CN1840592A - 用银钯合金纳米粒子制备印刷电路板的方法 - Google Patents
用银钯合金纳米粒子制备印刷电路板的方法 Download PDFInfo
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Abstract
根据本发明制备的PCB,通过喷射分散有银钯合金纳米粒子的导电墨水,并固化以形成布线,使Ag离子迁移减小。此外,本发明还提供了一种PCB制造方法,该方法表现出竞争性的价格以及极好的传导性和抗迁移性。作为本发明的一个方面,提供含有银钯合金纳米粒子的导电墨水,其中,银钯合金纳米粒子包括5-40重量%的Pd。
Description
技术领域
本发明是关于一种用导电墨水通过喷墨印刷方法形成电路图案来制备印刷电路板(PCB)的方法。
相关申请
本申请要求于2005年3月18日向韩国知识产权局递交的韩国申请2005-0022606的优先权,该申请的全部内容结合于本申请作为参考。
背景技术
印刷电路板(printed circuit board,PCB)的金属布线(mental wiring)技术按照蚀刻(etching)、丝网印刷(screen printing)和喷墨印刷(ink-jetprinting)的顺序得到发展。其中,包括用金属浆料进行丝网印刷并固化的丝网印刷技术已经公知并仍然被广泛使用。然而丝网印刷技术存在一些缺点:i)固化温度过高;并且ii)该技术需要过量使用昂贵并且有害的无水溶剂,因此不可能在PCB上使用简单而方便的金属布线。再者,通过丝网印刷方法的书写方法,应用于成形电路图案(formed circuit pattern)的宽度不是十分窄的领域,因此平均直径为0.5-20微米的金属粉末通过分散在热固树脂组合物中而用作导电墨水。
另一方面,近来在信息设备中存在持续小型化的趋势,因此这些设备上安装的PCB的布线间距变得更窄,同时还存在电路精密度和准确性的趋势,因此PCB上形成的电路图案的宽度变得更窄,层厚度变得更薄。在层厚度为几微米的情况下,当使用含有平均直径大于0.5微米的金属组分的常规金属浆料时,层厚度的分布变得相对较大,导电性变得不规律。而且,可能由于粒子间的接触不良破坏导电性。
因为喷墨方法(ink-jet method)为通过使用含有细金属粉末的液体金属墨的直写方法(direct-writing),所以它能缩小最小线宽度和最小线间距从而得到高密度电路图案。
在喷墨方法中,导电线路板(conductive wiring board)通过使用喷墨设备将导电墨水喷射在基材上,然后进行固化操作直接形成导电电路而制备,所述导电墨水中金属粒子如Ag或Cu分散在有机溶剂中。因为喷墨方法使用细喷嘴形成图案,因此墨水中的金属纳米粒子维持均一分散浓度非常重要。金属粒子的实例包括Au、Ag、Cu等,其中具有成本以及抗离子迁移(anti-ion migration)特性优势的Cu目前广泛应用。然而当粒子大小逐渐变小接近纳米大小时,随着Cu表面积的增加,很容易被氧化。结果通过与空气中的氧气反应,在表面形成二氧化硅膜。尤其含有水分的空气促进氧化反应。虽然已尝试用多种方法防止Cu氧化,但是仍很难完全避免表面氧化。
另一方面,当通过用Au或Ag纳米粒子制备的超细印刷墨形成细电路图案,并且进行固化操作以制造PCB时,使得布线的体积比电阻率(volumespecific resistivity)小于1×10-5欧姆(Ω),其线宽度/布线间距(L/S)约为5-50微米。然而,Au非常昂贵,以至于它导致制造单位成本上升。另一方面,使用Ag纳米粒子时,Ag降低制造成本并和提供良好的导电性。但是PCB暴露于高湿高温下,导致枝晶朝向(-)电极(阴极)生长,其中Ag离子镀出,缩小布线的线宽度/布线间距。结果导致电路之间或布线之间断路或短路,还可能进一步破坏产品。当迁移发生后去除高湿或高温条件,迁移的状态仍然存在,因此很难使产品有保障。
因而亟需得到用含有导电金属纳米粒子并提供抗离子迁移的导电墨水制备PCB的方法。
发明内容
作为克服常规技术相关缺陷的解决方案,本发明的一个目的是提供一种含有银钯合金纳米粒子的导电墨水。
本发明还提供了一种制造印刷电路板(PCB)的方法,所述PCB的布线表现出竞争性的价格以及极好的传导性和抗迁移性。
本发明还提供了一种具有成形为细电路图案的布线的PCB,所述PCB的布线表现出竞争性的价格以及极好的传导性和抗迁移性,并且在所需布线宽度和间距下也不会产生由金属离子迁移引起的断路或短路。
附图说明
图1为表示离子迁移机制的示意图;
图2为由离子迁移到基材电路内产生的枝晶分支结构的照片;
图3为基材电路内产生的枝晶的横截面示意图;
图4为由于所述离子迁移,绝缘电阻值随时间递减图;
图5图解说明了绝缘电阻值,根据本发明,当含有Ag纳米粒子的导电墨水以L/S100微米喷射在基材上且固化形成布线之后,在湿度85%和温度85℃的条件下,允许60秒2.5伏特的电压。
图6图解说明了绝缘电阻值,根据本发明,当含有银钯合金纳米粒子的导电墨水以L/S100微米喷射在基材上且固化形成布线之后,在湿度85%和温度85℃的条件下,允许60秒2.5伏特的电压。
具体实施方式
当使用含有Ag和Pd纳米粒子混合物而不是银钯合金纳米粒子的导电墨水制备PCB时,导致以下一些缺点:i)很难使混合物粉末均一地分散在墨水溶剂中;ii)通过覆盖基材和固化得到的电路在固化操作中,有斑点形成;并且iii)彻底防止粒子迁移存在限制。因此,本发明试图使用其中银钯合金纳米粒子分散于有机溶剂中的导电墨水解决上述问题。
根据本发明的优选实施方式,导电墨水含有银钯合金纳米粒子,其中所述银钯合金纳米粒子包括5-40重量%的Pd,更优选10-30重量%。所述导电墨水可以用作PCB的布线材料。
根据本发明的优选实施方式,导电墨水中含有的所述银钯合金纳米粒子可以为直径1-50纳米的纳米级大小,可以通过喷墨管嘴。
根据本发明的优选实施方式,所述导电墨水通过在十二烷基硫酸钠(SDS)水溶液中溶解乙酸钯和乙酸银并加热使所得溶液反应制得。在此情况下,所述导电墨水不用混合任何有机溶剂,就可以简单制备。加热反应优选在130℃的油浴中进行。
本发明提供了一种制造PCB的方法和由此制造的PCB,该方法包括以下步骤:在有机溶剂中分散银钯合金纳米粒子,制造导电墨水;用喷墨方法在基材上喷射导电墨水并固化所述基材,形成布线。所述银钯合金纳米粒子包括5-40重量%的Pd,更优选10-30重量%。
所述银钯合金纳米粒子为纳米级大小,可以通过喷墨管嘴,优选直径为1-50纳米。
在银钯合金纳米粒子中的Pd为5重量%或者更低时,不足以防止Ag+离子迁移。另一方面,在银钯合金纳米粒子中的Pd为40重量%或者更高时,布线的传导性下降,而且由于增加了昂贵的Pd的量,利润下降。
具有细电路图案的PCB特别更需要本发明的导电墨水。所述细电路图案具有窄的布线宽度和布线间距,并且还引起离子迁移。可能因离子迁移导致如上所述断路或短路的布线宽度和布线间距通常为100微米或100微米以下。因此本发明的导电墨水对具有100微米或100微米以下的布线宽度和布线间距(L/S)的PCB非常有用。
本发明用以分散纳米粒子的有机溶剂可以是任何导电墨水用有机溶剂。
离子迁移为在与PCB相邻的电极上离子化的金属离子迁移到另一电极,并在该电极上还原且沉淀为金属。图1表示了离子迁移的机制。
阴极上的反应为:
(1)
(2)
(3)
阳极上的反应为:
(4)
如上所述,在阴极产生的银离子移动到阳极,与电子结合并最终沉淀成金属银,结果导致枝晶分支结构向阴极方向生长。图2表示由于离子向阴极迁移,枝晶分支结构生长引起阴极与阳极之间短路。图3表示产生的枝晶的横截面示意图。
离子迁移是由于电极之间通过湿气接触,实际上常常发生阳极基质上的金属积累。上述离子迁移成为日益增加的问题,因为近来集成电路封装(ICpackage)内的布线趋向小型化。所述集成电路封装例如积层板(build-upboard)、球栅阵列(Ball Grid Array,BGA)等。布线小型化导致图案间的电场强度(Electric Field Strength)增强、绝缘距离缩短和便携电子设备容易吸收湿气。
通过检测绝缘电阻的下降可以测定离子迁移。如图4所示,如果离子迁移随时间不断产生,则绝缘电阻值下降。
按照图4所示,在起始阶段(A)中,绝缘电阻由于吸收湿气或绝缘材料而下降,在中间阶段(B)中,电阻变得稳定。在最终阶段(C)中,当离子迁移开始时所述电阻骤降,因此电阻的骤降点可被认为是离子迁移开始的点。
实施例
在下文中将通过下列实施例对本发明进行更加详细的描述,所述实施例并不限定本发明的范围。
对比例1:分散有Ag纳米粒子的导电墨水的制备
将乙酸银前体溶解于50毫升0.1摩尔/升十二烷基硫酸钠(SDS)水溶液中,使乙酸银前体的浓度为4.5×10-4摩尔。所得溶液在油浴中缓慢加热,在130℃下反应9小时,以获得分散有直径为1-50纳米的Ag纳米粒子的银墨水。
实施例1-5:分散有银钯合金纳米粒子的导电墨水的制备
将乙酸钯前体和乙酸银前体2种前体溶解于50毫升0.1摩尔/升十二烷基硫酸钠(SDS)水溶液中,使2种前体的浓度为4.5×10-4摩尔。所得溶液在油浴中缓慢加热,在130℃下反应9小时,以获得分散有直径为1-50纳米的银钯合金纳米粒子的墨水。在所述制备的墨水中基于所述银钯合金的重量Pd的重量百分数分别为:5重量%(实施例1)、10重量%(实施例2)、20重量%(实施例3)、30重量%(实施例4)和40重量%(实施例5)。
对比例2
用喷墨打印机将对比例1制备的含有Ag纳米粒子的导电墨水以L/S100微米喷射在基材上,并在250℃下固化以形成布线。在湿度85%和温度85℃的条件下,对上述基材施用2.5伏特的电压60秒。观察绝缘电阻的变化。所得结果如图5所示。绝缘电阻从起始阶段到60小时保持了最初的绝缘电阻。但是一旦超过60小时,所述电阻因离子迁移的发生而骤降。
实施例6-10
用喷墨打印机将实施例1-5制备的含有银钯合金纳米粒子的导电墨水以L/S100微米喷射在基材上,并在250℃下固化以形成布线。测定上述基质的传导性。在湿度85%和温度85℃的条件下,对上述基材施用2.5伏特的电压60秒。观察绝缘电阻的变化,检测起始绝缘电阻保持不变的时间(形成枝晶的时间),在表1中与对比例2的结果汇总。当银钯合金中Pd重量%为30重量%时,绝缘电阻的变化如图6所示。
表1
类别 | 组成(Ag重量%/Pd重量t%) | 传导性(微欧姆·厘米) | 枝晶形成时间(小时) |
对比例2 | Ag100 | 3.23 | 60 |
实施例6 | 95/5 | 5.85 | 60 |
实施例7 | 90/10 | 9.01 | 82.5 |
实施例8 | 80/20 | 15.89 | 95 |
实施例9 | 70/30 | 25.74 | 120 |
实施例10 | 60/40 | 48.3 | - |
根据表1,当Pd的量为5重量%或者更低时,不足以防止Ag+离子迁移,而在银钯合金纳米粒子中的Pd为40重量%或者更高时,虽然没有离子迁移,但是传导性明显下降。此外,引人注意的是,如表2和图6所示,当Ag/Pd合金总重量中Pd的量为30重量%时,表现出最稳定的传导性,并且120小时后发生离子迁移。引人注意的是,当使用30重量%的Pd时,抗迁移性比只使用Ag纳米粒子时提高了2倍。
工业实用性
根据本发明制备的PCB,通过喷射分散有银钯合金纳米粒子的导电墨水,并固化以形成布线,使Ag离子迁移减小。此外,本发明还提供了一种PCB制造方法,该方法表现出竞争性的价格以及极好的传导性和抗迁移性。
Claims (12)
1、一种含有银钯合金纳米粒子的导电墨水,其中,所述银钯合金纳米粒子包括5至40重量%的Pd。
2、如权利要求1所述的导电墨水,其中,所述银钯合金包括10至30重量%的Pd。
3、如权利要求1或2所述的导电墨水,其中,所述银钯合金纳米粒子的直径为1至50纳米。
4、如权利要求1或2所述的导电墨水,其中,所述导电墨水通过在十二烷基硫酸钠水溶液中溶解乙酸钯和乙酸银并加热使所得溶液反应制得。
5、如权利要求4所述的导电墨水,其中,所述导电墨水通过在十二烷基硫酸钠水溶液中溶解乙酸钯和乙酸银并在130℃油浴中加热9小时使所得溶液反应制得。
6、一种制造印刷电路板的方法,该方法包括:
制备权利要求1或2所述的导电墨水;并且
将所述导电墨水喷射在基材上并固化所述基材,形成布线。
7、如权利要求6所述的方法,其中,所述银钯合金纳米粒子的直径为1至50纳米。
8、如权利要求6所述的方法,其中,所述制备导电墨水的步骤包括如下步骤:
在十二烷基硫酸钠水溶液中溶解乙酸钯和乙酸银;和
加热使所得溶液反应。
9、如权利要求6所述的方法,其中,所述制备导电墨水的步骤包括如下步骤:
在十二烷基硫酸钠水溶液中溶解乙酸钯和乙酸银;和
在130℃油浴中加热9小时使所得溶液反应。
10、如权利要求6所述的方法,其中,所述形成布线的步骤包括通过喷墨打印的方法在基材上形成图案。
11、一种印刷电路板,该印刷电路板按照权利要求6-10中任意一项所述的方法制得。
12、如权利要求11所述的印刷电路板,其中,在该印刷电路板上形成的所述布线的布线宽度和布线间距为可能发生由离子迁移引起的短路的布线宽度和布线间距。
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Cited By (5)
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CN101357403B (zh) * | 2007-07-30 | 2010-12-22 | 三星电机株式会社 | 用于制造金属纳米颗粒的方法 |
CN103436100A (zh) * | 2013-09-04 | 2013-12-11 | 西安腾星电子科技有限公司 | 一种导电油墨及其制备方法 |
CN104795128A (zh) * | 2015-05-14 | 2015-07-22 | 刘飞全 | 一种无铅电阻浆料及其制造工艺和应用 |
CN106670495A (zh) * | 2015-11-06 | 2017-05-17 | 南京大学 | 一种网络状Ag-Au-Pd三金属多孔材料的制备方法 |
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JP2006257403A (ja) | 2006-09-28 |
KR20060100792A (ko) | 2006-09-21 |
KR100653251B1 (ko) | 2006-12-01 |
US20060208230A1 (en) | 2006-09-21 |
CN100537677C (zh) | 2009-09-09 |
JP4431543B2 (ja) | 2010-03-17 |
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