CN115442975B - 一种纳米银基柔性电子电路的制备方法 - Google Patents
一种纳米银基柔性电子电路的制备方法 Download PDFInfo
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Abstract
本发明公开了一种纳米银基柔性电子电路的制备方法,属于柔性印刷电子电路领域,其特征在于,包括以下步骤:(1)制备纳米银颗粒;(2)制备纳米银基柔性电子电路:将制备的纳米银颗粒分散在醇共溶剂中,超声震荡得到纳米银溶胶;将纳米银溶胶与胶粘剂乳液均匀混合,并在室温缓慢搅拌得到导电胶,将导电胶利用丝网印刷将印花图案均匀印在柔性衬底的表面,然后将印刷图案固化即得纳米银基柔性电子电路;本发明采用一步法完成溶剂蒸发和成型工艺,解决了金属柔性基材往往需要二次高温热处理的痛点,降低了成本和能耗有望实现低成本大规模生产;其次,通过对制备工艺的优化,获得具有良好导电性的纳米银基柔性电子电路。
Description
技术领域
本发明属于柔性印刷电子电路领域,具体地,涉及一种采用低温一步法成型纳米银基柔性电子电路的制备方法。
背景技术
随着微电子技术的不断发展,具有多功能集成特性的小型电子设备层出不穷,并应用于社会生活的各个方面(如人体生理信号监测、人机交互***、智能软体机器人技术等)。然而,目前流行的大多数可穿戴电子产品都是刚性的,主要依靠在晶片上制作微集成电路来实现各种电子功能,如智能手表、智能眼镜、运动监控腕带或手镯,但很难与不同几何形状或拓扑的表面贴合,这不符合真正的人性化设计理念。而克服目前刚性集成电路的关键即是发展柔性电子电路。
现有的柔性电子电路方案的分为两种:一种是代替传统的PCB基底,将铜箔线路利用激光焊接于柔性的聚亚酰胺基底上形成柔性PCB板。但这样的工艺造价十分昂贵,所用的基底有严格的耐高温限制造成基底单一。另一种方法是受印刷启发,制备纳米导电浆料或墨水,通过印刷的方式形成图案化的柔性电子电路。但制备导电浆料或墨水时,为了维持纳米金属在浆料/墨水中的稳定性,通常会使用稳定剂来防止纳米金属组分的团聚,从而提高导电浆料/墨水的稳定性。然而,稳定剂是电绝缘体,引入稳定剂的同时也将会影响导电墨水的导电性能。因此,针对提高印制电子电路的导电性能,常需要高温处理,但长时间的高温加热(>250℃)将会对柔性衬底带来毁灭性的损害,同时还有可能对热敏电子元件造成损害。
近年来,有报道发现通过化学试剂可以引发金属纳米颗粒在室温/低温自聚结从而实现纳米金属的烧结过程,研究表明,当纳米金属被阴离子聚合物包覆,在体系中加入含氯体系的溶液处理可以诱发吸附在纳米金属表面的稳定剂剥离达到形成烧结体的目的,但目前使用低温烧结的方法依然是两步法,造成后处理麻烦,工序复杂。
发明内容
本发明目的在于提供一种采用低温一步法制备纳米银基柔性电子电路的方法,以改善高温烧结对基底和元器件损伤的难题以及两步法低温烧结工序和后处理繁琐的问题。
为达到上述目的,本发明所采取的技术方案为:
一种纳米银基柔性电子电路的制备方法,其特征在于,包括以下步骤:
(1)制备纳米银颗粒:
将硝酸银溶解在去离子水中配置成10-20wt.%的前驱液,标记为溶液A;
将稳定剂溶解在去离子水中得到的溶液作为稳定液,紧接着将还原剂溶解在去离子水中作为还原液,将稳定液与还原液均匀混合,标记为溶液B,溶液B中,稳定剂浓度为10-40wt.%;
在15-60℃磁力搅拌下,将溶液B滴入到溶液A中并持续反应0.5-24h,然后将反应液离心,沉淀用NaNO3溶液洗涤,最后将沉淀在20-60℃下真空干燥12-48h,得到纳米银颗粒;
(2)制备纳米银基柔性电子电路:
将步骤(1)制备的纳米银颗粒分散在醇共溶剂中,并超声震荡30-60min后得到0.1-1gml-1的纳米银溶胶备用;
向反应容器中加入双羟乙基丙酸、聚四氢呋喃2000,将反应容器加热至100-150℃保温1-2h,然后将温度下降至60-80℃,向反应容器中加入异佛尔酮二异氰酸酯,反应1-3小时,然后加入双羟基功能氯盐进行扩链,反应4-6h后,加入三乙胺中和,将温度下降至25~50℃,向体系中缓慢加入去离子水,高速搅拌致使体系充分乳化得到胶粘剂乳液备用;上述反应中,双羟基丙酸:聚四氢呋喃2000:双羟基功能氯盐的摩尔比为1:1:0.5,NCO:OH的摩尔比为1~2.8:1;
将纳米银溶胶与胶粘剂乳液均匀混合,并在室温缓慢搅拌15-30min得到导电浆料,将导电浆料利用丝网印刷将印花图案均匀印在柔性衬底的表面,然后将印刷图案在25-80℃固化12-24h,即得纳米银基柔性电子电路。
进一步的设置在于:
步骤(1)中,所述稳定剂为二水合柠檬酸三钠或聚乙烯吡咯烷酮中的任意一种。
步骤(1)中,所述还原剂为七水合硫酸亚铁。
步骤(1)中,稳定剂与还原剂的质量比为0~20比1,优选为5:1。
步骤(1)中,溶液A前驱液浓度为10wt.%,溶液B中,稳定剂浓度为30wt.%;溶液A与溶液B混合的体积比优选为1:1。
步骤(2)中,所述醇共溶剂为去离子水:乙醇:丙三醇:乙二醇按照体积比18-24:8-12:20-50:10-40配置而成。
步骤(2)中,所述双羟基功能氯盐为双1-(2-羟乙基)-3-乙基咪唑氯盐、双1-(2-羟乙基)-3-丁基咪唑氯盐中的任意一种。
步骤(2)中,在扩链反应前,加入稀释剂调节黏度,所述稀释剂为丙酮、乙腈、N,N-二甲基甲酰胺、二甲基亚砜中的任意一种。
步骤(2)中,所述纳米银溶胶与胶粘剂乳液按照质量比1:1均匀混合,所述固化温度为60℃,固化时间24h。
所述柔性衬底无特别限制,可选自聚酯纤维、硅胶、橡胶、天然棉织物、尼龙织物、聚氨酯弹性体中的任意一种。
本发明的有益效果如下:
(1)本发明的一种纳米银基柔性电子电路的制备方法,通过优化纳米银颗粒的制备工艺,进一步制备的纳米银基导电浆料,可实现低温一步法完成溶剂蒸发和电子电路成型,同时,可以有效提高纳米银基柔性电子电路的导电率。
(2)本发明的一种纳米银基柔性电子电路的制备方法,以双羟基功能氯盐为硬段扩链剂,利用-OH将咪唑氯盐结构锚定于聚氨酯胶粘剂的分子骨架中,借助Cl-诱发包覆于纳米银的稳定剂剥离而引发纳米银颗粒聚集行为,实现了一步法完成溶剂蒸发和成型工艺,解决了金属柔性基材往往需要二次高温热处理的痛点,降低了成本和能耗有望实现低成本大规模生产;其次,借助咪唑离子液体的离子可置换性,可以将低温成型后的功能咪唑离子液体胶粘剂中的Cl-更替成其他功能离子,实现对胶粘剂二次功能的定制化开发,获得可靠性良好的纳米银基柔性电子电路。
以下结合附图和具体实施方式对本发明做进一步说明。
附图说明
图1为实施例1制备的纳米银颗粒的XRD;
图2为实施例1制备的纳米银颗粒的红外光谱;
图3为不同稳定剂含量制备的纳米银颗粒的SEM图;
图4为不同稳定剂含量制备的纳米银颗粒的粒径分析图;
图5为不同稳定剂含量制备的纳米银颗粒的稳定性对照图。
图5中:从左至右稳定剂含量依次为0wt.%、10wt.%、20wt.%、30wt.%、40wt.%。
具体实施方式
实施例1
(1)制备纳米银颗粒
配置溶液A:将硝酸银完全溶解在去离子水中配置成10wt.%前驱液(记为溶液A)。
配置溶液B:按稳定剂与还原剂质量比5:1的比例,分别配置稳定液和还原液。首先,将稳定剂二水合柠檬酸三钠溶解在去离子水中作为稳定液,紧接着将还原剂七水合硫酸亚铁溶解在去离子水中作为还原液,然后将稳定液和还原液均匀混合,记为溶液B,溶液B中,二水合柠檬酸三钠的浓度为30wt.%。
在25℃磁力搅拌下,按照溶液A与溶液B体积比为1:1,用恒压滴液漏斗将溶液B滴入到A溶液中并持续反应1h,将反应液经6000rpm离心15min,将沉淀用1M的NaNO3溶液洗涤三次,最后将沉淀在30℃下真空干燥48h,即可得到提纯后的纳米银颗粒。
制备的纳米银颗粒,其XRD和红外光谱如图1~图2所示。
(2)制备纳米银基柔性电子电路:
将上述制备的纳米银颗粒分散在醇共溶剂(去离子水:乙醇:丙三醇:乙二醇=20:10:30:20,V/V)中,并超声震荡60min后得到0.3g ml-1的纳米银溶胶备用。
向反应容器中加入双羟乙基丙酸、聚四氢呋喃2000,将反应容器加热至120℃保温1h除去醇中的水分,将温度下降至80℃,将反应容器中再加入异佛尔酮二异氰酸酯和一滴二月桂酸二丁基锡,反应2h后,加入丙酮调节黏度,然后加入双1-(2-羟乙基)-3-乙基咪唑氯盐进行扩链,反应继续持续4h后,加入三乙胺中和,将温度下降至25℃,向体系中缓慢加入大量的去离子水,高速搅拌致使体系充分乳化得到胶粘剂乳液待用;上述反应中,双羟基丙酸:四氢呋喃2000:双1-(2-羟乙基)-3-乙基咪唑氯盐的摩尔比为1:1:0.5,NCO:OH的摩尔比为1.25:1。
将前述制备的纳米银溶胶和胶粘剂乳液按质量比1:1均匀混合,并在室温缓慢搅拌30min得到纳米银基导电浆料,将导电浆料利用丝网印刷技术将印刷图案均匀印在柔性衬底表面,然后将印刷图案在60℃固化24h即可获得纳米银基柔性电子电路。
替换例1
根据实施例1的制备方法,区别在于:改变溶剂B中的稳定剂含量,并检测不同稳定剂含量对制备的纳米银颗粒的粒径、稳定性及导电性的影响。
表1、
序号 | 稳定剂(wt.%) | 粒径 | 稳定性 | 导电性 |
实施例1-1 | 0 | 5000nm | 极差 | 120×10-5Ω·m |
实施例1-2 | 10 | 1000nm | 差 | 76×10-5Ω·m |
实施例1-3 | 20 | 200nm | 较差 | 21×10-5Ω·m |
实施例1-4 | 30 | 30nm | 较好 | 2.3×10-5Ω·m |
实施例1-5 | 40 | 10nm | 好 | 1.3×10-5Ω·m |
表中:稳定剂(wt.%)为稳定剂在溶液B中的质量浓度。
结合表1、图3~图5所示:
(1)、当不添加稳定剂时,所制备的纳米银颗粒发生剧烈的团聚现象,导致稳定性极差,随着稳定剂含量的升高,纳米银颗粒的粒径得以改善,其稳定性也随着优化。
(2)、当不添加稳定剂时,所制备的纳米银颗粒发生剧烈的团聚现象,导致稳定性极差,制备的纳米银基柔性电子电路的导电率亦较差,随着稳定剂含量的升高,纳米银颗粒的粒径和稳定性得以改善,制备的纳米银基柔性电子电路的导电率有明显提升。
替换例2
根据实施例1的制备方法,区别在于:调整印刷图案的固化温度,并测试其对纳米银基柔性电子电路的导电性影响,如表2所示:
表2、
序号 | 固化温度 | 导电性 |
实施例2-1 | 25 | 62×10-5Ω·m |
实施例2-2 | 40 | 16×10-5Ω·m |
实施例2-3 | 60 | 2.3×10-5Ω·m |
实施例2-4 | 80 | 1.2×10-5Ω·m |
。
分析:
如表2所示,当固化温度为较低,仅为室温时,电导率较低,温度升高,有利于纳米银印刷电路导电性的提升。
对比例
将本发明实施例1的制备工艺,与现有技术进行对照,如表3所示。
表3、本发明与现有技术的应用效果对照
序号 | 成型方式 | 成型步骤 |
本发明实施例1 | 低温(60℃) | 一步 |
现有技术1(CN111117367A) | 紫外光(昂贵) | 两步 |
现有技术2(CN113689972A) | 高温(120℃) | 两步 |
现有技术3(CN107513310A) | 高温(150℃) | 两步 |
现有技术4(CN107135602A) | 高温(100℃) | 两步 |
。
分析:
如表3所示:与现有技术相比,本发明实现了低温一步法完成溶剂蒸发和电子电路成型,解决金属柔性基材需要二次高温热处理的痛点,同时降低成本和能耗。
Claims (10)
1.一种纳米银基柔性电子电路的制备方法,其特征在于,包括以下步骤:
(1) 制备纳米银颗粒:
将硝酸银溶解在去离子水中配置成10-20 wt.%的前驱液,标记为溶液A;
将稳定剂溶解在去离子水中得到的溶液作为稳定液,紧接着将还原剂溶解在去离子水中作为还原液,将稳定液与还原液均匀混合,标记为溶液B,溶液B中,稳定剂浓度为10-40wt.%;
在15-60℃磁力搅拌下,将溶液B滴入到溶液A中并持续反应0.5-24 h,然后将反应液离心,沉淀用NaNO3溶液洗涤,最后将沉淀在20-60℃下真空干燥12-48 h,得到纳米银颗粒;
(2) 制备纳米银基柔性电子电路:
将步骤(1)制备的纳米银颗粒分散在醇共溶剂中,并超声震荡30-60 min后得到0.1-1g ml-1的纳米银溶胶备用;
向反应容器中加入双羟乙基丙酸、聚四氢呋喃2000,将反应容器加热至100-150℃保温1-2 h,然后将温度下降至60-80℃,向反应容器中加入异佛尔酮二异氰酸酯,反应1-3小时,然后加入双羟基功能氯盐进行扩链,反应4-6h后,加入三乙胺中和,将温度下降至25~50℃,向体系中缓慢加入去离子水,高速搅拌致使体系充分乳化得到胶粘剂乳液备用;上述反应中,双羟基丙酸:聚四氢呋喃2000:双羟基功能氯盐的摩尔比为1:1:0.5, NCO:OH的摩尔比为1~2.8:1;
将纳米银溶胶与胶粘剂乳液均匀混合,并在室温缓慢搅拌15-30min得到导电浆料,将导电浆料利用丝网印刷将印花图案均匀印在柔性衬底的表面,然后将印刷图案在25-80℃固化12-24 h,即得纳米银基柔性电子电路。
2.根据权利要求1所述的一种纳米银基柔性电子电路的制备方法,其特征在于:步骤(1)中,所述稳定剂为二水合柠檬酸三钠或聚乙烯吡咯烷酮中的任意一种。
3.根据权利要求1所述的一种纳米银基柔性电子电路的制备方法,其特征在于:步骤(1)中,所述还原剂为七水合硫酸亚铁。
4.根据权利要求1所述的一种纳米银基柔性电子电路的制备方法,其特征在于:步骤(1)中,稳定剂与还原剂的质量比为0~20比1。
5.根据权利要求4所述的一种纳米银基柔性电子电路的制备方法,其特征在于:步骤(1)中,稳定剂与还原剂的质量比为5:1。
6.根据权利要求4所述的一种纳米银基柔性电子电路的制备方法,其特征在于:步骤(1)中,溶液A前驱液浓度为10 wt.%,溶液B中稳定剂浓度为30 wt.%;溶液A与溶液B混合的体积比为1:1。
7.根据权利要求1所述的一种纳米银基柔性电子电路的制备方法,其特征在于:步骤(2)中,所述双羟基功能氯盐为双1-(2-羟乙基)-3-乙基咪唑氯盐、双1-(2-羟乙基)-3-丁基咪唑氯盐中的任意一种。
8.根据权利要求1所述的一种纳米银基柔性电子电路的制备方法,其特征在于:步骤(2)中,扩链反应前,加入稀释剂调节黏度,所述稀释剂为丙酮、乙腈、N,N-二甲基甲酰胺、二甲基亚砜中的任意一种。
9.根据权利要求1所述的一种纳米银基柔性电子电路的制备方法,其特征在于:步骤(2)中,所述纳米银溶胶与胶粘剂乳液按照质量比1:1均匀混合,所述固化温度为60℃,固化时间24 h。
10.根据权利要求1所述的一种纳米银基柔性电子电路的制备方法,其特征在于:步骤(2)中,所述柔性衬底为聚酯纤维、硅胶、橡胶、天然棉织物、尼龙织物、聚氨酯弹性体中的任意一种。
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