CN104303243A - 导电膜形成方法和烧结助剂 - Google Patents
导电膜形成方法和烧结助剂 Download PDFInfo
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Abstract
在使用光烧结的导电膜形成方法中，容易地形成具有低电阻的导电膜。该导电膜形成方法是其中使用光烧结形成导电膜5的方法。该方法包括以下步骤：在基板上形成由烧结助剂2制成的层22，在烧结助剂2的层22上形成由铜颗粒分散体制成的液体膜3，将该液体膜3干燥以形成铜颗粒层4，并对该铜颗粒层4施以光烧结。烧结助剂2是从金属铜中除去氧化铜的化合物。由此，烧结助剂2在光烧结中除去铜颗粒31的表面氧化物膜。
Description
技术领域
本发明涉及使用光烧结的导电膜形成方法，以及使得光烧结能够在所述导电膜形成方法中进行的烧结助剂。
背景技术
迄今为止，存在其中在基板上通过光刻法形成由铜箔组成的电路的印刷电路板。光刻法需要蚀刻铜箔的步骤，处理蚀刻等产生的废液需要高昂的成本。
作为无需蚀刻的技术，以下方法是已知的：其中，使用含有分散在分散媒介中的铜颗粒(铜纳米粒子)的铜颗粒分散体(铜墨水)在基板上形成导电膜(参见例如专利文献1)。根据这种方法，在基板上形成铜颗粒分散体的液体膜，并将该液体膜干燥以形成铜颗粒层。该铜颗粒层通过光照经受光烧结，由此形成具有低电阻的导电膜。
但是，在上述方法中，光烧结可能不充分，即使光烧结中照射的光的能量很大，由此无法形成具有低电阻的导电膜。
现有技术文献
专利文献1：美国专利申请第2008/0286488号
发明内容
本发明所要解决的问题
提出本发明以解决上述问题，其目的在于在使用光烧结的导电膜形成方法中容易地形成具有低电阻的导电膜。
解决问题的手段
本发明的导电膜形成方法是其中使用光烧结形成导电膜的方法，其特征在于包括以下步骤：在基板上形成由烧结助剂制成的层，在烧结助剂层上形成由铜颗粒分散体制成的液体膜，将该液体膜干燥以形成铜颗粒层，并对该铜颗粒层施以光烧结，所述烧结助剂是从金属铜中除去氧化铜的化合物。
在该导电膜形成方法中，烧结助剂优选选自酰胺类、酰亚胺类、酮类、氨基甲酸酯类、硫醚类、羧酸类和磷酸类。
在该导电膜形成方法中，烧结助剂优选选自聚乙烯吡咯烷酮、聚酰胺酰亚胺树脂、聚氨酯树脂、聚苯硫醚树脂和羟基亚乙基二膦酸。
在该导电膜形成方法中，烧结助剂可以选自醇类、糖类、醛类、肼类、醌类、酚类和胺类。
在该导电膜形成方法中，烧结助剂可以选自聚乙烯醇、氢醌和硅烷偶联剂。
本发明的烧结助剂用于上述导电膜形成方法。
本发明的优点
根据本发明，由于烧结助剂在光烧结中除去铜颗粒的表面氧化物膜，已经从其上除去表面氧化物膜的铜颗粒被烧结，并且铜颗粒层发生块化(bulking)，由此容易地形成具有低电阻的导电膜。
附图说明
图1(a)至1(f)是以时间顺序显示通过本发明的实施方式的导电膜形成方法形成导电膜的横截面示意图。
具体实施方式
将参照图1(a)至1(f)描述根据本发明的一个实施方式的导电膜形成方法。如图1(a)和1(b)所示，在基板1上施加含有烧结助剂2的溶液21。如图1(c)所示，将溶液21的溶剂干燥以形成由烧结助剂2制成的层22。
通过将基底材料成型为板形来获得基板1。基底材料的实例包括，但不限于，玻璃、树脂、陶瓷、硅片等。
烧结助剂2是从金属铜中除去氧化铜的化合物。烧结助剂2可以是例如酰胺类、酰亚胺类、酮类、氨基甲酸酯类、硫醚类、羧酸类或磷酸类，其实例包括但不限于：酰胺类中的聚乙烯吡咯烷酮、酰亚胺类中的聚酰胺酰亚胺树脂、氨基甲酸酯类中的聚氨酯树脂、硫醚类中的聚苯硫醚树脂、和磷酸类中的羟基亚乙基二膦酸。可以认为，此类烧结助剂2通过蚀刻从金属铜中除去氧化铜。
烧结助剂2可以是醇类、糖类、醛类、肼类、醌类、酚类或胺类，其实例包括但不限于：醇类中的聚乙烯醇、醌类中的氢醌和胺类中的硅烷偶联剂等。此类烧结助剂2通过还原氧化铜从金属铜中除去氧化铜。
这些烧结助剂2可以单独使用，或者两种或多种类型的烧结助剂可以适当地混合和使用。
如图1(d)所示，由铜颗粒分散体制成的液体膜3在烧结助剂2的层22上形成。铜颗粒分散体是含有分散在其中的铜颗粒31的液体，并包括铜颗粒31、分散媒介和分散剂。铜颗粒31是例如，具有1nm或更大且小于100nm的中值粒径的铜纳米粒子。分散媒介是含有铜颗粒31的液体媒介。分散剂使得铜颗粒31能够分散在分散媒介中。由于粒子表面被空气中的氧气氧化，铜颗粒31覆有薄的表面氧化物膜。
例如通过印刷法形成液体膜3。在印刷法中，铜颗粒分散体用作印刷墨水，在烧结助剂2的层22上印刷预先确定的图案，并形成具有该图案的液体膜3。由于铜颗粒分散体用作墨水，其也称为铜墨水。烧结助剂2通过与液体膜3接触而洗提到液体膜3中。
接着，将液体膜3干燥。如图1(e)所示，通过干燥液体膜3以便在基板1上形成由铜颗粒31组成的铜颗粒层4，由此使铜颗粒31和烧结助剂2保留在基板1上。铜颗粒层4中的铜颗粒31的表面与烧结助剂2接触。在图1(e)中，省略了对烧结助剂2的图示。
接着，用光照射铜颗粒层4，并对铜颗粒层4施以光烧结。在室温下在大气空气下进行光烧结。用于光烧结的光源是例如氙灯。激光装置可用作光源。在光烧结中，除去铜颗粒31的表面氧化物膜，并将铜颗粒31烧结，铜颗粒层4经受块化。如图1(f)所示，铜颗粒层4经受块化以形成导电膜5。
迄今为止，已经考虑过，通过光烧结中的光能量造成的光还原反应将铜颗粒31的表面氧化物膜还原为铜并随后除去。
但是，根据本发明的发明人进行的试验，取决于铜颗粒分散体，铜颗粒层4可能经受不充分的块化，即使光烧结中照射的光的能量较大。由于照射在铜颗粒层4上的过大的光能量可能造成铜颗粒层4的破坏，对于光烧结中照射的光能量的量级存在限制。本发明的发明人考虑了存在某些情况，在这些情况中，仅通过光的能量不能充分去除铜颗粒31的表面氧化物膜，由此无法充分进行光烧结，导致铜颗粒层4的不充分块化。
本发明的发明人通过实验已经发现，通过使用从金属铜中除去氧化铜的化合物，能够进行光烧结。在本实施方式的导电膜形成方法中，烧结助剂2是从金属铜中除去氧化铜，并除去铜颗粒31的表面氧化物膜的化合物。对铜颗粒层4的光照射促进了其中烧结助剂2使得能够从铜颗粒31中除去氧化铜的化学反应。已经从其上除去表面氧化物膜的铜颗粒31被光的能量烧结，由此铜颗粒层4经受块化以形成具有导电性的导电膜5。
如上所述，根据本实施方式的导电膜形成方法，由于烧结助剂2能够在光烧结中除去铜颗粒31的表面氧化物膜，已经从其上除去表面氧化物膜的铜颗粒31被烧结，且铜颗粒层4经受块化，由此容易地形成具有低电阻的导电膜5。
在烧结助剂2能够蚀刻氧化铜的情况下，通过蚀刻除去铜颗粒31的表面氧化物膜。
在烧结助剂2能够还原氧化铜的情况下，通过还原除去铜颗粒31的表面氧化物膜。
在实施例中，使用本发明的导电膜形成方法形成导电膜5，并测量由此形成的导电膜5的电阻。
[实施例1]
无碱玻璃用作基板1。使用酰胺类如聚乙烯吡咯烷酮(分子量为630,000)作为烧结助剂2，并使用水作为溶剂，制备含有烧结助剂2的溶液。将烧结助剂2的浓度调节至10％。通过旋涂法将该溶液以预定厚度涂覆在基板1上。为了干燥溶液中的溶剂，涂有该溶液的基板1在大气空气中在100℃至250℃干燥30分钟以形成烧结助剂层22。通过旋涂法将铜颗粒分散体(由ISHIHARA CHEMICAL CO.,LTD.制造，商品名“CJ-0104”)以预定厚度涂覆在烧结助剂层22上。涂有铜颗粒分散体的基板1在大气空气中在100℃干燥30分钟，随后用具有氙灯的闪照射装置施以光烧结以制造样品基板。在0.5J/cm2至30J/cm2范围内的能量级下进行光烧结中的光照射0.1ms至10ms。铜颗粒层4在光烧结前呈黑色。在通过单次光照射进行的光烧结之后，表面的颜色变为铜色。该铜色是块状铜的颜色，从光烧结造成的颜色变化可以发现铜颗粒层4经受块化以形成导电膜5。无需进行超过一次的光照射。测试基板上的导电膜5的薄层电阻显示出200mΩ/□的低值。
[实施例2]
使用酰胺酰亚胺类中的聚酰胺酰亚胺树脂作为烧结助剂2，并使用碳酸丙烯酯作为溶剂，制备含有烧结助剂2的溶液。将烧结助剂2的浓度调节至10％。除上述之外，以与实施例1相同的方式制造测试基板。该铜颗粒层4在光烧结前呈黑色。在通过单次光照射进行的光烧结之后，表面的颜色变为铜色。测试基板上的导电膜5的薄层电阻显示出280mΩ/□的低值。
[实施例3]
使用胺类中的硅烷偶联剂(3-氨基丙基三乙氧基硅烷)作为烧结助剂2，并使用水作为溶剂，制备含有烧结助剂2的溶液。将烧结助剂2的浓度调节至1％。除上述之外，以与实施例2相同的方式制造测试基板。该铜颗粒层4在光烧结前呈黑色。在通过单次光照射进行的光烧结之后，表面的颜色变为铜色。测试基板上的导电膜5的薄层电阻显示为200mΩ/□。
[实施例4]
使用另一种硅烷偶联剂(N-2-(氨基乙基)-3-氨基丙基三乙氧基硅烷)作为烧结助剂2，并使用水作为溶剂，制备含有烧结助剂2的溶液。将烧结助剂2的浓度调节至1％。除上述之外，以与实施例3相同的方式制造测试基板。该铜颗粒层4在光烧结前呈黑色。在通过单次光照射进行的光烧结之后，表面的颜色变为铜色。测试基板上的导电膜5的薄层电阻显示为200mΩ/□。
[实施例5]
使用醇类中的聚乙烯醇(分子量为2,000)作为烧结助剂2，并使用水作为溶剂，制备含有烧结助剂2的溶液。将烧结助剂2的浓度调节至10％。除上述之外，以与实施例4相同的方式制造测试基板。该铜颗粒层4在光烧结前呈黑色。在通过单次光照射进行的光烧结之后，表面的颜色变为铜色。测试基板上的导电膜5的薄层电阻显示为300mΩ/□。
[实施例6]
使用氨基甲酸酯类中的聚氨酯树脂作为烧结助剂2，并使用碳酸丙烯酯作为溶剂，制备含有烧结助剂2的溶液。将烧结助剂2的浓度调节至35％。除上述之外，以与实施例5相同的方式制造测试基板。该铜颗粒层4在光烧结前呈黑色。在通过单次光照射进行的光烧结之后，表面的颜色变为铜色。测试基板上的导电膜5的薄层电阻显示为250mΩ/□。
[实施例7]
使用硫醚类中的聚苯硫醚树脂作为烧结助剂2，并使用2-丙醇作为溶剂，制备含有烧结助剂2的溶液(分散体)。将烧结助剂2的浓度调节至1％。除上述之外，以与实施例6相同的方式制造测试基板。该铜颗粒层4在光烧结前呈黑色。在通过单次光照射进行的光烧结之后，表面的颜色变为铜色。测试基板上的导电膜5的薄层电阻显示为170mΩ/□。
[实施例8]
使用磷酸类中的羟基亚乙基二膦酸作为烧结助剂2，并使用水作为溶剂，制备含有烧结助剂2的溶液。将烧结助剂2的浓度调节至49％。除上述之外，以与实施例7相同的方式制造测试基板。该铜颗粒层4在光烧结前呈黑色。在通过单次光照射进行的光烧结之后，表面的颜色变为铜色。测试基板上的导电膜5的薄层电阻显示为150mΩ/□。
[实施例9]
使用醌类中的氢醌作为烧结助剂2，并使用碳酸丙烯酯作为溶剂，制备含有烧结助剂2的溶液。将烧结助剂2的浓度调节至10％。除上述之外，以与实施例8相同的方式制造测试基板。该铜颗粒层4在光烧结前呈黑色。在通过单次光照射进行的光烧结之后，表面的颜色变为铜色。测试基板上的导电膜5的薄层电阻显示为300mΩ/□。
如上所述，使用烧结助剂2能够形成具有低电阻的导电膜5。
本发明不限于上述实施方式的配置，可以在不背离本发明的精神或范围的情况下进行各种修改。例如，基板1的表面形状不限于平面，可以是弯曲表面或多个平面的组合。
符号说明
1：基板
2：烧结助剂
3：液体膜
31：铜颗粒
4：铜颗粒层
5：导电膜
Claims (6)
1.一种导电膜形成方法，其中使用光烧结形成导电膜，其包括以下步骤：
在基板上形成由烧结助剂制成的层，
在烧结助剂的层上形成由铜颗粒分散体制成的液体膜，
将所述液体膜干燥以形成铜颗粒层，并
对所述铜颗粒层施以光烧结，其中
所述烧结助剂是从金属铜中除去氧化铜的化合物。
2.根据权利要求1所述的导电膜形成方法，其中所述烧结助剂选自酰胺类、酰亚胺类、酮类、氨基甲酸酯类、硫醚类、羧酸类和磷酸类。
3.根据权利要求2所述的导电膜形成方法，其中所述烧结助剂选自聚乙烯吡咯烷酮、聚酰胺酰亚胺树脂、聚氨酯树脂、聚苯硫醚树脂和羟基亚乙基二膦酸。
4.根据权利要求1所述的导电膜形成方法，其中所述烧结助剂选自醇类、糖类、醛类、肼类、醌类、酚类和胺类。
5.根据权利要求4所述的导电膜形成方法，其中所述烧结助剂选自聚乙烯醇、氢醌和硅烷偶联剂。
6.一种烧结助剂，其用于根据权利要求1至5中任一项所述的导电膜形成方法。
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| KR101785350B1 (ko) * | 2014-07-18 | 2017-10-17 | 한국화학연구원 | 광소결을 이용한 전도성 금속박막의 제조방법 |
| JP2018003068A (ja) * | 2016-06-29 | 2018-01-11 | Dic株式会社 | 金属ナノ粒子焼結膜の製造方法 |
| WO2019189251A1 (ja) * | 2018-03-28 | 2019-10-03 | 三井金属鉱業株式会社 | 導電膜形成用組成物及び導電膜の製造方法 |
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