CN105670392A - 一种导电油墨及制备方法 - Google Patents
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Abstract
本发明公开一种导电油墨及制备方法。其中,该导电油墨包括以质量份数表示的如下组分:主溶剂50-70份,改性聚氨酯树脂10-20份,氨基树脂5-10份,封闭型异氰酸酯1-3份,水性蜡0.2-0.5份,消泡剂0.02-0.05份,慢干剂0.02-0.05份,纳米NaV6O15粉末20-40份,导电助剂0.2-0.5份。本发明制备的导电油墨的伏安特性符合欧姆定律,具有很好的耐温性及耐湿性,稳定可靠,符合高温高湿度环境下导电油墨的使用需要。
Description
技术领域
本发明涉及油墨领域,尤其是涉及一种导电油墨及制备方法。
背景技术
近年来,将导电油墨涂覆在柔性的聚合物薄膜表面的成型技术已在电暖器、无线射频识别、印制线路板、电子屏显示器、传感器、太阳能电池及薄膜开关等领域得到了广泛的应用。
导电油墨作为一种新型的特种功能高分子材料,主要由基体树脂和导电填料组成。所用的导电填料多为金属或无机填料,如金、银、锗、石墨、氧化锡等,其中,金属银以良好的导电性、稳定性而应用最多。导电油墨中粘接料树脂通常选用环氧树脂、酚醛树脂、聚氨酯和丙烯酸树脂等。尤其是水性丙烯酸酯类因其热稳定性、抗氧化性良好、黏度低和粘接性能好等优点,已成为导电油墨中得以广泛采用且性能良好的粘接剂。
现有的导电油墨品类已经较多,且大多具有不错的性能,正满足印刷电路制造工艺及电取暖等飞速发展领域的需求。但导电油墨在质量上的要求越来越精细化、科学化,甚至需要满足特点使用环境下的使用需要,比如高温高湿度环境下,需要导电油墨不会在高温高湿度(比如蒸汽作用下)下发生附着力下降等不良反应。
发明内容
本发明提出一种适合在高温高湿度环境下使用的导电油墨及制备方法,其附着力强,性能稳定可靠。
一种导电油墨,包括以质量份数表示的如下组分:主溶剂50-70份,改性聚氨酯树脂10-20份,氨基树脂5-10份,封闭型异氰酸酯1-3份,水性蜡0.2-0.5份,消泡剂0.02-0.05份,慢干剂0.02-0.05份,纳米NaV6O15粉末20-40份,导电助剂0.2-0.5份,其中,纳米NaV6O15粉末的晶体为颗粒均匀且尺寸长度为1.~1.5um的纳米棒状结构。
其中,包括以质量份数表示的如下组分:主溶剂60份、改性聚氨酯树脂15份、氨基树脂6份、封闭型异氰酸酯2份、水性蜡0.3份、消泡剂0.04份、导电助剂0.4份、慢干剂0.04份和纳米NaV6O15粉末35份。
其中,主溶剂为乙酸甲酯、乙酸乙酯、乙酸丙酯或乙酸丁酯中的至少一种。
其中,导电助剂为盐酸二甲基胺、盐酸二丁基胺、四甲基碘化铵、醋酸四甲基铵或季铵盐类中的至少一种。
其中,性改性聚氨酯树脂为大分子二元醇改性聚氨酯、烷基异氰酸酯改性聚氨酯或芳香族异氰酸酯改性聚氨酯中的至少一种。
其中,氨基树脂为甲醚化三聚氰胺甲醛树脂、丁醚化三聚氰胺甲醛树脂、混合醚化三聚氰胺甲醛树脂、甲醚化脲醛树脂、丁醚化脲醛树脂、甲醚化苯代三聚氰胺树脂或丁醚化苯代三聚氰胺树脂中的至少一种。
其中,消泡剂为聚丙烯酸酯类聚合物或磷酸酯改性的聚丙烯酸酯类聚合物的一种或几种。
其中,慢干剂为乙醇胺。
所述导电油墨的制备方法包括:(1)取主溶剂50-70份、改性聚氨酯树脂10-20份、氨基树脂5-10份、封闭型异氰酸酯1-3份、水性蜡0.2-0.5份、消泡剂0.02-0.05份和导电助剂0.2-0.5份,加入搅拌釜中混合均匀,得到水性油墨;(2)在上述水性油墨中再加入慢干剂0.02-0.05份和纳米NaV6O15粉末20-40份,研磨20-60分钟使纳米NaV6O15粉末充分分散在水性油墨中,制备得到导电油墨。
与现有技术相比,本发明具有如下有益效果:
本发明制备的导电油墨的伏安特性符合欧姆定律,具有很好的耐温性及耐湿性,稳定可靠,符合高温高湿度环境下导电油墨的使用需要。
具体实施方式
一种导电油墨,包括以质量份数表示的如下组分:主溶剂50-70份,改性聚氨酯树脂10-20份,氨基树脂5-10份,封闭型异氰酸酯1-3份,水性蜡0.2-0.5份,消泡剂0.02-0.05份,慢干剂0.02-0.05份,纳米NaV6O15粉末20-40份,导电助剂0.2-0.5份。当然导电油墨还可以包括适量的着色剂、助溶剂等。
主溶剂为乙酸甲酯、乙酸乙酯、乙酸丙酯或乙酸丁酯中的至少一种。
助溶剂为乙酸异丙酯、乙二醇***醋酸酯、乙二醇丁醚醋酸酯或丙二醇甲醚醋酸酯类中的至少一种。
性改性聚氨酯树脂的相对分子量为10000-20000,固含量为30-70%,粘度为200-1800cP。性改性聚氨酯树脂为大分子二元醇改性聚氨酯、烷基异氰酸酯改性聚氨酯或芳香族异氰酸酯改性聚氨酯中的至少一种。
氨基树脂为甲醚化三聚氰胺甲醛树脂、丁醚化三聚氰胺甲醛树脂、混合醚化三聚氰胺甲醛树脂、甲醚化脲醛树脂、丁醚化脲醛树脂、甲醚化苯代三聚氰胺树脂或丁醚化苯代三聚氰胺树脂中的至少一种。
消泡剂为聚丙烯酸酯类聚合物或磷酸酯改性的聚丙烯酸酯类聚合物的一种或几种。消泡剂能让导电油墨在印刷后的干燥成膜过程中形成一个平整、光滑、均匀的涂膜,能有效降低油墨表面张力,提高其流平性和均匀性。
导电助剂为盐酸二甲基胺、盐酸二丁基胺、四甲基碘化铵、醋酸四甲基铵或季铵盐类中的至少一种。
助溶剂为乙酸异丙酯、乙二醇***醋酸酯、乙二醇丁醚醋酸酯或丙二醇甲醚醋酸酯类中的至少一种。
纳米NaV6O15粉末的晶体结构为尺寸均匀(尺寸的长度均约1.~1.5um)且纳米棒状结构,由质量比NH4VO3:NaCl:表面活性剂:去离子水=1:(1.5~2.5):(0.1~0.3):100的NH4VO3、NaCl、表面活性剂和去离子水在强酸性的水热条件下制备而成。比如,质量比NH4VO3:NaCl:表面活性剂:去离子水=1:2.5:0.3:100取NH4VO3、NaCl和去离子水,将NH4VO3、NaCl和表面活性剂溶于去离子水中,在60℃下不断搅拌至完全溶解,加入适量的强酸溶液(比如盐酸、硫酸等)调节混合容易的pH值至为1。将所得混合溶液倒入聚四氟乙烯衬里不锈钢高压釜,300℃条件下水热反应12小时,然后自然冷却至室温,将反应得产物进行真空抽滤,用去离子水和乙醇各洗涤两遍,真空干燥后,再放入高温炉中600℃煅烧6小时,制备得到为棕色粉末的NaV6O15。当纳米NaV6O15粉末的晶体为颗粒均匀且尺寸长度为1.~1.5um的纳米棒状结构时,具有最佳的导电性能。
慢干剂比如为乙醇胺。
实施例1
取主溶剂50份、烷基异氰酸酯改性聚氨酯20份、甲醚化三聚氰胺甲醛树脂5份、封闭型异氰酸酯1份、水性蜡0.2份、消泡剂0.02份、盐酸二甲基胺0.2份加入搅拌釜中混合均匀,得到水性油墨。在上述水性油墨中再加入乙醇胺0.02份和纳米NaV6O15粉末20份,研磨20分钟使纳米NaV6O15粉末充分分散在水性油墨中,得到本发明的导电油墨。
将制备得到的导电油墨印刷在陶瓷表面,风干成型后,利用扫描电镜对油墨涂层进行分析,表面油墨涂层具有高结构性空间导电网络,纳米NaV6O15颗粒均匀分布且被由改性聚氨酯树脂、氨基树脂构成的聚合物树脂像桥梁一样将棒状结构的纳米NaV6O15颗粒联接起来,形成导电性能稳定的导电网络。
经测试,油墨涂层的伏安特性符合欧姆定律。将热处理后的导电薄膜置于120℃的烘箱中烘烤24、48、72、96和120小时后取样,发现油墨涂层表面形貌稳定无裂纹或脱落现象,且表面电阻未发生明显变化,表明该导电油墨涂层具有很好的耐温性。将测试样条浸于去离子水中,分别于24、48、72、96和120小时后取样,发现样条的油墨涂层表面形貌稳定,无失光、变色、起泡、起皱或脱落现象;干燥后再次测试油墨涂层的表面电阻未发生变化,表明该导电油墨具有很好的耐湿性。
实施例2
取主溶剂70份、改性聚氨酯树脂20份、氨基树脂0份、封闭型异氰酸酯3份、水性蜡0.5份、消泡剂0.05份、导电助剂0.2-0.5份,加入搅拌釜中混合均匀,得到水性油墨。在上述水性油墨中再加入乙醇胺0.05份和纳米NaV6O15粉末40份,研磨60分钟使纳米NaV6O15粉末充分分散在水性油墨中,得到本发明的导电油墨。
经测试,油墨涂层的伏安特性符合欧姆定律。将热处理后的导电薄膜置于120℃的烘箱中烘烤24、48、72、96和120小时后取样,发现油墨涂层表面形貌稳定无裂纹或脱落现象,且表面电阻未发生明显变化,表明该导电油墨涂层具有很好的耐温性。将测试样条浸于去离子水中,分别于24、48、72、96和120小时后取样,发现样条的油墨涂层表面形貌稳定,无失光、变色、起泡、起皱或脱落现象;干燥后再次测试油墨涂层的表面电阻未发生变化,表明该导电油墨具有很好的耐湿性。
实施例3
取主溶剂60份、改性聚氨酯树脂15份、氨基树脂6份、封闭型异氰酸酯2份、水性蜡0.3份、消泡剂0.04份、导电助剂0.4份,加入搅拌釜中混合均匀,得到水性油墨。在上述水性油墨中再加入乙醇胺0.04份和纳米NaV6O15粉末35份,研磨60分钟使纳米NaV6O15粉末充分分散在水性油墨中,得到本发明的导电油墨。
经测试,油墨涂层的伏安特性符合欧姆定律。将热处理后的导电薄膜置于120℃的烘箱中烘烤24、48、72、96和120小时后取样,发现油墨涂层表面形貌稳定无裂纹或脱落现象,且表面电阻未发生明显变化,表明该导电油墨涂层具有很好的耐温性。将测试样条浸于去离子水中,分别于24、48、72、96和120小时后取样,发现样条的油墨涂层表面形貌稳定,无失光、变色、起泡、起皱或脱落现象;干燥后再次测试油墨涂层的表面电阻未发生变化,表明该导电油墨具有很好的耐湿性。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (9)
1.一种导电油墨,其特征在于,包括以质量份数表示的如下组分:主溶剂50-70份,改性聚氨酯树脂10-20份,氨基树脂5-10份,封闭型异氰酸酯1-3份,水性蜡0.2-0.5份,消泡剂0.02-0.05份,慢干剂0.02-0.05份,纳米NaV6O15粉末20-40份,导电助剂0.2-0.5份,其中,纳米NaV6O15粉末的晶体为颗粒均匀且尺寸长度为1.~1.5um的纳米棒状结构。
2.根据权利要求1所述导电油墨,其特征在于,包括以质量份数表示的如下组分:主溶剂60份、改性聚氨酯树脂15份、氨基树脂6份、封闭型异氰酸酯2份、水性蜡0.3份、消泡剂0.04份、导电助剂0.4份、慢干剂0.04份和纳米NaV6O15粉末35份。
3.根据权利要求1所述导电油墨,其特征在于,主溶剂为乙酸甲酯、乙酸乙酯、乙酸丙酯或乙酸丁酯中的至少一种。
4.根据权利要求1所述导电油墨,其特征在于,导电助剂为盐酸二甲基胺、盐酸二丁基胺、四甲基碘化铵、醋酸四甲基铵或季铵盐类中的至少一种。
5.根据权利要求1所述导电油墨,其特征在于,性改性聚氨酯树脂为大分子二元醇改性聚氨酯、烷基异氰酸酯改性聚氨酯或芳香族异氰酸酯改性聚氨酯中的至少一种。
6.根据权利要求1所述导电油墨,其特征在于,氨基树脂为甲醚化三聚氰胺甲醛树脂、丁醚化三聚氰胺甲醛树脂、混合醚化三聚氰胺甲醛树脂、甲醚化脲醛树脂、丁醚化脲醛树脂、甲醚化苯代三聚氰胺树脂或丁醚化苯代三聚氰胺树脂中的至少一种。
7.根据权利要求1所述导电油墨,其特征在于,消泡剂为聚丙烯酸酯类聚合物或磷酸酯改性的聚丙烯酸酯类聚合物的一种或几种。
8.根据权利要求1所述导电油墨,其特征在于,慢干剂为乙醇胺。
9.根据权利要求1-8任何一项所述导电油墨的制备方法,其特征在于,包括:
(1)取主溶剂50-70份、改性聚氨酯树脂10-20份、氨基树脂5-10份、封闭型异氰酸酯1-3份、水性蜡0.2-0.5份、消泡剂0.02-0.05份和导电助剂0.2-0.5份,加入搅拌釜中混合均匀,得到水性油墨;
(2)在上述水性油墨中再加入慢干剂0.02-0.05份和纳米NaV6O15粉末20-40份,研磨20-60分钟使纳米NaV6O15粉末充分分散在水性油墨中,制备得到导电油墨。
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