CN109076702A - 基材上无溶剂印刷电路的方法 - Google Patents

基材上无溶剂印刷电路的方法 Download PDF

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CN109076702A
CN109076702A CN201780019139.2A CN201780019139A CN109076702A CN 109076702 A CN109076702 A CN 109076702A CN 201780019139 A CN201780019139 A CN 201780019139A CN 109076702 A CN109076702 A CN 109076702A
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杨军
张腾元
郭秋泉
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Abstract

本发明公开了一种无溶剂制造电路的方法。首先采用激光印刷技术将含金属前体和还原剂前体的厚达13微米的厚图案层沉积到基材上；然后用新开发的高能强脉冲光(intense pulsed light，IPL)系统照射沉积的图案化前体材料，以将沉积的材料转变为导电的厚金属层电路。印刷图案易于金属化使本发明成为大规模生产柔性印刷电路的高效制造方法。

Description

基材上无溶剂印刷电路的方法
技术领域
本发明涉及印刷电子领域，尤其涉及一种在基材上制造厚导电层电路的无溶剂方法。
背景技术
具有改进电子工业和改变我们日常生活潜力的印刷电子、柔性电子和可穿戴电子构成了一个迅速增长的研究领域。喷墨印刷、凹版印刷、丝网印刷、气溶胶喷射印刷和激光诱导正向转移印刷等各种印刷技术已被用于制造各种应用的电气和电子器件。高效率、可扩展的印刷技术一直吸引着印刷电子界。近年来，印刷电子产品的研发得到了长足的发展。大多数现有印刷电子技术是基于涉及一种或多种溶剂的溶液方案。金属纳米颗粒、碳纳米管、导电/功能聚合物或离子凝胶等可溶性的导电和/或特殊功能材料通常会被配制成不同的印刷油墨。在金属纳米颗粒制作成导电油墨应用在印刷电子领域的深入探索中，银纳米颗粒扮演着重要的角色。然而，为了防止纳米颗粒聚集、沉降和氧化，由金属纳米颗粒组成的导电油墨中大量的稳定剂、封端剂和/或改性剂的使用会降低固体负载、提高杂质含量，结果导致印刷电路的高电阻。虽然选择性激光烧结、脉冲光烧结、等离子体和微波闪速烧结等许多有效的烧结方法用来制作印刷电路并获得高达60％的块材导电性，但由于导电层较薄(小于1μm)，这些印刷电路的电阻仍然很高，使得印刷电子仍难以满足电子工业的要求。此外，高质量油墨的制备通常较复杂和昂贵；在油墨配方方面，印刷工艺对粘度和表面张力有严苛要求。印刷质量容易受到针孔构造等内在限制的影响，并且油墨与基底的粘附也是所有湿加工技术的共同挑战。
近年来，喷墨印刷、纳米压印和丝网印刷等印刷技术已逐渐成为生产柔性可伸缩的电子/器件非常有前景的技术趋势。特别是增材制造工艺的材料或喷墨印刷具有高效率、低材料消耗和可编程控制的优点，通过直接书写方式制造柔性和可伸缩的电子器件已被证明是非常通用且具有成本效益。然而，印刷电路的低导电性、印刷材料与基底之间的弱粘附、低分辨率、基底材料的选择限制性和导电油墨使用Ag或Au纳米粒子的高成本等方面仍存在挑战。特别是低电导率和弱粘附性问题，直接影响到制造过程中的质量控制，以及器件在使用过程中的性能和寿命。如果能够提高印刷分辨率，则成本和材料消耗将降低，吞吐量将进一步增加，更多的应用将变得可用。
发明内容
光固化是使用闪光灯(通常是氙灯)产生的高能光脉冲对材料进行能量密集处理的过程。光固化允许不耐高温基材在比用烤箱(需要长达数小时)更短的时间周期(约1毫秒)内被处理，而不会对热敏基材造成损坏。强脉冲光能使热塑性不透明或其它不透明聚合物材料在气相中分解成醇和酸，并能提供在醇和酸环境中还原金属前体的能量。
激光印刷是一种无溶剂、高速、静电式的数字印刷工艺，它通过将激光束传递到带电鼓上快速地产生高质量的图案，以便定义差分带电图像，并且已经广泛应用于我们的日常生活中。虽然激光印刷广泛应用于图形印刷中，除了激光诱导正向转移印刷、控制碳纳米管生长的激光印刷图案和制备微流体器件等少数案例外，利用激光印刷进行器件制造的报道仍然很少。因为不需要溶剂从而不必考虑金属和调色剂粉末的溶解性，激光印刷有很大优势。与喷墨印刷不同，激光印刷采用干墨粉，因此不受粘度和表面张力的限制。自激光打印机问世以来，它们变得更加实惠，使它们成为印刷电子和个人使用的可行选择。激光诱导正向转移(Laser-induced forward transfer，LIFT)是一种在无相变情况下将激光推进到基底的技术，能在不降低性能的情况下沉积复合材料。利用LIFT技术，可以高精度地传输具有平滑均匀轮廓的银图案，同时可以获得具有高再现性的均匀圆形液滴。醇和酸还原机理被广泛应用于通过还原金属氧化物来合成金属。下列反应式(1-6)显示了这些反应的机理和热动力学。
Cu2O+CH3OH(g)→2Cu+H2O(g)+HCHO(g)
G(310℃)＝-69kJ (1)
Cu2O+C2H5OH(g)→2Cu+H2O(g)+CH3CHO(g)
G(310℃)＝-87kJ (2)
Cu2O+C3H7OH(g)→2Cu+H2O(g)+(CH3)2CO(g)
G(310℃)＝-102kJ (3)
Cu2O+C3H7CHO(g)→2Cu+C3H7COOH(g)
G(310℃)＝-86kJ (4)
Cu2O+1/4CH3COOH(g)→2Cu+1/2H2O(g)+1/2CO2(g)
G(310℃)＝-99kJ (5)
Cu2O+HCOOH(g)→2Cu+H2O(g)+CO2(g)
G(310℃)＝-161kJ (6)
根据本发明优选实施例合成的金属前体和还原剂前体材料是可激光印刷的。图案最初沉积在基材上，使得基材可以是柔性的、刚性的、有机的或无机的。然后用新开发的高能强光脉冲照射图案化的前体材料，以将前体材料转变为具有导电性的厚纯金属层电路。本发明的所有特征和优点将在以下详述的实施说明中得以体现。
具体实施方式
本发明涉及一种新型墨粉的制备、印刷电路的印刷和后处理方法。还原剂/金属前体被结合到常规墨粉中以形成新的墨粉，使得印刷图案能够进一步功能化。几种典型的热塑性聚合物和富含醇基和酸基的其他聚合物被选择作为还原剂前驱体。金属前体可以是但不限于金属络合物、金属盐、金属氧化物、金属晶体、金属氢氧化物。金属元素可以是银、金、铜、镍、铂、铟、锡、镓和任何其它可能的导电元素。这些还原剂前体具有的共同特征是可以在高功率脉冲光下分解为醇和酸。
在本公开发明中，上述还原剂前体与金属前体和常规墨粉混合。常规墨粉可以通过乳液聚合法合成或直接从市场上购买。还原剂和/或金属前体也可从商业市场获得或通过化学方法合成。在制备墨粉和还原剂/金属前体之后，在本公开发明中有两种方法来混合它们，液相混合和固态混合。在液相混合中，催化剂首先溶解在溶剂如去离子水中，墨粉在表面活性剂辅助下分散在同一溶剂中。然后将还原剂前体溶液或金属盐溶液在搅拌下缓慢滴入墨粉分散体中，以达到良好的混合效果。然而由于溶剂的影响，液相混合可能会改变墨粉颗粒的初始性能。当然，固态混合是制备新型墨粉的良好选择。固态混合主要涉及球磨、机械研磨、鼓风混合、搅拌等。
在本公开发明中，还原剂前体或金属前体首先被粉碎成粒径小于10微米的细粉。然后将制备好的粉末与墨粉颗粒混合。通常在此过程中，行星球磨用于粉碎还原剂/金属前体颗粒以及前体材料与墨粉颗粒的混合。行星球磨机的旋转通常需要保持低速以防止温度急剧升高。过高的温度会使墨粉熔化在一起，影响后续的印刷质量。
在本公开发明中，使用激光印刷将所制备的前体功能墨粉沉积到基材上。含有墨粉的还原剂/金属前体的印刷质量与混合物的均匀性和前体材料的负载量有关。催化剂的均匀混合有利于提高印刷质量。印刷质量也受印刷基材性能的影响。高表面能有助于其他物质在表面上的粘附。表面能与表面积和表面张力有关。显然，较大的粗糙度和高的表面张力有利于提高粘合稳定性。因此，印刷基材需要具有较大的粗糙度和表面张力。一些以提高表面粗糙度和表面张力的表面改性有助于提高印刷质量。对于激光印刷，墨粉颗粒通常被熔化到基材中。墨粉与基材间的相互作用是非共价力，因此增加氢键数目是提高粘附力的有效方法。将羟基、羧基和羰基引入基材中将有助于提高表面粘附性。
在本公开发明中，印刷的还原剂/金属前体图案被高功率强脉冲光照射以将前体材料转变为纯导电金属电路。在光脉冲照射期间，还原剂前体在气相中分解成醇和酸，形成部分还原环境。同时，脉冲光提供金属前体的醇/酸还原所需的能量，产生纯金属、水(气体)和二氧化碳。印刷电路在反应后展现良好的导电性。为了实现前体材料的均匀金属化，采用与移动基底同步的快速高功率脉冲序列。
1 Ming‐Shin Yeh,Yuh‐Sheng Yang,Yi‐Pei Lee,Hsiu‐Fang Lee,Ya‐Huey Yeh,and Chen‐Sheng Yeh,The Journal of Physical Chemistry B 103(33),6851(1999).
2 Jaehoon Lee,Dong‐Kuk Kim,and Weekyung Kang,Bulletin of the KoreanChemical Society 27(11),1869(2006).
3 Harveth Gil,Alejandro Echavarria,and Felix Echeverría,Electrochimica Acta 54(20),4676(2009).
4 PJ Soininen,K‐E Elers,V Saanila,S Kaipio,T Sajavaara,and S Haukka,Journal of The Electrochemical Society 152(2),G122(2005).

Claims (10)

1.一种用于在基材上无溶剂制造印刷电子器件的方法，所述方法包括：
I、合成含有可激光印刷墨粉的还原剂前体和金属前体；
II、将含有墨粉的前体沉积到基材上得到沉积前体图案；
III、用高能强脉冲光照射上述的沉积前体图案，将所述沉积前体图案转变为导电图案。
2.根据权利要求1所述的方法，其中所述沉积通过激光印刷来实现。
3.根据权利要求1所述的方法，其中所述基材是纸张、聚对苯二甲酸乙二醇酯、聚酰亚胺、聚醚酰亚胺或FR-4环氧玻璃布层压板。
4.根据权利要求1所述的方法，其中所述金属前体材料包含颗粒金属。
5.根据权利要求4所述的方法，其中所述金属前体可以是金属氧化物、金属络合物、金属盐、金属聚合物化合物、具有封端剂的金属纳米颗粒。
6.根据权利要求4所述的方法，其中所述颗粒金属是选自铜、镍、银、钴金、铂、钯中的一种及其一种以上的组合金属。
7.根据权利要求1所述的方法，其中所述还原剂前体包括可在高能脉冲光下分解为醇和酸的颗粒聚合物。
8.根据权利要求7所述的方法，其中所述颗粒聚合物选自聚酯、苯乙烯丁二烯共聚物、苯乙烯丙烯酸酯共聚物、聚乙烯吡咯烷酮、聚乙烯醇中的一种及其一种以上的组合。
9.根据权利要求1所述的方法，其中所述还原剂前体浓度范围为0.1wt％～90wt％。
10.根据权利要求1所述的方法，其中所述金属前体浓度范围为10wt％～90wt％。
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