CN114981348A - 导电浆料 - Google Patents
导电浆料 Download PDFInfo
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- CN114981348A CN114981348A CN202180009017.1A CN202180009017A CN114981348A CN 114981348 A CN114981348 A CN 114981348A CN 202180009017 A CN202180009017 A CN 202180009017A CN 114981348 A CN114981348 A CN 114981348A
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Abstract
本发明涉及一种导电浆料,包括弹性的粘结剂(A)和导电的填充剂(B),其中所述导电的填充剂(B)包括以下成分:至少一种导电的球状填充剂(B1)、至少一种导电的薄片状填充剂(B2)和至少一种导电的细棍状填充剂(B3)。
Description
发明领域
本发明涉及一种导电浆料,包括弹性的粘结剂(A)和导电的填充剂(B)。本发明还涉及一种制造导电浆料的方法以及一种导电浆料施覆至弹性体基底的应用。
背景技术
用于形成导电结构的导电浆料在工程技术中众所周知并且通常包括填充有金属颗粒、金属化颗粒或碳颗粒的粘结剂。这种浆料的缺点是,其大多数情况下只有轻微的可延展性或完全不可延展。
从EP3021329A1中获悉一种导电浆料,其中导电填充剂均匀地分散在树脂中,其中该树脂为橡胶且导电填充剂为平均粒径为0.5至10μm的金属粉末。得到长宽比为10至10000的导电材料。混合物以硫化工艺来制造。优选地,金属粉末以絮体、球体、树枝晶、聚集体(聚集成三维形状的球状原始粒子)的形式存在。这种浆料的缺点是,高导电性只在高填充度下实现,因为所使用的由导电粒子组成的材料组合体需要高填充度来形成足够数目的导电路径。为了实现良好的导电性,所需的填充度非常高,以至于无法实现复合材料的高延展性(例如,100%的延展性)。
US2019/0043638 A1描述一种导电浆料,该导电浆料包含溶剂、分子内不含不饱和键的粘结剂树脂,以及分散在粘结剂树脂中的作为导电填充剂的镀银树脂粒子。镀银树脂粒子包括含有硅橡胶粒子的芯树脂粒子和覆盖芯树脂粒子表面的银涂层。添加剂的固体含量在35-75wt%之间。这种涂层的缺点是不具备良好的延展特性。此外,其重点在于硅涂层。
Toyobo公司的US 9,761,349 B2描述一种导电浆料,其中导电填充剂均匀地分散在树脂中,其中该树脂为含有硫原子的橡胶和/或含有腈基的橡胶。导电填充剂是平均粒径为0.5至10μm的金属粉末和表面具有选自巯基、氨基和腈基的基团的导电材料。这种涂层的缺点是必须使用高含量的添加剂(在实施例中在75%wt%的范围内)。最大延展率为80%。
WO 2018/134411 A1/Francisco Alberto S.A.U描述一种可延展的导电油墨,其适于在可延展、可热成型、柔性的基底和纺织品上印刷电路。该油墨是水基的,且包括导电的材料、EVA共聚物、助溶剂和分散剂。这种涂层的缺点是必须使用高含量的添加剂。此外,最大延展率为80%。
发明内容
本发明的目的是提供一种导电浆料,该导电浆料即使在低填充度下也能实现高导电性并且由此实现高延展性。
一种导电浆料实现了本发明目的,其包括弹性的粘结剂(A)和导电的填充剂(B),其中导电的填充剂(B)包括以下成分:至少一种导电的球状填充剂(B1)、至少一种导电的薄片状填充剂(B2)和至少一种导电的细棍状填充剂(B3)。
出人意料的是,本发明发现:由弹性的粘结剂(A)与导电的填充剂(B)组成的特殊组合,包括至少一种球状填充剂(B1)、至少一种薄片状填充剂(B2)和至少一种细棍状填充剂(B3),能够提供即使在低填充度下也具有高导电性和与之相关的高延展性的导电浆料。
在不确定机制的情况下,假定这一点是通过以下机制实现:薄片状填充剂(B2)可以基于其较大的表面形成导电的“岛”,从而在所有空间方向上实现高导电性。细棍状填充剂(B3)可以基于其细长的结构而在这些岛之间形成导电桥,从而在粘结剂基质中形成导电的三维网络。由此可以将导电的填充剂(B)的比例保持在较低水平,这能够实现浆料的高延展性。球状填充剂(B1)可以附着在薄片状填充剂(B2)和细棍状填充料(B3)的表面上,且可以基于其形态填补粘结剂中的空隙。这导致填充剂的接触点整体上增加,且由此导致网络内的导电路径数目增加。球状填充剂(B1)可以单独或作为团聚体附着,并且还可以占据粘结剂中的空隙。其优点在于,在变形的情况下,球状填充剂受到更少破坏。由于接触点数目众多,浆料可以在干燥后变形而不又失去导电性。因此,由三种不同类型的填充剂组成的网络由于其特殊的结构而能够适应粘结剂的变形运动而不会失去其导电性。
根据本发明,球状填充剂(B1)被理解为近似呈球状的颗粒状粒子。其还应被理解为呈不规则、非理想球状的颗粒。
在本发明一种优选实施方式中,根据ISO 21501-2:2019-11测量(液体散射光颗粒计数器),球状填充剂(B1)具有最大200μm的平均粒径,优选0.02μm至200μm,进一步优选最大100μm、例如0.02μm至100μm,进一步优选0.02μm至50μm,特别是0.02μm至10μm。
如果平均粒径过大,则需要高填充度以实现良好的导电性。此外,过大的颗粒无法渗入导电路径中的小空隙。如果平均粒径过小,则无法很好地粘结至聚合物基质中。
优选地,球状填充剂(B1)具有选自由以下物质组成的组的材料:金属,特别是过渡金属、碱土金属及其盐类、金属化玻璃、金属化陶瓷、碳以及前述物质的混合物。特别优选的是碳颗粒。特别优选地,球状填充剂(B1)具有前述材料,且优选具有特别是比例大于90wt%的碳、特别是大于95wt%的碳。
进一步优选地,基于导电浆料的总重量,球状填充剂(B1)的比例为0.1wt%至50wt%,进一步优选1wt%至15wt%,进一步优选1wt%至10wt%,进一步优选1wt%至8wt%,特别是1wt%至5wt%。
根据本发明,薄片状填充剂(B2)被理解为大体上扁平的颗粒状的填充剂。其特别是被理解为具有至少1/10,且小于1/10^6的长宽比的扁平填充剂。薄片状填充剂(B2)也可以以层状布置的形式存在。
在本发明优选的实施方式中,根据ISO 21501-2:2019-11测量(液体散射光颗粒计数器),薄片状填充剂(B2)具有最大150μm的平均粒径,例如0.02μm至150μm,进一步优选最大100μm、例如2μm至100μm,特别是5μm至80μm。在使用这种大小的粒径且特别是在粒径(B2)为5μm至80μm的情况下,涂层的延展性特别好。如果平均粒径过大,则需要高填充度以实现良好的导电性。
薄片状填充剂(B2)具有优选选自由以下物质组成的组的材料:金属,特别是过渡金属,特别是金属化玻璃、金属化陶瓷、碳以及前述物质的混合物。特别优选地,薄片状填充剂具有前述材料,且特别是具有比例优选大于75wt%的金属化玻璃、特别是大于95wt%的金属化玻璃。特别优选的是薄片状碳颗粒和/或金属化玻璃。
针对碳基薄片状填充剂(B2),特别是针对薄片状碳颗粒,根据ISO 21501-2:2019-11测量(液体散射光颗粒计数器),优选平均粒径最大为2μm,例如2μm至0.01μm,且特别是最大为0.8μm,例如0.8μm至0.02μm。
进一步优选地,基于导电浆料的总重量,薄片状填充剂(B2)的比例为0.5wt%至50wt%,进一步优选5wt%至40wt%,特别是10wt%至25wt%。
细棍状填充剂(B3)被理解为由相对于其直径而言较长的颗粒形成的填充剂。薄片状填充剂的表面可以具有空隙、隆起、凹部,或者大体上是光滑的。也可以采用分支的、枝状的、弯曲的、分叉的细棍状。
在本发明一种优选实施方式中,细棍状填充剂(B3)具有至少0.1的平均长宽比、例如1/10至1/10^8,特别是10^2至10^8。如果平均长宽比过大,则需要高填充度以实现良好的导电性。
优选地,细棍状填充剂(B3)具有选自由以下物质组成的组的材料:金属、特别是过渡金属、金属化玻璃、碳、特别是单层的碳纳米管、优选石墨烯类碳纳米管以及多层的碳纳米管以及前述物质的混合物。特别优选地,细棍状填充剂具有前述材料,且特别是具有优选比例大于90wt%的碳纳米管、特别是大于95Wt%的碳纳米管。
基于导电浆料的总重量,细棍状填充剂(B3)的比例优选为0.01wt%至10wt%,进一步优选0.01wt%至5wt%,特别是0.1wt%至3wt%。
在一种优选实施方式中,基于导电浆料的总重量,填充剂(B)的比例为0.03wt%至30wt%,进一步优选0.03wt%至25wt%,特别是0.03wt%至20wt%。进一步优选地,填充剂(B)均匀地分布在导电浆料中。填充剂的均匀分布是通过光学分析(电子显微镜)来测定的。如果1mm2面积内的团聚体比例小于填充剂比例的20%,则分布是均匀的。
根据本发明,弹性的粘结剂(A)被理解为能够在力的作用下改变其形状并且在力作用停止时大体上恢复到其原始形状的粘结剂。根据标准ISO 527(2018-06-29)测得,粘结剂(A)优选具有至少100%的延展率,例如100%至700%,进一步优选至少200%、例如200%至700%,特别是至少300%、例如300%至700%。
进一步优选地,基于导电浆料的总重量,粘结剂(A)的比例为50wt%至99wt%,进一步优选60wt%至80wt%,特别是65wt%至80wt%。
在另一优选实施方式中,弹性的粘结剂(A)包括热塑性弹性体,该弹性体优选选自由以下物质组成的组:硅酮、聚氨酯、环氧树脂、酰胺、酯或前述物质的混合物。
在另一优选实施方式中,弹性的粘结剂(A)是不导电的。在这个实施方式中,弹性的粘结剂A优选包含选自以下物质的组的粘合剂:聚氨酯、硅酮、氟硅酮、聚碳酸酯、乙烯-醋酸乙烯(EVA)、丙烯腈-丁二烯-苯乙烯(ABS)、丙烯酸酯、聚氯乙烯(PVC)、聚苯醚、聚苯乙烯、聚酰胺、尼龙、聚烯烃、聚对苯二甲酸丁二醇酯(PBT)、聚对苯二甲酸乙二醇酯(PET)、氟聚合物、橡胶,特别是NR(天然橡胶)、BR(丁二烯橡胶)、IR(异戊二烯橡胶)、SBR(丁苯橡胶)、CR(氯丁橡胶)、BIIR(异丁烯-异戊二烯橡胶)、CM(氯化橡胶)、EP(D)M(三元乙丙橡胶)、EU、NBR(丁腈橡胶)、IIR(丁基橡胶)、CIIR(氯化丁基橡胶)、CSM(氯磺化乙烯橡胶)、AU(聚氨酯橡胶)、ECO(氯醚橡胶)、HNBR(氢化丁腈橡胶)、ACM(丙烯酸酯橡胶)、FKM(氟橡胶)、VMQ(硅橡胶)、EAM=AEM(乙烯丙烯酸酯橡胶)、FFKM全氟橡胶TFE+PFVE共聚物四氟乙烯和全氟烷基乙烯基醚、FVMQ(聚三氟丙基乙烯基甲基硅氧烷)、EVA(乙烯-醋酸乙烯橡胶)、聚酯、缩醛、聚甲基丙烯酸酯、前述物质的共聚物和混合物。其中,上述粘合剂在粘结剂(A)中的比例优选大于50wt%,例如为50wt%至100wt%。
在本发明的一种优选实施方式中,根据标准EN ISO 527-1(2012年2月)测得,导电浆料具有至少30%的延展性,例如30%至400%,进一步优选至少40%、例如40%至300%,特别是至少60%、例如80%至150%。
导电浆料可以施覆到基底、特别是弹性体基底上。优选的基底是橡胶,因为其本身具有弹性特性或是可延展的。优选的橡胶种类为:NR(天然橡胶)、BR(丁二烯橡胶)、IR(异戊二烯橡胶)、SBR(丁苯橡胶)、CR(氯丁橡胶)、BIIR(异丁烯-异戊二烯橡胶)、CM(氯化橡胶)、EP(D)M(三元乙丙橡胶)、EU、NBR(丁腈橡胶)、IIR(丁基橡胶)、CIIR(氯化丁基橡胶)、CSM(氯磺化乙烯橡胶)、AU(聚氨酯橡胶)、ECO(氯醚橡胶)、HNBR(氢化丁腈橡胶)、ACM(丙烯酸酯橡胶)、FKM(氟橡胶)、VMQ(硅橡胶)、EAM=AEM(乙烯丙烯酸酯橡胶)、FFKM全氟橡胶TFE+PFVE共聚物四氟乙烯和全氟烷基乙烯基醚、和/或FVMQ(聚三氟丙基乙烯基甲基硅氧烷)。
一种优选实施方式包括导电浆料施覆至弹性体基底的应用。
根据本发明,例如导电浆料可以借助一种包括以下处理步骤的方法来制造:
A)制造或提供包含弹性的粘结剂(A)的分散体;
B)将导电的填充剂(B)引入分散体,其中导电的填充剂(B)包括以下成分:至少一种导电的球状填充剂(B1)、至少一种导电的薄片状填充剂(B2)和至少一种导电的细棍状填充剂(B3)。
其中,已在本文中述及的内容比照适用于导电浆料、弹性的粘结剂(A)、导电的填充剂(B)、导电的球状填充剂(B1)、至少一种导电的薄片状填充剂(B2)和/或导电的细棍状填充剂(B3),且特别是其优选实施方式。
步骤A)中分散体的制造优选通过将弹性的粘结剂(A)分散在水或溶剂(例如烷烃、醇、酸、醚、酯、芳烃、杂芳烃、卤化溶剂、水以及前述物质的混合物)中来实现。优选在混合设备(例如高速混合机)中进行分散。
优选地,在步骤B)中通过混合过程(例如,通过静态和动态的混合系统)将导电的填充剂(B)引入到分散体中。
本发明另一个主题是一种用于制造导电结构(例如,传感器或致动器)的浆料的应用。在这些应用中,导电且可延展的表面特别有利,因为对于这些应用而言,同样需要导电性和延展性。
具体实施方式
下面结合更多实施例对本发明进行更详细的阐述。
实施例1:制造本发明的导电浆料(配方浆料B)
将Impranil DLU分散体(固体比例为60wt%的聚氨酯分散在水中,粘结剂A)称量到适合批量大小(11g)的高速混合机罐中。
接着,加入填充剂(B)的成分,首先是分散的填充剂(CNT(填充剂B3),5.5g)和或Birla Conductex SC(填充剂B1,1.49g),然后是固体填充剂(eConduct Cu或eConduct Glass(填充剂B2),1.75g),并用木铲进行粗略混合。在高速混合机中以2300rpm的速度搅拌一分钟,然后用木铲搅拌,并再次在高速混合机中混合(1分钟,2300rpm)。施覆至弹性体(TPU薄膜)后,将浆料在60℃下干燥2小时。
得到浆料B。通过对固化的浆料(B)进行四点测量来测量电阻。结果得到值860[Ω],这对于低填充剂比例来说是非常低的。
为了制造上述的BirlaConductex SC Ultra碳分散体,在高速混合机罐中预加89wt%的水,技术性添加1%的十二烷基苯磺酸钠,并在高速混合机中以2300rpm的速度预混合15秒。
结果是得到本发明的浆料B。通过对固化的浆料(B)进行四点测量来测量电阻,结果得到值860[Ω]。
接着,一次性称量待分散的碳粉末并将其再次在高速混合机中混合。然后,在每次使用前,用铲子搅动分散体,并在高速混合机中搅动(1分钟,2300rpm)。
实施例2:本发明的多种导电浆料(A、C、D、E)和对比浆料(F、G、H)的制造
使用类似于实施例1中描述的方法来制造本发明的浆料(A、C、D、E)和非本发明的浆料(F、G、H)。所使用的比例如下表所示。
表1
上表中列出的填充剂分别分散在Impranil DLU中。其中,配方是基于100gImpranil DLU分散体中的wt%而给出。
实施例3:测定本发明的浆料和对比浆料的电阻
借助于四点测量来测定本发明的浆料和对比浆料的电阻。结果见下表。
样品名称 | 电阻[Ω]4 |
本发明的浆料A | 2300 |
本发明的浆料C | 780 |
本发明的浆料D | 740 |
本发明的浆料E3 | 570 |
非本发明的浆料F | 40000 |
非本发明的浆料G | 7500 |
非本发明的浆料H | 13000 |
表2
从上表可以得出,本发明的浆料的电阻明显小于非本发明的对比浆料。这一点尤为值得注意,因为本发明的浆料基于低填充度而具有与非本发明的浆料相当的延展性。此外,还需要注意低电阻,因为对此通常需要更多的填充剂。
除非另有说明,本文中引用的标准适用申请日的有效标准。
Claims (15)
1.一种导电浆料,包括弹性的粘结剂(A)和导电的填充剂(B),其特征在于,所述导电的填充剂(B)包括以下成分:至少一种导电的球状填充剂(B1)、至少一种导电的薄片状填充剂(B2)和至少一种导电的细棍状填充剂(B3)。
2.根据权利要求1所述的导电浆料,其特征在于,根据ISO 21501-2:2019-11测量,所述球状填充剂(B1)具有最大200μm的平均粒径,优选0.02μm至200μm,进一步优选最大100μm、例如0.02μm至100μm,进一步优选0.02μm至50μm,特别是0.02μm至10μm。
3.根据上述权利要求中任一项或多项所述的导电浆料,其特征在于,基于所述导电浆料的总重量,所述球状填充剂(B1)的比例为0.1wt%至50wt%,进一步优选1wt%至15wt%,进一步优选1wt%至10wt%,进一步优选1wt%至8wt%,特别是1wt%至5wt%。
4.根据上述权利要求中任一项或多项所述的导电浆料,其特征在于,所述薄片状填充剂(B2)的长宽比为至少1/10,且小于1/10^6。
5.根据上述权利要求中任一项或多项所述的导电浆料,其特征在于,根据ISO21501-2:2019-11,所述薄片状填充剂(B2)具有最大150μm的平均粒径、例如0.02μm至150μm,进一步优选最大100μm、例如2μm至100μm,特别是5μm至80μm。
6.根据上述权利要求中任一项或多项所述的导电浆料,其特征在于,基于所述导电浆料的总重量,所述薄片状填充剂(B2)的比例为0.5wt%至50wt%,进一步优选5wt%至40wt%,特别是10wt%至25wt%。
7.根据上述权利要求中任一项或多项所述的导电浆料,其特征在于,所述细棍状填充剂(B3)具有至少0.1的平均长宽比、例如1/10至1/10^8,特别是10^2至10^8。
8.根据上述权利要求中任一项或多项所述的导电浆料,其特征在于,基于所述导电浆料的总重量,所述细棍状填充剂(B3)的比例为0.01wt%至10wt%,进一步优选0.01wt%至5wt%,特别是0.1wt%至3wt%。
9.根据上述权利要求中任一项或多项所述的导电浆料,其特征在于,基于所述导电浆料的总重量,所述填充剂(B)的比例为0.03wt%至30wt%,进一步优选0.03wt%至25wt%,特别是0.03wt%至20wt%。
10.根据上述权利要求中任一项或多项所述的导电浆料,其特征在于,基于所述导电浆料的总重量,所述粘结剂(A)的比例为50wt%至99wt%,进一步优选60wt%至80wt%,特别是65wt%至80wt%。
11.根据上述权利要求中任一项或多项所述的导电浆料,其特征在于,所述弹性的粘结剂(A)包括热塑性弹性体,所述弹性体优选选自由以下物质组成的组:硅酮、聚氨酯、环氧树脂、酰胺、酯或前述物质的混合物。
12.根据上述权利要求中任一项或多项所述的导电浆料,其特征在于,根据EN ISO527-1(2012年2月)测得的延展性为至少30%、例如30%至400%,进一步优选至少40%、例如40%至300%,特别是60%、例如60%至150%,进一步优选80%至150%。
13.根据上述权利要求中任一项或多项所述的导电浆料,其特征在于,所述浆料施覆在弹性体基底上。
14.一种根据上述权利要求中任一项或多项所述的导电浆料施覆至弹性体基底的应用。
15.一种制造导电浆料的方法,包括以下处理步骤:
a)制造或提供包含弹性的粘结剂(A)的分散体;
b)将导电的填充剂(B)引入所述分散体,其中所述导电的填充剂(B)包括以下成分:至少一种导电的球状填充剂(B1)、至少一种导电的薄片状填充剂(B2)和至少一种导电的细棍状填充剂(B3)。
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CA3163379A1 (en) | 2021-09-10 |
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EP4114893A1 (de) | 2023-01-11 |
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