合物(C-1)的酸價為103
mgKOH/g。
(合成例2:化合物(C-2))
共聚合比率(質量基準):環氧乙烷改質雙酚A二丙烯酸酯(FA-324A;日立化成工業(股)製造)/EA/GMA/AA=60/25/10/5
向氮氣環境的反應容器中裝入150g的DMEA,使用油浴升溫至80℃。於其中,用1小時滴加包含60g的環氧乙烷改質雙酚A二丙烯酸酯、25g的EA、5g的AA、0.8g的2,2'-偶氮雙異丁腈及10g的DMEA的混合物。滴加結束後,進而進行6小時聚合反應。其後,添加1g的對苯二酚單甲醚,停止聚合反應。繼而,用0.5小時滴加包含10g的GMA、1g的三乙基苄基氯化銨及10g的DMEA的混合物。滴加結束後,進而進行2小時加成反應。藉由利用甲醇對所得的反應溶液進行純化而將未反應雜質去除,進而進行24小時真空乾燥,藉此獲得具有羧基及不飽和雙鍵的化合物(C-2)。所得的化合物(C-2)的酸價為1.4mgKOH/g。
(合成例3:化合物(C-3))
向氮氣環境的反應容器中裝入123g的RE-310S(日本化藥(股)製造)、47g的AA、0.3g的對苯二酚單甲醚及0.5g的三苯基膦,於98℃的溫度下進行反應直至反應液的酸價成為0.5mgKOH/g以下,而獲得化合物(C-3)。所得的化合物(C-3)的酸價為0.4mgKOH/g。
(合成例4:化合物(C-4))
向氮氣環境的反應容器中裝入164g的卡必醇乙酸酯、287g
的EOCN-103S(日本化藥(股)製造)、96g的AA、2g的2,6-二-第三丁基-對甲酚及2g的三苯基膦,於98℃的溫度下進行反應直至反應液的酸價成為0.5mgKOH/g以下,獲得環氧羧酸酯化合物。繼而,於該反應液中裝入57g的卡必醇乙酸酯及67g的四氫鄰苯二甲酸酐,於95℃下反應4小時,而獲得化合物(C-4)。所得的化合物(C-4)的酸價為104mgKOH/g。
(合成例5:化合物(C-5))
向氮氣環境的反應容器中裝入123g的RE-310S(日本化藥(股)製造)、47g的AA、0.3g的對苯二酚單甲醚及0.5g的三苯基膦,於98℃的溫度下進行反應直至反應液的酸價成為0.5mgKOH/g以下,而獲得環氧羧酸酯化合物。其後,於該反應溶液中加入252g的卡必醇乙酸酯、89g的2,2-雙(二羥甲基)-丙酸、0.4g的2-甲基對苯二酚及47g的螺甘油(spiroglycol),升溫至45℃。於該溶液中,以反應溫度不會超過65℃的方式,緩緩滴加162g的三甲基六亞甲基二異氰酸酯。滴加結束後,使反應溫度上升為80℃,藉由紅外線吸收光譜測定法反應6小時,直至變為2250cm-1附近的吸收不存在,而獲得化合物(C-5)。所得的化合物(C-5)的酸價為80.0mgKOH/g。
(合成例6:化合物(C-6))
向氮氣環境的反應容器中裝入300g的代那考爾(Denacol)EX-203(長瀨化成(Nagase ChemteX)(股)製造)的丙烯酸加成物(分子量:368)、500g的DMEA、0.5g的2-甲基對苯二酚及
200g的2,2-雙(羥基甲基)丙酸,升溫至45℃。於該溶液中,以反應溫度不會超過50℃的方式,緩緩滴加201.3g的甲苯二異氰酸酯。滴加結束後,使反應溫度上升為80℃,藉由紅外線吸收光譜測定法反應6小時,直至變為2250cm-1附近的吸收不存在。向該溶液中加入120g的甲基丙烯酸縮水甘油酯,升溫至95℃並反應6小時,而獲得化合物(C-6)。所得的化合物(C-6)的酸價為83mgKOH/g。
[光聚合起始劑(D)]
豔佳固(IRGACURE)(注冊商標)OXE-01(以下為「OXE-01」;日本汽巴(Ciba Japan)(股)製造);豔佳固(IRGACURE)(注冊商標)369(以下為「IC-369」;日本汽巴(Ciba Japan)(股)製造)。
[溶劑(E)]
DMEA(東京化成工業(股)製造)。
[透明電極]
ITO膜(日東電工(股)製造);銀奈米線膜(日立化成(股)製造)。
(實施例1)
於100mL的潔淨瓶(clean bottle)中加入10.0g的化合物(C-1)、0.50g的OXE-01、5.0g的DMEA及2.0g的BP-4EA,藉由自轉-公轉真空混合機「去泡煉太郎」ARE-310(注冊商標;新基(Thinky)(股)製造)進行混合,而獲得17.5g的樹脂溶液
(固體成分71.4質量%)。
將所得的17.5g的樹脂溶液、85.0g的Ag粒子及2.5g的碳粒子(B)混合,使用三輥磨機(艾卡特(EXAKT)M-50;艾卡特(EXAKT)公司製造)進行混煉,而獲得105.0g的導電糊。
使用所得的導電糊,分別評價導電圖案的圖案成形性、比電阻及與ITO的連接可靠性。確認到:成為圖案成形性的評價指標的能夠顯影的L/S值為15μm/15μm,且達成良好的圖案加工。導電圖案的比電阻為5.5×10-5Ωcm。與ITO的連接可靠性評價中電阻變化率為1.03且良好。
(實施例2~實施例14)
藉由與實施例1相同的方法製造表1所示的組成的導電糊,將進行與實施例1相同的評價而得的結果示於表2。
(比較例1~比較例4)
藉由與實施例1相同的方法製造表1所示的組成的導電糊,將進行與實施例1相同的評價而得的結果示於表2。
關於實施例1~實施例14的導電糊,均可製造圖案成形性、比電阻及與ITO的連接可靠性優異的導電圖案。另一方面,關於比較例1的導電糊,高溫高濕度下與ITO的連接可靠性降低,關於比較例2及比較例4的導電糊,顯影中圖案流動而無法製造微細的配線,進而,使用比較例3的導電糊而製造的導電圖案未顯示出導電性。
[表1]
[產業上之可利用性]
本發明的導電糊可適宜地利用於觸控面板用周邊配線等的導電圖案的製造。
Claims (5)
- 一種導電糊,其含有:金屬粒子(A);碳粒子(B);具有不飽和雙鍵的化合物(C);光聚合起始劑(D);以及溶劑(E),且所述金屬粒子(A)相對於所述碳粒子(B)的質量比為100~1900,所述具有不飽和雙鍵的化合物(C)的酸價為30mgKOH/g~250mgKOH/g。
- 如申請專利範圍第1項所述的導電糊,其含有肟酯系化合物作為所述光聚合起始劑(D)。
- 如申請專利範圍第1項或第2項所述的導電糊,其中所述金屬粒子(A)的體積平均粒徑為0.1μm~10μm,且所述碳粒子(B)的一次粒子的體積平均粒徑為0.005μm~0.5μm。
- 一種觸控面板,其具備由如申請專利範圍第1項至第3項中任一項所述的導電糊所形成的導電圖案、與包含ITO的透明電極,且所述透明電極與所述導電圖案相連接。
- 一種導電圖案的製造方法,其是將如申請專利範圍第1項至第3項中任一項所述的導電糊塗佈於基板上並加以乾燥,於進行曝光、顯影後,以100℃~300℃加以固化。
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