CN106488821A - 金属微粒分散液和金属覆膜 - Google Patents

金属微粒分散液和金属覆膜 Download PDF

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CN106488821A
CN106488821A CN201580035493.5A CN201580035493A CN106488821A CN 106488821 A CN106488821 A CN 106488821A CN 201580035493 A CN201580035493 A CN 201580035493A CN 106488821 A CN106488821 A CN 106488821A
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metal particle
dispersion liquid
particle dispersion
metal
water
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冈田诚
冈田一诚
杉浦元彦
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Sumitomo Electric Industries Ltd
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Sumitomo Electric Industries Ltd
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Abstract

本发明公开了一种金属微粒分散液，所述金属微粒分散液用于通过涂布和烧结形成金属覆膜，所述金属微粒分散液包含具有200nm以下平均粒径的金属微粒和用于分散所述金属微粒的溶剂。所述金属微粒分散液还包含水溶性树脂。相对于100质量份的所述金属微粒，所述水溶性树脂的含量优选为0.1质量份以上且10质量份以下。

Description

金属微粒分散液和金属覆膜
技术领域
本发明涉及金属微粒分散液和金属覆膜。
背景技术
近年来，在制造印刷电路板等时已经越来越多地采用在基材的表面上形成金属覆膜的特殊方法。该方法涉及将含有溶剂和分散在溶剂中的纳米级金属微粒的金属微粒分散液涂布到基材表面形成涂膜，和将涂膜加热以干燥并将涂膜烧结为金属覆膜。
已经提出了一种用于形成这样的金属覆膜的金属微粒分散液。根据该方案，通过将具有0.001μm～0.1μm粒径的银或氧化银超细微粒与在室温下不易蒸发但在干燥和烧结期间蒸发的有机溶剂混合来制备金属微粒分散液，所述金属微粒分散液具有1000cP以下的室温粘度(参考专利文献1)。
现有技术文献
专利文献
专利文献1：日本特开2001-35814号公报
发明内容
技术问题
通过涂布诸如专利文献1中公开的金属微粒分散液并进行烧结而形成的金属覆膜易于因在烧结期间金属微粒分散液的涂膜的体积减小而在所有部分中具有小的裂纹。
这种有裂纹的金属覆膜有时使得难以在其上均匀地形成不同材料的其它层或与基材剥离。
鉴于上述情况，本发明的目的是提供一种能够形成具有较少裂纹的金属覆膜的金属微粒分散液、和具有较少裂纹的金属覆膜。
解决技术问题的技术方案
旨在解决上述问题的本发明的一个方面的金属微粒分散液为用于通过涂布和烧结形成金属覆膜的金属微粒分散液，所述金属微粒分散液包含具有200nm以下平均粒径的金属微粒和用于分散所述金属微粒的溶剂，其中所述金属微粒分散液还包含水溶性树脂。
有益效果
通过使用本发明的一个方面的金属微粒分散液，可以形成具有较少裂纹的金属覆膜。
附图说明
[图1]图1为显示本发明实施方案的金属覆膜的制造方法的流程图。
具体实施方式
[本发明实施方案的说明]
本发明一个实施方案的金属微粒分散液为用于通过涂布和烧结形成金属覆膜的金属微粒分散液，所述金属微粒分散液包含具有200nm以下平均粒径的金属微粒和用于分散所述金属微粒的溶剂，其中所述金属微粒分散液还包含水溶性树脂。换而言之，本发明一个实施方案的金属微粒分散液为用于通过涂布和烧结形成金属覆膜的金属微粒分散液，所述金属微粒分散液包含具有200nm以下平均粒径的金属微粒和用于分散所述金属微粒的溶剂(通过涂布金属微粒分散液并对涂布的金属微粒分散液进行烧结形成金属覆膜)，其中所述金属微粒分散液还包含水溶性树脂。
由于金属微粒分散液除了金属微粒和溶剂以外还包含水溶性树脂，所以在对金属微粒分散液的涂膜进行干燥(溶剂蒸发)期间由于水溶性树脂而使得涂膜的收缩变得缓和。因为在涂膜干燥之后在对金属微粒进行烧结期间水溶性树脂逐渐热解，所以烧结缓慢进行。因此，可以抑制金属覆膜破裂。当使用该金属微粒分散液时，可以形成在其上可以容易地层叠其它材料的具有较少裂纹的金属覆膜，特别地，可以形成具有良好可镀性的金属覆膜。
相对于100质量份的金属微粒，水溶性树脂的含量优选为0.1质量份以上且10质量份以下。当水溶性树脂的含量在该范围内时，可以有效抑制破裂，并且因为水溶性树脂在烧结期间热解，所以在烧结之后有机残余物很少残留在金属覆膜中。
优选水溶性树脂的数均分子量为1000以上且1000000以下。当水溶性树脂的数均分子量在该范围内时，可以抑制涂膜破裂，并且因为水溶性树脂在烧结期间热解，所以在烧结之后有机残余物很少残留在金属覆膜中。
优选水溶性树脂为聚乙烯醇、聚乙二醇和聚乙撑亚胺中的任意一种或它们的组合。当水溶性树脂为聚乙烯醇、聚乙二醇和聚乙撑亚胺中的任意一种或它们的组合时，不仅可以更有效地防止破裂，而且水溶性树脂通过烧结而容易地热解并且在烧结之后较少的有机残余物残留在金属覆膜中。
优选金属微粒由铜制成。当将铜用作金属微粒时，可以形成具有低电阻的金属覆膜并且可以提供低成本的金属覆膜。
通过涂布金属微粒分散液并对涂布的金属微粒分散液进行烧结，形成本发明另一个实施方案的金属覆膜。
由于金属覆膜是通过涂布金属微粒分散液并对涂布的金属微粒分散液进行烧结而形成的，所以金属覆膜具有较少的裂纹和较大的对基材的粘附力。
“平均粒径”是指通过在用扫描电子显微镜摄取的照片中对100个以上的粒子进行计数而确定的体积中值直径D50。“数均分子量”是通过凝胶过滤色谱法测定的值。
[本发明实施方案的详情]
现在将参照附图对本发明实施方案的金属覆膜的制造方法进行详细说明。
图1显示本发明实施方案的金属覆膜的制造方法的步骤。该金属覆膜制造方法包括：通过液相还原法产生金属微粒的步骤(步骤S1)；将产生的金属微粒分离的步骤(步骤S2)；通过使用分离的金属微粒制备金属微粒分散液的步骤(步骤S3)；将得到的金属微粒分散液涂布到基材表面的步骤(步骤S4)；以及通过对金属微粒分散液的涂膜进行烧结来形成金属覆膜的步骤(步骤S5)。
<金属微粒产生步骤>
通过液相还原法实施金属微粒产生步骤S1，在所述液相还原法中，通过在含有还原剂的水溶液中将金属离子还原而使金属微粒析出。例如，可以采用钛氧化还原法作为这样的液相还原法。
构成金属微粒的金属的实例包括铜、镍、金和银。其中，铜因其良好的导电性和相对低的成本而是优选的。
金属微粒产生步骤S1包括制备还原剂的水溶液的步骤(还原剂水溶液制备步骤)和通过金属离子的还原使金属微粒析出的步骤(金属微粒析出步骤)。在金属微粒析出步骤中，将含有金属离子的水溶液或通过电离产生金属离子的水溶性金属化合物添加到还原剂水溶液中，从而还原金属离子并使金属微粒析出。
[还原剂水溶液制备步骤]
在还原剂水溶液制备步骤中，制备含有具有金属离子还原作用的还原剂的水溶液。
(还原剂)
可以将能够在液相反应体系中通过还原金属元素的离子而使金属微粒析出的各种还原剂中的任意一种用作还原剂。还原剂的实例包括硼氢化钠、次磷酸钠、肼和过渡金属元素的离子(三价钛离子、二价钴离子等)。为了尽可能降低要析出的金属微粒的粒径，减小金属元素的离子的还原速率和减小金属微粒的析出速率是有效的。为了减小还原速率和析出速率，优选选择使用具有尽可能低的还原能力的还原剂。
当采用钛氧化还原法作为液相还原法时，将三价钛离子用作还原剂。通过将在水中能够产生三价钛离子的水溶性钛化合物溶解或通过利用阴极电解将含有四价钛离子的水溶液还原，得到三价钛离子。能够产生三价钛离子的水溶性钛化合物的实例为三氯化钛。可以将市售高浓度的三氯化钛水溶液用作这种三氯化钛。
还原剂水溶液可以还包含络合剂、分散剂、pH调节剂等。
可以将本领域内已知的各种络合剂用作添加到还原剂水溶液的络合剂。为了制造具有尽可能小的粒径和尽可能尖的粒度分布(尽可能窄的粒度分布)的金属微粒，在通过三价钛离子的氧化而将金属元素的离子还原并析出时尽可能地缩短还原反应所花费的时长是有效的。为了实现该目的，控制三价钛离子的氧化反应速率和金属元素离子的还原反应速率两者是有效的；为此，形成三价钛离子和金属元素离子两者的络合物是重要的。而且，为了在将金属元素离子的还原速率和金属微粒的析出速率调节至合适速率的同时尽可能地缩短还原反应所花费的时间，对离子浓度等进行调节是重要的。
具有这样的功能的络合剂的实例包括柠檬酸三钠(Na3C6H5O7)、酒石酸钠(Na2C4H4O6)、乙酸钠(NaCH3CO2)、葡萄糖酸(C6H12O7)、硫代硫酸钠(Na2S2O3)、氨(NH3)和乙二胺四乙酸(C10H16N2O8)。可以使用这些物质中的任意一种或它们的组合。其中，优选柠檬酸三钠。
可以将具有各种结构的分散剂如阴离子性分散剂、阳离子性分散剂和非离子性分散剂用作添加到还原剂水溶液中的分散剂。其中，优选阳离子性分散剂且更优选具有聚乙撑亚胺结构的阳离子性分散剂。
添加到还原剂水溶液中的pH调节剂的实例包括碳酸钠、氨和氢氧化钠。还原剂水溶液的pH可以例如为5以上且13以下。当还原剂水溶液的pH低时，金属微粒的析出速率减小且金属微粒的粒径减小。在极低析出速率下，粒度分布变宽。因此优选以不过度减小析出速率的方式调节pH。当还原剂水溶液的pH过高时，金属微粒的析出速率过度增大且析出的金属微粒可能会团聚而形成簇状或链状的粗大粒子。
[金属微粒析出步骤]
在金属微粒析出步骤中，将金属离子添加到还原剂水溶液中以通过用还原剂水溶液中的还原剂还原金属离子而引起金属微粒的析出。
(金属离子)
通过将水溶性金属化合物溶于水中、并因水溶性金属化合物的电离而形成金属离子。水溶性金属化合物的实例包括各种水溶性化合物如硫酸盐化合物、硝酸盐化合物、乙酸盐化合物和氯化物。
水溶性金属化合物的具体实例包括：铜化合物如硝酸铜(II)(Cu(NO3)2)、三水合硝酸铜(II)(Cu(NO3)2·3H2O)、五水合硫酸铜(II)(CuSO4·5H2O)、氯化铜(II)(CuCl2)；镍化合物如六水合氯化镍(II)(NiCl2·6H2O)和六水合硝酸镍(II)(Ni(NO3)2·6H2O)；金化合物如四水合四氯金(III)酸(HAuCl4·4H2O)；和银化合物如硝酸银(I)(AgNO3)和甲烷磺酸银(CH3SO3Ag)。
如果将水溶性金属化合物直接添加到还原剂水溶液中，则首先在添加的化合物周围局部地进行反应，这样金属微粒的粒径变得不均匀并且粒度分布可能变宽。因此，优选将水溶性金属化合物溶解在水中以制备含有金属离子的稀释水溶液并且优选将该水溶液添加到还原剂水溶液中。
优选析出的金属微粒的平均粒径的上限为200nm且更优选为150nm。优选金属微粒的平均粒径的下限为1nm且更优选为10nm。当金属微粒的平均粒径超过上述上限时，在得到的金属覆膜中形成的空隙变得较大且不能获得足够的导电性。当金属微粒的平均粒径低于所述下限时，在金属微粒分离步骤S2中的分离效率可能降低或者在金属微粒分散液制备步骤S3中金属微粒可能不易均匀地分散在溶剂中。
<金属微粒分离步骤>
在金属微粒分离步骤S2中，将在金属微粒析出步骤S1中在还原剂水溶液中析出的金属微粒分离。用于分离金属微粒的方法的实例包括过滤和离心分离。分离的金属微粒可以通过洗涤、干燥、粉碎等步骤制备成粉末，但是优选以其分散在水溶液中的形式使用而不形成粉末以防止团聚。
<金属微粒分散液制备步骤>
在金属微粒分散液制备步骤S3中，将在金属微粒分离步骤中从还原剂水溶液分离的金属微粒分散在溶剂中以制备金属微粒分散液。
(溶剂)
将水与一种以上高极性溶剂的混合物用作金属微粒分散液的溶剂。特别地，优选使用水和与水混溶的高极性溶剂的混合物。这样的金属微粒分散液的溶剂可以由析出金属微粒之后的还原剂水溶液制备。即，预先对含有金属微粒的还原剂水溶液进行诸如超滤、离心分离、水洗、电渗析等处理以除去杂质，然后向其中添加高极性溶剂以得到包含特定量的金属微粒的溶剂。
优选高极性溶剂为可以在烧结步骤S5中在短时间内蒸发的挥发性有机溶剂。当将挥发性有机溶剂用作高极性溶剂时，高极性溶剂在烧结步骤S5中在短时间内蒸发并且涂布到基材表面的金属微粒分散液的粘度可以快速增大而不会引起金属微粒的移动。
可以将在室温(5℃以上且35℃以下)下蒸发的各种有机溶剂中的任意一种用作该挥发性有机溶剂。其中，优选在大气压下具有例如60℃以上且140℃以下的沸点的挥发性有机溶剂并且优选具有高挥发性和与水的良好混溶性且包含1～5个碳原子的脂肪族饱和醇。包含1～5个碳原子的脂肪族饱和醇的实例包括甲醇、乙醇、正丙醇、异丙醇、正丁醇、异丁醇、仲丁醇、叔丁醇、正戊醇和异戊醇，这些可以单独使用或以组合的方式使用。
在全部溶剂中挥发性有机溶剂的含量的下限优选为10质量％且更优选为15质量％。在全部溶剂中挥发性有机溶剂的含量的上限优选为80质量％且更优选为70质量％。当在全部溶剂中挥发性有机溶剂的含量低于所述下限时，在烧结步骤S5期间金属微粒分散液的粘度可能不会在短时间内增大。当全部溶剂中的挥发性有机溶剂的含量超过所述上限时，水含量相对降低，这样金属微粒分散液对各种基材如玻璃、陶瓷和塑料基材的表面的润湿性可能变得不足。
相对于100质量份的金属微粒，金属微粒分散液中总溶剂含量的下限优选为100质量份且更优选为250质量份。相对于100质量份的金属微粒，金属微粒分散液中总溶剂含量的上限优选为3000质量份且更优选为1000质量份。当金属微粒分散液中总溶剂含量低于所述下限时，金属微粒分散液的粘度增大且在涂布步骤S4中分散液的顺利涂布可能变得困难。当金属微粒分散液中总溶剂含量超过所述上限时，金属微粒分散液的粘度减小且在涂布步骤S4中可能不能形成足够厚度的涂膜。
(水溶性树脂)
水溶性树脂在烧结步骤S5中在涂膜的干燥和烧结期间起到防止金属微粒移动的粘结剂的作用。由于水溶性树脂逐渐热解，所以金属微粒的烧结缓慢进行。由此，阻止金属覆膜破裂。
水溶性树脂的数均分子量的下限优选为1000且更优选为5000。水溶性树脂的数均分子量的上限优选为1000000且更优选为500000。当水溶性树脂的数均分子量低于所述下限时，在烧结步骤S5中水溶性树脂不合需要地快速热解，不能充分抑制金属微粒的移动，并且金属覆膜可能破裂。当水溶性树脂的数均分子量超过所述上限时，在烧结步骤S5中水溶性树脂不完全热解，水溶性树脂的残余物可能残留在金属覆膜中，并且金属覆膜的导电性可能会降低。
水溶性树脂的实例包括聚乙烯醇、聚乙二醇、甲基纤维素、聚乙撑亚胺和聚乙烯基吡咯烷酮。其中，优选单独或组合使用能够有效抑制涂膜的体积变化和相对容易热解的聚乙烯醇、聚乙二醇和聚乙撑亚胺。由于聚乙烯醇和聚乙二醇具有高极性，所以它们在水中具有优异的分散性。聚乙撑亚胺适合作为金属微粒的包覆材料并且与金属微粒具有高的相容性。因此，水溶性树脂特别优选为聚乙撑亚胺与选自聚乙烯醇和聚乙二醇中的至少一种的组合。
相对于100质量份的金属微粒，金属微粒分散液中水溶性树脂的含量的下限优选为0.1质量份且更优选为0.2质量份。相对于100质量份的金属微粒，金属微粒分散液中水溶性树脂的含量的上限优选为10质量份，更优选为2质量份，且进一步优选为1质量份。如果水溶性树脂的量低于所述下限，则水溶性树脂不能充分地起到粘结剂的作用且得到的金属覆膜可能破裂或收缩。当水溶性树脂的含量超过所述上限时，水溶性树脂的热解残余物作为杂质残留在金属覆膜中，因此金属覆膜的导电性可能降低。
<涂布步骤>
在涂布步骤S4中，将金属微粒分散液涂布到基材的表面。可以采用已知的涂布金属微粒分散液的方法，其实例包括旋涂法、喷涂法、刮棒涂布法、模缝涂布法、狭缝涂布法、辊涂法和浸涂法。或者，可以通过丝网印刷、通过使用分配器等将金属微粒分散液仅涂布到基材的一部分。
<烧结步骤>
在烧结步骤S5中，将在涂布步骤S4中形成的金属微粒分散液的涂膜加热以蒸发金属微粒分散液中的溶剂，然后对通过起到粘结剂作用的水溶性树脂保持在一起的金属微粒进行烧结。在对金属微粒进行烧结期间，将金属微粒保持在一起的水溶性树脂热解，因此仅对金属微粒进行烧结且形成不含任何有机物质的金属覆膜。
该烧结步骤中的加热温度取决于金属微粒的原料等，例如为150℃以上且500℃以下。
如上所述，根据图1中所示的金属覆膜的制造方法，在金属微粒分散液制备步骤S3中得到金属微粒分散液，所述金属微粒分散液用于通过涂布和烧结形成金属覆膜并且包含具有200nm以下平均粒径的金属微粒、用于分散金属微粒的溶剂、以及另外的水溶性树脂。通过在步骤S4中涂布该金属微粒分散液并在步骤S5中对涂布的金属微粒分散液进行烧结形成金属覆膜。
[优势]
由于本发明实施方案的金属微粒分散液包含上述量的水溶性树脂，所以在对金属微粒分散液的涂膜进行干燥(溶剂蒸发)期间水溶性树脂缓和涂膜的收缩，并且在随后的烧结金属微粒的步骤中，随水溶性树脂逐渐热解，烧结缓慢进行。由此，通过使用本发明实施方案的金属微粒分散液可以形成具有较少裂纹的金属覆膜。结果，可以更容易地在通过使用金属微粒分散液形成的金属覆膜上形成其它材料的层，特别是金属镀层。
[其它实施方案]
本文中公开的所有实施方案在各个方面都仅是示例性的并且不应认为是限制性的。本发明的范围不限于上述实施方案的特征，而是仅由权利要求书限定，并且在权利要求书及其等价物的含义和范围内的所有变体和替代都旨在包括在本发明的范围内。
金属微粒可以通过液相还原法以外的各种已知方法中的任意一种来制造，所述已知方法例如为被称为浸渍法的高温处理法、和气相法。然而，由于获得尺寸小且具有均匀粒子形状和尺寸的金属微粒，所以液相还原法是优选的。
通过在经由液相还原法使金属微粒析出之后从还原剂水溶液中除去杂质，浓缩得到的水溶液以降低水含量，并且根据需要向得到的浓缩溶液添加高极性溶剂，可以制造金属微粒分散液。当将通过在使金属微粒析出之后对还原剂水溶液进行调节和浓缩而制备的溶剂用作所述溶剂时，可以抑制金属微粒的团聚。除了对还原剂水溶液进行浓缩以外，如果需要可以进一步添加金属微粒。
实施例
现在将通过使用实施例对本发明进行说明。实施例的说明不限制本发明的解释。
通过经由上述实施方案的液相还原法还原铜离子而形成铜微粒并对其进行分离。通过使用分离的铜微粒制备金属微粒分散液。铜微粒的平均粒径为50nm。
相对于100质量份的铜微粒，将200质量份的水和50质量份的乙醇(乙基醇)的混合物用作金属微粒分散液的溶剂。将铜微粒分散在该溶剂中以得到1号金属微粒分散液。
向1号金属微粒分散液中，添加通过在相对于100质量份的铜微粒为49质量份的水中溶解相对于100质量份的铜微粒为1质量份的聚乙烯醇而预先制备的溶液作为金属微粒分散液的水溶性树脂。结果，得到2号金属微粒分散液。
将通过这样获得的各种金属微粒分散液涂布到聚酰亚胺膜上至平均厚度为0.5μm并且在350℃下在氮气气氛中对涂布的分散液进行烧结以在聚酰亚胺膜上形成金属覆膜。
用扫描电子显微镜观察金属覆膜的表面。观察发现，通过使用1号金属微粒分散液形成的金属覆膜具有许多长度为1μm以上的裂纹，而通过使用2号金属微粒分散液形成的金属覆膜基本上没有长度为1μm以上的裂纹。
该结果证实，向金属微粒分散液中添加水溶性树脂有效地抑制了金属覆膜中裂纹的形成。
对各个金属覆膜进行无电镀铜以形成平均总厚度为1μm的复合合金覆膜。测定复合合金覆膜的剥离强度以评价金属覆膜对聚酰亚胺膜的粘接强度。根据JIS-C-6481(1996)测定剥离强度。
结果显示，通过使用1号金属微粒分散液形成的金属覆膜对聚酰亚胺膜的粘接强度为150gf/cm，通过使用2号金属微粒分散液形成的金属覆膜对聚酰亚胺膜的粘接强度为500gf/cm。
该结果证实，向金属微粒分散液中添加水溶性树脂提高了金属覆膜对基材的粘接强度。
还公开了以下附记。
(附记1)
一种金属微粒分散液，其包含具有200nm以下平均粒径的金属微粒、用于分散所述金属微粒的溶剂和水溶性树脂。
由于金属微粒分散液除了金属微粒和溶剂以外还包含水溶性树脂，所以在对涂膜进行干燥(溶剂蒸发)期间水溶性树脂缓和金属微粒分散液的涂膜的收缩。由于水溶性树脂在金属微粒的烧结期间逐渐热解，所以烧结缓慢进行。由此，通过使用该金属微粒分散液可以形成具有较少裂纹的金属覆膜。
产业实用性
本发明可以广泛应用于金属覆膜的形成并且特别适合于制造诸如印刷电路板的电子部件。
标号说明
S1 金属微粒产生步骤
S2 金属微粒分离步骤
S3 金属微粒制备步骤
S4 涂布步骤
S5 烧结步骤

Claims (6)

1.一种金属微粒分散液，所述金属微粒分散液用于通过涂布和烧结形成金属覆膜，所述金属微粒分散液包含具有200nm以下平均粒径的金属微粒和用于分散所述金属微粒的溶剂，其中，
所述金属微粒分散液还包含水溶性树脂。
2.根据权利要求1所述的金属微粒分散液，其中，
相对于100质量份的所述金属微粒，所述水溶性树脂的含量为0.1质量份以上且10质量份以下。
3.根据权利要求1或2所述的金属微粒分散液，其中，
所述水溶性树脂的数均分子量为1000以上且1000000以下。
4.根据权利要求1～3中任一项所述的金属微粒分散液，其中，
所述水溶性树脂为聚乙烯醇、聚乙二醇和聚乙撑亚胺中的任意一种或它们的组合。
5.根据权利要求1～4中任一项所述的金属微粒分散液，其中，
所述金属微粒包含铜。
6.一种金属覆膜，其通过涂布权利要求1～5中任一项所述的金属微粒分散液并对涂布的金属微粒分散液进行烧结而形成。
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