CN102597321A - 涂覆物品及方法 - Google Patents

涂覆物品及方法 Download PDF

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Publication number
CN102597321A
CN102597321A CN2010800408148A CN201080040814A CN102597321A CN 102597321 A CN102597321 A CN 102597321A CN 2010800408148 A CN2010800408148 A CN 2010800408148A CN 201080040814 A CN201080040814 A CN 201080040814A CN 102597321 A CN102597321 A CN 102597321A
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layer
article
coating
microinchs
less
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CN102597321B (zh
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约翰·克海伦
艾伦·C·伦德
克里斯托弗·A·舒
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Xtalic Corp
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Xtalic Corp
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/48—Electroplating: Baths therefor from solutions of gold
    • 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
    • B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
    • 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
    • B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
    • B32B15/018—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of a noble metal or a noble metal alloy
    • 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
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • 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
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B15/043—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of metal
    • 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
    • B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
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    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C—CHEMISTRY; METALLURGY
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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    • C—CHEMISTRY; METALLURGY
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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    • Y10T428/1291—Next to Co-, Cu-, or Ni-base component
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10T428/12931—Co-, Fe-, or Ni-base components, alternative to each other
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

描述了经涂覆的物品及涂覆涂层的方法。一些情况下，所述经涂覆物品体现了耐用性、耐蚀性、及高导电性等理想的特性。例如，所述经涂覆物品可使用电沉积工艺。

Description

涂覆物品及方法
技术领域
本发明主要涉及涂覆物品及相关方法。一些实施例中，使用电沉积工艺对物品进行涂覆。
技术背景
可在基底材料上涂覆多种类型的涂层。电沉积系用于淀积此类涂层的常用技术。电沉积一般包括向放置在电沉积浴(electrodeposition bath)中的基底材料施加电压以减少电沉积浴中的以金属、或金属合金、涂层的形式沉积在基底材料上的金属离子物种。可使用电源在阳极与阴极之间施加电压。阳极与阴极中至少有一个用作待涂覆的基底材料。一些电沉积工艺中，可以脉冲电镀，交流电镀，或反向脉冲电镀之类的复杂波形施加电压。
可使用电沉积对各种金属和金属合金涂层进行沉积。例如，金属合金涂层可基于两种或两种以上的过渡金属，包括Ni、W、Fe、Co等。
一般而言，腐蚀工艺能够影响暴露于腐蚀环境下的电镀涂层的结构与组分。例如，腐蚀可包括涂层表面的原子直接溶解，通过选择性溶解或去合金化改变涂层的表面化学成分，或者例如通过氧化或形成钝化膜而改变涂层的表面化学成分与结构。其中一些过程可改变涂层的形貌、纹理、特性或外观。例如，涂层可能会发生蚀斑或者锈污。此类影响是不理想的，特别是当至少部分地涂覆涂层以改进导电性的时候，因为这些影响会增大涂层的电阻。
发明内容
提供了经涂覆的物品和相关方法。
一个方面，提供了一种方法。所述方法包括使用具有正向脉冲和反向脉冲的波形将涂层的第一层电沉积在基底材料上，其中所述基底材料含铜，所述第一层含Ni并且含W及/或Mo，并且所述第一层的厚度大于5微英寸。所述方法还包括在所述第一层上电沉积所述涂层的第二层，所述第二层含有选自由Au、Ru、Os、Rh、Ir、Pd、Pt、及/或Ag构成的组中的金属，其中所述第二层的厚度小于30微英寸。
另一方面，提供了一种物品。所述物品包括含铜的基底材料。所述物品还包括形成在所述基底材料上的涂层，所述涂层包括含Ni，并且含W及/或Mo的第一层，其中所述第一层的厚度大于5微英寸；及形成在所述第一层上的第二层，所述第二层含有选自由Au、Ru、Os、Rh、Ir、Pd、Pt、及/或Ag构成的组中的金属，其中所述第二层的厚度小于30微英寸。
结合附图，参考下文的详细描述可清楚本发明的其他方面、实施例、及特征。所述附图是示意性的并且未按比例绘制。简明起见，并未对每幅附图中的每个元件进行标号，并且在其附图说明并非本领域的普通技术人员理解本发明所必须的情况下，也未对本发明各实施例中的每个元件进行标号。通过引用的方式结合的所有专利申请或专利系全文引用。在发生冲突的情况下，以本份说明书(包括定义)为准。
附图说明
图1示出了根据本发明的一些实施例的经涂覆物品；
图2A～2C示出了示例1中所描述的经涂覆物品的照片；
图3A～3C示出了示例2中所描述的经涂覆物品的测试程序和照片；
图4A～4D示出了示例3中所描述的经涂覆物品的照片；
图5A～5D示出了示例4所描述的接触电阻测量的图表；
图6～7示出了示例5中所描述的经涂覆物品的照片；
图8A～8D及9A～9B示出了示例5所描述的接触电阻测量的图表。
具体实施方式
描述了经涂覆的物品以及涂覆涂层的方法。所述物品可包括基底材料和形成于其上的分多层的涂层。一些情况下，所述涂层包括含有合金(例如，镍-钨合金)的第一层和含有贵金属(例如，Ru、Os、Rh、Ir、Pd、Pt、Ag、及/或Au)的第二层。一些情况下，可使用电沉积工艺涂覆涂层。所述涂层可具有理想的特性与属性，例如耐用性、耐蚀性、及高导电性，而高电导率例如在电气应用中是有利的。某些情况下，存在第一层能在保存所需特性的同时减小第二层的厚度。
图1示出了根据实施例的物品10。所述物品具有形成在基底材料30上的涂层20。所述涂层包括形成在基底材料上的第一层40以及形成在第一层上的第二层50。可使用合适的工艺涂覆各层，下文将详述。应理解，所述涂层可为两层以上。然而，某些实施例中，所述涂层仅包括两层，如图所示。
某些实施例中，第一层包括一或多种金属。例如，第一层可包括金属合金。某些情况下，最好是包括镍的合金。此类合金还可包括钨及/或钼。某些情况下最好使用镍-钨合金。
某些情况下，合金中镍的重量百分比可为25～75重量百分比；并且，某些情况下，可为50～70重量百分比。这些情况下，合金的剩余部分可为钨及/或钼。也可使用这一范围之外的其它重量百分比。
第一层的厚度可为适于某一应用。例如，第一层厚度可为大于1微英寸(例如，约1微英寸～约100微英寸、约1微英寸～约50微英寸)；某些情况下，大于约5微英寸(例如，约5微英寸～约100微英寸、约5微英寸～约50微英寸)；大于约25微英寸(例如，约25微英寸～约100微英寸、约1微英寸～约50微英寸)。应理解，其他的第一层厚度也是合适的。某些实施例中，第一层的厚度可选择为第一层的表面基本为透明。可利用业界公知的技术测量厚度。
某些实施例中，第一层最好直接形成在基底材料上。较之采用位于第一层与基底材料之间的层的某些现有结构，此类实施例较佳，因为不设置中间层可降低总的材料成本。应理解，其他实施例中，仍然可在第一层与基底材料之间形成一或多层。
第二层可包括一或多种贵金属。合适的贵金属的例子包括Ru、Os、Rh、Ir、Pd、Pt、Ag、及/或Au。某些实施例中，最好使用金。一些实施例中，第二层基本有一种贵金属构成。一些实施例中，第二层最好不含锡。其他情况下，第二层可含有包括至少一种贵金属与至少一种其他金属的合金。所述金属可选自Ni、W、Fe、B、S、Co、Mo、Cu、Cr、Zn及Sn等。
第二实施例可具有合适的厚度。薄的第二层是有利的，例如，可降低材料成本。例如，第二层厚度可为小于30微英寸(例如，约1微英寸～约30微英寸；某些情况下，为约5微英寸～约30微英寸)；某些情况下，第二层厚度可小于约20微英寸(例如，约1微英寸～约20微英寸；某些情况下，约5微英寸～约20微英寸)；并且，某些情况下，第二层厚度可为小于约10微英寸(例如，约1微英寸～约10微英寸、在某些情况下，约5微英寸～约10微英寸)。一些实施例中，第二层的厚度可选择为第二层的表面基本为透明。应理解，其他的第二层厚度也是合适的。
第二层可覆盖整个第一层。然而，应理解，其他实施例中，第二层可仅覆盖部分的第一层。某些情况下，第二层至少覆盖第一层表面积的50％；其他情况下，至少覆盖第一层表面积的75％。某些情况下，可将第一层的元素结合入第二层，及/或将第二层的元素结合入第一层。
某些情况下，所述涂层(例如第一层及/或第二层)可具有特定的微结构。例如，所述涂层的至少一部分可具有纳米晶态微结构。如本文所使用的“纳米晶态”微结构系指这样的结构，即其中晶粒的数量平均尺寸小于一微米。晶粒的数量平均尺寸使得各晶粒具有相等的统计权重，并且由所有球形等效粒径之和除以主体的代表性体积中晶粒的总数而计算得到。一些实施例中，所述涂层的至少一部分可具有无定形结构。如本领域所公知的，无定形结构系指原子位置中没有大范围对称的非晶态结构。无定形结构的例子包括玻璃，或者玻璃之类的结构。一些实施例可提供基本上全部都是纳米晶态结构的涂层。一些实施例可提供基本上全部都是非定形结构的涂层。
一些实施例中，所述涂层可包括多种具有不同微结构的部分。例如，第一层的微结构可不同于第二层。所述涂层例如可包括具有一或多个纳米晶态结构的部分和一或多个具有非定形结构的部分。一组实施例中，所述涂层包括纳米晶态的晶粒和具有无定形结构的其他部分。一些情况下，所述涂层，或其一部分(即，第一层的一部分，第二层的一部分，或第一层与第二层的一部分)可包括这样的包含晶粒的一部分，即其大多数晶粒的粒径大于一微米。一些实施例中，所述涂层可单独包括其他结构或相，或者包括与纳米晶态部分或者无定形部分组合的其他结构或相。例如，金属、陶瓷、金属间化合物的颗粒，石墨或MoS2的固体润滑剂颗粒，或者可结合入具有纳米晶态部分或无定形部分之涂层的其他材料。本领域的普通技术人员应能够选择其他适用于本发明背景的结构或者相。
有利的是，所述涂层(即，第一层，第二层，或第一层与第二层)基本不含有具有高毒性或其他缺点的元素或化合物。一些情况下，同样有利的是，涂层基本不含有由高毒性或其他缺点的物种进行沉积而得到的元素或化合物。例如，一些情况下，所述涂层不含有铬(例如，氧化铬)，而之前常使用有毒的铬离子物种(例如，Cr6+)进行沉积。此类涂层较之先前的涂层，可具有多种处理、健康及环境优势。
一些实施例中，可将金属、非金属、及/或类金属材料、盐等(例如，磷酸盐或铁氰化钾之类的氧化还原介质，或其碎片)结合入所述涂层。
可使用业界公知的合适技术来表征所述涂覆或者其部分的成分，诸如，俄歇电子能谱(AES)、X射线光电子能谱(XPS)等。例如，AES及/或XPS可用于表征所述涂层表面的化学成分。
可对基底材料30进行涂覆以形成经涂覆的物品，如前所述。一些情况下，基底材料可包括导电材料，诸如金属、金属合金、金属间材料等。合适的基底材料包括钢、铜、铝、黄铜、青铜、镍、带有导电表面及/或表面处理的聚合物、透明导电氧化物等。一些实施例中，最好使用铜作为基底材料。
所述物品可有多种应用，包括电气接头(例如，插入型)之类的电气应用。所述涂层可使得物品具有理想的属性，例如耐用性、耐蚀性、及改进的导电性。这些特性在电气接头之类的电气应用中的物品特别有利，因为它们在与电路的连接及/或断开会承受摩擦应力，这这一应力会破坏或减损物品上导电层的电导性。一些实施例中，涂层存在第一层至少使得所述涂层具有一些耐用性和耐蚀性。此外，存在第一层可允许第二层的厚度减小，藉此显著减小物品的贵金属使用量。
可使用电沉积工艺形成涂层20。电沉积一般包括通过使得基底与电沉积浴接触并且使得电流经由电沉积浴而在两个电极之间流动(即因两个电极之间的电位差)，而将材料(例如，电镀物)沉积在基底上。例如，本文所述的方法可包括提供阳极、阴极、与所述阳极和阴极相关的电沉积浴(亦称为电沉积流体)、连接至所述阳极和阴极的电源。一些情况下，可驱动电源生成用于制造涂层的波形，下文将详述。
一般地，可使用分开的电沉积浴来涂覆所述涂层的第一层和第二层。某些情况下，可将一个个的物品连接在一起，依次暴露至分开的电沉积浴，例如，在卷轮式(reel-to-reel)工艺中。例如，可将多个物品连接至公用的导电基底(例如，一条状物)。一些实施例中，各电沉积浴可与不同的阳极相关，并且互联的一个个物品可共同连接至一个阴极。
可通过改变施加在电极之间的电位(例如，电位控制或电压控制)，或者通过改变允许流动的电流或电流密度(例如，电流或电流密度控制)，来调制电沉积工艺。一些实施例中，可使用直流(DC)电镀、脉冲电流电路、反向脉冲电流电镀、或它们的组合来形成(例如，电沉积)涂层。一些实施例中，例如最好使用反向脉冲电镀来形成第一层(例如，镍-钨合金)。也可在电沉积期间加入脉冲、振荡、及/或电压、电位、电流及/或电流密度的其他变化，下文将详述。例如，受控电压的脉冲可与受控电流或电流密度的脉冲交替。一般地，在电沉积处理期间，待涂覆的基底(例如，基底材料)上存在电位，并且所施加电压、电流或电流密度的变化会导致基底上该电位的变化。一些情况下，电沉积处理包括使用含有一或多个段的波形，其中各段包括一组具体的电沉积条件(例如，电流密度、电流持续时间、电沉积浴温度等)，下文将详述。
本发明的一些实施例涉及可对电沉积材料(例如，金属、合金等)的颗粒尺寸进行控制的电沉积方法。一些实施例中，选择具体的涂覆(例如，电镀)成分，诸如合金沉积的成分，可使得涂覆具有所需的颗粒尺寸。一些实施例中，本文所述的电沉积方法(例如，电沉积条件)可选择为制造具体的成分，藉此控制沉积材料的颗粒尺寸。本发明的方法可采用名称为“使用负电流脉冲电沉积制造合金沉积物及控制其纳米结构的方法，及结合所述沉积物的物品(Methodfor Producing Alloy Deposits and Controlling the Nanostructure Thereof usingNegative Current Pulsing Electro-deposition、and Articles Incorporating SuchDeposits)”的第2006/02722949美国专利公开以及申请于05/14/2008的、名称为“涂覆物品及相关方法(Coated Articles and Related Methods)的第12/120,564号美国专利申请所描述之方法的某些方面，通过全文引用的方式将它们合并在此。电沉积方法的其他方面亦可包括第2006/0154084号美国专利公开以及名称为“定制纳米晶态或无定形金属或合金的表面形貌的方法，及由所述方法形成的物品(Methods for Tailoring the Surface Topography of a Nanocrystalline orAmorphous Metal or Alloy and Articles Formed by Such Methods)、申请于11/15/07的第11/985,569号美国专利申请，通过全文引用的方式将所述文献合并在此。
一些实施例中，可使用直流(DC)电路来电沉积涂层或其一部分。例如，基底(例如，电极)可定位为与电沉积浴接触(例如，浸入)，所述电沉积浴含有一或多个要被沉积到所述基底上的物种。恒定、稳定的电流经过电沉积浴以在基底上制造涂层或其一部分。如前所述，也可使用反向脉冲电流。
电沉积工艺使用合适的电沉积浴。此类浴一般包括在施加电流时沉积到基底(例如，电极)的物种。例如，可在含有金属(例如，合金)之涂层的电沉积中，使用含有一或多种金属物种(例如，金属类、盐类、其他金属源)的电沉积浴。一些情况下，电化学浴包括镍物种(例如，硫酸镍)和钨物种(例如，钨酸钠)，并且可用于形成例如镍-钨合金涂层中。
一般地，电沉积浴包括水性流体载体(例如，水)。然而，应理解在本发明的背景下可使用其他的流体载体，包括但不限于熔盐、低温溶剂、乙醇浴等。本领域的普通技术人员应能够选择适用于电沉积浴的流体载体。一些情况下，电沉积浴可选择为具有约7.0～9.0的pH。一些情况下，电沉积浴可选择为具有约7.6～8.4的pH，或者，一些情况下，为约7.9～8.1。
电沉积浴还可包括其他添加剂，诸如湿润剂、增亮剂或匀涂剂等。本领域的普通技术人员应能够选择适用于具体应用的适当添加剂。一些情况下，电沉积浴包括柠檬酸盐离子作为添加剂。一些情况下，柠檬酸盐离子含量为约35～150g/L、40～80g/L，一些情况下，60～66g/L。
本发明的方法的优点在于可通过单个电沉积步骤容易地制造具有多种成分的涂层(例如，Ni-W合金涂覆)。例如，可在单个电沉积浴和单独的沉积步骤中，通过选择具有适当段的波形，制造含有分层成分、分级成分等的涂层。经涂覆的物品具有增强的耐蚀性和表面特性。
应理解，可使用其他技术来制造本文所述的涂覆，包括气相处理、溅镀、物理气相沉积、化学气相沉积、热氧化、离子植入、喷涂、粉基工艺、浆基工艺等。
一些实施例中，本发明提供这样的经涂覆物品，其在一或多种可能的腐蚀环境中能够耐腐蚀、及/或保护下层基底材料不腐蚀。此类腐蚀环境的例子包括但不限于水溶液、酸溶液、碱溶液、或他们的组合。例如，本文所述的经涂覆物品在暴露至(例如，接触、浸入等)腐蚀液体、蒸汽或潮湿环境之类的腐蚀环境时能够耐腐蚀。
可利用名称为“硝酸蒸汽测试金属基体上金涂层孔隙率的标准方法”的ASTM B735之类的测试来评估耐蚀性，并且依据IIa类协议的名称为“电触点的混流气体试验用标准导则”的ASTM B845也可用于评估经涂覆物品的耐蚀性。这些测试规定了将经涂覆的基底样本暴露至腐蚀气氛(即，硝酸蒸汽或NO2、H2S、Cl2、及SO2的混合物)的程序。流动气体的混合物可包括200+/-50ppb的NO2、10+/-5ppb的H2S、10+/-3ppb的Cl2、及100+/-20ppb的SO2。也可控制温度和相对湿度。例如，温度可为30+/-1℃，并且相对湿度可为70+/-2％。
物品暴露于气体或气体混合物的时间是可变的，并且一般由被测试产品或涂层的终端用户指定。例如，暴露时间可为至少30分钟，至少2小时，至少1天，至少5天，或至少40天。预定量的暴露时间之后，检查(例如，通过肉眼观察及/或如下地用仪器观察)样本是否有因腐蚀及/或蚀斑造成表面外观及/或导电性的变化迹象。暴露时间经过之后，可使用简单的通过/失败法报告测试结果。
例如，可通过测量涂层外观的变化来评估经受上述测试条件的涂层。例如，可规定临界表面积比例以及规定的时间。若，经过规定时间之后，由腐蚀所造成的涂层在外观上发生变化的表面积比例小于规定的临界值，则认为结果是通过的。若由腐蚀所造成涂层在外观上已经变化的表面积比例达到临界值，则认为结果是失败。例如，可确定腐蚀性蚀斑的程度。蚀斑的程度可通过规定时间后，蚀斑的数量密度及/或面积密度来量化。例如，可通过对单位面积内的蚀斑数量(例如，蚀斑数/cm2)进行计数而判定数量密度。可通过测量蚀斑所占据的表面积比例来评估蚀斑面积密度，例如，等于1的面积密度表示100％的表面积发生腐蚀，等于0.5的面积密度表示50％的表面积发生腐蚀，而等于0的面积密度表示没有表面积发生腐蚀。
一些情况下，根据ASTM B735暴露至硝酸蒸汽2小时的经涂覆物品，或者根据ASTM B845(IIa类协议)暴露至混合流动气体5天的经涂覆物品的腐蚀面积密度小于0.10；一些情况下，小于0.05；并且，一些情况下，为0。一些实施例中，暴露至这些条件的经涂覆物品的蚀斑数量密度为小于3个蚀斑/cm2；一些实施例中，小于2个蚀斑/cm2；并且，一些实施例中，为0个蚀斑/cm2。应理解，蚀斑面积密度与蚀斑数量密度可在上述范围之外。
可在根据其中一个上述测试将样本暴露至腐蚀环境达一段设定时间之前或之后，判定所述样本的低电平接触电阻。一些实施例中，可根据规范EIA 364、测试程序23判定低电平接触电阻。一般地，这样测量样本的接触电阻，即，使得样本在规定负载与电流下与测量探针接触，所述测量探针具有与所述样本接触的限定截面积。例如，可在25g、50g、150g、200g的负载下测量低电平接触电阻。一般地，随着负载增大，低电平接触电阻减小。
可将门限低电平接触电阻值设为，当样本的测量低电平接触电阻值大于所述门限值则说明样本的测试失败。例如，根据ASTM B735暴露至硝酸蒸汽2小时之后，或者根据ASTM B845(IIa类协议)暴露至混合流动气体5天之后，25g负载下的门限低电平接触电阻值可大于1mOhm，大于10mOhm，大于100mOhm，或大于1000mOhm。应理解也可达成其他门限低电平接触电阻值。
一些实施例中，经涂覆的物品具有降低的低电平接触电阻。对于电气接头之类的电气应用中所使用的物品，降低的低电平接触电阻是有用的。一些情况下，物品在25g负载下的低电平接触电阻小于约100mOhm；一些情况下，小于约10mOhm；一些情况下，小于约5mOhm；并且，一些情况下，小于约1mOhm。应理解，物品的低电平接触电阻也可在这一范围之外。应理解，与测量探针接触的截面积可影响测得的低电平接触电阻值。
也可测试经涂覆物品的耐用性。一些实施例中，可与上述腐蚀测试及/或接触电阻测试结合，进行耐用性测试。耐用性测试可包括用物体对经涂覆物品的表面摩擦一段时间，然后视觉检查涂层的损伤及/或测量涂层的接触电阻。耐用性测试的非限制性例子中，可以在设定负载下保持抵靠着经涂覆的物品表面的挡块，并且经涂覆物品往复移动以使得所述挡块抵靠着所述经涂覆物品的表面摩擦。例如，可以50g的负载抵靠着经涂覆物品的表面保持挡块。例如，可通过单元时间内的循环次数测量往复运动的持续时间。例如，可以每秒1次循环的速率进行500秒的往复运动。一些实施例中，可在对物品进行上文详述的腐蚀测试之前及/或之后进行耐用性测试。可如前所述地测量接触电阻。一些情况下，可视觉观察磨损痕迹。一些实施例中，可通过在规定负载下经规定循环数之后测量磨损痕迹之间的暴露基底材料的宽度来分析所述磨损痕迹。一些实施例中，所述分析可为“通过/失败”测试，其磨损痕迹之间的暴露基底材料的门限宽度设为，若暴露基底材料的宽度大于所述门限值，则说明所述物品的测试失败。
下列示例不应认为是限制，而应是本发明某些特征的阐述。
示例
示例1
本示例对包括根据本发明实施例制得的带有第一层的涂层的物品与具有现有涂层的两个物品进行了抗腐蚀性对比。图2A～2C分别示出了根据ASTMB0735-06暴露至硝酸蒸汽30分钟的物品。图2A示出了使用脉冲反向DC电流涂覆有Ni-W层(约40～50微英寸厚)的铜基材料，其基本不发生腐蚀；图2B示出了涂覆有镍(约40～50微英寸厚，以脉冲DC电流使用Ni-氨基磺酸盐浴进行电沉积)的铜基材料，其显著腐蚀；并且图2C示出了电镀有镍-磷(EP-NiP)(约40～50微英寸厚，以脉冲DC电流进行电沉积)的铜基材料，其显著腐蚀。本示例表明，较之现有的经涂覆物品，本发明的经涂覆物品具有改进的耐腐蚀性。
示例2
本示例对包括根据本发明实施例制得的带有第一层的涂层的物品的耐用性与具有现有涂层的两个物品的耐用性进行了对比。图3A示出分析经涂覆物品耐用性的示意测试程序。以50g的负载将电镀有与磨损表面相同材料的挡块100抵靠着经涂覆物品110固定保持，同时以每秒1次循环的频率沿路径120抵靠着所述挡块使得所述经涂覆物品往复运动。图3B示出了涂覆有镍(约40～50微英寸厚，以脉冲DC电流使用Ni-氨基磺酸盐浴进行电沉积)的铜基材料，其显示出大规模的摩擦痕迹130。图3C示出了电镀有Ni-W(约40～50微英寸厚，以脉冲反向DC电流进行电沉积)的铜基材料，其显示出明显少的多的磨损痕迹。本示例表明，较之现有的经涂覆物品，本发明的经涂覆物品具有改进的耐用性。
示例3
本示例对包括根据本发明实施例制得的带有两层的涂层的物品与具有现有涂层的两个物品进行了抗腐蚀性对比。图4A～4D分别示出了根据ASTMB0845-97R08E01暴露至混合流动气体5天之后的物品。图4A～4B示出了涂覆有第一层Ni-W(40微英寸厚，使用脉冲反向DC电流电沉积)以及20微英寸厚(图4A)或30微英寸厚(图4B)的Au-Co合金的第二层的铜基底材料，其基本不发生腐蚀。图4C～4D示出了涂覆有第一层镍(约40～50微英寸厚，以脉冲DC电流使用Ni-氨基磺酸盐浴进行电沉积)以及20微英寸厚(图4A)或30微英寸厚(图4B)的Au-Co合金的第二层的铜基底材料，其显著腐蚀。本示例表明，较之现有的经涂覆物品，本发明的经涂覆物品具有改进的耐腐蚀性。
示例4
本示例对暴露至腐蚀条件后的包括根据本发明实施例制得的带有两层的涂层的物品与暴露至腐蚀条件后的具有现有涂层的两个物品进行了接触电阻对比。图5A～5D量化了示例3的经涂覆物品的低电平接触电阻，并且分别示出了多个重复试验的结果。图5A示出了涂覆有Ni-W和20微英寸厚Au-Co合金的基底材料的接触电阻，图5B示出了涂覆有Ni-W和30微英寸厚Au-Co合金的基底材料的接触电阻。这两种情况下，接触电阻小于10mOhm，这一值定义为“通过”本测试的门限值。图5C～5D分别示出了涂覆有镍(使用Ni-氨基磺酸盐浴进行电沉积)以及分别为20微英寸厚的金或30微英寸厚的金的铜基底材料的接触电阻。这两个物品都未通过接触电阻测试，因为接触电阻大于10mOhm。本示例表明，较之现有的经涂覆物品，本发明的经涂覆物品在暴露至腐蚀条件之后具有改进的接触电阻。
示例5
本示例对暴露至腐蚀条件后的包括根据本发明实施例制得的带有两层的涂层的物品与暴露至腐蚀条件后的具有现有涂层的两个物品进行了接触电阻对比。图6示出了一组经涂覆物品的立体图像(10倍放大)，各经涂覆物品暴露至硝酸蒸汽2小时。第一层(Ni-W，使用脉冲反向DC电流电沉积)的厚度列在每列的顶部，并且与各列中各基底材料上的第一层的厚度(从左至右：20微英寸、30微英寸、40微英寸)相对应。第二层(Au-Co)的厚度列在每一行左侧，并且与各行中的各基底材料上的第二涂层的厚度(从上到下：4微英寸、10微英寸、20微英寸、30微英寸)相对应。图7示出了一组经涂覆物品的未放大图像，这一组的经涂覆物品的规格与图6相同，并且各经涂覆物品暴露至混合流动气体5天。图8A～8D示出了如图7所示的经涂覆物品的接触电阻测量。作为对照，图9A～9B示出了具有包括EP-NiP第一层(以脉冲DC电流进行电沉积)与Au-Co第二层的涂层的物品暴露至硝酸蒸汽2小时之后的接触电阻测量。本示例表明，较之现有的经涂覆物品，本发明的经涂覆物品在暴露至腐蚀条件之后具有改进的接触电阻。

Claims (24)

1.一种物品，包括：
含铜的基底材料；
形成在所述基底材料上的涂层，所述涂层包括：
含Ni，并且含W及/或Mo的第一层，其中所述第一层的厚度大于5微英寸；及
形成在所述第一层上的第二层，所述第二层含有选自由Au、Ru、Os、Rh、Ir、Pd、Pt、及/或Ag构成的组中的金属，其中所述第二层的厚度小于30微英寸。
2.如权利要求1所述的物品，其中所述涂层为纳米晶态。
3.如权利要求1所述的物品，其中所述第一层的厚度大于20微英寸。
4.如权利要求1所述的物品，其中所述第二层的厚度小于20微英寸。
5.如权利要求4所述的物品，其中所述第二层的厚度小于10微英寸。
6.如权利要求1所述的物品，其中所述第一层包括镍-钨合金。
7.如权利要求1所述的物品，其中所述第一层包括镍-钼合金。
8.如权利要求1所述的物品，其中，根据ASTM B0735暴露至硝酸蒸汽2小时之后，所述涂层的接触电阻小于约10mOhm。
9.如权利要求1所述的物品，其中，根据IIa类协议ASTM B0845暴露至混合流动气体5天之后，所述涂层的接触电阻小于约10mOhm。
10.如权利要求1所述的物品，其中，根据ASTM B0735暴露至硝酸蒸汽2小时之后，所述涂层的腐蚀密度小于约1个蚀斑/cm2。
11.如权利要求1所述的物品，其中所述第一层直接形成在所述基底材料上。
12.如权利要求1所述的物品，其中所述第一层与所述第二层是电沉积的。
13.一种方法，包括
使用具有正向脉冲和反向脉冲的波形将涂层的第一层电沉积在基底材料上，
其中所述基底材料含铜，所述第一层含Ni并且含W及/或Mo，并且所述第一层的厚度大于5微英寸；并且
在所述第一层上电沉积所述涂层的第二层，所述第二层含有选自由Au、Ru、Os、Rh、Ir、Pd、Pt、及/或Ag构成的组中的金属，其中所述第二层的厚度小于30微英寸。
14.如权利要求13所述的方法，其中所述第一层和所述第二层为纳米晶态。
15.如权利要求13所述的方法，其中使用具有正向脉冲和反向脉冲的波形电沉积所述第二层。
16.如权利要求13所述的方法，其中所述第一层的厚度大于20微英寸。
17.如权利要求13所述的方法，其中所述第二层的厚度小于20微英寸。
18.如权利要求13所述的方法，其中所述第二层的厚度小于10微英寸。
19.如权利要求13所述的方法，其中所述第一层包括镍-钨合金。
20.如权利要求13所述的方法，其中所述第一层包括镍-钼合金。
21.如权利要求13所述的方法，其中，根据ASTM B0735暴露至硝酸蒸汽2小时之后，所述物品的接触电阻小于约10mOhm。
22.如权利要求13所述的方法，其中，根据IIa类协议ASTM B0845暴露至混合流动气体5天之后，所述物品的接触电阻小于约10mOhm。
23.如权利要求13所述的方法，其中，根据ASTM B0735暴露至硝酸蒸汽2小时之后，所述涂层的腐蚀密度小于约1个蚀斑/cm2。
24.如权利要求13所述的方法，其中所述第一层直接形成在所述基底材料上。
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