CN102794453B - 一种超薄片状银粉的制备方法 - Google Patents
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Abstract
本发明公开了一种超薄片状银粉的制备方法,应用于低银含量的导电涂料。本发明以纯度为99.95%以上的球形或类球形银粉为原料,并对银粉添加其重量的0.2~5.0%的球磨保护剂,在2~50%的球磨附着剂的作用下,将银粉均匀的附着在球体上,在1~20%的球磨粘度调节剂的调节下,调节球体之间的相对独立,在卧式球磨机中进行球磨,球带着粉体一同运行,保证球磨的均匀性。球磨5~40h后,用无水乙醇将银粉洗涤2~6次,在20~100℃真空干燥4~10h,得到厚度在100nm左右的超薄片状银粉,该银粉在低银含量的情况下具有良好的导电性能。
Description
技术领域
本发明涉及一种超薄片状银粉的制备方法,属于电子导电涂料用粉体材料制备领域。
背景技术
在信息产业的发展中,导电涂料是必不可少的重要材料之一,而片状银粉作为功能相广泛应用于导电涂料中,其中,碳膜电位器、薄膜开关/柔性电路用银浆以及电磁屏蔽导电漆是常见的导电涂料之一。高性能、低成本不但可以提高产品的市场竞争力,也是其发展的必然趋势,降低银含量成为降低成本的途径之一。
由聚合物与银粉组成的导电涂料的导电原理,一般认为是通过3种形式来实现:一是通过导电填料间直接接触(导电微粒之间的间隙<1nm)来实现导电,即通道导电;另一是孤立粒子或小聚集体之间相距很近.只被很薄的聚合物薄层(10 nm左右)隔开,由热振动激活的电子就能越过聚合物薄层所形成的势垒跃迁到邻近导电微粒上形成隧道电流,即隧道效应;第三是电场发射理论,电压增加到一定值时.导电粒子绝缘层间的强电场促使电子越过势垒而产生场致发射电流,实际上也是一种隧道效应,只是激发源为电场。因此,银粉之间的聚合物薄层厚度直接影响涂料的导电性能。厚度簿、比表面积大的片状银粉单位面积内所吸附的聚合物重量与体积就少,银粉与银粉之间的聚合物膜就相对较簿,电子跃迁需要克服的势垒就低,通过通道导电与隧道效应形成的电流就大,涂料的导电性就越好,在相同导电性能的条件下,采用超薄的片状银粉来降低导电涂料银含量成为可能,因此超薄的片状银粉具有较大的实用价值。
发明内容
本发明的目的在于提供了一种超薄片状银粉的制备方法,在球磨保护剂和球磨附着剂的作用下,将银含量为99.95%及以上的球形或类球形银粉附着在球体上,在球磨粘度调节剂的调节下,在卧式球磨机中进行均匀球磨,球磨后的片状银粉用无水乙醇洗涤,真空干燥后得到厚度在100nm左右的超薄片状银粉,该银粉在低银含量的情况下具有良好的导电性能。
本发明采用一下技术来实现。
超薄片状银粉的生产工序由选料、球磨、洗涤与干燥三部分组成。
1、选料:原料为银含量在99.95%及以上银粉,粒度为0.5~5微米的超细银粉。
2、球磨:按质量比每公斤银粉添加2~50克球磨保护剂、20~500克球磨附着剂将银粉调节成一定粘度的粉浆,按球与银粉的质量比为5~20:1加入直径为ф1~10毫米球体,将粉浆附着在球体上,每公斤银粉再加入10~200克球磨粘度调节剂,调节球体之间的流动性,在卧式球磨机中进行球磨,球磨转速为10~100转/分钟,球磨5~40小时,球磨后用乙醇在过滤筛中将银粉与球体分离,得到乙醇-银粉浆。
所叙球磨保护剂为硬脂酸、油酸、丙烯酸、十六醇、十八醇、月桂酸、十二醇、聚乙二醇等中的一种或几种。
所叙球磨附着剂为丙二酸二乙酯、丙二醇碳酸酯、丙烯酸乙酯、丙烯酸丁酯、丙烯酸甲酯、丙酸乙酯、丙酸丙酯、丙酸丁酯、丙酸甲酯、乙二酸二乙酯、乙二酸二丁酯、乙二醇二甲酸酯、乙二醇邻苯二甲酸酯、乙二醇蓖麻酸酯中的一种或几种。
所叙球磨粘度调节剂为乙醇、丙二醇、丙三醇、乙二醇二乙醚、乙二醇二丁醚、烷基酚聚氧乙烯醚、苄基酚聚氧乙烯醚、苯乙基酚聚氧乙烯醚、月桂醇聚氧乙烯醚中的一种或几种。
3、银粉洗涤与干燥:将乙醇-银粉浆搅拌,沉降,抽取上清液,再加入乙醇,搅拌沉降反复洗涤2~6次,抽滤后真空烘干,烘干温度20-100℃,烘干时间4~10小时,得到超薄片状银粉。
与公知技术相比具有的优点:
1、本发明通过球磨分散剂、附着剂将银粉均匀附着在球体上,保证银粉与球体一同在球磨机中运行,球磨粘度调节剂调节球体之间的分散性,保证球与球之间的相互影响较小,银粉因此得到比较相同的球磨效果。
2、本发明得到的片状银粉厚度在100nm左右,在相同银含量的条件下的导电性能比其它银粉更优良,可以降低导电涂料的银含量。
附图说明
图1为本发明的实施1的形状和厚度的扫描电镜图,图2为本发明的实施2形状和厚度的扫描电镜图。
具体实施方式
实施例1
1、原料:要求超细银粉粒度为0.5~1.5微米,银含量为99.95~99.97%;
2、球磨:将容积为30升的卧式球磨机清理干净,加入原料银粉5公斤,添加50克球磨保护剂、1000克球磨附着剂将银粉调节成一定粘度的粉浆,加入50公斤直径为ф3毫米钢球,将粉浆附着在球体上,加入100克球磨粘度调节剂,调节球体之间的流动性,在卧式球磨机中进行球磨,球磨转速为70转/分钟,球磨16小时,球磨后用乙醇在过滤筛中将银粉与球体分离,得到乙醇-银粉浆。
所叙球磨保护剂为硬脂酸、十八醇、月桂酸三种。
所叙球磨附着剂为丙二酸二乙酯、丙烯酸甲酯、丙酸乙酯、丙酸丙酯中的两种。
所叙球磨粘度调节剂为丙三醇、乙二醇二乙醚、乙二醇二丁醚、烷基酚聚氧乙烯醚中的一种。
3、银粉洗涤与干燥:将乙醇-银粉浆搅拌,沉降,抽取上清液,再加入乙醇,搅拌沉降反复洗涤4次,抽滤后真空烘干,烘干温度50℃,烘干时间5小时,得到超薄片状银粉,所得银粉的片径为1.0-4.0微米,厚度为60-100纳米。
实施例2
1、原料:要求超细银粉粒度为1.0~2.5微米,银含量为99.95~99.97%;
2、球磨:将容积为30升的卧式球磨机清理干净,加入原料银粉5公斤,添加100克球磨保护剂、1300克球磨附着剂将银粉调节成一定粘度的粉浆,加入100公斤直径为ф3毫米钢球,将粉浆附着在球体上,加入200克球磨粘度调节剂,调节球体之间的流动性,在卧式球磨机中进行球磨,球磨转速为60转/分钟,球磨8小时,球磨后用乙醇在过滤筛中将银粉与球体分离,得到乙醇-银粉浆。
所叙球磨保护剂为油酸、十六醇、聚乙二醇等中的三种。
所叙球磨附着剂为丙酸乙酯、丙酸丙酯、乙二醇邻苯二甲酸酯、乙二醇蓖麻酸酯中的两种。
所叙球磨粘度调节剂为丙三醇、烷基酚聚氧乙烯醚、月桂醇聚氧乙烯醚中的一种。
3、银粉洗涤与干燥:将乙醇-银粉浆搅拌,沉降,抽取上清液,再加入乙醇,搅拌沉降反复洗涤4次,抽滤后真空烘干,烘干温度50℃,烘干时间5小时,得到超薄片状银粉,所得银粉的片径为2.0-6.0微米,厚度为70-90纳米。
Claims (1)
1. 一种超薄片状银粉的制备方法,其特征在于含有以下工艺步骤:
1)、选料:选择银含量大于或等于99.95%,粒度为0.5~5微米的超细银粉;
2)、球磨:按质量比添加球、银粉、球磨保护剂、球磨附着剂和球磨粘度调节剂,球与银粉的质量比为5~20:1,采用直径为ф1~10毫米球,每公斤银粉添加2~50克球磨保护剂、20~500克球磨附着剂、10~200克球磨粘度调节剂,球磨转速为10~100转/分钟,球磨5~40小时,球磨后用乙醇在过滤筛中将银粉与球体分离,得到乙醇-银粉浆;
3)、银粉洗涤与干燥:将乙醇-银粉浆搅拌,沉降,抽取上清液,再加入乙醇,搅拌沉降反复洗涤2~6次,抽滤后真空烘干,烘干温度20-100℃,烘干时间4~10小时,得到超薄片状银粉,
所述球磨保护剂为硬脂酸、油酸、丙烯酸、十六醇、十八醇、月桂酸、十二醇、聚乙二醇中的一种或几种,
所述球磨附着剂为丙二酸二乙酯、丙二醇碳酸酯、丙烯酸乙酯、丙烯酸丁酯、丙烯酸甲酯、丙酸乙酯、丙酸丙酯、丙酸丁酯、丙酸甲酯、乙二酸二乙酯、乙二酸二丁酯、乙二醇二甲酸酯、乙二醇邻苯二甲酸酯、乙二醇蓖麻酸酯中的一种或几种,
所述球磨粘度调节剂为乙醇、丙二醇、丙三醇、乙二醇二乙醚、乙二醇二丁醚、烷基酚聚氧乙烯醚、苄基酚聚氧乙烯醚、苯乙基酚聚氧乙烯醚、月桂醇聚氧乙烯醚中的一种或几种。
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