CN115029769B - 一种纳米孪晶铜膜转变为单晶铜膜的制备方法 - Google Patents
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Abstract
本发明公开了一种纳米孪晶铜膜转变为单晶铜膜的制备方法,包括以下步骤:(1)采用酸溶液对纳米孪晶铜膜进行预处理;(2)将预处理后的纳米孪晶铜膜沿厚度方向夹持于冷夹板和热夹板中进行热处理,冷夹板的温度为‑20℃至30℃,热夹板的温度为200‑300℃;(3)保持步骤(2),待热处理结束后,即得单晶铜膜,所述纳米孪晶铜膜为沿厚度方向具有(111)择优晶体取向,所述单晶铜膜为沿厚度取向为(100)晶面取向。本发明所采用的制备方法可在低温下实现由纳米孪晶铜膜到单晶铜膜的转变,可避免热损失,简单易实现,成本低,适合大规模生产。
Description
技术领域
本发明涉及膜的制备方法,具体涉及一种纳米孪晶铜膜转变为单晶铜膜的制备方法。
背景技术
在三维系统封装技术中,键合是实现多层芯片堆叠和垂直互连的关键技术。在众多键合技术中,Cu-Cu直接键合凭借其优良的导热导电性能、抗电迁移性能、结合界面的机械强度高以及封装制造中的兼容性和低成本等优势,成为3D封装中硅通孔(TSV)互连的主要键合方式。Cu-Cu直接键合是在真空条件下,通过热压的方式使Cu原子相互扩散形成界面互连。然而,Cu-Cu直接键合虽然具有诸多优点,但键合过程通常需要较高的键合温度(>350℃),极易对芯片造成热损伤。因此,降低键合温度成为了该领域的技术瓶颈。
为克服这一挑战,高度(111)择优晶体取向的纳米孪晶铜成为了研究人员和企业界关注的焦点。使用(111)择优晶体取向纳米孪晶铜进行键合,键合温度可以降低到200℃。但键合完成后,在微凸点键合处留下一个键合界面,该界面的存在使微凸点的剪切强度较低。因此,如果能够消除键合界面,这将对微凸点的剪切性能有很大的改善。在电镀(111)择优晶体取向纳米孪晶中存在一层由纳米尺度的晶粒组成的过渡层,该层具有热不稳定性,因此,电镀(111)择优晶体取向纳米孪晶铜薄膜在400℃温度下退火60min后,其晶粒向(100)晶体取向方向转变,同时伴随着晶粒的异常长大,这种转变对消除Cu-Cu直接键合的键合界面具有重要意义。此外,这种转变对铜膜在凸点下金属化层(UBM)和再布线层(RDL)中的应用同样具有积极地影响,利用力学与电学性能优异、工艺简单、成本低廉的(100)晶体取向单晶铜,作为凸点下UBM或再布线层RDL,可以解决电子工业中的单晶铜工艺繁琐、成本昂贵、难以实际应用等问题。然而,对于该方法在微互连中的应用,这一转变温度明显过高。因此,有必要通过必要的技术手段降低(111)择优晶体取向纳米孪晶铜薄膜的晶粒取向转变温度,避免其对芯片造成的热损伤。
发明内容
发明目的:为了解决现有技术存在的技术问题,本发明旨在提供一种加工温度低、简单易实现的纳米孪晶铜膜转变为单晶铜膜的制备方法。
技术方案:本发明所述纳米孪晶铜膜转变为单晶铜膜的制备方法,包括以下步骤:
(1)采用酸溶液对纳米孪晶铜膜进行预处理;
(2)将预处理后的纳米孪晶铜膜沿厚度方向夹持于冷夹板和热夹板中进行热处理,冷夹板的温度为-20℃至30℃,热夹板的温度为200-300℃;
(3)保持步骤(2),待热处理结束后,即得单晶铜膜。
进一步地,所述步骤(1)中的纳米孪晶铜膜的厚度为10-50μm,纳米孪晶铜膜为沿厚度方向具有(111)择优晶体取向,形状为圆柱形、线形、矩形或不规则形,纳米孪晶铜膜为单独存在或附着在基板上,基板为铜或硅。
进一步地,所述步骤(1)中的酸溶液为柠檬酸水溶液,浓度为4-6%,本发明通过柠檬酸水溶液预处理去除纳米孪晶铜膜表面的氧化膜,既可达到有效去除氧化膜的作用,又不损伤纳米孪晶铜膜的表面。
进一步地,所述步骤(2)中冷夹板和热夹板之间的温度梯度为1×103-6×104℃/cm,在此温度梯度范围内,既可加快(111)择优晶体取向的纳米孪晶铜膜向(100)晶体取向的单晶铜膜的转变过程,又不至于使加热温度过高(>300℃)。
进一步地,所述步骤(3)中的单晶铜膜为沿厚度取向为(100)晶面取向,晶粒尺寸达300-400μm,步骤(2)的保持时间为10-60min。
发明原理:本发明将(111)择优晶体取向的纳米孪晶铜膜沿厚度方向夹持于冷、热两夹板中间,通过合理的冷、热夹板温度设定,使择优晶体取向纳米孪晶铜膜两侧产生一定的温度梯度并保持一定时间,温度梯度促使金属原子发生热迁移,加速(111)择优晶体取向的纳米孪晶铜膜转变为沿厚度方向为(100)晶体取向的单晶铜膜,显著提高键合效率。
有益效果:与现有技术相比,本发明具有以下显著优点:
(1)加工温度低,与现有400℃的加工温度相比,本发明选择的热板最高温度为300℃,显著降低了工艺温度,减少了微电子制造过程中的热损伤;
(2)简单易实现,本发明中(100)晶体取向的单晶铜膜只需通过简单的对(111)择优晶体取向的纳米孪晶铜膜进行电镀及温度梯度老化即可制得,克服了提拉法制备单晶铜的复杂性;此外,(100)晶体取向的单晶铜膜可以做到数微米至数十微米厚,可获得任意厚度、形状的样品,克服了提拉法制备的单晶铜尺寸的限制;
(3)与现有半导体及封装工艺兼容性好,工艺简单易实现,成本低,适合大规模生产。
附图说明
图1为本发明实施例1晶面为(111)的纳米孪晶铜膜的XRD图;
图2为本发明实施例1制得的晶面为(100)的单晶铜膜的XRD图。
具体实施方式
下面,结合具体实施例和附图进一步对本发明进行说明。
实施例1:本发明所述纳米孪晶铜膜转变为单晶铜膜的制备方法,包括以下步骤:
(1)采用5%柠檬酸水溶液对单独存在、不规则形状、厚度为40μm、沿厚度方向具有(111)择优晶体取向的纳米孪晶铜膜进行预处理,图1为本发明实施例1晶面为(111)的纳米孪晶铜膜的XRD图;
(2)将预处理后的纳米孪晶铜膜沿厚度方向夹持于冷夹板和热夹板中进行热处理,冷夹板的温度为0℃,热夹板的温度为200℃,温度梯度为5×104℃/cm;
(3)将步骤(2)保持20min,即得沿厚度方向为(100)晶体取向的单晶铜膜,晶粒尺寸可达400μm,图2为本发明在温度梯度为5×104℃/cm下保持20min制得的晶面为(100)的单晶铜膜的XRD图,图中Cu的强衍射峰为(200),(200)面与(100)面都是一个方向的晶面,属于同一晶面族。在XRD测试中,因为Cu的点阵结构为面心立方结构,只有当衍射面(hkl)指数为全奇数或全偶数时才产生衍射,而当其衍射面(hkl)指数为奇偶混杂时,其衍射消光。因此,在单晶铜膜的XRD图中,强衍射峰为(200),而不是(100)。
实施例2:本发明所述纳米孪晶铜膜转变为单晶铜膜的制备方法,包括以下步骤:
(1)采用5%柠檬酸水溶液对附着在厚度为100μm的铜基板上、矩形、厚度为12μm、沿厚度方向具有(111)择优晶体取向的纳米孪晶铜膜进行预处理;
(2)将预处理后的纳米孪晶铜膜沿厚度方向夹持于冷夹板和热夹板中进行热处理,冷夹板的温度为-20℃,热夹板的温度为200℃,温度梯度为1.96×104℃/cm;
(3)将步骤(2)保持45min,即得沿厚度方向为(100)晶体取向的单晶铜膜,晶粒尺寸可达300μm。
实施例3:本发明所述纳米孪晶铜膜转变为单晶铜膜的制备方法,包括以下步骤:
(1)采用5%柠檬酸水溶液对单独存在、圆柱形、厚度为50μm、沿厚度方向具有(111)择优晶体取向的纳米孪晶铜膜进行预处理;
(2)将预处理后的纳米孪晶铜膜沿厚度方向夹持于冷夹板和热夹板中进行热处理,冷夹板的温度为20℃,热夹板的温度为300℃,温度梯度为5.6×104℃/cm;
(3)将步骤(2)保持10min,即得沿厚度方向为(100)晶体取向的单晶铜膜,晶粒尺寸可达400μm。
实施例4:本发明所述纳米孪晶铜膜转变为单晶铜膜的制备方法,包括以下步骤:
(1)采用5%柠檬酸水溶液对附着在厚度为100μm的硅基板上、矩形、厚度为20μm、沿厚度方向具有(111)择优晶体取向的纳米孪晶铜膜进行预处理;
(2)将预处理后的纳米孪晶铜膜沿厚度方向夹持于冷夹板和热夹板中进行热处理,冷夹板的温度为0℃,热夹板的温度为200℃,温度梯度为1.67×104℃/cm;
(3)将步骤(2)保持60min,即得沿厚度方向为(100)晶体取向的单晶铜膜,晶粒尺寸可达400μm。
Claims (7)
1.一种纳米孪晶铜膜转变为单晶铜膜的制备方法,其特征在于,包括以下步骤:
(1)采用酸溶液对纳米孪晶铜膜进行预处理;
(2)将预处理后的纳米孪晶铜膜沿厚度方向夹持于冷夹板和热夹板中进行热处理,冷夹板的温度为-20℃至30℃,热夹板的温度为200-300℃;
(3)保持步骤(2),待热处理结束后,即得单晶铜膜;
所述步骤(1)中的纳米孪晶铜膜的厚度为10-50μm,纳米孪晶铜膜为沿厚度方向具有(111)择优晶体取向;
所述步骤(3)中的单晶铜膜为沿厚度取向为(100)晶面取向。
2.根据权利要求1所述的制备方法,其特征在于,所述步骤(1)中的纳米孪晶铜膜的形状为矩形或不规则形。
3.根据权利要求1所述的制备方法,其特征在于,所述步骤(1)中的纳米孪晶铜膜为单独存在或附着在基板上。
4.根据权利要求3所述的制备方法,其特征在于,所述基板为铜或硅。
5.根据权利要求1所述的制备方法,其特征在于,所述步骤(1)中的酸溶液为柠檬酸水溶液。
6.根据权利要求1所述的制备方法,其特征在于,所述步骤(2)中冷夹板和热夹板之间的温度梯度为1×103-6×104℃/cm。
7.根据权利要求1所述的制备方法,其特征在于,所述步骤(3)中,步骤(2)的保持时间为10-60min。
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