CN1732291B - 无铅凸点及该凸点的形成方法 - Google Patents

无铅凸点及该凸点的形成方法 Download PDF

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CN1732291B
CN1732291B CN2003801074750A CN200380107475A CN1732291B CN 1732291 B CN1732291 B CN 1732291B CN 2003801074750 A CN2003801074750 A CN 2003801074750A CN 200380107475 A CN200380107475 A CN 200380107475A CN 1732291 B CN1732291 B CN 1732291B
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salient point
concentration
alloy
plating
unleaded
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CN1732291A (zh
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下山正
横田洋
黄海冷
栗山文夫
斋藤信利
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Ebara Corp
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Abstract

本发明涉及一种通过将调整了镀膜中的Ag浓度的Sn-Ag类焊锡合金镀膜进行回流得到的抑制空隙产生的无铅凸点及该凸点的形成方法。本发明的无铅凸点是通过电镀形成Ag含量比Sn-Ag的共晶形成浓度低的Sn-Ag类合金膜，并通过回流该合金镀膜得到的。

Description

无铅凸点及该凸点的形成方法
技术领域
本发明涉及无铅凸点及该凸点的形成方法，更具体地讲，涉及通过将调整了镀膜中的Ag浓度的Sn-Ag类焊锡合金镀膜进行回流所得到的抑制空隙产生的无铅凸点及该凸点的形成方法，以及形成无铅凸点形成用电镀装置。
背景技术
在半导体元件等的表面安装技术中，可靠性良好地进行焊锡加工是非常重要的。迄今为止，作为焊锡广泛使用的是含有铅的共晶焊锡(Sn∶Pn＝63∶37)，但是由于环境污染和由铅产生的α射线问题，因此正在进行无铅焊锡的开发。
例如正在进行通过印刷法和电镀法的无铅焊锡的研究，但是在印刷法中存在与通过金属掩模形成的精细节距所对应的界限，因此在形成晶片凸点中，电镀法正成为主流。
可是以电镀法形成晶片凸点(bump)的情况下，为了使形成的镀膜成为球形，通常进行加热操作(回流，reflowing)。为了避免对基板上存在的其它部件造成热损伤，该回流温度优选为尽可能低的温度。因此可以认为在多数合金的开发中，利用共晶点，使合金的组成比非常接近共晶组成。
但是在回流通过电镀法形成的凸点时，存在所谓在凸点内产生空隙的问题。特别是在Sn-Ag类合金的凸点情况下，空隙的产生率高，从而使得作为凸点的可靠性显著降低。
发明内容
因而本发明的课题是：寻求一种通过电镀法形成在回流后不产生空隙的Sn-Ag类的无铅凸点的方法的开发，并提供这样的方法。
本发明者们为了得到不产生空隙的无铅凸点进行了研究，结果发现在通过电镀Sn-Ag类焊锡合金形成凸点的情况下，该镀膜所含有的Ag浓度对于空隙的产生影响较大。更具体地讲，如果Sn-Ag类无铅凸点所含有的Ag浓度由Sn-Ag的共晶组成比附近变为组成比或以上，则可以判定回流后在凸点内产生空隙。并且进行了进一步地研究，结果发现，在凸点中使用Sn-Ag类焊锡合金镀膜时，为了确实防止凸点内空隙的产生，必需使用Ag浓度比Sn-Ag的共晶组成比(重量比、Sn∶Ag＝96.5∶3.5/Ag含量为3.5质量％)低的合金镀膜，从而形成凸点。
并且可以认为，如果Ag浓度比Sn-Ag的共晶组成比还低，回流温度上升，即使Ag含有浓度下降，也没有发现熔点有大的上升，也没有必要使得回流温度大大地上升。
本发明是基于上述发现完成的，提供一种无铅凸点，其是通过电镀形成Ag含量比Sn-Ag的共晶形成浓度低的Sn-Ag类合金膜，并通过回流该合金镀膜得到的。
另外，本发明提供一种无铅凸点的形成方法，其是在欲形成凸点的部分中，一边控制镀浴组成和电析条件一边进行Sn-Ag类合金电镀，以形成Ag含量比Sn-Ag的共晶形成浓度低的Sn-Ag类合金膜，接着回流得到的该合金镀膜。
再者，本发明提供一种无铅凸点形成用电镀装置，其具有装有含有Ag离子和Sn离子的镀液的镀槽、阳极、保持被处理物并对该被处理物供电的电极夹、对上述阳极和用上述电极夹保持的各个被处理物供电的电析用电源、补充Ag离子和Sn离子的补偿机构、监测Ag离子和Sn离子的分析装置、和基于来自上述分析装置的分析信息而将在上述被处理物的表面上形成的Sn-Ag类合金镀膜中的Ag含量控制到低于Sn-Ag的共晶形成浓度的控制机构。
附图说明
图1是表示合金镀液中Ag离子和Sn离子浓度比和镀膜中的Ag含有浓度的关系的图。
图2是表示在连续地外加直流进行电镀时的电流密度和镀膜中的Ag的含有浓度的关系的图。
图3是表示在连续地外加直流进行电镀时(连续直流电镀)和间歇地外加直流进行电镀时(间歇电镀)镀膜中的Ag的含有浓度的差异的图。
图4是表示一例本发明电镀装置的图。
图5是表示一例回流处理中使用的红外线加热炉的图。
图6A是表示在实施例1中进行Ag的定量分析时试样回流前的采集部分的图，图6B表示在实施例1中进行Ag的定量分析时试样回流后的采集部分的图。
图7A是表示实施例1中回流前的凸点的SEM照片，图7B是图7A中所示的凸点在225℃下回流后的SEM照片，图7C是图7A中所示的凸点在230℃下回流后的SEM照片，图7D是图7A中所示的凸点在238℃下回流后的SEM照片。
图8是Ag浓度为2.6质量％的Sn-Ag类合金镀膜在238℃下回流而形成的凸点截面的SEM照片。
图9是Ag浓度为3.4质量％的Sn-Ag类合金镀膜在238℃下回流而形成的凸点截面的SEM照片。
具体实施方式
本发明的无铅凸点，是通过控制电析条件以使Ag浓度为低于Sn-Ag的共晶形成浓度中的含量(3.5质量％或以下)的Sn-Ag类合金电镀(以下简单称为“合金电镀”)来使Sn-Ag类合金镀膜析出，接着通过将其回流而得到的。
从防止空隙产生的观点来看，只控制合金镀膜中的Ag浓度的上限为上述浓度即可，但是如果Ag浓度在2.6～3.5质量％之间，有时产生空隙有时不产生空隙，因此从完全避免空隙的角度考虑，合金镀膜中的Ag浓度优选在2.6质量％或以下。
另外从实用性方面来看，优选回流温度基本不升高(例如最高回流温度在240℃或以下)。为此合金镀膜所含有的Ag浓度的下限优选为1.6质量％。即，为了在实际应用中形成优选的凸点，合金镀膜中的Ag浓度优选为1.6～2.6质量％，
象这样地，在本发明中，必需一边将合金镀膜中的Ag浓度控制在3.5质量％或以下、优选为1.6～2.6质量％，一边进行电镀。
另外如上所述，通过回流合金镀膜所得到的无铅凸点，其表面放出的α射线放出量优选在0.02cph/cm2或以下。
在铅中，存在含有天然放射线元素的多个同位素。铅的同位素是铀和钍衰变系列中的中间产物或者最终产物，在衰变过程中放出α射线。α射线在作用于半导体集成电路的半导体元件时存在引起软错误的问题。对于Sn和其它元素也少量含有这些天然放射性元素，因此在Sn-Ag类无铅凸点中将α射线放出及其放出量抑制到较低也是很重要的。因此通过控制由无铅凸点的表面放出的α射线放出量低至0.02cph/cm2或以下，可以抑制由于α射线对半导体集成电路元件的影响而产生的软错误。
一般在合金电镀中的析出成分的组成取决于镀液中各种成分的浓度和电析条件。因此在本发明的合金电镀中，也可以通过调整合金镀液中的Ag离子和Sn离子的浓度比或控制电析条件，使得合金镀膜中的Ag浓度在上述范围内。具体地讲可以通过(a)固定镀浴中Ag离子和Sn离子的浓度比、改变电析条件来控制合金镀膜中的Ag浓度的方法，或(b)固定电析条件、改变镀浴中的Ag离子和Sn离子的浓度比来控制合金镀膜中的Ag浓度。
即在合金镀液中，除了形成合金的金属离子以外，还可以混合使得金属离子稳定化的络合剂、用于完美地形成镀膜表面的光泽剂或者其它添加剂。但是主要决定合金镀膜中的Ag浓度的是合金镀浴中的Ag离子和Sn离子的浓度比，由此发现了实验上的优选的范围，通过一边维持该浓度比一边进行电镀，可以制得Ag浓度被控制的合金镀膜。实际上，在固定电析条件的状态下进行合金电镀的情况下，如图1所示意地表示的那样，所示合金镀膜中的Ag浓度，与镀液中存在的Ag离子和Sn离子的浓度比存在比例关系。
因此，如果在Ag离子和Sn离子浓度为预定浓度比的合金镀液中浸渍被处理物，并且在一定的电析条件下电镀，可以制得控制了Ag浓度的合金镀膜，通过将其回流，可以得到没有产生空隙的凸点。
作为本发明中使用的一例合金镀液，可以列举以下的镀液。组成：
Sn离子(Sn2+)：10～100g/L(优选的是35～50g/L)
Ag离子(Ag+)：0.3～8g/L(优选的是0.6～4g/L)
甲磺酸：100g/L
另外，在合金电镀中，已知的是由于电析条件的不同导致析出成分的组成不同，在本发明的合金电镀中也可以通过改变电析条件而改变合金镀膜中的Ag浓度。
本发明的合金电镀可以在各种电流模式下进行，既可以是连续地外加直流电流进行电镀的直流电镀，也可以是通过间歇地外加直流电流进行电镀的周期性的存在停止期的间歇电镀。
在连续地外加直流电流进行电镀的直流电镀情况下，如图中2示意地表示的那样，由于存在电流密度越高则合金镀膜中的Ag的含有浓度越低的关系，因此根据实验确定优选的电流条件，只要一边维持该条件一边电镀即可。直流电镀时优选的电流密度是10～100mA/cm2左右。
另外，在通过间歇地外加直流电流进行电镀周期性地存在停止期的间歇电镀的情况下，如图3示意地所表示的那样，连续地外加直流时与间歇地外加同样电流时Ag的含有浓度不同，因此在这种情况下，也通过实验决定优选的外加电压和间隙时间的比例等，一边维持该条件一边进行电镀即可。这种间歇电镀时的优选外加时电流密度是10～200mA/cm2左右，间隙时间(0电流)在外加时间的1/10～1的范围。
上述两种电镀中的外加电压是根据电流强度、底层材料、厚度、电镀液、阳极等条件也会有变动，但是优选为1～5V左右。
作为用于实施上述合金电镀的装置，没有特别的限制，可以使用一般浸渍式电镀装置等。但是在实际操作时，优选使用考虑了被处理物的机械条件的夹具结构、用于向晶片(wafer)等被处理物的整个表面均匀并且迅速供给金属离子的搅拌机构(桨片结构)、考虑用于使得电场分布均匀的掩模的形状和大小、除去杂物、防止镀液的变质、用于均匀并且迅速向被处理物整个表面提供金属离子的镀液循环系统等的装置。
另外如上所述，由于需要一边调整镀液中Ag离子和Sn离子的浓度以及控制电析条件一边进行合金电镀，因此优选使用补充Ag离子以及Sn离子的补充机构、监测Ag离子和Sn离子的分析装置和具有将在来自分析装置的分析信息基础上，用于调整合金镀液中Ag离子和Sn离子的浓度和/或控制电析条件的控制机构的电镀装置。该电镀装置的一例如图4中所示。
图4中，1表示电镀装置，2表示电镀槽，3表示阳极，4表示夹具，5表示被处理物，6表示电析用电源，7表示导电线，8a～8c表示补充机构，9表示分析装置，10表示控制机构，11表示自动取样器，12a～12c表示送液泵，13表示开关阀，14表示排液口。
其中分析装置9是作为控制电镀的指针，其是对由于电镀装置运转中消耗或损失所产生的Ag离子和Sn离子浓度变化进行定期或者连续地分析并监测的装置，例如可以使用原子吸光分析装置等。
另外，控制机构10例如是控制用的计算机，根据来自分析装置9的分析信息，求得Ag离子(溶液)、Sn离子(溶液)等的最佳补充量，使得与补充机构8a～8c连接的送液泵12a～12c运转，向镀液中添加Ag离子(溶液)和Sn离子(溶液)等。
另外，在补充机构8a～8c中，除了补充Ag离子溶液和Sn离子溶液部分之外，还可以追加补充用于调整镀液组成的水和添加剂的部分。
上述阳极3、夹具4和电镀槽2是用可以将α射线放出量抑制到较低的材料构成的，以使从由电镀装置1形成的Sn-Ag类合金镀膜表面上放出的α射线放出量在0.02cph/cm2或以下。这样一来，通过将在由电镀形成的合金镀膜构成的凸点中放出的上述天然放射线元素抑制到较低，从而将由凸点放出的α射线量抑制到较低，进而可以抑制由于α射线对半导体集成电路元件的影响所产生的软错误。
阳极3既可以是不溶解性阳极，也可以是溶解性阳极。通过将阳极3设定为不溶解性阳极，不用交换即可以继续使用。另外在使用溶解性阳极作为阳极3的情况下，通过使用Sn阳极，可以在由阳极电镀Sn离子的过程中供给镀液，由此可以减轻镀液的管理和金属离子的补给操作。
上述控制机构10优选控制为相对于镀液组成最佳的电析条件(上述外加电流密度和电压外加方法)，必须至少维持根据上述Ag离子和Sn离子的补充量进行控制的任何一方。
实际电镀的析出操作，不仅受到上述合金镀液中的Ag离子和Sn离子的浓度比和电析条件的影响，还要受到多种因素的影响。例如根据镀液中添加的多种添加剂，也会使得合金镀膜中的Ag浓度发生改变。但是在多数情况下，这些添加剂的物质名和添加量作为添加剂制造商的窍门而未公开。
因而，在形成本发明的凸点时，在一定的合金镀液中，必须预先通过改变电镀的电流密度、电压外加方法、镀液中的Ag离子和Sn离子的浓度比进行实验，测定形成的凸点所含有的Ag的重量浓度，在此基础上求得最佳条件进行合金电镀。
由此可以使得镀液的组成稳定化，另外可以稳定地形成具有所希望的Ag含有浓度的凸点。
将按照上述形成的合金镀膜，接着进行回流处理使之成为凸点。该回流处理例如通过使用图5中所示的装置(红外线加热炉)、在惰性气体氛围(例如氮和氩气氛)中加热进行。图5中20表示红外线加热炉，21表示燃烧室，22表示载物台，23表示石英玻璃窗，24表示红外灯，25表示被处理物。
通过该装置的回流，例如通过在燃烧室21中固定进行合金电镀的被处理物25，向该燃烧室21中以8～30L/min左右的速度通入氮气，进行充分地气体交换后，通过石英玻璃窗23，用红外灯24加热来进行。
在本发明的凸点形成中，回流温度是重要的。凸点在印刷电路板等上形成，但一般电子部件的耐热温度通常认为是240℃。因此在通过合金电镀形成的合金镀膜的回流工序中的最高温度需要控制在240℃或以下。另外一般来说Sn-Ag类焊锡的熔点是221℃，一般可以回流的最低温度是需要在熔点+10℃下保持15秒～45秒。作为考虑这种条件时的回流温度条件的一例，可以列举出，在231℃下保持30秒钟、最高到达温度为238℃的温度条件。
以上所说明的本发明的无铅凸点，例如可以用作实装基板中的配线衬垫上的球状凸点。
该球状凸点的形成，首先在形成金属焊垫(bond pad)后，残留凸点的形状涂覆抗蚀剂，形成抗蚀剂图案。接着根据上述方法形成Ag浓度被控制的Sn-Ag类合金镀膜。然后剥离抗蚀剂，通过在规定的回流温度下处理来进行。
在上述方法中，金属焊垫的形成、抗蚀剂图案的形成和抗蚀剂的去除，可以根据该技术领域中任何一种常规方法进行。
另外本发明的无铅凸点是为了在各种半导体基板上形成配线衬垫而被使用的。具体地讲，通过如下(I)～(IV)的工序可以在半导体元件的半导体基板上形成无铅凸点。
(I)在半导体元件的半导体基板上形成配线衬垫的工序。
(II)在形成的配线衬垫上形成阻障金属(barrier metal)的工序。
(III)在阻障金属上形成Sn-Ag类镀层的工序。
(IV)将Sn-Ag类镀层回流的工序。
作为上述(I)的半导体元件，包含集成电路(IC)等。另外作为配线衬垫中形成的(II)的阻障金属，可以使用公知的阻障金属。
其次列举实施例和比较例更详细地说明本发明，但是本发明并不受到这些实施例的任何限制。
实施例1
(1)Sn-Ag类凸点的调制
在晶片上涂覆120μm厚的抗蚀剂以形成多个开口径Φ为100μm的孔，作为试样。该试样的电镀面积是149.63cm2。针对该试样在如下的工序和条件下进行电镀。
(电镀工序)
脱气(10分钟)→用10％硫酸前洗涤(1分钟)→镀铜→水洗→镀Ni→水洗→电镀Sn-Ag类合金
(电镀条件)
(a)镀铜
镀浴组成：
Cu2+              220g/L
H28O4           200g/L
HCl                5mL/L
添加剂             5mL/L
电镀温度：25℃
搅拌：机械搅拌(桨片搅拌速度10m/min)
镀液循环：流量2.5L/min
电极：铜阳极、电极间距离约7.5mm、阳极掩模Φ250mm
阴极电流密度(总电流)：5A/dm2(7.48A)
镀层厚度：2μm
(b)镀Ni
镀浴组成：
Ni(NH2SO4)·4H2O       450g/L
H3BO3                   30g/L
NiCl2·6H2O             10g/L
添加剂                     2mL/L
电镀温度：50℃
搅拌：机械搅拌(桨片搅拌速度10m/min)
镀液循环：流量2.5L/min
电极：镍阳极、电极间距离约75mm、阳极掩模Φ250mm
阴极电流密度(总电流)：3A/dm2(4.49A)
镀层厚度：3μm
(c)镀Sn-Ag
镀浴组成：
Sn2+                      40g/L
Ag+                       1.5g/L
甲磺酸                     100g/L
添加剂                     10g/L
(将聚氧乙烯类表面活性剂、硫脲、邻苯二酚以重量比计为2∶2∶1的物质)
电镀温度：25℃
搅拌：机械搅拌(桨片搅拌速度10m/min)
镀液循环：流量2.5L/min
电极：钛阳极、电极间距离约7.5mm、阳极掩模Φ250mm
阴极电流密度(总电流)：10A/dm2(14.9A)、直流电镀
镀层厚度：140μm
(2)回流处理
上述(1)电镀后，除去抗蚀剂，使得电镀部分露出。针对该电镀部分，使用图5中所示的红外线加热炉进行回流处理。红外线加热炉的温度控制是通过将在中心最外层中埋入的热电偶的2英寸硅晶片(SensArray公司制造、温度测量晶片)置于红外线加热炉的载物台上来进行。另外，回流试样置于接近其硅晶片上的热电偶的位置。回流温度条件是在150～170℃下预先加热90秒，然后用30秒升温至最高温度。最高温度为238℃，在可以回流的最低温度即231℃或以上保持30秒钟后，冷却。
另外该加热炉氛围气体用氮气置换，在加热时也一边以8L/min的流量通入氮气一边进行。红外线加热炉由于具有所谓容易进行快速加热、快速冷却的特征而被使用。
(3)凸点的组成分析
按照如下方法评价Sn-Ag合金的元素组成比。将该凸点埋入树脂中，刮平截面并研磨后，用电子线微量分析(电子探针微量分析：EPMA)进行元素映射，同时在图6A和图6B中所示的截面内约10μm×10μm的微小区域中的3个地方(l、c、r)进行Ag的定量分析，其平均值作为Ag的含量。
还有，如果使用μ荧光X线分析装置，即使不刮平截面，也可以粗略测定组成比，另外也可以将凸点溶解在酸中，通过电感耦合等离子体质量分析计(电感耦合等离子体质谱：ICP-MS)进行晶片内组成分布的分析。
(4)凸点形状的确认
在进行Sn-Ag合金电镀后，用SEM观察除去例如抗蚀剂的电镀部分和在各温度下回流后的凸点形状。图7A表示回流前的凸点的SEM照片，图7B表示在225℃下回流后的SEM照片，图7C表示在230℃下回流后的SEM照片，图7D表示在238℃下回流后的SEM照片。
(5)空隙的确认
用SEM观察在回流温度为238℃下回流后的凸点的截面形状。观察是在连晶片一起埋入树脂、刮平截面、研磨后进行。其结果是，在该实施例的Ag浓度为2.6质量％的合金镀膜(凸点)中，如图8中所示没有空隙，与此相反在通过Ag浓度为3.4质量％的合金镀膜形成的凸点中，有时产生图9中所示的空隙。
实施例2
使得相对于合金镀液中整个金属的Ag的比例、电镀时的电流密度、电流外加法分别改变进行合金电镀，再使之在238℃下回流。针对得到的凸点，与实施例1同样调查凸点中Ag的含量、形状和有无空隙。该结果显示在表1中。
【表1】
 镀液Ag/Sn (％)   电镀条件  电流密度  (A/dm<sup>2</sup>)   电压外加法   凸点  Ag的含有  浓度(wt％) 空隙 有(×)无(○)   在238℃   下的球化
 4.3   3   DC   5.2 ×   ○
 4.4   3   DC   6.4 ×   ○
 4.4   20   CHOP   4.0 ×   ○
 4.3   3   DC   7.7 ×   ○
 4.3   20   CHOP   5.1 ×   ○
 1.3   3   DC   1.8 ○   ○
 1.3   8   DC   0.9 ○   ×
 1.3   20   CHOP   1.4 ○   ×
 2.2   3   DC   3.4 ×   ○
 镀液Ag/Sn (％)   电镀条件  电流密度  (A/dm<sup>2</sup>)   电压外加法   凸点  Ag的含有  浓度(wt％) 空隙 有(×)无(○)   在238℃   下的球化
 2.2   20   CHOP   2.1 ○   ○
 4.1   3   DC   4.9 ×   ○
 3.1   20   CHOP   2.9 ○   ○
 3.1   10   CHOP   3.6 ×   ○
 3.1   3   DC   5.0 ×   ○
 3.2   3   DC   5.8 ×   ○
 3.2   20   CHOP   2.7 ×   ○
 2.3   3   DC   3.5 ×   ○
 2.3   20   CHOP   2.6 ○   ○
注)表中，DC是指直流电镀，CHOP是指间歇电镀。
由该结果可以明显看出，在凸点(合金镀膜)中的Ag含量在2.9％或以下的情况下不会出现空隙，特别是在Ag含量为1.8～2.6％的情况下，在最高回流温度为238℃下球化并且不会出现空隙，因此可以得到实用性高的无铅凸点。
本发明的无铅凸点不会产生空隙，并且即使上升不到那样的温度，也会形成优选形状的凸点。另外该凸点不含铅，不会由于放出α射线导致集成电路的误操作和对环境产生影响。
这样一来本发明的无铅凸点可以广泛应用于半导体元件等表面安装技术(SMT)中，无铅的同时也可以很可靠地进行焊锡。
本发明涉及一种通过将调整了镀膜中的Ag浓度的Sn-Ag类焊锡合金镀膜进行回流而得到的抑制空隙产生的无铅凸点及该凸点的形成方法。

Claims (4)

1.一种无铅凸点的形成方法，其特征在于，一边控制镀浴组成和电析条件一边进行电镀，在欲形成凸点的部分上形成膜中的Ag浓度为1.6～2.6质量％的Sn-Ag类合金镀膜，接着回流所得到的该合金镀膜。
2.根据权利要求1所记载的无铅凸点的形成方法，其中回流所述合金镀膜时的最高温度在Sn-Ag系焊锡的熔点+10℃～240℃。
3.根据权利要求1所记载的无铅凸点的形成方法，其中镀浴组成和电析条件的控制是通过固定镀浴中的Ag离子和Sn离子的浓度比并改变电析条件来进行的。
4.根据权利要求1所记载的无铅凸点的形成方法，其中镀浴组成和电析条件的控制是通过固定电析条件并改变镀浴中的Ag离子和Sn离子的浓度比来进行的。
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