CN106489199A - 半导体装置用接合线 - Google Patents

半导体装置用接合线 Download PDF

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Publication number
CN106489199A
CN106489199A CN201580002424.4A CN201580002424A CN106489199A CN 106489199 A CN106489199 A CN 106489199A CN 201580002424 A CN201580002424 A CN 201580002424A CN 106489199 A CN106489199 A CN 106489199A
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China
Prior art keywords
line
alloy
coating
endurance
closing line
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Granted
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CN201580002424.4A
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CN106489199B (zh
Inventor
山田隆
小田大造
榛原照男
大石良
斋藤和之
宇野智裕
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Nippon Steel & Sumitomo New Materials Co.,Ltd.
Nippon Steel Chemical and Materials Co Ltd
Original Assignee
Kanae Co Ltd
Nippon Micrometal Corp
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Publication of CN106489199A publication Critical patent/CN106489199A/zh
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    • H—ELECTRICITY
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    • H01L24/42—Wire connectors; Manufacturing methods related thereto
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
    • B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
    • B23K35/0227—Rods, wires
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
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    • B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/24—Selection of soldering or welding materials proper
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    • B23K35/3013—Au as the principal constituent
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    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
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    • B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/24—Selection of soldering or welding materials proper
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    • B23K35/302—Cu as the principal constituent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
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Abstract

本发明涉及一种具有Cu合金芯材和在其表面形成的Pd被覆层的半导体装置用接合线，谋求提高175℃～200℃的HTS中的球接合部的接合可靠性和使耐力比(＝最大耐力/0.2％耐力)为1.1～1.6。通过使线中含有总计为0.03～2质量％的Ni、Zn、Rh、In、Ir、Pt中的1种以上，来提高HTS中的球接合部的接合可靠性，进而，在对与接合线的线轴垂直的方向的芯材截面测定晶体取向所得到的结果中，使线长度方向的晶体取向之中、相对于线长度方向角度差为15度以下的晶体取向<100>的取向比率为50％以上，且与接合线的线轴垂直的方向的芯材截面中的平均结晶粒径为0.9～1.3μm，由此使耐力比为1.6以下。

Description

半导体装置用接合线
技术领域
本发明涉及为了将半导体元件上的电极与外部引线等的电路布线基板的布线连接而被利用的半导体装置用接合线。
背景技术
现在，作为将半导体元件上的电极与外部引线之间接合的半导体装置用接合线(以下称为接合线)，主要使用线径15～50μm左右的细线。接合线的接合方法一般为并用超声波的热压接方式，可使用通用接合装置、将接合线通到其内部而用于连接的毛细管工具等。接合线的接合工艺通过下述过程来完成：通过电弧热输入将线尖端加热熔融，利用表面张力形成球(FAB：Free Air Ball，无空气的球)后，使该球部压接接合于在150℃～300℃的范围内加热了的半导体元件的电极上(以下称为球接合)，接着，形成环路之后，将线部压接接合于外部引线侧的电极(以下称为楔接合)。作为接合线的接合对象，半导体元件上的电极可以使用在Si基板上形成了以Al为主体的合金膜的电极结构，外部引线侧的电极可以使用在Si基板上施加了镀Ag层、镀Pd层的电极结构等。
迄今为止，接合线的材料中Au是主流，但以LSI用途为中心，替代为Cu的工作正在推进。另一方面，以近年来的电动汽车、混合动力汽车的普及为背景，在车载用装置用途中，对于从Au向Cu的替代的需求也在提高。
关于Cu接合线，曾提出了使用高纯度Cu(纯度：99.99质量％以上)的Cu接合线(例如，专利文献1)。Cu与Au相比具有易氧化的缺点，存在接合可靠性、球形成性、楔接合性等较差的问题。作为防止Cu接合线的表面氧化的方法，曾提出了用Au、Ag、Pt、Pd、Ni、Co、Cr、Ti等金属被覆Cu芯材表面的结构(专利文献2)。另外，曾提出了在Cu芯材的表面被覆Pd，再将其表面用Au、Ag、Cu或它们的合金被覆的结构(专利文献3)。
在先技术文献
专利文献
专利文献1：日本特开昭61-48543号公报
专利文献2：日本特开2005-167020号公报
专利文献3：日本特开2012-36490号公报
发明内容
车载用装置与一般的电子设备相比，要求在严酷的高温高湿环境下的接合可靠性。特别是，将线的球部接合于电极的球接合部的接合寿命成为最大的问题。
在作为半导体装置的外壳的塑模树脂(环氧树脂)中，包含硅烷偶联剂。硅烷偶联剂具有提高有机物(树脂)与无机物(硅、金属)的密合性的作用，因此，能够提高与硅基板、金属的密合性。进而，在要求在更高温下的可靠性的面向车载的半导体等、要求高密合性的情况下，添加“含硫的硅烷偶联剂”。塑模树脂中包含的硫，如果在175℃以上(例如，175℃～200℃)的条件下使用，则会游离出来。而且，如果在175℃以上的高温下游离出的硫与Cu接触，则Cu的腐蚀变得剧烈，生成硫化物(Cu2S)、氧化物(CuO)。如果在使用了Cu接合线的半导体装置中发生Cu的腐蚀，则特别是球接合部的接合可靠性会下降。
作为评价在170℃以上的高温环境下的球接合部的接合可靠性的方法，可以使用HTS(High Temperature Storage Test)(高温放置试验)。通过对于暴露在高温环境中的评价用样品，测定球接合部的电阻值的经时变化、或者测定球接合部的剪切强度的经时变化，来评价球接合部的接合寿命。近年来，在车载用的半导体装置中，要求提高在175℃～200℃的HTS中的球接合部的接合可靠性。
在本发明中，已判明：当接合线包含选自Ni、Zn、Rh、In、Ir、Pt中的至少1种以上的元素，相对于线整体，上述元素的浓度总计为0.03～2质量％时，球接合部在高温环境下的接合可靠性中，在175℃以上的HTS中的成绩改善。
在此，由下述(1)式定义耐力比。
耐力比＝最大耐力/0.2％耐力(1)
在楔接合中，接合线严重变形。如果变形时线发生加工硬化，则接合后的线***，其结果是楔接合的接合强度下降。为了维持楔接合强度，优选由上述(1)式定义的耐力比为1.6以下。但是，为了提高175℃～200℃的HTS中的球接合部的接合可靠性而使线中含有上述元素时，耐力比增大，变得超过1.6。因此，会造成楔接合的接合强度下降。
本发明的目的是提供一种半导体装置用接合线，其具有Cu合金芯材和在其表面形成的Pd被覆层，在所述接合线中可含有总计为0.03～2质量％的选自Ni、Zn、Rh、In、Ir、Pt中的至少1种以上的元素，且由(1)式定义的耐力比可为1.1～1.6。
即，本发明的要旨如下。
(1)一种半导体装置用接合线，其特征在于，具有Cu合金芯材和在上述Cu合金芯材的表面形成的Pd被覆层，
所述接合线包含选自Ni、Zn、Rh、In、Ir、Pt中的至少1种以上的元素，相对于线整体，上述元素的浓度总计为0.03～2质量％，
在对与上述接合线的线轴垂直的方向的芯材截面测定晶体取向所得到的结果中，线长度方向的晶体取向之中，相对于线长度方向角度差为15度以下的晶体取向<100>的取向比率为50％以上，
与上述接合线的线轴垂直的方向的芯材截面中的平均结晶粒径为0.9～1.3μm。
(2)根据上述(1)所述的半导体装置用接合线，其特征在于，由下述(1)式定义的耐力比为1.1～1.6，
耐力比＝最大耐力/0.2％耐力 (1)。
(3)根据上述(1)或(2)所述的半导体装置用接合线，其特征在于，所述Pd被覆层的厚度为0.015～0.150μm。
(4)根据上述(1)～(3)的任一项所述的半导体装置用接合线，其特征在于，在上述Pd被覆层上还具有包含Au和Pd的合金表皮层。
(5)根据上述(4)所述的半导体装置用接合线，其特征在于，上述包含Au和Pd的合金表皮层的厚度为0.0005～0.050μm。
(6)根据上述(1)～(5)的任一项所述的半导体装置用接合线，其特征在于，上述接合线包含选自Ga、Ge、As、Te、Sn、Sb、Bi、Se中的至少1种以上的元素，相对于线整体，上述元素的浓度合计为0.1～100质量ppm，Sn≤10质量ppm、Sb≤10质量ppm、Bi≤1质量ppm。
(7)根据上述(1)～(6)的任一项所述的半导体装置用接合线，其特征在于，上述接合线还包含选自B、P、Mg、Ca、La中的至少1种以上的元素，相对于线整体，上述元素的浓度分别为1～100质量ppm。
(8)根据上述(1)～(7)的任一项所述的半导体装置用接合线，其特征在于，在上述接合线的最表面存在Cu。
本发明，对于具有Cu合金芯材和在该Cu合金芯材的表面形成的Pd被覆层的半导体装置用接合线，通过使线中含有总计为0.03～2质量％的选自Ni、Zn、Rh、In、Ir、Pt中的至少1种以上的元素，能够提高175℃～200℃的HTS中的球接合部的接合可靠性，进而，在对与接合线的线轴垂直的方向的芯材截面测定晶体取向所得到的结果中，使线长度方向的晶体取向之中、相对于线长度方向角度差为15度以下的晶体取向<100>的取向比率为50％以上，且与接合线的线轴垂直的方向的芯材截面中的平均结晶粒径为0.9～1.3μm，由此能够使由(1)式定义的耐力比为1.1～1.6。
具体实施方式
如前所述，在作为半导体装置的外壳的塑模树脂(环氧树脂)中，包含硅烷偶联剂。硅烷偶联剂具有提高有机物(树脂)与无机物(硅、金属)的密合性的作用，因此，能够提高与硅基板、金属的密合性。进而，在要求在更高温下的可靠性的面向车载的半导体等、要求高密合性的情况下，添加“含硫的硅烷偶联剂”。塑模树脂中包含的硫，如果在175℃以上(例如，175℃～200℃)的条件下使用，则会游离出来。而且，如果在175℃以上的高温下游离出的硫与Cu接触，则Cu的腐蚀变得剧烈，生成硫化物(Cu2S)、氧化物(CuO)。如果在使用了Cu接合线的半导体装置中发生Cu的腐蚀，则特别是球接合部的接合可靠性会下降。
如前所述，近年来，在车载用半导体装置中，要求提高175℃～200℃的HTS(High Temperature Storage Test)(高温放置试验)中的球接合部的接合可靠性。
本发明将具有Cu合金芯材和在上述Cu合金芯材的表面形成的Pd被覆层的半导体装置用接合线作为对象。在本发明中，通过使该接合线包含选自Ni、Zn、Rh、In、Ir、Pt中的至少1种以上的元素，且相对于线整体，上述元素的浓度总计为0.03～2质量％，从而关于球接合部在高温环境中的接合可靠性，在175℃以上的HTS中的成绩改善。具有该特定的构成的本发明的接合线能够改善车载用装置中所要求的高温高湿环境中的球接合部的接合可靠性。
从改善球接合部在高温环境中的接合可靠性(特别是在175℃以上的HTS中的成绩)的观点出发，相对于线整体，上述元素的浓度的总计优选为0.030质量％以上，更优选为0.050质量％以上，进一步优选为0.070质量％以上、0.090质量％以上、0.10质量％以上、0.15质量％以上、或0.20质量％以上。
如前所述，由下述(1)式定义耐力比。
耐力比＝最大耐力/0.2％耐力 (1)
在楔接合中，接合线严重变形。如果变形时线发生加工硬化，则接合后的线***，其结果是楔接合的接合强度下降。为了维持良好的楔接合强度，优选由上述(1)式定义的耐力比为1.6以下。但是，为了提高175℃～200℃的HTS中的球接合部的接合可靠性而使线中含有总计为0.03质量％以上的Ni、Zn、Rh、In、Ir、Pt中的1种以上时，耐力比增大，变得超过1.6。可以认为，在芯材的Cu中含有上述合金成分的结果是发生耐力比的增大、即硬度的增加。因此，会造成楔接合的接合强度下降。另一方面，在以往的制造方法的范围内想要降低耐力比的结果是耐力比变得小于1.1，楔接合性变差。
因此，对于即使接合线含有上述合金成分，也能够将(1)式的耐力比保持在1.1～1.6的合适范围的结晶组织进行了研究。其结果发现，在将(1)式的耐力比保持在合适范围时，控制接合线中的芯材的结晶结构、特别是(i)对与接合线的线轴垂直的方向的芯材截面测定晶体取向所得到的结果中的、线长度方向的晶体取向之中、相对于线长度方向角度差为15度以下的晶体取向<100>的取向比率(以下也简称为“<100>取向比率”。)、和(ii)与接合线的线轴垂直的方向的芯材截面中的平均结晶粒径(以下也简称为“平均结晶粒径”。)是重要的。详细而言，已知：如果利用通常的制造方法制造接合线，则不能同时确保<100>取向比率为50％以上、和平均结晶粒径为0.9μm以上且1.3μm以下，作为其结果，耐力比变为小于1.1或超过1.6。与此相对，明确了以下情况：通过如后所述那样研究制造方法，能够使与接合线的线轴垂直的方向的芯材截面中的线长度方向的晶体取向之中、包含相对于线长度方向角度差为15度以内的<100>的取向比率为50％以上，且与接合线的线轴垂直的方向的芯材截面中的平均结晶粒径为0.9～1.3μm，其结果是，能够使(1)式的耐力比为1.1～1.6。
当<100>取向比率为50％以上时，与楔接合时的变形相伴的线的加工硬化小，因此能够使耐力比为1.6以下。然而，即使是该情况，当平均结晶粒径小于0.9μm时，由于0.2％耐力高(缺乏延展性)，因此耐力比变得小于1.1，楔接合性差。在平均结晶粒径超过1.3μm的情况下，推定由于<100>取向比率变得小于50％，而且0.2％耐力低，因此耐力比超过1.6，楔接合性差。
再者，关于线的结晶结构，即使在满足上述条件的情况下，如果线中的上述元素含量过多，则耐力比也仍会增大。从实现耐力比为1.6以下、抑制接合线的硬质化从而抑制楔接合性下降的观点出发，相对于线整体，选自Ni、Zn、Rh、In、Ir、Pt中的至少1种以上的元素的浓度的总计优选为2.0质量％以下、1.8质量％以下、或1.6质量％以下。
在使接合线中含有Ni、Zn、Rh、In、Ir、Pt时，不论采用使Cu芯材中含有这些元素的方法、使这些元素覆着于Cu芯材或线表面而含有的方法中的哪种方法都能够发挥上述本发明的效果。由于这些成分的添加量是极微量的，因而添加方法的变化(variation)广，无论用怎样的方法添加，只要包含指定的浓度范围的成分，就能显现效果。
在本发明的接合线中，Pd被覆层的厚度，从获得良好的FAB形状的观点以及更进一步改善车载用装置所要求的在高温高湿环境中的球接合部的接合可靠性的观点出发，优选为0.015μm以上，更优选为0.02μm以上，进一步优选为0.025μm以上、0.03μm以上、0.035μm以上、0.04μm以上、0.045μm以上、或0.05μm以上。另一方面，由于即使Pd被覆层的厚度过厚，FAB形状也会下降，因此Pd被覆层的厚度优选为0.150μm以下，更优选为0.140μm以下、0.130μm以下、0.120μm以下、0.110μm以下、或0.100μm以下。
对上述接合线的Cu合金芯材、Pd被覆层的定义进行说明。Cu合金芯材和Pd被覆层的边界以Pd浓度为基准来判定。将Pd浓度为50原子％的位置作为边界，将Pd浓度为50原子％以上的区域判定为Pd被覆层，将Pd浓度小于50原子％的区域判定为Cu合金芯材。其根据是由于在Pd被覆层中如果Pd浓度为50原子％以上，则能够从Pd被覆层的结构获得特性的改善效果。Pd被覆层可以包含仅为Pd的层的区域、Pd和Cu在线的深度方向具有浓度梯度的区域。在Pd被覆层中，具有该浓度梯度的区域形成的原因是，有时通过制造工序中的热处理等，Pd和Cu的原子会扩散。在本发明中，浓度梯度是指在深度方向上的浓度变化的程度是每0.1μm为10mol％以上。进而，Pd被覆层可以包含不可避免的杂质。
本发明的接合线，也可以在Pd被覆层的表面进一步具有包含Au和Pd的合金表皮层。由此，本发明的接合线能够在更加提高接合可靠性的同时进一步改善楔接合性。
对上述接合线的包含Au和Pd的合金表皮层的定义进行说明。包含Au和Pd的合金表皮层与Pd被覆层的边界以Au浓度为基准来判定。将Au浓度为10原子％的位置作为边界，将Au浓度为10原子％以上的区域判定为包含Au和Pd的合金表皮层，将Au浓度小于10原子％的区域判定为Pd被覆层。另外，即使是Pd浓度为50原子％以上的区域，只要存在10原子％以上的Au，就判定是包含Au和Pd的合金表皮层。这样判定的根据是因为，如果Au浓度为上述的浓度范围，就能够从Au表皮层的结构期待特性的改善效果。包含Au和Pd的合金表皮层为Au-Pd合金，为包含Au和Pd在线的深度方向具有浓度梯度的区域的区域。在包含Au和Pd的合金表皮层中，具有该浓度梯度的区域形成的原因是通过制造工序中的热处理等，Au和Pd原子进行扩散。进而，包含Au和Pd的合金表皮层可以包含不可避免的杂质和Cu。
在本发明的接合线中，包含Au和Pd的合金表皮层与Pd被覆层反应，能够提高包含Au和Pd的合金表皮层、Pd被覆层、Cu合金芯材之间的密合强度，能够抑制楔接合时的Pd被覆层、包含Au和Pd的合金表皮层的剥离。由此，本发明的接合线能够进一步改善楔接合性。从获得良好的楔接合性的观点出发，包含Au和Pd的合金表皮层的厚度优选为0.0005μm以上，更优选为0.001μm以上、0.002μm以上、或0.003μm以上。从抑制偏芯、获得良好的FAB形状的观点出发，包含Au和Pd的合金表皮层的厚度优选为0.050μm以下，更优选为0.045μm以下、0.040μm以下、0.035μm以下、或0.030μm以下。再者，包含Au和Pd的合金表皮层能够采用与Pd被覆层的形成方法同样的方法形成。
优选：本发明的接合线还包含选自Ga、Ge、As、Te、Sn、Sb、Bi、Se中的至少1种以上的元素，相对于线整体，上述元素的浓度合计为0.1～100质量ppm，Sn≤10质量ppm、Sb≤10质量ppm、Bi≤1质量ppm。由此，能够进一步改善车载用装置所要求的在高温高湿环境中的球接合部的接合可靠性。特别是提高了在温度为130℃、相对湿度为85％的高温高湿环境下的球接合部的接合寿命、改善接合可靠性，因而优选。相对于线整体，上述元素的浓度的合计优选为0.1质量ppm以上，更优选为0.5质量ppm以上，进一步优选为1质量ppm以上，更进一步优选为1.5质量ppm以上、2质量ppm以上、2.5质量ppm以上、或3质量ppm以上。另一方面，从获得良好的FAB形状的观点出发，相对于线整体，上述元素的浓度的合计优选为100质量ppm以下，更优选为95质量ppm以下、90质量ppm以下、85质量ppm以下、或80质量ppm以下。另外，在Sn浓度、Sb浓度超过10质量ppm的情况下，或者，在Bi浓度超过1质量ppm的情况下，FAB形状变得不良，因此通过设为Sn≤10质量ppm、Sb≤10质量ppm、Bi≤1质量ppm，能够更加改善FAB形状，因而优选。
优选：本发明的接合线还包含选自B、P、Mg、Ca、La中的至少1种以上的元素，相对于线整体，上述元素的浓度分别为1～100质量ppm。由此，能够改善高密度安装中所要求的球接合部的压溃形状，即，能够改善球接合部形状的圆形性。相对于线整体，上述元素的浓度分别优选为1质量ppm以上，更优选为2质量ppm以上、3质量ppm以上、4质量ppm以上、或5质量ppm以上。从抑制球的硬质化、抑制球接合时的芯片损伤的观点出发，相对于线整体，上述元素的浓度分别优选为100质量ppm以下，更优选为95质量ppm以下、90质量ppm以下、85质量ppm以下、或80质量ppm以下。
如本发明那样，在被覆有Pd的Cu接合线含有规定量的Ni、Zn、Rh、In、Ir、Pt的情况下，如果进而在接合线的最表面存在Cu，则有接合部中的Cu9Al4金属间化合物的生成被进一步抑制的倾向。在被覆有Pd的Cu接合线含有规定量的Ni、Zn、Rh、In、Ir、Pt的情况下，如果进而在接合线的最表面存在Cu，则通过接合线中包含的Ni、Zn、Rh、In、Ir、Pt与Cu的相互作用，在形成FAB时FAB表面的Pd浓化被促进，球接合界面的Pd浓化更显著地显现。由此推定：由Pd浓化层引起的抑制Cu与Al的相互扩散的效果进一步变强，由于Cl的作用而容易腐蚀的Cu9Al4的生成量变少，球接合部在高温高湿环境中的接合可靠性进一步提高。
在Pd被覆层的最表面存在Cu的情况下，如果Cu的浓度达到30原子％以上，则线表面的耐硫化性下降，接合线的使用寿命下降，因此有时会不适于实用。因此，在Pd被覆层的最表面存在Cu的情况下，优选Cu的浓度小于30原子％。
另外，在Au表皮层的最表面存在Cu的情况下，如果Cu的浓度达到35原子％以上，则线表面的耐硫化性下降，接合线的使用寿命下降，因此有时会不适于实用。因此，在Au表皮层的最表面存在Cu的情况下，优选Cu的浓度小于35原子％。
在此，最表面是指在不实施溅射等的状态下，利用俄歇电子能谱分析装置测定到的接合线表面的区域。
对于Pd被覆层、包含Au和Pd的合金表皮层的浓度分析，一边利用溅射等从接合线的表面向深度方向削除一边进行分析的方法、或者使线截面露出而进行线分析、点分析等的方法是有效的。用于这些浓度分析的解析装置，可以利用装备在扫描型电子显微镜或透射型电子显微镜中的俄歇电子能谱分析装置、能量色散型X射线分析装置、电子射线显微分析仪等。作为使线截面露出的方法，可以利用机械研磨、离子蚀刻法等。关于接合线中的Ni、Zn、Rh、In、Ir、Pt等的微量分析，可以利用ICP发射光谱分析装置、ICP质量分析装置来分析用强酸溶解接合线而得到的液体，作为接合线整体中包含的元素的浓度而检测出。
(制造方法)
接着，对本发明的实施方式涉及的接合线的制造方法进行说明。接合线是通过制造用于芯材的Cu合金，然后加工成细线状，形成Pd被覆层、Au层，进行热处理而获得的。形成Pd被覆层、Au层后，有时会进行再次拉丝和热处理。对Cu合金芯材的制造方法、Pd被覆层、包含Au和Pd的合金表皮层的形成方法、热处理方法进行详细说明。
用于芯材的Cu合金，是通过将成为原料的Cu与添加的元素一起熔化，使其凝固而获得的。对于熔化，可以利用电弧加热炉、高频加热炉、电阻加热炉等。为了防止从大气中混入O2、H2等气体，优选在真空气氛或Ar、N2等惰性气氛中进行熔化。
在Cu合金芯材的表面形成Pd被覆层、Au层的方法，有镀敷法、蒸镀法、熔融法等。镀敷法可以应用电解镀敷法、无电解镀敷法中的任何方法。在被称为触击镀、闪镀的电解镀敷中，镀敷速度快、与基底的密合性也良好。在无电解镀敷中使用的溶液分为置换型和还原型，在厚度要较薄的情况下仅用置换型镀敷就足够了，在厚度要较厚的情况下在置换型镀敷之后阶段性地实施还原型镀敷是有效的。
在蒸镀法中，可以利用溅射法、离子镀法、真空蒸镀等物理吸附、和等离子体CVD等化学吸附。都是干式方法，不需要形成Pd被覆层、Au层后的洗涤，不用担心洗涤时的表面污染等。
在形成Pd被覆层、Au层后，通过进行热处理，Pd被覆层的Pd向Au层中扩散，形成包含Au和Pd的合金表皮层。也可以从最初就被覆包含Au和Pd的合金表皮层，而不是在形成Au层后通过热处理来形成包含Au和Pd的合金表皮层。
对于Pd被覆层、包含Au和Pd的合金表皮层的形成，在拉丝到最终线径为止然后进行形成的方法、和在形成于粗径的Cu合金芯材上后数次拉丝直到目标线径为止的方法中的任何方法都是有效的。在前者的在最终线径下形成Pd被覆层、包含Au和Pd的合金表皮层的情况下，制造、品质管理等很简便。在后者的将Pd被覆层、包含Au和Pd的合金表皮层与拉丝组合的情况下，在与Cu合金芯材的密合性提高这点上是有利的。作为各形成法的具体例，可举出：对于最终线径的Cu合金芯材，一边使线在电解镀敷溶液中连续地扫掠通过一边形成Pd被覆层、包含Au和Pd的合金表皮层的方法；或者，将粗的Cu合金芯材浸渍在电解镀浴或无电解镀浴中来形成Pd被覆层、包含Au和Pd的合金表皮层，然后将线进行拉丝而达到最终线径的方法；等等。
形成Pd被覆层、包含Au和Pd的合金表皮层后，有时进行热处理。通过进行热处理，在包含Au和Pd的合金表皮层、Pd被覆层、Cu合金芯材之间原子进行扩散，密合强度提高，因此能够抑制加工中的包含Au和Pd的合金表皮层、Pd被覆层的剥离，在生产率提高这点上是有效的。为了防止从大气中混入O2，优选在真空气氛或Ar、N2等惰性气氛中进行热处理。
如前所述，通过调整对接合线实施的扩散热处理、退火热处理的条件，芯材的Cu通过晶界扩散、粒内扩散等在Pd被覆层、包含Au和Pd的表皮合金层中扩散，能够使Cu到达接合线的最表面，能够使Cu存在于最表面。作为用于使Cu存在于最表面的热处理，如上所述，可以使用用于形成包含Au和Pd的合金表皮层的热处理。在进行用于形成合金表皮层的热处理时，通过选择热处理温度和时间，能够使Cu存在于最表面、或不使Cu存在于最表面。进而，也能够将最表面的Cu浓度调整为规定的范围(例如，1～50原子％的范围)。也可以通过在形成合金表皮层时以外进行的热处理来使Cu扩散到最表面。
如前所述，在使接合线中含有Ni、Zn、Rh、In、Ir、Pt时，不论采用使Cu芯材中含有这些元素的方法、使这些元素覆着于Cu芯材或线表面而含有的方法中的哪种方法都能够发挥上述本发明的效果。对于Ga、Ge、As、Te、Sn、Sb、Bi、Se、B、P、Mg、Ca、La也是同样的。
作为上述成分的添加方法，最简便的是预先添加到Cu合金芯材的起始材料中的方法。例如，将高纯度的铜和上述成分元素原料作为起始原料进行称量，然后将其在高真空下或氮气、氩气等惰性气氛下加热、熔化，从而制成添加有目标浓度范围的上述成分的锭，将其作为包含目标浓度的上述成分元素的起始材料。因此，在优选的一个实施方式中，本发明的接合线的Cu合金芯材包含选自Ni、Zn、Rh、In、Ir、Pt中的至少1种以上的元素，使得相对于线整体，上述元素的浓度总计为0.03～2质量％。该浓度合计的优选的数值范围如上所述。在其他优选的一个实施方式中，本发明的接合线的Cu合金芯材包含选自Ga、Ge、As、Te、Sn、Sb、Bi、Se中的至少1种以上的元素，使得相对于线整体，上述元素的浓度合计为0.1～100质量ppm、Sn≤10质量ppm、Sb≤10质量ppm、Bi≤1质量ppm。该浓度的优选的数值范围如上所述。在优选的一个实施方式中，Cu合金芯材的Cu纯度为3N以下(优选为2N以下)。以往的被覆有Pd的Cu接合线，从接合性的观点出发，存在使用高纯度(4N以上)的Cu芯材、避免使用低纯度的Cu芯材的倾向。含有特定元素的本发明的接合线，特别适合于使用如上述那样Cu纯度低的Cu合金芯材的情况，从而实现了车载用装置所要求的在高温高湿环境中的球接合部的接合可靠性。在其他优选的一个实施方式中，本发明的接合线的Cu合金芯材包含选自B、P、Mg、Ca、La中的至少1种以上的元素，使得相对于线整体，上述元素的浓度分别为1～100质量ppm。该浓度的优选的数值范围如上所述。
也可以通过在线制造工序的途中使上述成分覆着于线表面来含有上述成分。在该情况下，可以在线制造工序的任一时间点编入该覆着步骤，可以反复编入多次。可以编入到多个工序中。可以向Pd被覆前的Cu表面添加，可以向Pd被覆后的Pd表面添加，可以向Au被覆后的Au表面添加，也可以编入到各被覆工序中。作为覆着方法，可以从(1)水溶液的 (2)镀敷法(湿式)、(3)蒸镀法(干式)中选择。
在采用水溶液的的方法的情况下，首先用包含上述成分元素的水溶性化合物调制出适当浓度的水溶液。由此，能够将上述成分纳入线材料中。可以在线制造工序的任一时间点编入该覆着方法，可以反复编入多次。可以编入到多个工序中。可以向Pd被覆前的Cu表面添加，可以向Pd被覆后的Pd表面添加，可以向Au被覆后的Au表面添加，也可以编入到各被覆工序中。
在使用镀敷法(湿式)的情况下，镀敷法可以应用电解镀敷法、无电解镀敷法中的任何方法。在电解镀敷法中，除了通常的电解镀敷以外，还可以应用被称为闪镀的镀敷速度快且与基材的密合性也良好的镀敷法。用于无电解镀敷的溶液有置换型和还原型。一般而言，在镀层厚度要较薄的情况下可应用置换型镀敷，在镀层厚度要较厚的情况下可应用还原型镀敷，但是哪种都可以应用，按照想要添加的浓度来选择，调节镀液浓度、时间即可。电解镀敷法、无电解镀敷法均可以在线制造工序的任一时间点编入，可以反复编入多次。可以编入到多个工序中。可以向Pd被覆前的Cu表面添加，可以向Pd被覆后的Pd表面添加，可以向Au被覆后的Au表面添加，也可以编入到各被覆工序中。
在蒸镀法(干式)中有溅射法、离子镀法、真空蒸镀法、等离子体CVD等。由于是干式的，因此不需要预处理和后处理，不用担心污染，这是优点。一般而言，蒸镀法，存在目标元素的添加速度慢的问题，但是上述成分元素的添加浓度比较低，因此它是适合本发明的目的的方法之一。
各蒸镀法，可以在线制造工序的任一时间点编入，可以反复编入多次。可以编入到多个工序中。可以向Pd被覆前的Cu表面添加，可以向Pd被覆后的Pd表面添加，可以向Au被覆后的Au表面添加，也可以编入到各被覆工序中。
对用于实现下述目标的制造方法进行说明：在对与接合线的线轴垂直的方向的芯材截面测定晶体取向所得到的结果中，线长度方向的晶体取向之中，相对于线长度方向角度差为15度以下的晶体取向<100>的取向比率为50％以上，与接合线的线轴垂直的方向的芯材截面中的平均结晶粒径为0.9～1.3μm。
本发明的接合线，在Cu合金芯材中含有总计为0.03质量％以上的Ni、Zn、Rh、In、Ir、Pt中的1种以上，因此线的材料强度(硬度)变高。因此，在对Cu芯线的接合线进行拉丝加工时，将拉丝时的减面率设为5～8％的低的减面率。另外，在拉丝后的热处理中，硬度仍然高，因此为了软质化到能够作为接合线使用的水平，在600℃以上的温度下进行了热处理。由于是高的热处理温度，因此线长度方向的<100>取向比率变为小于50％，同时，芯材截面中的平均结晶粒径变为超过1.3μm，耐力比变为超过1.6。另一方面，如果想要降低耐力比而降低热处理温度的话，则芯材截面中的平均结晶粒径变为小于0.9μm，耐力比变为小于1.1，楔接合性变差。
与此相对，在本发明中，在使用了拉模的拉丝时，在拉模总数之中的一半以上的拉模中，减面率设为10％以上，进而将拉丝后的热处理中的热处理温度设为500℃以下的低的温度。其结果是能够实现下述目标：在对与接合线的线轴垂直的方向的芯材截面测定晶体取向所得到的结果中，线长度方向的晶体取向之中，相对于线长度方向角度差为15度以下的晶体取向<100>的取向比率为50％以上，与接合线的线轴垂直的方向的芯材截面中的平均结晶粒径为0.9～1.3μm。通过应用最新的拉丝加工技术，作为润滑液设计成使润滑液中包含的非离子系表面活性剂的浓度比以往高，作为拉模形状设计成使拉模的主偏角比以往的拉模的主偏角平缓，将拉模的冷却水温度设定成比以往低等等的协同效应，尽管Cu合金芯材中含有总计为0.03质量％以上的Ni等成分而硬质化，但是能够实现减面率为10％以上的拉丝加工。
在测定线截面的晶体取向时，优选使用电子射线背散射衍射法(EBSD，Electron Backscattered Diffraction)。EBSD法具有能够观察观察面的晶体取向，能够图示在相邻的测定点间的晶体取向的角度差这样的特征，即使是如接合线那样的细线，也能够比较简便且高精度地观察晶体取向。关于粒径测定，可针对EBSD法的测定结果，利用装于装置中的解析软件来求出。本发明中规定的结晶粒径是将在测定区域内包含的晶粒的等效直径(与晶粒面积对应的圆的直径；等效圆直径)进行算术平均而得到的值。
本发明并不被上述实施方式限定，可以在本发明的主旨的范围内进行适当变更。
实施例
以下一边示出实施例一边对本发明的实施方式涉及的接合线进行具体说明。
(样品)
首先，对样品的制作方法进行说明。成为芯材的原材料的Cu，使用了纯度为99.99质量％以上且其余量由不可避免的杂质构成的Cu。Au、Pd、Ni、Zn、Rh、In、Ir、Pt使用了纯度为99质量％以上且其余量由不可避免的杂质构成的材料。调合作为向芯材添加的元素的Ni、Zn、Rh、In、Ir、Pt，使得线或芯材的组成成为目标组成。关于Ni、Zn、Rh、In、Ir、Pt的添加，可以是用单质来进行调合，但是在为单质具有高熔点的元素、和/或添加量为极微量的情况下，也可以预先制作包含添加元素的Cu母合金，再进行调合使得成为目标的添加量。另外，在下述表3所示的本发明例中，还含有Ga、Ge、As、Te、Sn、Sb、Bi、Se、B、P、Mg、Ca、La中的1种以上。
芯材的Cu合金通过连铸而制成数mm的线径。对于所得的数mm的合金，进行拉拔加工，制作出Ф0.3～1.4mm的线。在拉丝中使用市售的润滑液，将拉丝速度设为20～150m/分钟。为了除去线表面的氧化膜，利用盐酸等进行酸洗处理，然后以覆盖芯材的Cu合金的表面整体的方式形成了1～15μm厚度的Pd被覆层。进而，一部分线在Pd被覆层上形成了0.05～1.5μm厚度的包含Au和Pd的合金表皮层。对于Pd被覆层、包含Au和Pd的合金表皮层的形成，使用了电解镀敷法。镀液使用了市售的半导体用镀液。然后，主要使用减面率为10～21％的拉模进行拉丝加工，而且在途中在200～500℃下进行1～3次的热处理，由此加工到直径20μm。加工后，最终进行了热处理使得断裂伸长率约为5～15％。热处理方法，是一边使线连续地扫掠通过一边进行，一边流通N2或Ar气一边进行。送线速度设为10～90m/分钟，热处理温度为350～500℃，热处理时间设为1～10秒。
(评价方法)
关于线中的Ni、Zn、Rh、In、Ir、Pt、Ga、Ge、As、Te、Sn、Sb、Bi、Se、B、P、Mg、Ca、La的含量，利用ICP发射光谱分析装置，以接合线整体中所包含的元素的浓度的形式来分析。
作为Pd被覆层、包含Au和Pd的合金表皮层的浓度分析，是一边从接合线的表面向深度方向利用溅射等削除一边实施俄歇电子能谱分析。从所得的深度方向的浓度廓线，求出Pd被覆层厚度、包含Au和Pd的合金表皮层厚度。
关于与接合线的线轴垂直的方向的芯材截面中的线长度方向的晶体取向之中，相对于线长度方向角度差为15度以下的晶体取向<100>的取向比率，在利用EBSD法观察观察面(即，与线轴垂直的方向的芯材截面)的晶体取向的基础上算出。作为EBSD测定数据的解析，利用了专用软件(TSLソリューションズ制OIM analisis等)。关于与线轴垂直的方向的芯材截面中的平均结晶粒径，在利用EBSD法观察观察面的晶体取向的基础上算出。作为EBSD测定数据的解析，利用了专用软件(TSLソリューションズ制OIM analisis等)。结晶粒径，是将在测定区域内包含的晶粒的等效直径(与晶粒的面积对应的圆的直径；等效圆直径)进行算术平均而得到的值。
关于0.2％耐力(产生0.2％残余应变时的应力；条件屈服强度)和最大耐力，是通过将标点间距离设为100mm进行拉伸试验来评价的。作为拉伸试验装置，使用了インストロン公司制的万能材料试验机5542型。0.2％耐力使用在装置中安装的专用软件算出。另外，将断裂时的载荷作为最大耐力。由下述(1)式算出耐力比。
耐力比＝最大耐力/0.2％耐力 (1)
线接合部中的楔接合性的评价，是在BGA基板的楔接合部进行1000根的接合，利用接合部的剥离发生频度来判定的。使用的BGA基板是施加了Ni以及Au的镀层的基板。在本评价中，设想比通常严格的接合条件，将台(stage)温度设定为比一般的设定温度域低的150℃。在上述的评价中，在发生了11个以上的不良的情况下，判断为有问题，记为×符号；如果不良为6～10个，则能够实用但稍有问题，记为△符号；在不良为1～5个的情况下，判断为无问题，记为○符号；在没有发生不良的情况下，判断为优异，记为◎符号，都标记在表1的“楔接合性”栏中。
高温高湿环境或高温环境中的球接合部的接合可靠性，是制作接合可靠性评价用的样品，进行HTS评价，根据球接合部的接合寿命来判定的。接合可靠性评价用的样品，是在一般的金属框上的Si基板上形成厚度0.8μm的Al-1.0％Si-0.5％Cu的合金膜而形成电极，对该电极使用市售的线焊接机进行球接合，利用市售的环氧树脂进行封装而制作的。球是一边使N2+5％H2气体以0.4～0.6L/min的流量流通一边形成的，其大小设为Ф33～34μm的范围。
关于HTS评价，将所制作的接合可靠性评价用的样品，使用高温恒温器，暴露在温度200℃的高温环境中。球接合部的接合寿命设为，每500小时实施球接合部的剪切试验，剪切强度的值变为初期所获得的剪切强度的1/2的时间。高温高湿试验后的剪切试验，是通过酸处理来除去树脂，使球接合部露出后进行的。
HTS评价的剪切试验机使用了DAGE公司制的试验机。剪切强度的值，采用随机选择的球接合部的10处位置的测定值的平均值。在上述的评价中，如果接合寿命为500小时以上且小于1000小时，则判断为能够实用但希望改善，记为△符号；如果接合寿命为1000小时以上且小于3000小时，则判断为实用上无问题，记为○符号；如果接合寿命为3000小时以上，则判断为特别优异，记为◎符号。
球形成性(FAB形状)的评价，是采取进行接合之前的球进行观察，判定球表面有无气泡、本来作为圆球的球有无变形。在发生了上述任一现象的情况下都判断为不良。关于球的形成，为了抑制熔融工序中的氧化，一边以0.5L/min的流量吹N2气一边进行。球的大小设为34μm。对于1个条件观察50个球。观察时使用了SEM。关于球形成性的评价，在发生了5个以上的不良的情况下，判断为有问题，记为×符号；如果不良为3～4个，则能够实用但稍有问题，记为△符号；在不良为1～2个的情况下判断为无问题，记为○符号；在没有发生不良的情况下，判断为优异，记为◎符号，都标记在表1的“FAB形状”栏中。
关于温度为130℃、相对湿度为85％的高温高湿环境下的球接合部的接合寿命，可以利用以下的HAST评价来进行评价。关于HAST评价，将制作出的接合可靠性评价用的样品，使用不饱和型压力锅蒸煮试验机，暴露在温度130℃、相对湿度85％的高温高湿环境中，施加5V的偏电压。球接合部的接合寿命设为，每48小时实施球接合部的剪切试验，剪切强度的值变为初期所获得的剪切强度的1/2的时间。高温高湿试验后的剪切试验，是通过酸处理来除去树脂，使球接合部露出后进行的。
HAST评价的剪切试验机使用了DAGE公司制的试验机。剪切强度的值，采用了随机选择的球接合部的10处位置的测定值的平均值。在上述的评价中，如果接合寿命为144小时以上且小于288小时，则判断为实用上无问题，记为○符号；如果接合寿命为288小时以上且小于384小时，则判断为优异，记为◎符号；如果接合寿命为384小时以上，则判断为特别优异，记为◎◎符号，都标记在表1的“HAST”栏中。
球接合部的压溃形状的评价，是从正上方观察进行了接合的球接合部，根据其圆球性来判定。接合对象使用了在Si基板上形成厚度1.0μm的Al-0.5％Cu的合金膜而成的电极。观察时使用光学显微镜，对于1个条件观察200处。将与圆球的偏差大的椭圆状的情况、变形具有异向性的情况判断为球接合部的压溃形状不良。在上述的评价中，在不良为1～3个的情况下判断为无问题，记为○符号；在全部获得了良好的圆球形的情况下，判断为特别优异，记为◎符号，都标记在表1的“压溃形状”栏中。
(评价结果)
表1的本发明例1～26涉及的接合线，具有Cu合金芯材和在Cu合金芯材的表面形成的Pd被覆层，Pd被覆层的厚度在作为合适范围的0.015～0.150μm的范围，FAB形状均良好。另外，接合线包含选自Ni、Zn、Rh、In、Ir、Pt中的至少1种以上的元素，相对于线整体，上述元素的浓度合计为0.03～2质量％，因此确认到HTS评价中的球接合部高温可靠性良好。
另外，关于本发明例1～26，将拉丝时的减面率设为10％以上，拉丝后的热处理中的热处理温度设为500℃以下的低的温度，因此能够实现下述目标：在对与接合线的线轴垂直的方向的芯材截面测定晶体取向所得到的结果中，线长度方向的晶体取向之中，相对于线长度方向角度差为15度以下的晶体取向<100>的取向比率为50％以上，与接合线的线轴垂直的方向的芯材截面中的平均结晶粒径为0.9～1.3μm。其结果是，尽管在线中含有Ni、Zn、Rh、In、Ir、Pt，但是耐力比(＝最大耐力/0.2％耐力)都在1.1～1.6的范围内。因此，得到了楔接合性都良好的结果。
另一方面，表2的比较例4～6，将热处理温度设为600℃以上的高的温度，因此线长度方向的<100>取向比率小于50％。另外，比较例2、7～9，将热处理温度设为620℃以上的高的温度，因此线长度方向的<100>取向比率小于50％，并且，芯材截面中的平均结晶粒径超过1.3μm。因此，比较例2、4～9都是耐力比超过1.6，楔接合性都不良。
另外，比较例1、3，将拉模的减面率设为小于10％，因此芯材截面中的平均结晶粒径小于0.9μm，耐力比小于1.1，楔接合性都不良。

Claims (8)

1.一种半导体装置用接合线，其特征在于，具有Cu合金芯材和在所述Cu合金芯材的表面形成的Pd被覆层，
所述接合线包含选自Ni、Zn、Rh、In、Ir、Pt中的至少1种以上的元素，相对于线整体，所述元素的浓度总计为0.03～2质量％，
在对与所述接合线的线轴垂直的方向的芯材截面测定晶体取向所得到的结果中，线长度方向的晶体取向之中，相对于线长度方向角度差为15度以下的晶体取向<100>的取向比率为50％以上，
与所述接合线的线轴垂直的方向的芯材截面中的平均结晶粒径为0.9～1.3μm。
2.根据权利要求1所述的半导体装置用接合线，其特征在于，由下述(1)式定义的耐力比为1.1～1.6，
耐力比＝最大耐力/0.2％耐力 (1)。
3.根据权利要求1或2所述的半导体装置用接合线，其特征在于，所述Pd被覆层的厚度为0.015～0.150μm。
4.根据权利要求1～3的任一项所述的半导体装置用接合线，其特征在于，在所述Pd被覆层上还具有包含Au和Pd的合金表皮层。
5.根据权利要求4所述的半导体装置用接合线，其特征在于，所述包含Au和Pd的合金表皮层的厚度为0.0005～0.050μm。
6.根据权利要求1～5的任一项所述的半导体装置用接合线，其特征在于，所述接合线包含选自Ga、Ge、As、Te、Sn、Sb、Bi、Se中的至少1种以上的元素，相对于线整体，所述元素的浓度合计为0.1～100质量ppm，Sn≤10质量ppm、Sb≤10质量ppm、Bi≤1质量ppm。
7.根据权利要求1～6的任一项所述的半导体装置用接合线，其特征在于，所述接合线还包含选自B、P、Mg、Ca、La中的至少1种以上的元素，相对于线整体，所述元素的浓度分别为1～100质量ppm。
8.根据权利要求1～7的任一项所述的半导体装置用接合线，其特征在于，在所述接合线的最表面存在Cu。
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