CN114101661A - 一种填充有微纳米金属颗粒的混合浆料的制备方法及其产品和应用 - Google Patents
一种填充有微纳米金属颗粒的混合浆料的制备方法及其产品和应用 Download PDFInfo
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- CN114101661A CN114101661A CN202111411756.1A CN202111411756A CN114101661A CN 114101661 A CN114101661 A CN 114101661A CN 202111411756 A CN202111411756 A CN 202111411756A CN 114101661 A CN114101661 A CN 114101661A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- Powder Metallurgy (AREA)
Abstract
本发明涉及一种填充有微纳米金属颗粒的混合浆料的制备方法及其产品和应用,属于半导体芯片封装技术领域。本发明公开了一种填充有微纳米金属颗粒的混合浆料的制备方法,主要是将粒径大的微纳米金属颗粒I制成微纳米金属颗粒基体浆料,采用物理火花烧蚀法制备微纳米金属颗粒核,将包覆材料通过雾化喷嘴的形式对微纳米金属颗粒核进行表面改性处理,在微纳米金属颗粒核表面形成具有防氧化和防团聚作用的包覆层,得到粒径小的微纳米金属颗粒Ⅱ,通过对微纳米金属颗粒Ⅱ赋予动能,利用物理冲击的方式填充进基体浆料中,制备填充有微纳米金属颗粒的混合浆料。该方法可以提高填充有微纳米金属颗粒的混合浆料的致密度,从而提导电、导热的性能和烧结性能。
Description
技术领域
本发明属于半导体芯片封装技术领域,具体涉及一种填充有微纳米金属颗粒的混合浆料的制备方法及其产品和应用。
背景技术
目前电力电子器件向着大功率、高密度、高可靠性以及微型化的方向发展,也对半导体芯片的封装技术提出了更高的要求。在封装技术领域,寻求低温互连、高温服役且热膨胀系数相匹配,可靠性高的互连材料成为急需解决的问题。由于“尺寸效应”,使得微纳米金属颗粒能够实现封装中低温连接、高温服役的要求。目前国内外封装中使用最多是纳米银烧结材料,实现了对大功率芯片的有效连接。然而,金属银价格昂贵,且抗电迁移能力较差,使得纳米银烧结材料难以长时间大规模使用。同时银与芯片背面热膨胀系数不同,需要添加其他中间金属层提高其互连能力,导致连接工艺复杂且增加了封装成本。金属铜价格低廉,具有较好的抗电迁移的能力、高导电、导热,以及良好的机械性能。因此,微纳米金属铜成为代替纳米烧结银、金,含铅焊料等昂贵、有害的互连材料的最佳选择。然而,随着铜颗粒尺寸越小,表面能越大,在制备过程中容易发生氧化、团聚的现象,导致其烧结性能变差。为解决微纳米铜颗粒的氧化、团聚现象,普遍采用在铜颗粒表面进行包覆来防止颗粒的氧化、团聚。但是由于在颗粒保存、运输或制备过程中,依旧会造成部分颗粒的氧化以及颗粒间的团聚,影响了所制备的烧结膏体的均匀性,难以实现对芯片有效、可靠、均匀的连接。
其次,单一尺寸微纳米铜膏进行烧结连接时,由于烧结首先发生在颗粒之间,通过“颈连”而发生烧结连接,在烧结体中容易形成较大空隙而降低烧结层的导电、导热等性能。通常需要更高的能量输入来实现进一步的致密化,从而导致连接温度或时间或压力较高,增加了连接成本。因此,亟需一种能够适应于快速、有效、可靠的互连工艺的烧结封装互连材料。
发明内容
有鉴于此,本发明的目的之一在于提供一种填充有微纳米金属颗粒的混合浆料的制备方法;目的之二在于提供一种填充有微纳米金属颗粒的混合浆料;目的之三在于提供一种填充有微纳米金属颗粒的混合浆料的应用。
为达到上述目的,本发明提供如下技术方案:
1.一种填充有微纳米金属颗粒的混合浆料的制备方法,所述制备方法如下:
采用物理冲击的方法将表面具有防氧化和防团聚作用包覆层的微纳米金属颗粒Ⅱ填充进微纳米金属颗粒基体浆料中,即可得到填充有微纳米金属颗粒的混合浆料;
所述物理冲击的方法为:在微纳米金属颗粒Ⅱ上施加电场、磁场或气流中的任意一种或几种。
优选的,所述微纳米金属颗粒Ⅱ的制备方法如下:采用雾化的方法将包覆材料对微纳米金属颗粒核进行表面改性处理,在微纳米金属颗粒核表面形成具有防氧化和防团聚作用的包覆层,即可得到微纳米金属颗粒Ⅱ。
优选的,所述微纳米金属颗粒核的材质为铜、金、钯、银、铝、银钯合金、金钯合金、铜银合金、铜银镍合金或铜铝合金中的任意一种。
优选的,所述微纳米金属颗粒核的直径为1nm≤d≤50nm。
优选的,所述包覆材料包括材料I和材料Ⅱ。
优选的,所述材料I为乙二醇、丙三醇、二甘醇、三甘醇中的任意一种或几种。
优选的,所述材料Ⅱ为聚乙烯吡咯烷酮、聚乙二醇、聚丙烯酸、羧酸、磷酸、水合肼、草酸、油酸、柠檬酸、C6~C18的脂肪酸中的任意一种或几种。
优选的,所述C6~C18的脂肪酸包括具有直链或支链的饱和脂肪酸、具有直链或支链的不饱和脂肪酸。
优选的,所述材料I与材料Ⅱ的质量比为1:10~9:10。
优选的,所述微纳米金属颗粒基体浆料的制备方法如下:将直径为50nm≤D≤500um的微纳米金属颗粒I倒入有机载体中,搅拌混合均匀,即可得到微纳米金属颗粒基体浆料。
优选的,所述有机载体包括溶剂、增稠剂、活性剂和触变剂。
优选的,所述溶剂为松油醇或乙二醇。
优选的,所述增稠剂为酚醛树脂或环氧树脂。
优选的,所述活性剂为松香或月桂酸。
优选的,所述触变剂为氢化蓖麻油。
优选的,所述微纳米金属颗粒I与有机载体的质量比为3:2~4:1。
优选的,所述微纳米金属颗粒I的材质为铜、金、钯、银、铝、银钯合金、金钯合金、铜银合金、铜银镍合金或铜铝合金中的任意一种。
优选的,所述微纳米金属颗粒I与微纳米金属颗粒基体浆料中的微纳米金属颗粒Ⅱ的质量比为1:2~2:1。
2、根据上述方法制备的填充有微纳米金属颗粒的混合浆料。
3、上述填充有微纳米金属颗粒的混合浆料在封装半导体芯片中的应用。
本发明的有益效果在于:本发明提供的一种填充有微纳米金属颗粒的混合浆料的制备方法,本发明将微纳米金属颗粒I制成微纳米金属颗粒基体浆料,采用物理火花烧蚀法制备微纳米金属颗粒核,将包覆材料经加热、加压、超声或三者同时应用的条件下进行雾化,通过雾化喷嘴的形式对微纳米金属颗粒核进行表面改性处理在微纳米金属颗粒核表面形成具有防氧化和防团聚作用的包覆层,得到微纳米金属颗粒Ⅱ,通过对微纳米金属颗粒Ⅱ赋予动能,利用物理冲击的方式填充进基体浆料中,并辅助高速搅拌、超声工艺,使大小颗粒在浆料中充分混合,避免了常规搅拌混合制备时,微纳米金属颗粒Ⅱ发生氧化、团聚的现象,使微纳米金属颗粒Ⅱ与微纳米金属颗粒基体浆料快速、充分的混合,得到填充有微纳米金属颗粒的混合浆料。该方法可以提高填充有微纳米金属颗粒的混合浆料的致密度,从而提高填充有微纳米金属颗粒的混合浆料的导电、导热的性能。同时,由于微纳米金属颗粒Ⅱ的加入,使混合浆料中金属颗粒的平均粒径减小,降低填充有微纳米金属颗粒的混合浆料烧结时的温度,提高填充有微纳米金属颗粒的混合浆料的烧结性能。
本发明的其他优点、目标和特征在某种程度上将在随后的说明书中进行阐述,并且在某种程度上,基于对下文的考察研究对本领域技术人员而言将是显而易见的,或者可以从本发明的实践中得到教导。本发明的目标和其他优点可以通过下面的说明书来实现和获得。
附图说明
为了使本发明的目的、技术方案和优点更加清楚,下面将结合附图对本发明作优选的详细描述,其中:
图1为实施例1中微纳米金属颗粒基体浆料的制备流程示意图;
图2为实施例1中填充有微纳米金属颗粒的混合浆料的制备流程示意图;
图3为实施例1中基板的侧视图;
图4为实施例1中填充有微纳米金属颗粒的混合浆料印刷于基板上的示意图
图5为实施例1中待封装的半导体芯片封装在基板上的混合浆料上的示意图;
图6为实施例1中填充有微纳米金属颗粒的混合浆料的烧结示意图;
图7为实施例1中封装后的半导体芯片示意图;
图8为实施例1中填充有微纳米金属颗粒的混合浆料的烧结电镜图;
图9为实施例2中填充有微纳米金属颗粒的混合浆料的烧结电镜图。
图中序号:1为微纳米金属颗粒基体浆料,2为微纳米金属颗I,3为纳米粒子发生器,4为微纳米金属颗粒核,5为雾化装置,6为雾化喷嘴,7为微纳米金属颗粒Ⅱ,8为填充有微纳米金属颗粒的混合浆料,9为基板,10为印刷在基板上的填充有微纳米金属颗粒的混合浆料,11为待封装的半导体芯片,12为已封装的半导体芯片。
具体实施方式
以下通过特定的具体实例说明本发明的实施方式,本领域技术人员可由本说明书所揭露的内容轻易地了解本发明的其他优点与功效。本发明还可以通过另外不同的具体实施方式加以实施或应用,本说明书中的各项细节也可以基于不同观点与应用,在没有背离本发明的精神下进行各种修饰或改变。需要说明的是,以下实施例中所提供的图示仅以示意方式说明本发明的基本构想,在不冲突的情况下,以下实施例及实施例中的特征可以相互组合。
实施例1
1、填充有微纳米金属颗粒的混合浆料的制备方法,包括如下步骤:
(1)采用具有物理火光烧蚀的纳米粒子发生器,制备原材料为铜的微纳米金属颗粒核;
(2)将乙二醇、丙三醇、聚乙烯吡咯烷酮、聚乙二醇和聚丙烯酸混合均匀后,通过雾化装置进行雾化处理,再经雾化喷嘴均匀喷洒至纳米粒子发生器制备的原材料为铜的微纳米金属颗粒核表面形成具有防氧化和防团聚作用的包覆层,得到直径为1nm的微纳米金属颗粒Ⅱ,其中乙二醇、丙三醇与聚乙烯吡咯烷酮、聚乙二醇和聚丙烯酸质量比为1:10;
(3)将原材料为铜、直径为50nm的微纳米金属颗粒I倒入松油醇、酚醛树脂、松香和氢化蓖麻油的混合物中,搅拌混合均匀,即可得到微纳米金属颗粒基体浆料(其制备流程图如图1所示,图中1为微纳米金属颗粒基体浆料,2为微纳米金属颗I),其中微纳米金属颗粒I与松油醇的质量比为3:2;
(4)采用物理冲击的方法将微纳米金属颗粒Ⅱ填充进微纳米金属颗粒基体浆料中,得到填充有微纳米金属颗粒的混合浆料(其制备流程图如图2所示,图中2为微纳米金属颗I,3为纳米粒子发生器,4为微纳米金属颗粒核,5为雾化装置,6为雾化喷嘴,7为微纳米金属颗粒Ⅱ,8为填充有微纳米金属颗粒的混合浆料),所述物理冲击方式为:在微纳米金属颗粒Ⅱ上施加电场、磁场或气流中的任意一种或几种;通过调整电场、磁场强度,气流流量,施加时间,控制打入的微纳米金属颗粒Ⅱ的量,其中微纳米金属颗粒基体浆料中微纳米金属颗粒I与微纳米金属颗粒Ⅱ的质量比为1:2。
2、填充有微纳米金属颗粒的混合浆料在封装半导体芯片中的应用,所述封装半导体芯片包括如下步骤:
(1)采用高精度丝印台将上述混合浆料印刷于DBC基板上(其侧视图如图3所示,图中9为基板;填充有微纳米金属颗粒的混合浆料印刷于基板上的示意图如图4所示,图中10为印刷在基板上的填充有微纳米金属颗粒的混合浆料),并在干燥箱中进行烘干,使混合浆料中的部分有机载体挥发;
(2)将待封装的半导体芯片贴于步骤(1)中挥发后的混合浆料上(待封装的半导体芯片封装在基板上的混合浆料上的示意图如图5所示,图中11为待封装的半导体芯片),在280℃和20MPa下烧结5min即可(填充有微纳米金属颗粒的混合浆料的烧结示意图如图6所示;封装后的半导体芯片示意图如图7所示,图中12为已封装的半导体芯片;填充有微纳米金属颗粒的混合浆料的烧结电镜图如图8所示)。
实施例2
1、填充有微纳米金属颗粒的混合浆料的制备方法,包括如下步骤:
(1)采用具有物理火光烧蚀的纳米粒子发生器,制备原材料为铝的微纳米金属颗粒核;
(2)将二甘醇、三甘醇、羧酸、水合肼和油酸混合均匀后,通过雾化装置进行雾化处理,再经雾化喷嘴均匀喷洒至纳米粒子发生器制备的原材料为铝的微纳米金属颗粒核表面形成具有防氧化和防团聚作用的包覆层,得到直径为50nm的微纳米金属颗粒Ⅱ,其中乙二醇、丙三醇与聚乙烯吡咯烷酮、聚乙二醇和聚丙烯酸质量比为9:10;
(3)将原材料为铝、直径为500um的微纳米金属颗粒I倒入乙二醇、环氧树脂、月桂酸和氢化蓖麻油的混合物中,搅拌混合均匀,即可得到微纳米金属颗粒基体浆料,其中微纳米金属颗粒I与松油醇的质量比为4:1;
(4)采用物理冲击的方法将微纳米金属颗粒Ⅱ填充进微纳米金属颗粒基体浆料中,得到填充有微纳米金属颗粒的混合浆料,所述物理冲击方式为:在微纳米金属颗粒Ⅱ上施加电场、磁场或气流中的任意一种或几种;通过调整电场、磁场强度,气流流量,施加时间,控制打入的微纳米金属颗粒Ⅱ的量,其中微纳米金属颗粒基体浆料中微纳米金属颗粒I与微纳米金属颗粒Ⅱ的质量比为2:1。
2、填充有微纳米金属颗粒的混合浆料在封装半导体芯片中的应用,所述封装半导体芯片包括如下步骤:
(1)采用高精度丝印台将上述混合浆料印刷于DBC基板上,并在干燥箱中进行烘干,使混合浆料中的部分有机载体挥发;
(2)将待封装的半导体芯片贴于步骤(1)中挥发后的混合浆料上,在220℃和20MPa下烧结5min即可(填充有微纳米金属颗粒的混合浆料的烧结电镜图如图9所示)。
材料性能测试
本申请中实施例1和2中制备的填充有微纳米金属颗粒的混合浆料的测试数据如表1所示:
表1实施例1和2制备的试样性能的测试数据
试样 | 剪切强度 | 孔隙率 |
实施例1 | 95.04MPa | 0.9% |
实施例2 | 17.59MPa | 5.3% |
由表1中数据可得到如下结论:
实施例1和2中方法制备的填充有微纳米金属颗粒的混合浆料,具有低的孔隙率,可以提高填充有微纳米金属颗粒的混合浆料的致密度,从而提高填充有微纳米金属颗粒的混合浆料的导电、导热的性能。
在上述实施例中,将实施例1-2中微纳米金属颗粒核和微纳米金属颗粒I的原材料分别为铜和铝替换成金、钯、银、银钯合金、金钯合金、铜银合金、铜银镍合金或铜铝合金中的任意一种;将实施例1-2中包覆材料中的材料Ⅱ分别为聚乙烯吡咯烷酮、聚乙二醇、聚丙烯酸和羧酸、水合肼、油酸替换成磷酸、草酸、柠檬酸、C6~C18的脂肪酸中的任意一种或几种;鉴于上述材料具有相似的物化性能,其相互替换后制备的产物与实施例1-2中的产品性能相似,得到填充有微纳米金属颗粒的混合浆料。
综上所述:本发明将微纳米金属颗粒I制成微纳米金属颗粒基体浆料,采用物理火花烧蚀法制备微纳米金属颗粒核,将包覆材料经加热、加压、超声或三者同时应用的条件下进行雾化,通过雾化喷嘴的形式对微纳米金属颗粒核进行表面改性处理在微纳米金属颗粒核表面形成具有防氧化和防团聚作用的包覆层,得到微纳米金属颗粒Ⅱ,通过对微纳米金属颗粒Ⅱ赋予动能,利用物理冲击的方式填充进基体浆料中,并辅助高速搅拌、超声工艺,使大小颗粒在浆料中充分混合,避免了常规搅拌混合制备时,微纳米金属颗粒Ⅱ发生氧化、团聚的现象,使微纳米金属颗粒Ⅱ与微纳米金属颗粒基体浆料快速、充分的混合,得到填充有微纳米金属颗粒的混合浆料。该方法可以提高填充有微纳米金属颗粒的混合浆料的致密度,从而提高填充有微纳米金属颗粒的混合浆料的导电、导热的性能。同时,由于微纳米金属颗粒Ⅱ的加入,使混合浆料中金属颗粒的平均粒径减小,降低填充有微纳米金属颗粒的混合浆料烧结时的温度,提高填充有微纳米金属颗粒的混合浆料的烧结性能。
最后说明的是,以上实施例仅用以说明本发明的技术方案而非限制,尽管参照较佳实施例对本发明进行了详细说明,本领域的普通技术人员应当理解,可以对本发明的技术方案进行修改或者等同替换,而不脱离本技术方案的宗旨和范围,其均应涵盖在本发明的权利要求范围当中。
Claims (10)
1.一种填充有微纳米金属颗粒的混合浆料的制备方法,其特征在于,所述制备方法如下:
采用物理冲击的方法将表面具有防氧化和防团聚作用包覆层的微纳米金属颗粒Ⅱ填充进微纳米金属颗粒基体浆料中,即可得到填充有微纳米金属颗粒的混合浆料;
所述物理冲击的方法为:在微纳米金属颗粒Ⅱ上施加电场、磁场或气流中的任意一种或几种。
2.根据权利要求1所述的方法,其特征在于,所述微纳米金属颗粒Ⅱ的制备方法如下:采用雾化的方法将包覆材料对微纳米金属颗粒核进行表面改性处理,在微纳米金属颗粒核表面形成具有防氧化和防团聚作用的包覆层,即可得到微纳米金属颗粒Ⅱ。
3.根据权利要求2所述的方法,其特征在于,所述微纳米金属颗粒核的材质为铜、金、钯、银、铝、银钯合金、金钯合金、铜银合金、铜银镍合金或铜铝合金中的任意一种;
所述微纳米金属颗粒核的直径为1nm≤d≤50nm。
4.根据权利要求2所述的方法,其特征在于,所述包覆材料包括材料I和材料Ⅱ;
所述材料I为乙二醇、丙三醇、二甘醇、三甘醇中的任意一种或几种;
所述材料Ⅱ为聚乙烯吡咯烷酮、聚乙二醇、聚丙烯酸、羧酸、磷酸、水合肼、草酸、油酸、柠檬酸、C6~C18的脂肪酸中的任意一种或几种;
所述C6~C18的脂肪酸包括具有直链或支链的饱和脂肪酸、具有直链或支链的不饱和脂肪酸。
5.根据权利要求4所述的方法,其特征在于,所述材料I与材料Ⅱ的质量比为1:10~9:10。
6.根据权利要求1所述的方法,其特征在于,所述微纳米金属颗粒基体浆料的制备方法如下:将直径为50nm≤D≤500um的微纳米金属颗粒I倒入有机载体中,搅拌混合均匀,即可得到微纳米金属颗粒基体浆料。
7.根据权利要求6所述的方法,其特征在于,所述有机载体包括溶剂、增稠剂、活性剂和触变剂;
所述溶剂为松油醇或乙二醇;
所述增稠剂为酚醛树脂或环氧树脂;
所述活性剂为松香或月桂酸;
所述触变剂为氢化蓖麻油;
所述微纳米金属颗粒I与有机载体的质量比为3:2~4:1;
所述微纳米金属颗粒I的材质为铜、金、钯、银、铝、银钯合金、金钯合金、铜银合金、铜银镍合金或铜铝合金中的任意一种。
8.根据权利要求7所述的方法,其特征在于,所述微纳米金属颗粒I与微纳米金属颗粒基体浆料中的微纳米金属颗粒Ⅱ的质量比为1:2~2:1。
9.根据权利要求1~8任一项所述的制备方法制得的填充有微纳米金属颗粒的混合浆料。
10.权利要求9所述的填充有微纳米金属颗粒的混合浆料在封装半导体芯片中的应用。
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