CN111117517B - 导电银胶及其制备方法 - Google Patents
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Abstract
本发明公开了一种导电银胶及其制备方法,所述导电银胶以重量计份包括如下成分:改性酚类树脂80‑100份;脂肪族聚酰胺55‑60份;稀释剂30‑40份;金属粉末1‑3份;促进剂1.2‑1.8份;添加剂0.6‑1份;组合助剂0.2‑0.5份,本发明将镀银玻璃微珠与石墨的混合物引入体系中,一方面具有节能和节约成本的作用,另一方面层状结构的石墨与球状镀银玻璃微珠的混合使用,实现疏松的片状石墨中加入粒度较小的球状微珠,改变了粉末的粒度分散特点和堆积状态,颗粒间实现了片与片、点与点、片与点几种接触形式,从而提高导电银胶的导电性能。
Description
技术领域
本发明涉及一种导电银胶及其制备方法,属于电子材料领域。
背景技术
导电胶是将提供导电性能的导电填料填充到提供机械性能的聚合物粘料中制得的电子化学品。它起源于20世纪70年代早期,最初主要用在陶瓷基板上IC晶片以及被动元器件的精细间距引脚连接,并未获得广泛工业应用。在现代社会中,导电银胶在电子、信息、电镀等行业被广泛应用,主要用作物体间的导电粘接。导电银胶通常采用环氧树脂或聚氨酯作为导电银胶的基体树脂,添加橡胶等柔性大分子,利用长链柔性胺作为固化剂改善环氧树脂的脆性得到柔弹性的导电银胶。导电银胶主体有机聚合物在加热过程中的物理化学反应,可以分为热固性导电银胶和热塑性导电银胶。热固性树脂在浆料中是单体线性分子或预聚体,在固化过程中发生聚合接枝反应,线型高分子交联形成三维体形结构,形成不溶物;热塑性树脂有大分子线性聚合链,不形成交联的三维网状结构,在高温下或溶剂中能重新熔融或溶解。其中热固性导电银胶虽然膜层固化后的附着力和电性能等性能都不错,但是经过焊接银层爆肚、开裂、膜层完全失效。随着电子器件向微型化方向发展,许多传感器材料都要求薄膜化,导电胶成为连接薄膜和其引线材料的首选材料,但是现有的导电胶存在电导率低、耐热型差、粘接强度弱等缺陷,难以满足现代社会电子行业发展的需要。
发明内容
本发明所要解决的技术问题在于针对上述现有技术中的不足,提供一种导电银胶及其制备方法。
为解决上述技术问题,本发明采用的技术方案是:一种导电银胶,所述导电银胶以重量计份包括如下成分:
优选的是,其中,所述脂肪族聚酰胺包括聚乙二酰乙二胺、聚乙内酰胺、聚癸二酰己二胺、聚ω-氨基十一酰、聚十二内酰胺中的至少一种。
优选的是,其中,所述改性酚类树脂的制备方法如下:将苯酚以及混合无机强碱混合,以500r/min搅拌30-45min,加入双酚A和甲醛,升温至60℃,将温度控制在60-65℃,保温2h,冷却至室温后加入L-肉羧酸,恒温75-90℃搅拌1.5-2h,降温出料即得到改性酚类树脂。
双酚A改性酚醛树脂,不仅可以提高酚醛树脂的耐热性,还可以改善其韧性和抗湿性,因为芳香杂环引入到分子结构中,可以提高其玻璃化转变温度和热稳定性,可以改善耐热性能尤其是耐高温性能,并且双酚A属活性较强但耐热性能较好的柔性段,用其对酚醛树脂进行改性,增加网链分子的活动能力,从而获得理想的增韧效果。
优选的是,其中,所述稀释剂包括乙醇、正丙醇、异丙醇、丁醇中的一种或多种的混合物。
优选的是,其中,所述促进剂包括二甲基苯胺、二乙基苯胺、N,N-二甲基对甲苯胺、三乙醇胺、2,4,6-三(二甲胺基甲基)苯酚中的一种或多种的混合物。
优选的是,其中,所述添加剂包括二甲基胺硼烷、苯基二硫代丙烷磺酸钠、聚二硫丙烷磺酸钠、N,N-二甲基硫代胺基甲酰基丙烷磺酸钠、噻唑啉基二硫代丙烷磺酸钠、2-巯基苯骈咪唑中的一种或多种的组合物。
优选的是,其中,所述金属粉末为片状金属粉末与球状金属粉末的混合物,其中,所述金属粉末为金、银、锑中的一种或多种的组合。
优选的是,其中,所述组合助剂为镀金属玻璃微球与石墨的混合物。
优选的是,其中,所述金属纳米粒子包括银纳米粒子、金纳米粒子、铜纳米粒子中的至少一种。
优选的是,其中,一种制备如权利要求1-9任意一项所述的导电银胶的制备方法,包括以下步骤:
(1)将改性酚树脂、脂肪族聚酰胺加入分散剂中加热搅拌至完全溶解,在80-90℃的恒温条件下加热20-40min,缓慢加入添加剂、促进剂以及组合助剂缓慢,搅拌加热至完全溶解,冷却得到导电银胶基体;
(2)将所述金属粉末与所述导电银胶基体混合,研磨分散后轧制成为均匀的膏状物体,即得到所述导电银胶。
本发明的有益效果是:(1)金属粉末结合片状和球状金属粉末,改变粉末的粒度分散特点和堆积状态,颗粒间实现了片与片、点与点、片与点几种接触形式,显著提高导电胶的导电性能;(2)双酚A改性的酚类树脂使得制备的导电银胶具有很高的导热率,能够应用于极端高温环境;(3)组合助剂采用石墨与镀银玻璃微珠,在节省生产成本的基础上,通过将层状结构石墨与球状镀银玻璃微球混合使用,发挥二者协同效应,石墨片在镀银玻璃微球之间搭桥,从而提高导电银胶的导电性能。
具体实施方式
实施例1:
一种导电银胶,导电银胶以重量计份包括如下成分:
其中,改性酚类树脂的制备方法如下:将苯酚以及混合无机强碱混合,以500r/min搅拌30-45min,加入双酚A和甲醛,升温至60℃,将温度控制在60-65℃,保温2h,冷却至室温后加入L-肉羧酸,恒温75-90℃搅拌1.5-2h,降温出料即得到改性酚类树脂。
其中,脂肪族聚酰胺为聚乙二酰乙二胺,稀释剂为正丙醇,促进剂为二甲基苯胺,添加剂为二甲基胺硼烷,金属粉末为片状银粉末与球状银粉末的混合物,组合助剂为镀银玻璃微球与石墨的混合物。
一种制备导电银胶的制备方法,包括以下步骤:
(1)将改性酚树脂、脂肪族聚酰胺加入分散剂中加热搅拌至完全溶解,在80-90℃的恒温条件下加热20-40min,缓慢加入添加剂、促进剂以及组合助剂缓慢,搅拌加热至完全溶解,冷却得到导电银胶基体;
(2)将所述金属粉末与所述导电银胶基体混合,研磨分散后轧制成为均匀的膏状物体,即得到所述导电银胶。
实施例2:
一种导电银胶,导电银胶以重量计份包括如下成分:
其中,改性酚类树脂的制备方法如下:将苯酚以及混合无机强碱混合,以500r/min搅拌30-45min,加入双酚A和甲醛,升温至60℃,将温度控制在60-65℃,保温2h,冷却至室温后加入L-肉羧酸,恒温75-90℃搅拌1.5-2h,降温出料即得到改性酚类树脂。
其中,脂肪族聚酰胺为聚乙内酰胺,稀释剂为正丙醇,促进剂为N,N-二甲基对甲苯胺,添加剂为二甲基胺硼烷,金属粉末为片状银粉末与球状银粉末的混合物,组合助剂为镀银玻璃微球与石墨的混合物。
一种制备导电银胶的制备方法,包括以下步骤:
(1)将改性酚树脂、脂肪族聚酰胺加入分散剂中加热搅拌至完全溶解,在80-90℃的恒温条件下加热20-40min,缓慢加入添加剂、促进剂以及组合助剂缓慢,搅拌加热至完全溶解,冷却得到导电银胶基体;
(2)将所述金属粉末与所述导电银胶基体混合,研磨分散后轧制成为均匀的膏状物体,即得到所述导电银胶。
实施例3:
本实施例与实施例1的原料和工艺基本相同,唯一不同之处在于,将添加剂二甲基胺硼烷改为苯基二硫代丙烷磺酸钠。
实施例4:
本实施例与实施例1的原料和工艺基本相同,唯一不同之处在于,将片状银粉末与球状银粉末的混合物改为片状金粉末与球状金粉末的混合物。
对比例1:
本对比例与实施例1的原料和工艺基本相同,唯一不同之处在于,将改性酚类树脂改为酚类树脂或单一的石墨。
对比例2:
本对比例与实施例1的原料和工艺基本相同,唯一不同之处在于,将组合助剂改为单一的镀银玻璃微球。
对比例3:
本对比例与实施例1的原料和工艺基本相同,唯一不同之处在于,将片状金属粉末和球状金属粉末的混合物改为单一片状金属粉末或单一球状金属粉末。
以上实施例1-4及对比例1-3的产品性能如下表所示,以下为性能测试结果:
粘接强度(MPa) | 体积电阻率(Ω.cm) | 导热率(w/k.m) | |
实施例1 | 12.9 | 1.21x10<sup>-4</sup> | 6.11 |
实施例2 | 13.3 | 1.27x10<sup>-4</sup> | 6.27 |
实施例3 | 13.6 | 1.24x10<sup>-4</sup> | 5.94 |
实施例4 | 13.4 | 1.29x10<sup>-4</sup> | 6.01 |
对比例1 | 7.5 | 1.65x10<sup>-4</sup> | 4.56 |
对比例2 | 8.2 | 1.73x10<sup>-4</sup> | 4.37 |
对比例3 | 6.0 | 1.60x10<sup>-4</sup> | 4.35 |
剪切强度测试:采用GB 7124-86标准测试。
体积电阻率测试:按照GB/T 1410-2006标准测试。
电导率测试:采用3651-2008标准进行测试。
实施例1与对比例1相比,导热率由4.56增大到6.11w/k.m,这是因为双酚A改性酚类树脂,将芳杂环引入分子结构中,可以提高酚类树脂的玻璃化转变温度与热稳定性,增加网链分子的活动能力,从而改善导电银胶的耐高温性能。
实施例1与对比例2相比,导电银胶的体积电阻率由1.73x10-4Ω.cm减小至1.21x10-4Ω.cm,石墨具有层状结构,其耐压力的程度受到了一定的限制,当将层状结构的石墨与球状镀银玻璃微球混合使用时,石墨的片可以在镀银玻璃微球之间搭桥,从而有利于提高导电银胶的导电性能。
实施例1与对比例3相比,1.60x10-4减小至1.21x10-4Ω.cm,疏松的片状金粉中加入粒度较小的球状金粉,改变了粉末的粒度分散特点和堆积状态,颗粒间实现了片与片、点与点、片与点几种接触形式,从而提高导电胶的导电性能。
尽管本发明的实施方案已公开如上,但其并不仅仅限于说明书和实施方式中所列运用,它完全可以被适用于各种适合本发明的领域,对于熟悉本领域的人员而言,可容易地实现另外的修改,因此在不背离权利要求及等同范围所限定的一般概念下,本发明并不限于特定的细节。
Claims (4)
2.根据权利要求1所述的导电银胶,其特征在于,所述添加剂包括二甲基胺硼烷、聚二硫丙烷磺酸钠、N ,N-二甲基硫代胺基甲酰基丙烷磺酸钠、噻唑啉基二硫代丙烷磺酸钠、2-巯基苯骈咪唑中的一种或多种的组合物。
3.根据权利要求1所述的导电银胶,其特征在于,其中,所述金属粉末为金、银、锑中的一种或多种的组合。
4.一种制备如权利要求1-3任意一项所述的导电银胶的制备方法,其特征在于,包括以下步骤: 1)将改性酚树脂、脂肪族聚酰胺加入稀释剂中加热搅拌至完全溶解,在80-90℃的恒温条件下加热20-40min,缓慢加入添加剂、促进剂以及组合助剂缓慢搅拌加热至完全溶解,冷却得到导电银胶基体; 2)将所述金属粉末与所述导电银胶基体混合,研磨分散后轧制成为均匀的膏状物体,即得到所述导电银胶。
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