CN109979904A - 一种多尺寸纳米颗粒混合金属膜及其制备方法 - Google Patents
一种多尺寸纳米颗粒混合金属膜及其制备方法 Download PDFInfo
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Abstract
本发明提供一种多尺寸纳米颗粒混合膜及其制备方法,包括形成有机包覆层的有机介质材料,所述有机介质材料中配置至少两种尺寸的纳米金属颗粒;通过在大尺寸纳米金属颗粒的间隙中用物理冲击方式打入小尺寸纳米金属颗粒,实现大尺寸纳米铜颗粒间的空隙填充,所述纳米金属颗粒优选使用纳米铜材料,避免现有复合银膜高孔隙率、低热导率、高成本、与Si、SiC基芯片热失配、高电迁移率等问题,提高功率器件整体可靠性性能,同时具备易于装配的特点,可有效降低成本。
Description
技术领域
本发明涉及芯片封装互连领域,更具体地涉及烧结用金属膜及其制备技术。
背景技术
在功率半导体封装领域,寻求低温工艺、高温服役、热膨胀系数相匹配、高导热导电、低成本的互连材料成为现在急需解决的问题。以焊接及引线键合的传统材料工艺存在熔点低、高温蠕变失效、引线缠绕、寄生参数等无法解决的问题,新型互连材料正从焊接向烧结技术发展。通过减小烧结颗粒的尺寸,降低烧结温度,纳米金属颗粒烧结技术已经成为功率半导体器件新型互连材料中最有前景的技术。
目前以纳米银烧结为代表的先进工艺已逐渐成为功率半导体器件封装互连的主流,国内外主要封装应用厂商已进入实用化和规模化使用中。然而纳米银烧结专利、材料、工艺及设备主要由国外厂商控制,在国内的发展受到较大限制。同时纳米银烧结技术也存在不足:1)银材料本身价格较高,限制其不能被广泛使用。2)银和SiC芯片背面材料热膨胀系数的不同,需要添加其它中间金属层提高互连性能,从而增加了工艺复杂性和成本。3)银层存在电迁移现象,不利于功率器件长期可靠应用。与纳米银近似的纳米铜颗粒可以在低温条件下熔融,烧结后熔点接近铜单质材料(1083℃),可构筑稳定的金属互连层。其单组分金属的特性,避免了合金材料热循环效应下的服役可靠性问题,实现铜铜键合,解决芯片和基板之间热膨胀系数匹配的问题,同时避免电迁移现象导致可靠性问题。对比纳米银颗粒,有效降低互连封装的材料和加工成本。更重要的是能够从芯片封装应用领域,进一步推进“全铜化”(All copper)理念的实际应用和产业化,推动半导体产业的创新发展。
专利文献CN103262172A,其公开了一种烧结材料和烧结材料制备的薄层,以及该材料的附着方法,薄层是由金属粉末、焊膏、粘合剂和溶剂组成。其中金属粉末包括金、钯、银、铜、铝、银钯合金或者金钯合金,可进一步包括一种或更多的功能性添加物。金属粉末包括纳米颗粒。金属粉末被适用到基片上,对基片上的材料进行干燥形成薄层。基片材料包括聚酯纤维,该现有技术的缺点在于基片上的纳米金属层成分尺寸单一,由此造成烧结后孔隙率较大,导电导热效果差等后果。
专利文献CN105492198A,其公开了一种用于电气部件和机械部件的复合和多层银膜,其中在可烧结银层中加入了增强颗粒或纤维,以提高其强度。然而该现有技术的问题的多层银膜的纳米银烧结材料存在诸多不足:1)银材料本身价格较高,限制其不能被广泛使用。2)银和SiC芯片背面材料热膨胀系数的不同,需要添加其它中间金属层提高互连性能,从而增加了工艺复杂性和成本。3)银层存在电迁移现象,不利于功率器件长期可靠应用。
专利文献CN107705869A,其公开了一种导电材料、打印墨水以及导电结构的制备方法。该导电材料是由多个导电金属纳米片和填充在所述多个导电金属纳米片之间的间隙中的导电金属纳米颗粒制成,可以提高烧接后致密度。然而,一方面该文献所述材料混合是在墨水制备之前,在后续保存中,纳米颗粒有团聚风险。
本发明解决的技术问题在于提供一种多尺寸纳米颗粒混合金属膜的快速、高效、简易的制备方法。利用金属膜可省略在应用端印刷干燥、步骤,直接用于电气互连的可烧结;由该方法制备的金属膜,可以方便准确的控制大小尺寸纳米铜颗粒混合比例,避免现有复合金属膜高孔隙率、低热导率、高成本、与Si基芯片热失配、高电迁移率等问题,提高功率器件整体可靠性性能,同时具备易于装配、低烧结温度的特点,可有效降低成本。
发明内容
本发明提供一种多尺寸纳米颗粒混合金属膜,包括:
有机介质材料,形成有机包覆层;
所述有机介质材料中配置至少两种尺寸的纳米金属颗粒;
用物理冲击方式将小尺寸纳米金属颗粒打入大尺寸纳米金属颗粒的空隙,通过设定物理冲击参数控制打入的小尺寸纳米金属颗粒量。
优选的,所述物理冲击方式为:施加在小尺寸纳米金属颗粒上的电场、磁场、气流或其组合。
优选的,所述纳米金属颗粒的金属为金、钯、银、铜、铝、银钯合金、金钯合金、铜银合金、铜银镍合金或铜铝合金。
优选的,所述纳米金属颗粒的金属膜为纳米铜膜。
优选的,所述大尺寸纳米金属颗粒是颗粒直径在1nm<D<10um的纳米金属铜颗粒,所述小尺寸纳米金属颗粒是颗粒直径在0.5nm<d<20nm的小尺寸纳米金属铜颗粒。
优选的,所述金属膜烧结前厚度为10微米至200微米。
优选的,所述大尺寸纳米金属颗粒和所述小尺寸纳米金属颗粒的形状是球型、纤维状、片状、雪花状和/或线状。
优选的,所述金属膜还包括支撑基材,其中支撑基材包括有机硅涂覆的聚酯纤维、陶瓷、玻璃和/或金属材料;
所述支撑基材包括带式、片式、板式结构;
所述带式支撑基材,在制备好金属膜后,可以收纳为成一卷。
优选的,所述支撑基材和纳米颗粒接触的一面具有有机硅涂覆。
优选的,介质材料包括有机溶剂、助焊剂、焊膏、和/或粘合剂。
一种单层多尺寸纳米颗粒混合金属膜制备方法,包括:
步骤1:配置大尺寸纳米金属溶液;
步骤2:通过上述大尺寸纳米金属溶液制备大尺寸纳米金属膏;
步骤3:将所述大尺寸纳米金属膏适用到支撑基材上,通过干燥所述金属膏在所述支撑基材上形成大尺寸纳米金属膜;
步骤4:利用物理法纳米粒子发生器制备小尺寸纳米金属颗粒;
步骤5:利用电场、磁场或气流给小尺寸纳米金属颗粒赋予动能,以物理冲击方式将小尺寸纳米金属颗粒打入所述大尺寸纳米金属膜,填充大尺寸纳米金属颗粒之间的间隙,形成单层多尺寸纳米颗粒混合金属膜。
优选的,所述纳米金属膏为通过离心、沉淀、分离、洗涤、干燥步骤制备。
优选的,所述纳米金属颗粒的金属为金、钯、银、铜、铝、银钯合金、金钯合金、铜银合金、铜银镍合金或铜铝合金。
优选的,所述的纳米金属颗粒的形状包括球型、纤维状、雪花状、片状和/或线状。
优选的,所述金属膏通过100-150℃,10-25分钟的干燥,在所述支撑基材上形成金属膜。
优选的,所述支撑基材包括有机硅涂覆的聚酯纤维、陶瓷、玻璃和/或金属材料。
优选的,所述金属膏通过丝网印制、涂覆、或喷涂方法适用到支撑基材上。
优选的,所述大尺寸纳米金属颗粒直径1nm<D<10um,所述小尺寸纳米金属颗粒直径0.5nm<d<20nm。
通过本发明上述技术方案,可以至少实现下列所述一点益处:
1)烧结后提升金属层致密性、降低孔隙率;
2)同时小尺寸纳米金属颗粒的混入可以拉低材料平均粒度,进一步降低烧结温度;
3)本发明的铜膜能够使用含有有机包覆层的纳米铜材料代替纳米银材料制备烧结膜,进一步降低成本。
4)使用带式存储纳米金属膜,在使用时可以按需求取用并裁剪,降低了操作复杂度。
附图说明
图1为本发明的纳米铜薄膜的透视图。
图2为本发明的铜膜制备流程。
附图标记:有机介质材料1,大尺寸纳米金属颗粒2,小尺寸纳米金属颗粒3,支撑层材料4,纳米铜溶液5;纳米铜膏6;印刷丝网7;印刷刮刀8;纳米粒子发生器9;磁线圈10。
具体实施方式
下面详细说明本发明的具体实施,有必要在此指出的是,以下实施只是用于本发明的进一步说明,不能理解为对本发明保护范围的限制,该领域技术熟练人员根据上述本发明内容对本发明做出的一些非本质的改进和调整,仍然属于本发明的保护范围。
本发明提供了一种单层多尺寸纳米颗粒混合金属膜及其制备方法,其中本发明的多尺寸纳米颗粒混合金属膜如图1所示,包括:
有机介质材料1,形成有机包覆层;
所述有机介质材料中配置至少两种尺寸的纳米金属混合物;通过在大尺寸纳米金属颗粒2的间隙中打入小尺寸纳米金属颗粒3,实现了空隙填充,所述大尺寸纳米金属颗粒是指颗粒直径在1nm<D<10um的纳米金属铜颗粒,所述小尺寸纳米金属颗粒是颗粒直径在0.5nm<d<20nm的小尺寸纳米金属铜颗粒。其中必要条件是D>d。上述金属颗粒尺寸的设计达到在烧结后提升金属层致密性、降低孔隙率的效果,是其他直径尺寸的纳米金属颗粒组合所不能达到的。
优选地,纳米金属混合物是纳米铜混合物,形成单层多尺寸纳米铜颗粒混合的铜膜,使用纳米铜材料制备铜膜,具有降低成本、有效避免纳米银膜烧结后高电子迁移、降低与芯片热失配的效果。与纳米银近似的纳米铜颗粒可以在低温条件下熔融,烧结后熔点接近铜单质材料(1083℃),可构筑稳定的金属互连层。其单组分金属的特性,避免了合金材料热循环效应下的服役可靠性问题,实现铜铜键合,用纳米铜替代现有技术中的纳米银能够解决芯片和基板之间热膨胀系数匹配的问题,同时避免电迁移现象导致可靠性问题。对比纳米银颗粒,有效降低互连封装的材料和加工成本。由纳米铜粉体、膏体制成的烧结用纳米铜膜,在具备铜材料的优良特性同时,也同时具备金属烧结膜的便携性、易成型性等特点。
不同尺寸纳米金属混合物为不同尺寸的纳米铜;所述至少两种尺寸的纳米金属混合物包括大尺寸纳米金属铜颗粒和小尺寸纳米金属铜颗粒,所述大尺寸铜颗粒的缝隙中填充小尺寸纳米铜颗粒。通过在大尺寸纳米铜颗粒的间隙中打入小尺寸纳米铜颗粒,形成了通过小尺寸纳米铜颗粒填充大尺寸纳米铜颗粒的间隙的效果,从而达到在烧结后提升金属层致密性、提升导电导热率、降低孔隙率的效果。
所述铜膜还包括支撑基材4,其中支撑基材包括聚酯纤维、陶瓷、玻璃和/或金属材料。
至少两种尺寸的纳米金属混合物的所述尺寸数量可以为两种、三种或四种。
介质材料包括有机溶剂、助焊剂、焊膏、和/或粘合剂。
其中所述的纳米金属颗粒是多种形状的,包括球型、纤维、雪花状以及线状。
本发明的一种单层多尺寸纳米颗粒混合金属膜制备方法,其流程步骤如图2所示,具体地,
1)在罐中混合0至5wt.%的树脂或聚合物、0至1wt.%的成膜剂和30wt.%溶剂混合物以得到均匀溶液;
2)将0至2wt.%润湿剂、0至2wt.%有机过氧化物添加至所述均匀溶液,然后添加90wt.%的由大尺寸纳米铜颗粒构成的大尺寸(D50=10um)金属粉末,并且使用轨道式混合器进行混合,支撑纳米铜溶液5;
3)在混合后,在研磨机中研磨混合物,持续几分钟以获得均匀的纳米铜膏6;
4)将所述铜膏6适用到支撑基材上4;
5)所述铜膏6通过在130℃,10-15分钟的干燥,在所述支撑基材4上形成铜膜;
6)利用物理法纳米粒子发生器9制备小尺寸(D50=50nm)纳米铜颗粒;
7)通过保护性氮气气流给小尺寸纳米铜颗粒3赋予动能,使小尺寸纳米铜颗粒3以物理冲击方式以图2中打入所述铜膜,使其填充大尺寸纳米铜颗粒的间隙,形成单层多尺寸纳米颗粒混合铜膜。
测试结果表明,利用所述方法制备的混合纳米铜膜,烧接后孔隙率小于20%,导热率大于100(W/mK),剪切应力大于15MPa。在至少某些测试结果中,在-40到150℃的温度条件下,在1000次的热循环之后,剪切应力仍然大于10MPa。
表1本发明与现有技术获得的纳米金属膜的相关性能对比如下:
封装领域通过化学方法制备的纳米金属颗粒直径通常在30nm以上,难以实现20nm以下甚至1nm以下粒径的纳米金属颗粒制备及后续的稳定留存。此外,采用化学制备方法制备的纳米金属颗粒,尽管对操作及环境严格控制,其同批次制备的粒径范围依然存在分布集中性差,离散程度大的技术问题,这将不同程度的影响金属膜的烧结后性能。本发明采用的物理法制备纳米金属粒径范围为0-20nm,为克服化学方法制备的粒径尺寸上的限制带来的烧结性能上的瓶颈,将物理法制备的小尺寸金属纳米金属颗粒与化学法制备的大尺寸金属颗粒结合,在90um的烧结厚度下,实现如上表所示的高热导率电导率,高剪切力的技术突破。
本发明的纳米金属颗粒的较大和较小颗粒的尺寸的具体选择,使得小尺寸纳米金属颗粒在大尺寸纳米金属颗粒的间隙的填补效果好,致密性显著提升。上述金属颗粒尺寸的设计达到在烧结后提升金属层致密性、降低孔隙率的效果,是其他直径尺寸的纳米金属颗粒组合所不能达到的。此外,小尺寸纳米金属颗粒的混入可以拉低材料平均粒度,进一步降低烧结温度。
尽管为了说明的目的,已描述了本发明的示例性实施方式,但是本领域的技术人员将理解,不脱离所附权利要求中公开的发明的范围和精神的情况下,可以在形式和细节上进行各种修改、添加和替换等的改变,而所有这些改变都应属于本发明所附权利要求的保护范围,并且本发明要求保护的产品各个部门和方法中的各个步骤,可以以任意组合的形式组合在一起。因此,对本发明中所公开的实施方式的描述并非为了限制本发明的范围,而是用于描述本发明。相应地,本发明的范围不受以上实施方式的限制,而是由权利要求或其等同物进行限定。
Claims (18)
1.一种多尺寸纳米颗粒混合金属膜,其特征在于,包括:
有机介质材料,形成有机包覆层;
所述有机介质材料中配置至少两种尺寸的纳米金属颗粒;
用物理冲击方式将小尺寸纳米金属颗粒打入大尺寸纳米金属颗粒的空隙,通过设定物理冲击参数控制打入的小尺寸纳米金属颗粒量。
2.如权利要求1所述的多尺寸纳米颗粒混合金属膜,其特征在于:所述物理冲击方式为施加在小尺寸纳米金属颗粒上的电场、磁场、气流或其组合。
3.如权利要求1所述的多尺寸纳米颗粒混合金属膜,其特征在于:所述纳米金属颗粒的金属为金、钯、银、铜、铝、银钯合金、金钯合金、铜银合金、铜铝合金或铜银镍合金。
4.如权利要求1所述的多尺寸纳米颗粒混合金属膜,其特征在于:所述纳米金属颗粒的金属膜为纳米铜膜。
5.如权利要求1所述的多尺寸纳米颗粒混合金属膜,其特征在于:所述大尺寸纳米金属颗粒是颗粒直径在1nm<D<10um的纳米金属铜颗粒,所述小尺寸纳米金属颗粒是颗粒直径在0.5nm<d<20nm的小尺寸纳米金属铜颗粒。
6.如权利要求1所述的多尺寸纳米颗粒混合金属膜,其特征在于,所述金属膜烧结前厚度为10微米至200微米。
7.如权利要求1所述的多尺寸纳米颗粒混合金属膜,其特征在于:所述大尺寸纳米金属颗粒和所述小尺寸纳米金属颗粒的形状是球型、纤维状、雪花状、片状和/或线状。
8.如权利要求1至3任一项所述的多尺寸纳米颗粒混合金属膜,其特征在于:所述金属膜还包括支撑基材,其中支撑基材材质为聚酯纤维、陶瓷、玻璃和/或金属材料或其组合;
所述支撑基材包括线式、带式、片式、板式结构;
所述线式或带式支撑基材,在制备好金属膜后,收纳为成一卷。
9.如权利要求8任一项所述的多尺寸纳米颗粒混合金属膜,其特征在于:所述支撑基材和纳米颗粒接触的一面具有有机硅涂覆。
10.如权利要求1至3任一项所述的多尺寸纳米颗粒混合金属膜,其特征在于:有机介质材料包括有机溶剂、助焊剂、焊膏、和/或粘合剂。
11.一种多尺寸纳米颗粒混合金属膜制备方法,其特征在于,包括:
步骤1:配置大尺寸纳米金属溶液;
步骤2:通过上述大尺寸纳米金属溶液制备大尺寸纳米金属膏;
步骤3:将所述大尺寸纳米金属膏适用到支撑基材上,通过干燥所述金属膏在所述支撑基材上形成大尺寸纳米金属膜;
步骤4:利用物理法纳米粒子发生器制备小尺寸纳米金属颗粒;
步骤5:利用电场、磁场或气流给小尺寸纳米金属颗粒赋予动能,以物理冲击方式将小尺寸纳米金属颗粒打入所述大尺寸纳米金属膜,填充大尺寸纳米金属颗粒之间的间隙,形成多尺寸纳米颗粒混合金属膜。
12.如权利要求11所述的多尺寸纳米颗粒混合的金属膜制备方法,其特征在于,所述纳米金属膏为通过离心、沉淀、分离、洗涤、干燥步骤制备。
13.如权利要求11所述的多尺寸纳米颗粒混合金属膜制备方法,其特征在于:所述纳米金属颗粒的金属为金、钯、银、铜、铝、银钯合金、金钯合金、铜银合金、铜银镍合金或铜铝合金。
14.如权利要求11所述的多尺寸纳米颗粒混合金属膜制备方法,其特征在于:
所述的纳米金属颗粒的形状包括球型、纤维状、雪花状、片状和/或线状。
15.如权利要求11所述的多尺寸纳米颗粒混合金属膜制备方法,其特征在于:所述金属膏通过100-150℃,10-25分钟的干燥,在所述支撑基材上形成金属膜。
16.如权利要求11所述的多尺寸纳米颗粒混合金属膜制备方法,其特征在于:所述支撑基材包括有机硅涂覆的聚酯纤维、陶瓷、玻璃和/或金属材料。
17.如权利要求11所述的多尺寸纳米颗粒混合金属膜制备方法,其特征在于:所述金属膏通过丝网印制、涂覆或喷涂方法适用到支撑基材上。
18.如权利要求11至17任一项所述的金属膜制备方法,其特征在于:所述大尺寸纳米金属颗粒直径1nm<D<10um,所述小尺寸纳米金属颗粒直径0.5nm<d<20nm。
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