CN113874551A - 层叠体及其制造方法 - Google Patents

层叠体及其制造方法 Download PDF

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Publication number
CN113874551A
CN113874551A CN202080037305.3A CN202080037305A CN113874551A CN 113874551 A CN113874551 A CN 113874551A CN 202080037305 A CN202080037305 A CN 202080037305A CN 113874551 A CN113874551 A CN 113874551A
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China
Prior art keywords
plating
nickel
layer
gold
mass
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CN202080037305.3A
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CN113874551B (zh
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古谷章
小岛忠昭
铃木广志
那贺文彰
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Resonac Holdings Corp
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Showa Denko KK
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    • B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
    • B32B15/013—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of an iron alloy or steel, another layer being formed of a metal other than iron or aluminium
    • B32B15/015—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of an iron alloy or steel, another layer being formed of a metal other than iron or aluminium the said other metal being copper or nickel or an alloy thereof
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Abstract

本发明的课题是提供一种可适用于半导体制造装置的构成部件且耐腐蚀性、特别是对酸和高温蒸汽的耐腐蚀性优异的金属材料。本发明涉及的层叠体具有金属基材、在所述金属基材上形成的含镍镀敷被膜层、以及在所述含镍镀敷被膜层上形成的镀金被膜层，并且，所述镀金被膜层的针孔被厚度为15nm以上的钝态被膜封孔。

Description

层叠体及其制造方法
技术领域
本发明涉及层叠体及其制造方法。更具体而言，涉及适合作为半导体制造装置等的构成部件的层叠体及其制造方法。
背景技术
以往，在半导体制造工艺中，在干蚀刻工序和制造装置的清洁等中，使用氟、氯化氢、三氯化硼、三氟化氮、三氟化氯、溴化氢等卤素类的反应性和腐蚀性强的特殊气体(以下也称为“腐蚀性气体”)。
但是，上述腐蚀性气体与气氛下的水分反应而水解时，会产生氟化氢、草酸和氯化氢等生成物。上述生成物容易腐蚀使用上述腐蚀性气体时的阀、接头、配管和反应室等构成部件的金属表面，因此成为问题。
迄今为止，为了谋求耐腐蚀性的提高，进行了对金属基材实施镍-磷合金镀敷、形成镍的氟化钝态膜的方法(例如，参照专利文献1～3)，但这些方法有时不充分。
另外，在使用上述腐蚀性气体实施清洁的情况下，由于在冷却配管后导入腐蚀性气体，因此在生产线上会产生时间损失。所以，作为配管等构成部件的金属材料，要求开发能够不冷却而转移到清洁工序、即使在高温区域耐腐蚀性也不变差的新的金属材料。
另外，近年来，作为半导体制造的新工艺，以发展CVD法的形式，即作为能够在高纵横比的深冲压部以高精度进行膜厚控制的成膜的工艺，ALD(AtomicLayerDeposition：原子层沉积)法的开发得到发展。目前，在ALD法中主要使用H2O，成膜时的温度区域达到约150～400℃，所以H2O必然成为高温蒸汽。因此，要求半导体装置的构成部件的耐腐蚀性进一步提高。作为防止高温蒸汽气氛下的耐腐蚀的方法，在ALD工艺中使用哈斯特洛伊C(注册商标)等，但存在价格昂贵且加工性困难的问题。
此外，镀层表面的针孔也会成为腐蚀加剧的原因。针孔的产生原因，可以认为是例如通过镀敷反应产生的H2在形成镀敷被膜时成为气泡而阻碍成膜，或者残留在基材上的杂质(氧化膜、污垢、油分等)在前处理工序中未被除去而阻碍成膜等多种原因。对此，专利文献4中公开了在金属基材上实施镀金，通过在氧化气氛下加热而用氧化膜覆盖针孔的方法。
在先技术文献
专利文献1：日本特许第2954716号公报
专利文献2：日本特许第3094000号公报
专利文献3：日本特开2004-360066号公报
专利文献4：日本特开2008-260646号公报
发明内容
发明要解决的课题
根据本发明人的研究，了解到如专利文献1～3那样在镍-磷合金镀层表面形成镍的氟化钝态膜的方法中，有时耐蒸汽腐蚀性不充分。另外，在专利文献4的方法中，由于形成的氧化膜是极薄的膜，因此根据环境的不同，氧化膜有可能容易消失。因此，存在难以作为实用上的部件适用的问题。
因此，本发明的课题在于提供一种金属材料，其可适用于半导体制造装置的构成部件，且耐腐蚀性、特别是对酸和高温蒸汽的耐腐蚀性优异。
用于解决课题的手段
本发明涉及例如以下的[1]～[12]。
[1]一种层叠体，具有金属基材、在所述金属基材上形成的含镍镀敷被膜层、以及在所述含镍镀敷被膜层上形成的镀金被膜层，并且，所述镀金被膜层的针孔被厚度为15nm以上的钝态被膜封孔。
[2]根据上述[1]记载的层叠体，所述金属基材包含选自不锈钢、铁、铝、铝合金、铜和铜合金中的至少一种金属。
[3]根据上述[1]或[2]记载的层叠体，在所述金属基材与所述含镍镀敷被膜层之间具有镍触击电镀层。
[4]根据上述[1]～[3]中任一项记载的层叠体，所述含镍镀敷被膜层从所述金属基材侧起依次包含磷浓度为8质量％以上且小于10质量％的镍-磷合金镀层(1)、和磷浓度为10质量％以上且12质量％以下的镍-磷合金镀层(2)。
[5]根据上述[1]～[4]中任一项记载的层叠体，所述镀金被膜层从所述含镍镀敷被膜层侧起依次包含置换型镀金被膜层和还原型镀金被膜层。
[6]一种半导体制造装置的构成部件，由上述[1]～[5]中任一项记载的层叠体制成。
[7]一种层叠体的制造方法，包括：在金属基材上形成含镍镀敷被膜层的工序(A)；在所述含镍镀敷被膜层上形成镀金被膜层的工序(B)；以及在所述镀金被膜层的针孔上形成厚度为15nm以上的钝态被膜的封孔处理工序(C)。
[8]根据上述[7]记载的层叠体的制造方法，所述封孔处理工序(C)在氧气浓度为50体积％以上且温度为140～200℃的气氛下进行。
[9]根据上述[7]或[8]记载的层叠体的制造方法，所述金属基材包含选自不锈钢、铁、铝、铝合金、铜和铜合金中的至少一种金属。
[10]根据上述[7]～[9]中任一项记载的层叠体的制造方法，在所述工序(A)之前，包括对金属基材以电流密度为5～20A/dm2的条件实施镍触击电镀处理的工序。
[11]根据上述[7]～[10]中任一项记载的层叠体的制造方法，所述工序(A)包括形成磷浓度为8质量％以上且小于10质量％的镍-磷合金镀层(1)的工序(a1)、和在该工序(a1)之后形成磷浓度为10质量％以上且12质量％以下的镍-磷合金镀层(2)的工序(a2)。
[12]根据上述[7]～[11]中任一项记载的层叠体的制造方法，所述工序(B)包括形成置换型镀金被膜层的工序(b1)、和在该工序(b1)之后形成还原型镀金被膜层的工序(b2)。
发明的效果
根据本发明，能够提供一种耐腐蚀性、特别是对酸和高温蒸汽的耐腐蚀性优异的层叠体。
附图说明
图1是表示封孔处理前后的层叠体的概略图((a)：封孔处理前，(b)：封孔处理后)。
具体实施方式
以下，对本发明的一个实施方式进行具体说明。
本发明的一个实施方式的层叠体，具有金属基材、在所述金属基材上形成的含镍镀敷被膜层、以及在所述含镍镀敷被膜层上形成的镀金被膜层，并且，所述镀金被膜层的针孔被厚度为15nm以上的钝态被膜封孔。
本发明的一个实施方式的层叠体的制造方法，包括：在金属基材上形成含镍镀敷被膜层的工序(A)；在所述含镍镀敷被膜层上形成镀金被膜层的工序(B)；以及在所述镀金被膜层的针孔上形成厚度为15nm以上的钝态被膜的封孔处理工序(C)。
[金属基材]
本发明的一个实施方式所使用的金属基材是至少表面由金属制成的基材。作为所述金属基材，没有特别限定，可举出半导体制造装置的构成部件通常使用的金属，优选为不锈钢、铁、铝、铝合金、铜和铜合金。
所述金属基材，为了与含镍镀敷被膜层的密合性牢固，作为工序(A)的前处理，可以实施脱脂、酸洗或镍触击电镀处理等与基材相应的处理。镍触击电镀处理是使用含镍镀浴的预镀敷处理，镍触击电镀处理中的电流密度优选为5～20A/dm2，更优选为6～10A/dm2。另外，镍触击电镀处理的时间优选为5秒以上且5分钟以下。
[含镍镀敷被膜层]
含镍镀敷被膜层通过工序(A)而形成在所述金属基材上。再者，在对所述金属基材实施镍触击电镀处理的情况下，在金属基材与镍镀敷被膜层之间具有镍触击电镀层。
从提高耐腐蚀性的观点出发，含镍镀敷被膜层优选含有磷，更优选从所述金属基材侧起依次包含磷浓度为8质量％以上且小于10质量％的镍-磷合金镀层(1)、和磷浓度为10质量％以上且12质量％以下的镍-磷合金镀层(2)。
在将含镍镀敷被膜层整体设为100质量％时，含镍镀敷被膜层中的镍含量优选为80质量％以上，更优选为85～95质量％，特别优选为88～92质量％。通过镍含量为上述范围，被膜层中的磷的比率增加，能够发挥优异的耐腐蚀性。另外，如果使改变了磷浓度的无电解镀(化学镀)镍-磷合金镀敷被膜层叠，则针孔缺陷在不同的位置形成并进行成膜，因此外部干扰难以直接到达基材，能够期待耐腐蚀性提高。
＜工序(A)＞
含镍镀敷被膜层可以使用包含镍盐和作为还原剂的磷化合物的无电解镀浴在金属基材上形成。作为镍盐，例如可举出硫酸镍、氯化镍、乙酸镍、碳酸镍等。作为磷化合物，例如可举出次磷酸钠、次磷酸钾等。
所述工序(A)优选包括形成镍-磷合金镀层(1)的工序(a1)、和在该工序(a1)之后形成镍-磷合金镀层(2)的工序(a2)。
所述镍-磷合金镀层(1)的成膜速度优选为20～30μm/h(小时)，更优选为22～25μm/h(小时)，所述镍-磷合金镀层(2)的成膜速度优选为10～15μm/h(小时)，更优选为11～13μm/h(小时)。通过这样形成镍-磷合金镀层(1)和(2)，能够提高耐腐蚀性。镍-磷合金镀层(1)和(2)的膜厚分别优选为5μm以上，更优选为7～25μm，从不易产生针孔的被膜性能和成本的观点出发，进一步优选为10～20μm。
[镀金被膜层]
镀金被膜层通过工序(B)形成在上述含镍镀敷被膜层上。
在将镀金被膜层整体设为100质量％的情况下，镀金被膜中的金含量优选为90质量％以上，更优选为99质量％以上，特别优选为99.9质量％以上。通过使金含量在上述范围内，本申请发明的层叠体的耐腐蚀性稳定。金含量通过杂质定量法求出，即、用王水溶解镀金，用原子吸光分析和高频诱导耦合等离子体(ICP)发射光谱分析来测定。
从难以产生针孔的被膜性能和成本的观点出发，镀金被膜的厚度优选为0.1μm～1μm，更优选为0.2～0.9μm，特别优选为0.3～0.8μm。现有技术已知如果加厚贵金属镀敷被膜则针孔减少，虽然可期待高的耐腐蚀性，但价格变高，因此实用上不优选。
＜工序(B)＞
作为所述镀金被膜层的形成方法，没有特别限定，但优选无电解镀金法。在无电解镀金法中，优选在进行置换型镀金之后进行还原型镀金。即、所述工序(B)优选包括形成置换型镀金被膜层的工序(b1)、和在该工序(b1)之后形成还原型镀金被膜层的工序(b2)。
在置换型镀金中，镍从镍被膜溶解，并且溶液中的金离子被此时释放的电子还原，从而作为镀金被膜析出。在还原型镀金中，溶液中的金离子被还原剂的氧化反应中释放的电子还原，从而析出镀金被膜。
作为无电解镀金液例如可举出含有氰化金钾、氯化金、亚硫酸金、硫代硫酸金等的镀浴等，作为还原剂例如可举出氢氧化钠、二甲胺硼烷、六亚甲基四胺、具有碳原子数为3个以上的烷基和多个氨基的链状多胺等。
置换型镀金优选以50～90℃实施3～7分钟，更优选以65～75℃实施3～7分钟，还原型镀金优选以55～65℃实施7～15分钟，更优选以58～62℃实施7～15分钟，由此可以形成镀金被膜层。
[钝态被膜]
通过在工序(C)中对所述镀金被膜层表面进行氧化处理，所述镀金被膜层的针孔被钝态被膜封孔。
钝态被膜的厚度通常为15nm以上，优选为18～50nm，更优选为20～40nm，特别优选为25～35nm。通过使钝态被膜的厚度在上述范围，钝态被膜的耐久性等在实用上变得合适。
＜工序(C)＞
在工序(C)中，通过对从经过所述工序(A)和(B)的镀金被膜层的针孔露出的含镍镀敷被膜层表面进行强制氧化，形成钝态被膜，对针孔进行封孔处理。
工序(C)在氧气浓度优选为50体积％以上、更优选为70～100体积％的气氛下进行，氧化温度优选为140～200℃、更优选为150～180℃。作为伴随氧气的气体，可举出氮气、氩气等惰性气体。在金属基材为不锈钢的情况下，优选在150～190℃、更优选在155℃～175℃下氧化，在金属基材为铝合金的情况下，优选在140～160℃、更优选在145～155℃下氧化。通过使成膜温度在上述范围，无电解镀镍-合金和镀金的热扩散的平衡良好。
氧化处理时间根据要形成的钝态被膜的厚度而不同，但为了发挥优异的耐腐蚀性，优选为20～100小时，更优选为30～80小时。
实施例
以下，基于实施例对本发明进行更具体的说明，但本发明不限定于这些实施例。
[实施例1]
＜工序(A)＞
对于不锈钢(SUS316L)的表面，作为前处理实施了脱脂、酸洗和镍触击电镀处理。在实施了镍触击电镀处理的不锈钢的表面，使用无电解镍-磷镀敷药剂“ニムデン(商标)NSX”(上村工业(株)制)在镀敷温度为90℃、pH值为4.5～4.8的条件下，以成膜速度为10μm/25分钟，形成了成膜时的磷含量为8～10质量％的无电解镀镍-磷合金镀敷被膜层(1)。接着，使用无电解镀镍-磷镀敷药剂“ニムデン(商标)HDX”(上村工业(株)制)，以成膜速度为10μm/50分钟，形成了成膜时的磷含量为10～12质量％的无电解镀镍-磷合金镀敷被膜层(2)。由此，在实施了镍触击电镀处理的不锈钢上形成总计20μm厚的含镍镀敷被膜层。
＜工序(B)＞
依次使用两种无电解镀金液“フラッシュゴールドNC(置换型)”和“セルフゴールドOTK-IT(还原型)”(均为奥野制药工业(株)制)，在工序(A)中形成的含镍镀敷被膜层上，依次分别进行置换型镀敷温度70℃下5分钟和还原型镀敷温度60℃下10分钟的处理，形成合计0.6μm厚的镀金被膜层。
＜工序(C)＞
将具有在工序(A)和(B)中形成的含镍镀敷被膜层和镀金被膜层的不锈钢安装在常压气相流通式反应炉的内部，使炉内温度升温至165℃。然后，用氮气置换大气，接着导入100体积％氧气，将氮气置换为氧气。完全置换后，保持该状态36小时，将因实施镀金时产生的针孔导致的基底的无电解镀镍-磷被膜的露出部分强制氧化，形成钝态被膜。用W-SEM“JSM-IT200”(日本电子株式会社(制))对所得到的钝态被膜进行分析，确认钝态被膜的膜厚为20nm。
[实施例2]
除了将实施例1的工序(C)中使用100体积％氧气的强制氧化时间变更为72小时以外，采用与实施例1同样的方法形成钝态被膜。与实施例1同样地求出所得到的钝态被膜的膜厚，确认为30nm。
[实施例3]
代替实施例1中的不锈钢(SUS316L)而使用铝合金(A5052)，作为前处理实施脱脂、活性化处理、酸洗和锌置换处理后，采用与实施例1同样的方法实施了工序(A)和(B)。所述活性化处理使用酸性氟化铵和硝酸的混合酸作为处理剂，在室温下进行30秒。所述酸洗使用硝酸作为清洗剂，在室温下进行25秒。所述锌置换处理使用锌酸盐浴作为处理剂，在室温下进行25秒。再者，所述酸洗和所述锌置换处理在上述条件下分别各进行2次。
除了在工序(C)中将强制氧化温度设为150℃以外，与实施例1同样地在镀金被膜上形成钝态被膜。与实施例1同样地求出所得到的钝态被膜的膜厚，确认为20nm。
[比较例1]
仅进行实施例1的工序(A)，在不锈钢的表面形成含镍镀敷被膜层20μm。
[比较例2]
在进行实施例1的工序(A)和(B)后，使具有含镍镀敷被膜层和镀金被膜层的不锈钢暴露在大气中，形成自然氧化被膜。与实施例1同样地求出所得到的自然氧化被膜的膜厚，确认为7nm。
[比较例3]
在进行实施例1的工序(A)后进行以下的处理。将具有含镍镀敷被膜层的不锈钢安装在常压气相流通式反应炉的内部，使炉内温度升温至300℃。然后，用氮气置换大气，接着导入100体积％氧气，将氮气置换为氧气。完全置换后，保持该状态12小时。接着，导入10体积％F2气体，保持该状态12小时，由此在含镍镀敷被膜层上形成氟化镍(NiF2)膜。然后，为了实现成膜稳定化，注入氮气12小时。
[评价]
对于上述实施例1～3和比较例1～3中得到的金属基材表面上的被膜，采用下述方法进行评价。评价结果示于表1。
＜盐酸耐腐蚀试验＞
将长15mm×宽15mm×厚1mm的试验片在25℃浸渍于35质量％盐酸溶液中5小时。基于浸渍前后的质量减少量[mg/dm2]，以下述基准评价盐酸耐腐蚀性。
(评价基准)
A：小于0.1mg/dm2
B：0.1mg/dm2以上且小于3mg/dm2
C：3mg/dm2以上
＜蒸汽耐腐蚀试验＞
将长15mm×宽15mm×厚1mm的试验片在190℃饱和水蒸气气氛下放置144小时。基于试验前后的质量减少量[mg/dm2]，以下述基准评价耐蒸汽腐蚀性。
(评价基准)
A：小于0.1mg/dm2
B：0.1mg/dm2以上且小于3mg/dm2
C：3mg/dm2以上
表1
实施例1 实施例2 实施例3 比较例1 比较例2 比较例3
金属基材 SUS SUS Al SUS SUS SUS
含镍镀敷被膜层 有 有 有 有 有 有
镀金被膜层 有 有 有 无 有 无
是否具有封孔处理 有 有 有 无 有 无
钝态被膜的厚度[nm] 20 30 20 - 7
Ni F<sub>2</sub>处理 无 无 无 无 无 有
耐盐酸腐蚀性 B A B C C C
耐蒸汽腐蚀性 B A B C B C
表1中，SUS表示不锈钢(SUS316L)，Al表示铝合金(A5052)。
附图标记说明
1···金属基材
2···含镍镀敷被膜层
2a···镍-磷合金镀层(1)
2b···镍-磷合金镀层(2)
3···镀金被膜层
4···针孔
5···钝态被膜

Claims (12)

1.一种层叠体，具有金属基材、在所述金属基材上形成的含镍镀敷被膜层、以及在所述含镍镀敷被膜层上形成的镀金被膜层，并且，
所述镀金被膜层的针孔被厚度为15nm以上的钝态被膜封孔。
2.根据权利要求1所述的层叠体，所述金属基材包含选自不锈钢、铁、铝、铝合金、铜和铜合金中的至少一种金属。
3.根据权利要求1或2所述的层叠体，在所述金属基材与所述含镍镀敷被膜层之间具有镍触击电镀层。
4.根据权利要求1～3中任一项所述的层叠体，所述含镍镀敷被膜层从所述金属基材侧起依次包含磷浓度为8质量％以上且小于10质量％的镍-磷合金镀层1、和磷浓度为10质量％以上且12质量％以下的镍-磷合金镀层2。
5.根据权利要求1～4中任一项所述的层叠体，所述镀金被膜层从所述含镍镀敷被膜层侧起依次包含置换型镀金被膜层和还原型镀金被膜层。
6.一种半导体制造装置的构成部件，由权利要求1～5中任一项所述的层叠体制成。
7.一种层叠体的制造方法，包括：
在金属基材上形成含镍镀敷被膜层的工序A；
在所述含镍镀敷被膜层上形成镀金被膜层的工序B；以及
在所述镀金被膜层的针孔上形成厚度为15nm以上的钝态被膜的封孔处理工序C。
8.根据权利要求7所述的层叠体的制造方法，所述封孔处理工序C在氧气浓度为50体积％以上且温度为140～200℃的气氛下进行。
9.根据权利要求7或8所述的层叠体的制造方法，所述金属基材包含选自不锈钢、铁、铝、铝合金、铜和铜合金中的至少一种金属。
10.根据权利要求7～9中任一项所述的层叠体的制造方法，在所述工序A之前，包括对金属基材以电流密度为5～20A/dm2的条件实施镍触击电镀处理的工序。
11.根据权利要求7～10中任一项所述的层叠体的制造方法，所述工序A包括形成磷浓度为8质量％以上且小于10质量％的镍-磷合金镀层1的工序a1、和在该工序a1之后形成磷浓度为10质量％以上且12质量％以下的镍-磷合金镀层2的工序a2。
12.根据权利要求7～11中任一项所述的层叠体的制造方法，所述工序B包括形成置换型镀金被膜层的工序b1、和在该工序b1之后形成还原型镀金被膜层的工序b2。
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