CN100513641C - 环境适应型电子元件用表面处理钢板 - Google Patents

环境适应型电子元件用表面处理钢板 Download PDF

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CN100513641C
CN100513641C CNB02805265XA CN02805265A CN100513641C CN 100513641 C CN100513641 C CN 100513641C CN B02805265X A CNB02805265X A CN B02805265XA CN 02805265 A CN02805265 A CN 02805265A CN 100513641 C CN100513641 C CN 100513641C
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steel plate
alloy layer
steel sheet
surface treated
alloy
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CN1492946A (zh
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吉原良一
白川时次
三浦泰彦
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Nippon Steel Corp
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Abstract

本发明是提供不含环境负荷有害物质的铅，特别是同时满足经曲颈甑处理后的焊料浸润性、耐锈性和耐晶须性的电子元件用表面处理钢板。即，本发明是具有焊料浸润性、耐锈性、耐晶须性的环境适应型电子元件用表面处理钢板，它是通过在钢板或镀镍钢板上镀锡和锌后进行热扩散处理，或者是通过在钢板或镀镍钢板上镀Sn-Zn合金而形成的具有Sn-Zn合金层的电子元件用表面处理钢板，其特征在于，所述Sn-Zn合金层的附着量是3g/m2以上，Zn/Sn的比率以重量比计是0.01～10，优选是0.01～0.1且该Sn-Zn合金层上形成以磷酸镁为主体的无机涂膜，该无机涂膜的量以P+Mg附着量计在1～100mg/m2的范围内。

Description

环境适应型电子元件用表面处理钢板
技术领域
本发明涉及电气制品的电子元件用表面处理钢板，其具有优异的焊料浸润性、耐锈性、耐晶须性的特性，并且不含铅等环境负荷物质。
背景技术
对于电气制品的电子元件，特别是可焊性优异的表面处理钢板，通常使用镀锡铁板、镀铅锡钢板以及镀焊锡钢板等。
这样，使用一种表面处理钢板，它具有在熔融焊料浴中短时间浸渍而可附着焊料层的优异的焊料浸润性，且钢板表面须附着有8.4～11.2g/m2镀锡层的表面处理钢板(以下称之为#75～#100镀锡铁板)，但是近年来电气制品的小型化使得电子元件的间隔变窄，结果在镀锡铁板上出现直接短路或绝缘层的破坏等问题，这些是由于从镀锡层生长的针状单晶体(晶须)导致的，所以不会生长晶须的镀铅锡钢板和镀焊锡钢板成为主流。
对于阻止晶须的生长，目前已提出实施合金电镀(特公昭58—2598号公报、特开昭49—129号公报等)和电镀后的后处理(特公昭56—47955号公报、特公昭56—47956号公报、特开昭59—143089号公报、特开昭62—77481号公报等)方法。但是，在这些方法中，由于通过实施合金电镀或后处理妨碍了可焊性，所以这些方法几乎不能实现实用化，但在特开平2—270970号公报、特开平3—183796号公报中通过合金组成和铬酸盐处理层的优化而得以实用化。
最近，基于地球环境问题的考虑，正在规定对环境负荷有害物质的限制，特别是6价铬和铅成为限制的对象，所以迫切需要代替铅—锡焊料材料之外，还需要作为电镀钢板的镀锡铁板或镀焊锡钢板的代替材料。特别是在小型电子元件中，为了有效地被覆焊料，即在熔融的焊料浴中短时间浸渍而被覆焊料。
又，因为电子元件在加工后有时需要长期保管，所以用再现长期保管状态的曲颈甑促进处理等实验方法加速评价长期保管性，助焊剂也转变成活性度低的不含氯的类型。对于电子元件用表面处理钢板，要求极其优异的焊料浸润性，包括上述加速促进试验后的焊料浸润性。
如上所述，强烈要求焊料浸润性和耐晶须性均优异的环境适应型电子元件用表面处理钢板。
本发明的目的是提供不含环境负荷有害物质的铅，特别是满足经曲颈甑处理后的焊料浸润性、耐锈性和耐晶须性的电子元件用表面处理钢板。
发明内容
本发明是一种表面处理钢板，确保在熔融焊料浴中短时间浸渍而被覆焊料的电子元件用的镀铅锡钢板有优异的经曲颈甑处理后的焊料浸润性，且确保耐晶须性和耐锈性(而这正是镀锡铁板的缺点)。
可以通过如下的方法得到上述表面处理钢板：在钢板或者镀镍钢板上镀锡和锌后，进行热扩散处理，或者是通过镀Sn—Zn合金而形成具有Sn—Zn合金层，且镀Sn—Zn合金层的电子元件用表面处理钢板中，设定Sn—Zn合金量和Zn/Sn比率，以及在钢板上形成以磷酸镁为主体的无机涂膜来代替以前的铬酸盐涂膜。
即，本发明是具有焊料浸润性、耐锈性、耐晶须性的环境适应型电子元件用表面处理钢板，其是有，在钢板或镀镍钢板上镀锡和锌后进行热扩散处理，或者通过镀Sn—Zn合金而形成的具有Sn—Zn合金层，其特征在于，所述Sn—Zn合金层的附着量是3g/m2以上，Zn/Sn的比率以重量比计是0.01～10，更优选是0.01～0.1，且该Sn—Zn合金层上形成磷酸镁为主体的无机涂膜，无机涂膜的量以P+Mg附着量计在1～100mg/m2的范围内。
附图说明
图1是表示本发明中表面处理钢板的镀层断面表层的结构示意图。
图2是表示无机涂膜的P+Mg附着量与Sn—Zn合金层的Zn/Sn比率和焊料浸润性的关系。
图3是表示Sn—Zn合金层的Zn/Sn比率和耐晶须性的关系。
具体实施方式
下面对本发明进行详细地说明。首先，对本发明的表面处理钢板的限定理由进行说明。
在图1中，以示意图的形式表示本发明的表面处理钢板的镀层断面表层结构。图中的记号1是钢板或镀镍钢板(未图示出)镀锡和锌后进行热扩散处理，或者是通过镀Sn—Zn合金而形成的Sn—Zn合金层，而记号2是表示Sn—Zn合金层上的以磷酸镁为主体的无机涂膜，也是本发明中最本质的特征。
Sn—Zn合金层是本发明的基本的镀膜，从焊料浸润性和耐锈性考虑，它的附着量最低限至少3.0g/m2以上，其上限在本发明中不特别限定，但从成本考虑，优选是50g/m2左右。
Sn—Zn合金层的制备方法，除了在钢板或镀镍钢板上电镀Sn、Zn后，通过进行热扩散处理而得到Sn—Zn合金层之外，也可以通过在钢板上直接电镀而被覆Sn—Zn合金的方法，或者通过熔融浸渍涂镀法，即，将钢板浸渍在熔融Sn—Zn合金浴中而镀层的方法。另外，在上述的三种方法中，如特开平2—270970号公报、特开平3—183796号公报中记载的那样，通过使用实施基底镀镍层的钢板作为上述钢板，可以在钢板界面上制备镀镍层或Fe—Ni扩散层，在表层上制备Sn—Zn合金层，本发明并不特别限定Sn—Zn合金层的制造方法。
另外，在本发明中的Sn—Zn合金层是在钢板或镀镍钢板的两表面上形成的。
当Sn—Zn合金层薄时，由于基底表面的镀镍层，Sn—Zn合金层均匀，进而可以改善耐锈性。
接着，就对Sn—Zn合金层的Zn/Sn比率(重量比)和防氧化涂膜的限定进行解释，将附着量在3g/m2以上，Zn/Sn比率(重量比)在10.0以下的Sn—Zn合金层，浸渍在磷酸二氢镁溶液为主体的浴中，使之干燥后，在合金层表面形成以磷酸镁为主体的薄的无机涂膜，它的P+Mg附着量在1～100mg/m2的范围内，如图2中所示，通过以上方法可以抑制曲颈甑处理等的加速处理后的氧化膜生成，且可以确保优异的焊料浸润性以及与铬酸盐涂膜等同的耐锈性。
另外，如图3所示，将Zn/Sn比率(重量比)的下限设定在0.01以上，这样可以确保耐晶须性。
图2是表示，当Sn—Zn合金量为5.0～20.0g/m2时，磷酸镁为主体的无机涂膜的P+Mg附着量与Sn—Zn合金层的Zn/Sn比率(重量比)和焊料浸润性间的关系。这种情况下，焊料浸润性的评价是使用记录焊料弯月面随时间变化的装置，焊料是Sn—Ag系无铅焊料，助焊剂是非活性型和活性型两种，将试样在105℃的曲颈甑中加速试验8小时后，试验它的浸润性。
评价方法是，在非活性助焊剂中浸渍时间(零交叉时间)在3秒以内的记为◎，在活性助焊剂中浸渍时间在3秒以内的记为○，在活性助焊剂中浸渍时间在3～5秒的记为△，在活性助焊剂中浸渍时间在5秒以上的记为×。
如图2中所示，要确保优异的焊料浸润性，则Zn/Sn比率在10.0以下，特别是在0.1以下时，即使在非活性助焊剂中也能表现出非常优异的浸润性。关于P+Mg附着量，在该附着量为0时，当Zn/Sn比率在0.01～0.1时记为△，当Zn/Sn比率在1以上时记为×。为了具有防氧化涂膜的功能，P+Mg附着量必须在1mg/m2以上。至于该附着量的上限，随着涂布方法的不同有变化，当超过100mg/m2时，会影响焊料浸润性，因此P+Mg附着量优选是100mg/m2以下。
图3表示Sn—Zn合金层的Zn/Sn比率(重量比)和耐晶须性的结果。耐晶须性试验是将试样进行弯曲90°和凸出加工(bulgingprocessing)后，在与耐湿性试验相同的60℃、90％RH的气氛中放置3个月。试验的评价是通过目测法和扫描电子显微镜进行，评价基准是，○：晶须生长不足50微米，×：晶须生长为50微米以上。
如图3中所示，对于耐晶须性，Zn/Sn比率(重量比)在0.01以上时，晶须生长是不足50微米。因此，从耐晶须性的方面考虑，Zn/Sn比率(重量比)的范围限定在0.01以上，在使用活性助焊剂时，从焊料浸润性方面考虑，Zn/Sn比率(重量比)的范围限定在10.0以下，而在使用非活性焊料时，从焊料浸润性方面考虑，Zn/Sn比率(重量比)的范围限定在0.1以下。
实施例
下面通过实施例对本发明的内容进一步说明。在表1中，汇集了有关在实施例中所涉及的具体条件的变化和比较例，以及它们特性的评价结果。
实施例1
对用通常的方法进行冷轧和退火的低碳冷轧钢板以通常的方法进行脱脂、酸洗后，依次以(1)中所示的处理条件进行镀镍，以(2)中所示的条件实施镀锡，以(3)中所示的条件实施镀锌。之后，通过电加热方式，在大气中实施以钢板表面温度为250～350℃的温度加热处理0.5秒以上，形成以Sn—Zn二元合金为主体的镀膜。另外，在以(4)、(5)所示的条件后处理之后，作为试样进行各种评价试验。
(1)镀镍
①浴条件   NiSO4·7H2O：200～300g/L
           H2SO4：0～50g/L
             H3BO3：40g/L
②电镀条件   浴温度：40～50℃
             电流密度：5～30A/dm2
(2)镀锡
①浴条件     硫酸锡：20～30g/L
             苯酚磺酸：20～30g/L
             乙氧化α—萘酚磺酸：2～3g/L
②电镀条件   浴温度：35～45℃
             电流密度：2～30A/dm2
(3)镀锌
①浴条件     ZnSO4·7H2O：200～400g/L
             Na2SO4：50～150g/L
②电镀条件   浴温度：40～50℃
             电流密度：5～30A/dm2
(4)除去表层氧化膜的处理浸   渍时间：3秒
①浴条件    H2SO4：10～20g/L
②浴温度    常温(20～30℃)
(5)防氧化涂膜处理
①浴条件     磷酸二氢镁溶液：1～20g/L
②处理条件   浴：常温～50℃(浸渍3～5秒)
实施例2
对用通常的方法进行冷轧和退火的低碳冷轧钢板以通常的方法进行脱脂、酸洗后，依次以实施例1的(1)中所示的处理条件镀镍，以下述(6)中所示的处理条件镀Sn—Zn合金，以实施例1的(4)中所示的条件除去表层氧化膜。之后，以实施例1的(5)中所示的条件实施防氧化涂膜处理之后，作为试样进行各种评价试验。
(6)镀Sn—Zn熔融合金
①浴条件       Sn—Zn合金
②电镀条件     浴温度：250～300℃
               浸渍时间：1秒
               镀层附着量：30～40g/m2(擦拭控制)
实施例3
对用通常的方法进行冷轧和退火的低碳冷轧钢板以通常的方法进行脱脂、酸洗后，依次以实施例1的(1)中所示的处理条件镀镍，以下述(7)中所示的处理条件镀Sn—Zn合金，以实施例1的(4)中所示的条件除去表层氧化膜。之后，以实施例1的(5)中所示的条件实施防氧化涂膜处理之后，作为试样进行各种评价试验。
(7)Sn—Zn合金电镀
①浴条件     链烷醇磺酸：10～200g/L
             2价Zn：1～50g/L
             2价Sn：100～500g/L
②电镀条件   浴温度：50～60℃
             电流密度：10～200A/dm2
比较例1—1
除了以下述(8)所示的铬酸盐处理条件代替实施例1中的(4)、(5)之外，其它项目与实施例1相同。
(8)铬酸盐处理
①浴条件      CrO3：50～100g/L
②浴温度      ：40～50℃(5秒钟浸渍)
比较例1—2
除了省略比较例1—1中的铬酸盐处理条件(8)之外，其它项目与实施例1相同。
比较例2
将每个单面的镀锡量为11.2g/m2的电镀镀锡铁板(称之为#100镀锡铁板)作为试样进行各种特性评价试验。
比较例3
将每个单面的镀铅量为30g/m2的电镀镀铅钢板(称之为镀铅锡钢板)作为试样进行各种特性评价试验。
对以上本发明的实施例和比较例，进行以下所示为(a)～(c)的评价试验，比较各自的特性。另外，对于实施例在评价前用下述的(1)～(3)的方法测定Sn—Zn合金层(g/m2)、Zn/Sn比率(重量比)、P+Mg附着量(mg/m2)。
(a)焊料浸润性试验
焊料浸润性试验是使用记录焊料弯月面随时间变化的装置(由Tarutin Kester Co.制的SWET—2100)、使用Sn-Ag-Bi系无铅焊料(由Tarutin Kester Co.制的SA2515)和非氯系助焊剂(由Tamura Giken Co.，Ltd.制的NA200)以及含氯的活性助焊剂(由Nihon Superior Co.，Ltd.制的NS828)，将试样进行曲颈甑加速试验105℃×8小时后，试验浸润性。
评价方法是，在非活性助焊剂中浸渍时间(零交叉时间)在3秒以内的记为◎，在活性助焊剂中浸渍时间在3秒以内的记为○，在活性助焊剂中浸渍时间在3～5秒的记为△，在活性助焊剂中浸渍时间在5秒以上的记为×。
(b)耐晶须试验
耐晶须性试验是将试样进行弯曲90°和凸出加工(bulgingprocessing)后，在与耐湿性试验相同的60℃、90％RH的气氛中放置3个月。试验的评价是通过目测法和扫描电子显微镜进行，评价基准是，○：晶须生长不足50微米，×：晶须生长为50微米以上。
(c)耐锈性试验
实施JIS Z 2371规定的盐水喷雾72小时连续试验，以％测定红锈发生面积率。
1)Sn—Zn合金量(g/m2)的测定
使用荧光X线分光分析装置，由预先制备的Sn和Zn的重量检测线测出各自的重量，以它们之和作为Sn—Zn合金量。
2)Zn/Sn比率(重量比)的测定
由与1)相同方法测Sn和Zn的重量后，计算Zn/Sn比率(重量比)。
3)P+Mg附着量(mg/m2)的测定
对于P，使用荧光X线分光分析装置，由预先制备的重量检测线测出重量；对于Mg，将以酸溶解涂膜得到的溶液使用高频诱导结合等离子体发光分析装置，由预先制备的重量检测线测出重量，以两者重量之和作为P+Mg附着量。
表1中汇集示出了实施例的具体条件和比较例，以及它们的特性评价结果。
实施例1—1～1—4是电镀Sn、Zn后，进行热扩散合金化处理而形成Sn—Zn合金层的例子，实施例2—1和2—2是以熔融浸渍法来制备Sn—Zn合金层的例子，而实施例3是以合金电镀法制备Sn—Zn合金层的例子。并且给出了这些实施例的特性评价结果。
比较例1—1是电镀后，进行热扩散处理，进而使表面形成铬酸盐涂膜的例子，而比较例1—2是没有进行铬酸盐处理的例子。比较例2和3是分别表示现行比较材#100镀锡铁板和镀铅锡钢板的结果。
正如这些实施例所述，P+Mg无机涂膜的曲颈甑加速处理后的焊料浸润性比铬酸盐处理更良好，耐锈性也具有同等的性能，表现出比作为比较材的#100镀锡铁板和镀铅锡钢板更优异的特性。
如以上所述，本发明具有优异的经曲颈甑处理后的焊料浸润性、耐锈性和耐晶须性。根据本发明，可提供环境适应型的电子元件用表面处理钢板。

Claims (2)

1、一种具有焊料浸润性、耐锈性、耐晶须性的环境适应型电子元件用表面处理钢板，其是有通过在钢板或镀镍钢板上镀锡和锌后进行热扩散处理，或者通过在钢板或镀镍钢板上镀Sn—Zn合金而形成的具有Sn—Zn合金层，其特征在于，所述Sn—Zn合金层的附着量是3g/m2以上，Zn/Sn的比率以重量比计为0.01～10，且该Sn—Zn合金层上形成以磷酸镁为主体的无机涂膜，该无机涂膜的量以P和Mg各自的附着量的总和计在1～100mg/m2的范围内。
2、根据权利要求1所述的具有焊料浸润性、耐锈性、耐晶须性的环境适应型电子元件用表面处理钢板，其特征在于，Sn—Zn合金层的Zn/Sn的比率以重量比计在0.01～0.1的范围内。
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