CN107922767B - 具有改进导电性的油墨组合物 - Google Patents
具有改进导电性的油墨组合物 Download PDFInfo
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- CN107922767B CN107922767B CN201680047649.6A CN201680047649A CN107922767B CN 107922767 B CN107922767 B CN 107922767B CN 201680047649 A CN201680047649 A CN 201680047649A CN 107922767 B CN107922767 B CN 107922767B
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- Non-Insulated Conductors (AREA)
Abstract
本文提供具有改进导电性的油墨组合物。改进的导电性归因于向组合物中添加有机卤素化合物。
Description
背景
领域
本文提供具有改进导电性的油墨组合物。改进的导电性归因于向组合物中添加有机卤素化合物。
相关技术简介
导电的油墨组合物是已知的。用于向那些组合物赋予导电性的主要成分之一是银。银价近来波动极大,使得制造商难以管理他们的产品线。因此,最近盛行涉及导电性的研究和开发调查。
迄今为止,已经使用各种方法来形成导电油墨组合物并改进此类组合物的导电性。例如,已将银络合物引入所述组合物中然后使所述组合物经历升高的温度条件如大于150℃,以使银络合物分解。在银络合物分解之后,原位形成银纳米颗粒,其能够增强导电性。然而,许多热敏的应用要求低于150℃的加工温度。
已经使用水性体系,其中离子性卤素盐、酸和离子性卤素聚合物形成导电油墨组合物的成分。已知离子组分会导致电子设备过早失效,特别是在苛刻的环境条件下。
随着热敏基材的使用在电子工业中变得越来越盛行,对在低于150℃的温度下加工后具有高导电性的材料存在强烈的需求。例如,随着移动技术的进步,存在降低触摸屏传感器上的边框宽度(bezel width)和改进边框线导电性的迫切需要。降低的边框宽度增加了在所有其他保持相同下使屏幕尺寸最大化的机会。然而,随着边框宽度降低,边框线导电性也降低,从而导致较不敏感的触控板。
因此,理想的是提供一种所述需求的替代性解决方案,以对获得导电油墨组合物的导电性的方式提供改进。
概述
本发明提供这样的解决方案。
广泛地说,本发明提供一种导电油墨组合物,所述导电油墨组合物包含银组分,其中至少约50%的银组分由具有大于约100nm且小于约1μm的粒径的银组成;载体;和有机卤素化合物。
所述有机卤素化合物用于改进所述油墨组合物的导电性,且在减少所述银组分的负载的同时维持导电性。
在另一方面,本发明提供一种改进油墨组合物的导电性的方法,所述方法包括下述步骤:
提供包含下述组分的油墨组合物:
银组分,其中至少约50%的银组分由具有大于约100nm且小于约1μm的粒径的银组成;和
载体;和
将有机卤素化合物提供至所述银组分和所述载体,
其中所述有机卤素化合物接触所述银组分以改进当电流通过所述油墨组合物时的导电性。
详细说明
如上所述,本发明提供一种导电油墨组合物,其包含银组分,其中至少约50%的银组分由具有大于约100nm且小于约1μm的粒径的银组成;载体;和有机卤素化合物。
所述有机卤素化合物用于改进所述油墨组合物的导电性,且在减少所述银组分的负载的同时维持导电性。
所述银组分可以是适合于目前商业应用的任何形状。例如,球形、长方形(oblong)、粉末和薄片形状的银是可用的。银可以作为在适合的液体介质中的分散体或作为干燥形式的固体提供和维持。
银可来源自各种商业供应商,如Ames Goldsmith Corporation,Glenn Falls,NY、Inframat Advanced Materials,Manchester,CT或Metalor Technologies USACorporation,North Attleboro,MA。也可以使用不同尺寸的银薄片的混合物,如可从Ames商购获得的11000-25与可从Inframat Advanced Materials,Manchester,CT商购获得的47MR-23S的混合物。D50和D95是具有某种特定粒径的银的工业公认标识。例如,D50具有大约50%的银颗粒小于特定尺寸;D95具有大约95%的银颗粒小于特定尺寸。
所述银组分可以所述组合物的约40重量%至约80重量%的范围内使用,如所述组合物的约60重量%至约75重量%的范围内。
所述载体为所述银组分和所述有机卤素化合物分散在其中的介质。所述载体可以是热塑性树脂或热固性树脂。适合用作所述载体的热塑性树脂的实例包括热塑性聚氨酯,如可从The Lubrizol Company,Cleveland,OH根据商品名ESTANE商购获得的那些,如ESTANE 5700系列,其实例是ESTANE 5703。
也可以使用其它热塑性树脂,如表氯醇与双酚的热塑性聚合物,可作为苯氧基树脂从InChem Corp,Rocky Hill,SC商购获得;聚酯树脂,如可从Bostik,Wauwatosa,WI根据商品名VITEL商购获得的那些,如VITEL 2000系列,其实例是VITEL 2700B;纤维素,如乙基纤维素(EC),如来自Ashland,Wilmington,DE的EC N7;乙酸丁酸纤维素,如例如来自Eastman Chemicals,Kingsport,TN的CAB-531-1;丙烯酸树脂,可从Dow Chemical,Midland,MI根据Paraloid商品名商购,如Paraloid A14;来自Sekisui Chemical Co.,Tokyo,Japan的聚乙烯醇缩丁醛树脂,如S-LEC B系列,例如S-LEC BL-1;和来自SekisuiChemical Co.,Tokyo,Japan的聚乙烯醇缩乙醛树脂,如S-LEC k系列,例如S-LEC KS-1。
所述组合物可任选地进一步包含一种或多种选自由下述组成的组的热固性树脂:环氧官能化树脂、丙烯酸酯、氰酸酯、聚硅氧烷、氧杂环丁烷、马来酰亚胺和它们的任意混合物。
各种环氧官能化树脂是适合的,包括基于双酚A的液体型环氧树脂、基于双酚A的固体型环氧树脂、基于双酚F的液体型环氧树脂、基于苯酚-酚醛清漆树脂的多官能环氧树脂、二环戊二烯型树脂、萘型环氧树脂和它们的任意混合物。示例性的环氧官能化树脂包括环脂族醇的双环氧化物、氢化双酚A、六氢邻苯二甲酸酐的二官能化环脂族缩水甘油酯和它们的任意混合物。
适合的(甲基)丙烯酸酯包括具有如下通式结构I的化合物:
其中R为H或甲基,和X选自(a)具有8至24个碳原子范围内的烷基,或(b)
其中R为H或甲基,R'独立地选自H或甲基,并且x为2至6的整数。理想地,(甲基)丙烯酸酯选自甲基丙烯酸十三烷酯、二甲基丙烯酸1,6-己二醇酯、二丙烯酸1,10-癸二醇酯、二甲基丙烯酸1,10-癸二醇酯、二丙烯酸1,12-十二烷二醇酯、二甲基丙烯酸1,12-十二烷二醇酯和它们的任意混合物。
适合的氰酸酯含有两个或更多个形成氰酸酯(-O-C=N)基团的环,其在加热时形成取代的三嗪环。可使用的氰酸酯选自1,1-双(4-氰酰苯基)甲烷、1,1-双(4-氰酰苯基)乙烷、2,2-双(4-氰酰苯基)丙烷、双(4-氰酰苯基)-2,2-丁烷、1,3-双2-(4-氰酰苯基)丙基苯、双(4-氰酰苯基)醚、4,4'-二氰酰二苯基、双(4-氰酰-3,5-二甲基苯基)甲烷、三(4-氰酰苯基)乙烷、氰化酚醛清漆、1,3-双-4-氰酰苯基-1-(1-甲基亚乙基)苯、氰化苯酚-二环戊二烯加合物和它们的任意混合物。
适合的聚硅氧烷包括氢化物封端的(一种或多种)聚硅氧烷和乙烯基封端的(一种或多种)聚硅氧烷的基本上化学计量混合物,其中氢化物封端的聚硅氧烷为氢化物封端的聚二甲基硅氧烷并且乙烯基封端的聚硅氧烷为二乙烯基封端的聚二甲基硅氧烷。
适合的树脂还包括含有氧杂环丁烷的单体和/或低聚物。
适合的马来酰亚胺树脂包括双马来酰亚胺,如来自Designer Molecules Inc.,San Diego,CA的BMI-1500和BMI-3000,以下提供其结构。
其中n=1至10
其中n=1至10
所述载体应以约0.5重量%至15重量%的量使用。
所述有机卤素化合物在室温下应为液体。通常,所述有机卤素化合物具有低于约150℃、例如低于约120℃、理想地低于约100℃和适合地高于约70℃的沸点。
所述有机卤素化合物理想地具有一个或多个连接其上的碘原子。理想地,仅一个碘原子连接至所述有机碘化合物。
所述有机卤素化合物的有机部分可以是烷基或芳基。当其为烷基时,其应为烷基部分至多十二个碳原子的低级烷基。
所述有机卤素化合物的代表实例包括2-碘丙烷、1-碘丙烷、2-碘-2-甲基丙烷、2-碘丁烷、2-氟三氟甲苯、3-氟三氟甲苯、4-氟三氟甲苯、氟苯、2-氟乙醇、1-氟十二烷、1-氟己烷、1-氟庚烷和三氟乙酸。当然,也可以使用这些有机卤素化合物中任意两种或更多种的混合物。
所述有机卤素化合物应以≤5重量%的量使用。理想地,如约0.05-2重量%。例如,约0.25重量%已证明是特别有效的。
为了使本发明的导电油墨组合物更容易地可分配,经常理想的是将所述组合物稀释在适合的溶剂中。所述稀释应为约1份组合物比约5份溶剂。许多溶剂适合用于本发明的组合物,在溶剂选择上没有特别的限制,只要溶剂与所述有机卤素化合物相容。
溶剂的代表实例包括二丙二醇甲基醚、乙酸卡必醇酯、己二酸二甲酯和它们的任意混合物。
根据需要,可使用各种增稠剂或触变剂调节所述导电油墨组合物的粘度。例如,在一些商业应用中,理想的是本发明的油墨组合物具有约10Pa·s至约100Pa·s范围内的粘度,以优化其在高速印刷工艺中的使用。
适合的增稠剂和触变剂的实例包括根据各种商品名的氢化蓖麻油,如ISCATHIXISP;根据各种商品名的有机酰胺,如来自ISCA UK Lte,Wales,UK的ISCATHIX SR;气相法二氧化硅,包括来自Cabot Corp.,Boston,MA的Cab-O-Sil TS720。这些增稠剂和触变剂应以约0.05%-2重量%的量使用。
根据需要,也可以使用各种分散剂调节所述导电油墨组合物的粘度,以适当地分散导电填料,从而确保均匀的填料和使结块最小化。适合的分散剂的实例包括可根据DISPERBYK商品名从Altana获得的那些,如DISPERBYK 111和DISPERBYK 168。
表面张力改性剂经常用于所述配制物,以改进加工和固化后的基材润湿和表面质地。表面张力改性剂的实例为:氟化表面活性剂,如来自Dupont,Willmington,DE的Capstone系列;来自Dow Chemical,Midland,MI的非离子型辛基苯酚乙氧基化物Triton系列;和含有表面添加剂的聚二甲基硅氧烷,如来自Altana的BYK 333。
本发明的导电油墨组合物适合于其中在塑料基材如PET和PC上要求高导电性的应用。
实施例
表I提供可用作本发明范围内的导电促进剂的有机卤素化合物的列表。具有低于约150℃的沸点的有机卤素化合物促进在固化的导电油墨中最少的残留物。
表I
表II提供具有和不具有有机卤素导电促进剂的导电油墨组合物。通过将各成分添加至容器并将混合物在室温下匀化约1小时的时间来制备样品。
表II
!聚酯型热塑性聚氨酯,可从The Lubrizol Company,Cleveland,OH商购获得
@用于溶剂型和不含溶剂的涂料和印刷油墨以稳定无机颜料的不含溶剂的润湿和分散添加剂,特别是二氧化钛,可从BYK-Chemie GmbH,Wesel,Germany商购获得
与对照样品相比,如从样品B和C可见,当它们在120℃的温度下固化30分钟的时间后,体积电阻率降低的效果在0.2重量%和0.3重量%的2-碘丙烷负载下非常显著。那些样品分别显示出比对照好10-20倍的导电性。更具体地说,以Ω·cm测量,对于对照,体积电阻率测定为2.9×10-4和对于样品A、B以及C,体积电阻率分别测定为2.1×10-4、2.5×10-5和1.4×10-5。
根据下述方式测量体积电阻率:
1.取三片清洁的载玻片
2.将一片3M Scotch Magic胶带放置于每片载玻片,以使整个长度和约40%的宽度被覆盖
3.将第二片3M Scotch Magic胶带平行于第一片胶带放置,以使胶带的边缘相隔约3mm。
4.将第二层3M Scotch Magic胶带放置在第一层的上面,确保胶带之间以及胶带与玻璃之间没有截留任何异物或空气。
5.在3mm的沟槽中施加材料。使用另一片载波片以通过跨越胶带移动载玻片来刮掉过量材料。
6.移去胶带,并在给定时间和温度下固化材料
7.在测试前,使载玻片冷却至室温
8.将万用表的探针以5.0cm间隔放置于材料条的中心,测量电阻,以Ω计
9.使用显微镜或卡尺测量线宽度
10.通过卡尺测量厚度
11.计算VR(Ω-cm)=R(Ω)×宽度(cm)×厚度(cm)/5(cm)
在表III中,示出导电油墨的不同固化条件对体积电阻率的影响。
表III
固化条件对体积电阻率的影响示出在表III中,其中在80℃至120℃范围的温度下固化油墨后,2-碘丙烷能够将体积电阻率降低1个数量级。当100℃下的固化时间从5分钟变化至30分钟时,也观察到导电性增强。对于热敏的塑料基材如PET和PC,低固化温度和短固化时间下的高导电性是非常理想的。
在表IV中,示出Ag体积%对体积电阻率的影响。
表IV
在导电油墨组合物中使用有机卤素显著地改进导电性,甚至在低银负载下。通常,在导电油墨组合物中,银将以约55-约75体积%的范围存在。1号样品为具有基于(V/W)的69.5的银含量的代表性导电油墨组合物。(1-6号样品的残留成分为树脂、溶剂和分散剂。)1-4号样品表明,在不含有机卤素例如2-碘丙烷的情况下,随着银体积百分比从69.5%降低至48.7%,体积电阻率增大。在48.7%下,体积电阻如此高,以致所述材料不再记录为导电的。但是,当0.25重量%的碘丙烷添加至4号样品(变成5号样品)时,5号样品变成非常导电,具有1.67×10-5ohm.cm的体积电阻率测量值。该值比1号样品更导电,1号样品具有超过20体积%的更多负载水平的银(69.5体积%)。在6号样品中,在添加0.25重量%的碘丙烷的情况下,银体积百分比进一步降低至44%。6号样品达到与1号样品所示的相同体积电阻率,1号样品具有超过25体积%的更多负载水平的银(69.5体积%)。
Claims (12)
1.一种导电油墨组合物,包含:
银组分,其中至少50%的银组分由具有大于100nm且小于1μm的粒径的银组成;
载体;和
有机卤素化合物,所述有机卤素化合物选自2-碘丙烷、1-碘丙烷、2-碘-2-甲基丙烷、2-碘丁烷、2-氟三氟甲苯、3-氟三氟甲苯、4-氟三氟甲苯、氟苯、2-氟乙醇、1-氟十二烷、1-氟己烷、1-氟庚烷和其任意混合物;
其中所述银组分在所述导电油墨组合物中的含量为40重量%-80重量%,
所述载体在所述导电油墨组合物中的含量为0.5重量%-15重量%,和
所述有机卤素化合物在所述导电油墨组合物中的含量为小于等于5重量%。
2.权利要求1所述的油墨组合物,其中所述有机卤素化合物在室温下为液体。
3.权利要求1所述的油墨组合物,其中所述卤素为碘。
4.权利要求1所述的油墨组合物,其中所述有机卤素化合物为低级烷烃卤化物。
5.权利要求1所述的油墨组合物,其中所述有机卤素化合物由具有至多十二个碳原子的卤代化合物表示。
6.权利要求1所述的油墨组合物,其中所述有机卤素化合物具有低于150℃的沸点。
7.权利要求1所述的油墨组合物,其中所述有机卤素化合物接触所述银组分以改进导电性。
8.权利要求1所述的油墨组合物,其中所述载体为热塑性树脂。
9.权利要求1所述的油墨组合物,其中所述载体为热固性树脂。
10.权利要求1所述的油墨组合物,进一步包含溶剂。
11.一种改进油墨组合物的导电性的方法,包括下述步骤:
提供包含下述组分的油墨组合物:
银组分,其中至少50%的银组分由具有大于100nm且小于1μm的粒径的银组成;和
载体;和
将有机卤素化合物提供至所述银组分和所述载体,其中所述有机卤素化合物接触所述银组分以改进当电流通过所述油墨组合物时的导电性;
其中,所述有机卤素化合物选自2-碘丙烷、1-碘丙烷、2-碘-2-甲基丙烷、2-碘丁烷、2-氟三氟甲苯、3-氟三氟甲苯、4-氟三氟甲苯、氟苯、2-氟乙醇、1-氟十二烷、1-氟己烷、1-氟庚烷和其任意混合物;
其中所述银组分在所述油墨组合物中的含量为40重量%-80重量%,
所述载体在所述油墨组合物中的含量为0.5重量%-15重量%,和
所述有机卤素化合物在所述油墨组合物中的含量为小于等于5重量%。
12.一种基材,其上配置有权利要求1所述的油墨组合物。
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JP6869227B2 (ja) | 2021-05-12 |
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EP3337861B1 (en) | 2020-12-02 |
US10836922B2 (en) | 2020-11-17 |
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