CN107735212B - 软钎料材料、焊接接头和软钎料材料的检查方法 - Google Patents

软钎料材料、焊接接头和软钎料材料的检查方法 Download PDF

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CN107735212B
CN107735212B CN201680039077.7A CN201680039077A CN107735212B CN 107735212 B CN107735212 B CN 107735212B CN 201680039077 A CN201680039077 A CN 201680039077A CN 107735212 B CN107735212 B CN 107735212B
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core
ball
core ball
solder material
solder
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CN107735212A (zh
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川崎浩由
西野友朗
六本木贵弘
佐藤勇
川又勇司
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Senju Metal Industry Co Ltd
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Senju Metal Industry Co Ltd
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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
    • B23K35/0244—Powders, particles or spheres; Preforms made therefrom
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/065—Spherical particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/102—Metallic powder coated with organic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14—Treatment of metallic powder
    • B22F1/142—Thermal or thermo-mechanical treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/17—Metallic particles coated with metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/18—Non-metallic particles coated with metal
    • 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
    • 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
    • B23K35/0233—Sheets, foils
    • B23K35/0238—Sheets, foils layered
    • 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
    • B23K35/0244—Powders, particles or spheres; Preforms made therefrom
    • B23K35/025—Pastes, creams, slurries
    • 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
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • 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
    • B23K35/26—Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
    • B23K35/262—Sn as the principal constituent
    • 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
    • B23K35/22—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
    • B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
    • B23K35/302—Cu as the principal constituent
    • 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
    • B23K35/22—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
    • B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
    • B23K35/3033—Ni as the principal constituent
    • 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
    • B23K35/22—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
    • B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
    • B23K35/3046—Co as the principal constituent
    • 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
    • B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
    • B23K35/3601—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest with inorganic compounds as principal constituents
    • B23K35/3602—Carbonates, basic oxides or hydroxides
    • 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
    • B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
    • B23K35/365—Selection of non-metallic compositions of coating materials either alone or conjoint with selection of soldering or welding materials
    • 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
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    • 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
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    • B32B15/00—Layered products comprising a layer of metal
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    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C13/00—Alloys based on tin
    • 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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    • 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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    • C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
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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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    • H01L23/49811—Additional leads joined to the metallisation on the insulating substrate, e.g. pins, bumps, wires, flat leads
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    • H—ELECTRICITY
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    • H01L24/13—Structure, shape, material or disposition of the bump connectors prior to the connecting process of an individual bump connector
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    • H05K3/32—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits
    • H05K3/34—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits by soldering
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Abstract

准确地辨别不易氧化的软钎料材料。Cu芯球具备：Cu球，其具有规定的大小，用于在半导体封装体与印刷电路基板之间确保间隔；以及，被覆铜球的软钎料层。就Cu芯球而言，在位于温度为25℃、湿度为40％的室内的150℃的恒温槽中的72小时的烘烤试验后，在L*a*b*表色系统中的亮度为62.5以上，烘烤试验前的软钎料材料在L*a*b*表色系统中的亮度为65以上且在L*a*b*表色系统中的黄色度为7.0以下。

Description

软钎料材料、焊接接头和软钎料材料的检查方法
技术领域
本发明涉及软钎料材料、焊接接头和软钎料材料的检查方法。
背景技术
近年来，由于小型信息设备的发展，所搭载的电子部件正在迅速小型化。电子部件中，为了应对由于小型化的要求而进行的连接端子的狭小化、安装面积的缩小而应用将电极设置于背面的球栅阵列(以下称为“BGA”。)。
在应用BGA的电子部件中，有例如半导体封装体。半导体封装体例如将具有电极的半导体芯片介由软钎料凸块接合于印刷电路基板的导电性焊盘、并利用树脂将这些密封而构成。近年来，为了应对进一步的高密度安装要求，开发了半导体封装体沿着高度方向堆叠而成的3维高密度安装。
作为软钎料凸块，例如开发了Cu芯球。专利文献1记载了一种Cu芯球，其具备：成为核的Cu球和被覆Cu球的表面的软钎料层。就使用Cu芯球构成的软钎料凸块而言，将电子部件安装于印刷电路基板时，即使半导体封装体的重量施加于软钎料凸块，也能通过在软钎料的熔点下不熔融的Cu球支撑半导体封装体。由此能够防止软钎料凸块由于半导体封装体的自重而碎裂的情况。
但是，有时Cu芯球的软钎料表面会形成氧化膜。由于该氧化膜的影响，软钎料与电极之间发生润湿不良，结果发生Cu芯球安装不良，存在半导体封装体的生产率和成品率大幅下降的问题。因此，要求Cu芯球具有耐氧化性。
该Cu芯球的氧化膜问题有时是由于Cu芯球制作后的保管环境的温度、湿度而产生的。即使将形成了氧化膜的Cu芯球安装于半导体封装体的电极上、然后进行回流焊处理，也同样产生软钎料的润湿不良，构成Cu芯球的软钎料无法润湿扩散到电极整体，呈现电极露出的状态，存在由于Cu芯球与电极的位置偏移等而发生Cu芯球安装不良的问题。因此，Cu芯球制作后的氧化膜厚管理也成为重要的问题。
于是，本申请人着眼于黄色度和亮度这两个指标来作为在软钎料熔融前事先管理氧化膜厚的指标，并提出了如下方法：选择黄色度和亮度符合预先设定的值的Cu芯球，从而准确地管理形成于Cu芯球的表面的氧化膜厚。通过使用利用该Cu芯球的氧化膜厚的管理方法得到的Cu芯球，可以良好地进行半导体芯片与印刷电路基板的接合。
现有技术文献
专利文献
专利文献1：国际公开第95/24113号
发明内容
发明要解决的问题
但是，在对Cu球实施镀覆处理后，一般会实施洗涤处理，以除去残留于Cu芯球的表面的镀覆液中的有机络合剂、pH调节剂、pH缓冲剂、促进剂、稳定剂、表面活性剂、光泽剂、半光泽剂、平滑剂等镀覆液残渣。但是，即使是制作后的黄色度和亮度符合预先设定的值的Cu芯球，当洗涤处理不充分时，Cu芯球的表面会残留较多的镀覆液残渣，即使在合适的保管条件下保管，在长期保管Cu芯球后等，与通常情况相比会相应于残留的镀覆液残渣量而促进Cu芯球表面的软钎料氧化。其结果是，即使使用制作后的黄色度和亮度符合预先设定的值的Cu芯球，在半导体芯片与印刷电路基板接合时，有时由于形成于Cu芯球的表面的氧化膜而发生接合不良。
因此，本发明是鉴于上述问题而作出的，其目的在于，提供一种即使长期保管后也不易氧化的软钎料材料和焊接接头。此外，本发明提供软钎料材料的检查方法，其能够准确地辨别即使长期保管后也不易氧化的软钎料材料。
用于解决问题的方案
本发明人们发现，对于在Cu芯球的洗涤处理后、通过在规定的温度和大气湿度条件下进行加热处理来有意识地促进氧化的Cu芯球而言，当满足烘烤试验后在L*a*b*表色系统中的亮度(L＊值)为62.5以上的条件时，能得到镀覆液残渣量少、即不易氧化的Cu芯球。需要说明的是，在本发明中，烘烤试验是用于有意识地促进相应于Cu芯球1的洗涤后残留的镀覆液量而形成的氧化膜的生长的试验，例如是指将制作后的Cu芯球在位于温度为25℃、湿度为40％的室内的150℃的恒温槽中加热保管72小时的试验。制作后的Cu芯球也包括例如进行加速试验等后的Cu芯球。
(1)一种软钎料材料，其具备：用于在接合物与被接合物之间确保间隔的芯；以及，被覆前述芯的由Sn或以Sn为主要成分的软钎料合金构成的被覆层，其特征在于，在位于温度为25℃、湿度为40％的室内的150℃的恒温槽中的72小时的烘烤试验后，在L*a*b*表色系统中的亮度为62.5以上，前述烘烤试验前的前述软钎料材料在L*a*b*表色系统中的亮度为65以上且在L*a*b*表色系统中的黄色度为7.0以下。
(2)根据上述(1)的软钎料材料，其特征在于，被覆有由选自Ni和Co中的1种以上元素形成的层的前述芯被前述被覆层被覆。
(3)根据上述(1)或(2)的软钎料材料，其特征在于，前述软钎料材料在前述烘烤试验后在L*a*b*表色系统中的前述亮度为70.2以上。
(4)根据上述(1)～(3)中的任一软钎料材料，其特征在于，前述芯由球状的选自由Cu、Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg组成的组中的至少1种元素或树脂材料构成。
(5)根据上述(1)～(3)中的任一软钎料材料，其特征在于，前述芯由圆柱状的选自由Cu、Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg组成的组中的至少1种元素或树脂材料构成。
(6)一种焊接接头，其使用了上述(1)～(5)中的任一软钎料材料。
(7)一种软钎料材料，其具备：用于在接合物与被接合物之间确保间隔的芯；以及，被覆前述芯的由Sn或以Sn为主要成分的软钎料合金构成的被覆层，其特征在于，在位于温度为25℃、湿度为40％的室内的150℃的恒温槽中进行72小时加热后，氧化膜厚为4.9nm以下。
(8)根据上述(7)的软钎料材料，其特征在于，被覆有由选自Ni和Co中的1种以上元素形成的层的前述芯被前述被覆层被覆。
(9)根据上述(7)或(8)的软钎料材料，其特征在于，前述烘烤试验后，前述氧化膜厚为3.1nm以下。
(10)根据上述(7)～(9)中的任一软钎料材料，其特征在于，前述芯由球状的选自由Cu、Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg组成的组中的至少1种元素或树脂材料构成。
(11)根据上述(7)～(9)中的任一软钎料材料，其特征在于，前述芯由圆柱状的选自由Cu、Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg组成的组中的至少1种元素或树脂材料构成。
(12)一种焊接接头，其使用了上述(7)～(11)中的任一软钎料材料。
(13)一种软钎料材料的检查方法，其特征在于，具有如下工序：将具备用于在接合物与被接合物之间确保间隔的芯、和被覆该芯的由Sn或以Sn为主要成分的软钎料合金构成的被覆层的软钎料材料在温度为25℃、湿度为40％的室内在设为150℃的恒温槽中加热72小时的工序；以及，获得在前述工序中加热后的前述软钎料材料在L*a*b*表色系统中的亮度为62.5以上的软钎料材料的工序。
发明的效果
根据本发明的软钎料材料、焊接接头和软钎料材料的检查方法，能够准确且在短时间内辨别出长期保管后也不易氧化的Cu芯球。
附图说明
图1是示出本发明的一实施方式中Cu芯球的构成例的剖视图。
图2是示出烘烤试验前的Cu芯球的黄色度与氧化膜厚的关系的图。
图3是示出烘烤试验前的Cu芯球的亮度与氧化膜厚的关系的图。
图4是示出烘烤试验后的Cu芯球的黄色度与保管期的关系的图。
图5是示出烘烤试验后的Cu芯球的亮度与氧化膜厚的关系的图。
具体实施方式
以下参照附图来详细说明本公开的优选实施方式。需要说明的是，以下说明中，所有的亮度和黄色度均是指L*a*b*表色系统中的亮度和黄色度。
[关于Cu芯球]
图1是示出本发明的Cu芯球1的构成的一例的剖视图。如图1所示，本发明的Cu芯球1具有规定的大小，具备：Cu球(芯)2，其用于在半导体封装体(接合物)和印刷电路基板(被接合物)之间确保间隔；以及，被覆Cu球2的软钎料层(被覆层)3。
·烘烤试验前的Cu芯球1的亮度和黄色度
就本发明的Cu芯球1而言，烘烤试验前在L*a*b*表色系统中的亮度为65以上且在L*a*b*表色系统中的黄色度为7.0以下。通过选择亮度和黄色度在上述范围内的Cu芯球1，可以将形成于软钎料层3的表面的氧化膜厚管理为一定值以下。
在本发明中，就烘烤试验前的Cu芯球1而言，仅用黄色度一个指标或仅用亮度一个指标不能进行氧化膜厚的准确管理，因此利用黄色度和亮度两个指标来管理Cu芯球1的氧化膜厚。以下首先说明仅用黄色度不能管理Cu芯球1的氧化膜厚的理由。
图2是示出Cu芯球1和软钎料球的黄色度(b＊值)与氧化膜厚的关系的图。纵轴表示黄色度，横轴表示氧化膜厚。如图2所示，就软钎料球而言，随着表面的氧化膜厚度变厚，黄色度也逐渐上升，氧化膜厚与黄色度大致成比例关系。因此，如果是软钎料球，在一定膜厚以内是可以通过黄色度来管理氧化膜厚的。
与此相对地，就Cu芯球1而言，比软钎料球更快地进行氧化，伴随氧化黄色度也上升，但是，此后氧化膜厚增加黄色度反而下降，氧化膜厚与黄色度不成正比关系。例如氧化膜厚为4nm时黄色度为7.2，而氧化膜厚为8.7nm时黄色度为2.9，氧化膜厚与黄色度之间相关关系不成立。我们认为，被覆Cu球的表面的软钎料镀层中的杂质是主要原因。因此，在仅利用黄色度进行管理的情况下，存在不能准确地管理氧化膜厚的问题。
然后说明仅用亮度不能管理Cu芯球1的氧化膜厚的理由。图3是示出Cu芯球1和软钎料球的氧化膜厚与亮度的关系的图表。纵轴表示亮度，横轴表示氧化膜厚。如图3所示，Cu芯球1的氧化膜厚与亮度处于氧化膜越厚则亮度越低的相关关系。求出此时的氧化膜厚与亮度的相关系数R。在-1～1的范围内求出相关系数R。然后将计算出的相关系数进行平方而求出贡献率(Contribution rate)R2。在0～1的范围内求出贡献率R2，其越接近1则表示亮度与氧化膜厚越具有相关关系。
Cu芯球1的氧化膜厚与亮度的贡献率R2＝0.8229，为比1小的值。与此相对地，当仅使用图2所示的黄色度下降前的值通过上述方法求出氧化膜厚与黄色度的贡献率时，利用黄色度进行管理时贡献率R2＝0.9523，变为接近1的值。因此，仅利用亮度进行管理的情况下，存在测定值偏差大、不能高精度地管理氧化膜厚的问题。因此，本发明中使用亮度和黄色度两个指标来进行烘烤试验前的Cu芯球1的氧化膜厚的准确管理。
·烘烤试验后的Cu芯球1的亮度和黄色度
就本发明的Cu芯球1而言，烘烤试验后在L*a*b*表色系统中的亮度为62.5以上。在150℃的大气湿度下将Cu芯球1加热72小时的理由是：即使不进行长期、例如1个月的保管试验，也可以在短时间内形成相应于Cu芯球1的洗涤后残留的镀覆液残渣量而形成的氧化膜。此外，之所以将Cu芯球1的亮度设为62.5以上，是为了准确地辨别、管理由于烘烤试验而氧化膜超过规定的膜厚(4.9nm)的Cu芯球1。需要说明的是，Cu芯球1在L*a*b*表色系统中的亮度更优选为70.2以上。这种情况下，可以更严格地管理氧化膜厚。通过满足上述2个条件，可以简单且容易地辨别Cu芯球1的洗涤后的镀覆液残渣量少、长期保管后也不易氧化的Cu芯球1。
然后说明管理烘烤试验后的Cu芯球1的氧化膜厚的指标。烘烤试验后的Cu芯球1可以仅用亮度这1个指标进行氧化膜厚的准确管理，因此仅用亮度来管理Cu芯球1的氧化膜厚。首先说明通过黄色度的指标不能管理Cu芯球1的氧化膜厚的理由。
图4是示出Cu芯球1的黄色度和保管期的关系的图。纵轴表示黄色度，横轴表示保管期。就Cu芯球1而言，比一般的软钎料球更快地进行氧化，伴随氧化黄色度也上升，但是，此后保管期延长黄色度反而下降，黄色度与保管期不成正比关系。在此，保管期为1天以上的Cu芯球1的保管天数与黄色度的贡献率R2＝0.589，为远小于1的值。因此，在利用黄色度进行管理的情况下，存在测定值偏差大、不能高精度地管理氧化膜厚的问题。
然后说明仅通过亮度指标就能够管理Cu芯球1的氧化膜厚的理由。图4是示出Cu芯球1的氧化膜厚与亮度的关系的图表。纵轴表示亮度，横轴表示氧化膜厚。Cu芯球1的氧化膜厚与亮度处于氧化膜越厚则亮度越低的相关关系。Cu芯球1的氧化膜厚与亮度的贡献率R2＝0.9332，为接近1的值。因此，如果利用亮度来进行管理，测定值偏差小，可以高精度地管理氧化膜厚。
我们认为，在烘烤试验前仅利用亮度进行管理时测定值偏差大而不能高精度地管理Cu芯球1的氧化膜厚、但在烘烤试验后仅利用亮度进行管理就可以高精度地管理Cu芯球1的氧化膜厚的理由如下。烘烤试验前进行的试验如后文详述那样改变了温度、湿度、加热时间等各种条件而假设了各种类型的氧化行为，其目的在于，制造在任一氧化行为下、如果制造后立即进行安装则能够抑制氧化膜厚的形成的Cu芯球。
相对地，本发明的烘烤试验假设可以抑制“长期保管后的”氧化膜厚的生长的Cu芯球，因此不需要像烘烤试验前进行的试验那样假设各种氧化行为，而仅关注高温保管下的氧化行为。因此，详细如后所述，本发明的烘烤试验将加热温度规定为150℃以上的某一恒定值、仅改变加热时间并将此外的条件统一而进行实验，从而仅观察高温保管时的氧化行为。所谓的假设的氧化行为仅为高温保管时这一点是指氧化膜厚的生长行为也是类似的。并且，所谓的氧化膜厚的生长行为是类似的这一点是指亮度变化也是类似的，明确了亮度与氧化膜厚的相关关系良好。因此，在本发明中，使用亮度这一个指标来进行烘烤试验后的Cu芯球1的氧化膜厚的准确管理。
[关于Cu球2]
然后，详细说明构成本发明的Cu芯球1的Cu球2。需要说明的是，Cu球2的构成等在烘烤试验前后是通用的，因此以下一并进行说明。Cu球2在将Cu芯球1用于软钎料凸块时在软钎焊的温度下不会熔融，因此具有抑制焊接接头的高度偏差的功能。因此，Cu球2优选球形度高、直径的偏差少的Cu球。
·Cu球2的组成
Cu球2既可以由Cu单质的组成来构成，也可以由以Cu为主要成分的合金组成来构成。在由合金来构成Cu球2时，Cu的含量为50质量％以上。此外，作为成为芯的球，除了Cu以外，还可以由Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg的金属单质或者合金、金属氧化物或金属混合氧化物来构成。
·Cu球2的纯度
对Cu球2的纯度没有特别限定，从抑制纯度下降所致的Cu球2的电导率、热导率劣化、此外根据需要抑制α射线量的观点出发，为99.9％以上。作为Cu球2中所含的杂质元素，可以列举Sn、Sb、Bi、Ni、Zn、Fe、Al、As、Ag、In、Cd、Pb、Au、P、S、Co等。
·Cu球2的球形度
从控制焊点高度的观点出发，Cu球2的球形度为0.95以上。当Cu球2的球形度小于0.95时，Cu球2成为不规则形状，因此在凸块形成时会形成高度不均匀的凸块，发生接合不良的可能性变高。进而，将Cu芯球1搭载于电极并进行回流焊时，Cu芯球1发生位置偏移，自对准性也会恶化。球形度更优选为0.990以上。在本发明中，球形度表示与完美球形的偏差。球形度例如可以通过最小二乘中心法(LSC法)、最小区域中心法(MZC法)、最大内切中心法(MIC法)、最小外切中心法(MCC法)等各种方法来求出。详细而言，球形度例如为将500个各Cu球2的直径除以长径时算出的算术平均值，值越接近上限1.00表示越接近完美球形。本发明中的长径的长度和直径的长度是指用三丰公司制的ULTRA QUICK VISION、ULTRA QV350-PRO测定装置测定的长度。
·Cu球2的直径
Cu球2的直径为1～1000μm。当Cu球2的直径在该范围时，可以稳定地制造球状的Cu球2，此外可以抑制端子间为窄间距时的连接短路。
在此，例如本发明的Cu芯球1的直径为1～300μm左右时，“Cu芯球”的集合体可以称为“Cu芯粉末”。其中，“Cu芯粉末”为具有上述特性的各个Cu芯球1所具备的多个Cu芯球1的集合体。与例如焊膏中的作为粉末而配混等单一的Cu芯球1在使用形态方面不同。同样地，在用于软钎料凸块的形成时也通常以集合体的形式来处理，因此以这种形态使用的“Cu芯粉末”与单一的Cu芯球1不同。
[关于软钎料层3]
然后详细说明构成本发明的Cu芯球1的软钎料层3。需要说明的是，软钎料层3的构成等在烘烤试验前后是通用的，因此以下一并进行说明。软钎料层3在将Cu芯球1用于软钎料凸块时会由于回流焊时的温度而熔融，发挥将半导体封装体的电极与印刷电路基板的电极电接合的接合构件的功能。
·软钎料层3的组成
软钎料层3既可以设为Sn单质的组成，也可以设为以Sn为主要成分的无铅软钎料合金的合金组成，还可以设为Sn-Pb软钎料合金的组成。在由合金构成软钎料层3时，Sn的含量为40质量％以上。作为无铅软钎料组成的一例，可以列举例如：Sn、Sn-Ag合金、Sn-Cu合金、Sn-Bi合金、Sn-Ag-Cu合金、Sn-In合金和在这些中添加有规定的合金元素的合金。作为所添加的合金元素，可以列举例如：Ag、Cu、In、Ni、Co、Sb、P、Fe等。关于所添加的合金元素的添加量，优选抑制为使无铅软钎料合金的黄色度和亮度与Sn单质的黄色度和亮度达到几乎同程度的量。这些中，从热疲劳寿命的观点出发，软钎料层3的合金组成优选为Sn-3Ag-0.5Cu。对软钎料层3的厚度没有特别限制，为例如100μm(单侧)以下是充分的。通常可以为20～50μm。需要说明的是，本发明中的以Sn为主要成分的无铅软钎料合金的Sn的含量优选Sn为80％以上，更优选Sn为90％以上。
需要说明的是，在Cu球2的表面与软钎料层3之间，还可以设置被覆Cu球2的由选自Ni和Co中的1种以上元素形成的层，例如镀Ni层、镀Co层等。由此，在与电极接合时，可以降低Cu向软钎料中的扩散，可以抑制Cu球2的Cu蚀。镀Ni层、镀Co层等的膜厚例如为单侧0.1～20μm。此外，可以在Cu芯球1的表面被覆助焊剂。
[Cu芯球1的制造方法]
然后说明本发明的Cu芯球1的制造方法的一例。首先，准备陶瓷之类的耐热性板，即底部设有呈半球状的多个圆形的槽的耐热板。槽的直径、深度可根据Cu球2的粒径适当设定，例如直径为0.8mm，深度为0.88mm。然后，将通过切断作为材料的Cu细线而得的芯片形状的Cu材(以下称为“芯片材”。)逐一放入耐热板的槽内。
然后，将槽内投入有芯片材的耐热板在填充有还原性气体、例如氨分解气体的炉内升温到1100～1300℃并进行30～60分钟加热处理。此时，当炉内温度达到Cu的熔点以上时，芯片材会熔融并形成球状。然后，通过使炉内冷却而使Cu球2在耐热板的槽内成型。冷却后，以低于Cu熔点的温度即800～1000℃再次对成型后的Cu球2进行加热处理。
此外，作为其它方法，有如下方法：使熔融Cu从设于坩埚底部的孔滴落，使该液滴冷却而制造Cu球2的雾化法；利用热等离子体将Cu切割金属加热到1000℃以上而制造球的方法。由此制造的Cu球2可以分别在800～1000℃的温度下实施30～60分钟再加热处理。此外，在制造Cu球2之前，可以将作为Cu球2的原料的Cu材在800～1000℃进行加热处理。
就作为Cu球2的原料的Cu材而言，例如可以使用颗粒、线、柱等。从不过度降低Cu球2的纯度的观点出发，Cu材的纯度可以为99.9～99.99％。
进而，在使用高纯度Cu材的情况下，可以不进行上述加热处理而将熔融Cu的保持温度与以往同样地降低到1000℃左右。像这样前述加热处理可以根据Cu材的纯度而适当省略、变更。
作为使按照上述方式制作的Cu球2、镀覆液流动而在Cu球2上形成软钎料层3的方法，有如下方法：公知的转筒滚镀等电镀法；连接于镀覆槽的泵使镀覆液在镀覆槽中产生高速紊流，通过镀覆液的紊流在Cu球2上形成软钎料层3的方法；在镀覆槽中设置振动板并使其以规定频率振动，从而对镀覆液进行高速紊流搅拌，利用镀覆液的紊流在Cu球2上形成软钎料层3的方法等。
然后，在直径100μm的Cu球2上被覆膜厚(单侧)2μm的镀Ni层后，形成膜厚(单侧)18μm的Sn-Ag-Cu的软钎料层3，从而制作直径约140μm的Cu芯球1。
本发明的一实施方式的含Sn-Ag-Cu镀覆液在以水为主体的介质中含有磺酸类和作为金属成分的Sn、Ag和Cu作为必需成分。
金属成分在镀覆液中以Sn离子(Sn2+和/或Sn4+)、Ag离子(Ag+)和Cu离子(Cu+和/或Cu2+)形式存在。镀覆液通过将主要含有水和磺酸类的镀覆母液与金属化合物混合而得到，为了金属离子的稳定性，优选含有有机络合剂。
作为镀覆液中的金属化合物，例如可以例示以下物质。作为Sn化合物的具体例子，可以列举出甲磺酸、乙磺酸、2-丙醇磺酸、对苯酚磺酸等有机磺酸的锡盐；硫酸锡、氧化锡、硝酸锡、氯化锡、溴化锡、碘化锡、磷酸锡、焦磷酸锡、乙酸锡、甲酸锡、柠檬酸锡、葡萄糖酸锡、酒石酸锡、乳酸锡、琥珀酸锡、氨基磺酸锡、氟硼酸锡、氟硅酸锡等亚锡化合物。这些Sn化合物可以单独使用一种或将两种以上混合使用。
作为Cu化合物，可以列举上述的有机磺酸的铜盐、硫酸铜、氧化铜、硝酸铜、氯化铜、溴化铜、碘化铜、磷酸铜、焦磷酸铜、乙酸铜、甲酸铜、柠檬酸铜、葡萄糖酸铜、酒石酸铜、乳酸铜、琥珀酸铜、氨基磺酸铜、氟硼酸铜、氟硅酸铜等。这些Cu化合物可以单独使用一种或将两种以上混合使用。
作为Ag化合物，可以列举上述有机磺酸的银盐、硫酸银、氧化银、氯化银、硝酸银、溴化银、碘化银、磷酸银、焦磷酸银、乙酸银、甲酸银、柠檬酸银、葡萄糖酸银、酒石酸银、乳酸银、琥珀酸银、氨基磺酸银、氟硼酸银、氟硅酸银等。这些Ag化合物可以单独使用一种或将两种以上混合使用。
此外，在直径100μm的Cu球2上形成膜厚(单侧)20μm的Sn-Ag-Cu的软钎料层3时，需要约0.0108库伦的电量。
关于镀覆液中的各金属的配混量，作为Sn2+，为0.21～2mol/L，优选为0.25～1mol/L；作为Ag+，为0.01～0.1mol/L，优选为0.02～0.05mol/L；作为Cu2+，为0.002～0.02mol/L，优选为0.003～0.01mol/L。在此，由于参与镀覆的是Sn2+，因此本发明中调整Sn2+的量即可。
此外，优选Ag离子浓度相对于Cu离子浓度(Ag/Cu摩尔比)在4.5～5.58的范围。如果为该范围，可以形成Sn-3Ag-0.5Cu合金这种熔点低的Sn-Ag-Cu软钎料层3。需要说明的是，根据法拉第电解定律，利用下述式(1)估计出期望的软钎料镀覆的析出量，计算出电量，按照达到计算出的电量的方式将电流通入到镀覆液中，一边使Cu球2和镀覆液流动一边进行镀覆处理。镀覆槽的容积可以根据Cu球2和镀覆液的总投料量来确定。
w(g)＝(I×t×M)/(Z×F)···式(1)
式(1)中，w表示电解析出量(g)，I表示电流(A)，t表示通电时间(秒)，M表示所析出的元素的原子量(Sn时为118.71)，Z表示原子价(Sn时为2价)，F表示法拉第常数(96500库伦)，电量Q(A·秒)以(I×t)来表示。
在本发明中，一边使Cu球2和镀覆液流动一边进行镀覆，对使其流动的方法没有特别限定。例如可以如转筒式电镀法那样通过利用转筒的旋转使Cu球2和镀覆液流动。
镀覆处理后，在大气中、N2氛围中干燥，从而可以得到本发明的Cu芯球1。
在此，当如上操作对Cu球2进行软钎料镀覆时，有时镀覆液的残渣会残留在Cu芯球1的表面上。因此，为了去除Cu芯球1的表面残留的镀覆液残渣，通常实施洗涤处理。作为洗涤液，可以使用例如纯水、异丙醇等醇，酮(丙酮)等有机溶剂；磷酸三钠等酸性洗涤液；碱性洗涤液等。洗涤液既可以单独使用也可以将多种洗涤液组合使用。
作为洗涤方法，可以采用例如：浸渍洗涤、超声波洗涤、喷雾洗涤、喷淋洗涤、喷射洗涤、真空洗涤、脱气洗涤、转筒式洗涤、揺动刷洗、喷流鼓泡洗涤、微细鼓泡洗涤等。就洗涤方法而言，既可以根据所要求的洗涤效果采用单一的洗涤方法，也可以将多种洗涤方法组合。根据洗涤方法、洗涤液、洗涤时间的不同，洗涤后残留于Cu芯球1的表面的镀覆残渣也不同，保管时的氧化水平也不同，因此通过充分实施洗涤处理，可以得到长期保管后也不易氧化的Cu芯球1。
[软钎料材料的其它构成例(其1)]
此外，构成本发明的Cu芯球1的芯也可以由树脂球构成。作为树脂材料，可以列举例如含有氨基树脂、丙烯酸类树脂、乙烯-乙酸乙烯酯树脂、苯乙烯-丁二烯嵌段共聚物、聚酯树脂、三聚氰胺树脂、酚醛树脂、醇酸树脂、聚酰亚胺树脂、氨基甲酸酯树脂、环氧树脂、交联树脂等的树脂材料。其中，优选使用聚乙炔、聚吡咯、聚噻吩、聚苯胺等导电性塑料等。在将芯设为树脂材料时，可以利用树脂球和被覆树脂球的表面的Sn-Ag-Cu系软钎料镀覆层(被覆层)来构成Cu芯球。需要说明的是，上述被覆层的种类、层叠结构不限于上述例子。
[软钎料材料的其它构成例(其2)]
在上述实施方式中对利用亮度和黄色度来管理Cu芯球1的氧化水平的例子进行了说明，但并非仅限于此。例如，也可以通过直接管理形成于Cu芯球的表面的氧化膜的膜厚来管理洗涤后的Cu芯球的氧化水平。本发明的其它Cu芯球具备：用于在半导体封装体与印刷电路基板之间确保间隔的Cu球和被覆铜球的软钎料层，在150度、大气湿度下的72小时的烘烤试验后的氧化膜厚为4.9nm以下。通过将烘烤试验后的Cu芯球的氧化膜厚管理为4.9nm以下，可以辨别、获得充分实施了洗涤、不易氧化的(氧化膜薄的)Cu芯球。Cu芯球的氧化膜厚更优选为3.1nm以下。需要说明的是，为了方便，对于与上述Cu芯球1实质相同的构成功能省略说明。
[软钎料材料的其它构成例(其3)]
上述实施方式中对软钎料材料的形状为球状的情况进行了说明，但在软钎料材料的形状为柱形的情况下也可以应用本发明。在将软钎料材料设为柱形的情况下，软钎料材料由呈圆柱状的柱和被覆柱的表面的软钎料层构成。该软钎料材料在150℃、大气湿度下的72小时的烘烤试验后在L*a*b*表色系统中的亮度为62.5以上，烘烤试验前的软钎料材料在L*a*b*表色系统中的亮度为65以上且在L*a*b*表色系统中的黄色度为7.0以下。
作为柱的材料，可以使用Cu、Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg的金属单质、合金、金属氧化物或金属混合氧化物或者树脂材料。软钎料层既可以设为Sn单质的组成，也可以设为以Sn为主要成分的无铅软钎料合金的合金组成，还可以设为Sn-Pb软钎料合金的组成。在由合金构成软钎料层时，Sn的含量为40质量％以上。作为无铅软钎料组成的一例，可以列举例如：Sn、Sn-Ag合金、Sn-Cu合金、Sn-Bi合金、Sn-Ag-Cu合金、Sn-In合金和在这些中添加有规定的合金元素的合金。作为所添加的合金元素，可以列举例如：Ag、Cu、In、Ni、Co、Sb、P、Fe等。需要说明的是，除了形状(球形度)以外与上述Cu芯球1实质上为相同的构成功能，因为了方便而省略说明。
需要说明的是，本发明的Cu芯球1可以用于电子部件的焊接接头。在本例中，焊接接头例如是指在印刷电路基板的电极上安装有软钎料凸块的结构。此外，软钎料凸块例如是指在半导体芯片的电极上安装有Cu芯球1的结构。
实施例
以下说明本发明的实施例，但本发明不受这些实施例限定。
·Cu球的制作
准备纯度为99.995％以下的Cu线。将所准备的各Cu线投入坩埚中后，将坩埚的温度升温到1200℃，进行45分钟加热处理。然后使熔融Cu的液滴从设置于坩埚底部的孔滴落，将滴落的液滴冷却，从而制造平均粒径为100μm的Cu球。
·球形度
所制作的Cu球的球形度用CNC图像测定系统来测定。具体而言，使用三丰公司制的ULTRA QUICK VISION、ULTRA QV350-PRO测定装置。在本实施例中，利用上述测定装置测定Cu球长径的长度和直径的长度，计算出将500个各Cu球的直径除以长径而得的值的算术平均值，从而求出球形度。值越接近上限1.00表示越接近完美球形。
·烘烤试验前的Cu芯球的氧化膜厚、亮度和黄色度
然后，在所制作的直径100μm的Cu球的表面形成膜厚(单侧)2μm的镀Ni层，从而制作直径104μm的镀Ni的Cu球，进而在镀Ni层的表面形成膜厚18μm的软钎料层，从而制作直径140μm的Cu芯球。软钎料层使用Sn-3Ag-0.5Cu合金。然后将所制作的Cu芯球投入装有纯水的烧杯中，利用搅拌机搅拌洗涤10分钟。然后，在下述各实施例和比较例所示的条件下分别测定Cu芯球的氧化膜厚、亮度和黄色度。
实施例1中，使用刚洗涤后的Cu芯球。实施例2中，将搅拌洗涤后的Cu芯球在常温(大气暴露)且湿度30～40％的状态下保管2天。实施例3中，将搅拌洗涤后的Cu芯球在常温且湿度30～40％的状态下保管5天。实施例4中，将搅拌洗涤后的Cu芯球在常温且湿度30～40％的状态下保管7天。实施例5中，将搅拌洗涤后的Cu芯球在常温且湿度30～40％的状态下保管10天。实施例6中，将搅拌洗涤后的Cu芯球在常温且湿度30～40％的状态下保管14天。实施例7中，将搅拌洗涤后的Cu芯球在40℃且湿度90％的状态下保管1天。实施例8中，将搅拌洗涤后的Cu芯球在常温且湿度30～40％的状态下保管20天。实施例9中，将搅拌洗涤后的Cu芯球在40℃且湿度90％的状态下保管2天。实施例10中，将搅拌洗涤后的Cu芯球在200℃的状态下保管1小时。需要说明的是，常温为20～30℃。
比较例1中，将搅拌洗涤后的Cu芯球在40℃且湿度90％的状态下保管5天。比较例2中，将搅拌洗涤后的Cu芯球在40℃且湿度90％的状态下保管7天。比较例3中，将搅拌洗涤后的Cu芯球在40℃且湿度90％的状态下保管10天。比较例4中，将搅拌洗涤后的Cu芯球在40℃且湿度90％的状态下保管14天。比较例5中，将搅拌洗涤后的Cu芯球在200℃的状态下保管1天。比较例6中，将搅拌洗涤后的Cu芯球在200℃的状态下保管2天。
然后，将按照上述条件进行了保管的实施例1～10、比较例1～6的各Cu芯球回收，分别测定所回收的各Cu芯球的亮度、黄色度和氧化膜厚。Cu芯球的亮度和黄色度使用柯尼卡美能达制CM-2600d型分光测色计来测定。Cu球的氧化膜厚使用ULVAC PHI700的FE―AES测定装置来测定。测定装置的加速电压设为10kV，照射电流设为10nA。氧化膜厚(深度)由用离子(Ar)削去试样表面的速度(蚀刻速率)来求出，使用成为来自氧的强度(Intensity)的1/2峰值的蚀刻深度作为氧化膜厚近似值。蚀刻速率是以削去SiO2标准试样的速度换算的SiO2换算值。将所测定的各实施例1～10、比较例1～6的Cu芯球的亮度和黄色度与氧化膜厚的关系示于表1。表1中，氧化膜厚的单位为(nm)。
[表1]
如表1的实施例1～10所示，当选择亮度为62.5以上且黄色度为7.0以下的Cu芯球时，氧化膜厚达到3.8nm以下。此外，如表1的实施例1～5所示，当选择亮度为70以上且黄色度为5.1以下的Cu芯球时，氧化膜厚达到1.9nm以下，与此外的实施例6～10相比，得到了氧化膜厚更薄的Cu芯球。
另一方面，如比较例1～6所示，当Cu芯球的亮度小于62.5或黄色度超过7.0时，氧化膜厚达到3.9nm以上，变得比目标氧化膜厚更厚。由以上可知，通过选择亮度为65以上且黄色度为7.0以下的Cu芯球，可以提供氧化膜厚较薄的Cu芯球。
需要说明的是，也测定了红色度(a＊值)，但红色度(a＊值)与氧化膜厚的相关系数和红色度(a＊值)与氧化膜厚的贡献率小于1，确认不能使用红色度来作为氧化膜厚管理的指标。
此外，测定了各实施例1～10的Cu芯球的α射线量，结果虽然未在上述表1中示出，但全部Cu芯球的α射线量均为0.0010cph/cm2以下，低于所要求的0.0200cph/cm2。
·烘烤试验后的Cu芯球的氧化膜厚、亮度和黄色度
然后，使用上述实施例1的烘烤试验前的Cu芯球，为了在短期内使Cu芯球达到长期保管状态，对该Cu芯球实施烘烤试验。然后，分别测定进行烘烤试验后的Cu芯球的氧化膜厚、亮度和黄色度。需要说明的是，所使用的Cu芯球按照上述方式实施了10分钟的搅拌洗涤。
·洗涤条件和烘烤试验的条件
首先，在温度25℃(室温)、湿度40％下将恒温槽设为150℃，使该状态维持1小时以上。实施例1A中，将搅拌洗涤后的Cu芯球进一步用第1洗涤方法洗涤后，将洗涤后的Cu芯球放入上述恒温槽中，在150℃下保管3天。实施例1B中，将搅拌洗涤后的Cu芯球进一步用第2洗涤方法洗涤后，将洗涤后的Cu芯球放入上述恒温槽中，在150℃下保管3天。实施例1C中，将搅拌洗涤后的Cu芯球进一步用第3洗涤方法洗涤后，将洗涤后的Cu芯球放入上述恒温槽中，在150℃下保管3天。比较例1A中，将上述搅拌洗涤后的Cu芯球放入上述恒温槽中，在150℃下保管3天。
需要说明的是，第1洗涤方法为：向装有纯水的烧杯中投入所制作的Cu芯球，将投入了Cu芯球的烧杯设置在超声波洗涤机中，进行10秒超声波洗涤。第2洗涤方法为：向装有纯水的烧杯中投入所制作的Cu芯球，将投入了Cu芯球的烧杯设置在超声波洗涤机中，进行60秒超声波洗涤。第3洗涤处理为：向装有纯水的烧杯中投入所制作的Cu芯球，将投入了Cu芯球的烧杯设置在超声波洗涤机中，进行180秒超声波洗涤。需要说明的是，在本实施例中，将第1～第3洗涤方法分类为可以充分除去镀覆液残渣的洗涤效果高的洗涤方法。此外，将仅搅拌洗涤的洗涤方法分类为不能充分除去镀覆液残渣的洗涤效果低的洗涤方法。
然后，将按照上述条件进行了洗涤和加热保管的实施例1A、1B、1C、比较例1A的各Cu芯球回收，分别测定所回收的各Cu芯球的亮度、黄色度和氧化膜厚。Cu芯球的亮度和黄色度使用柯尼卡美能达制CM-2600d型分光测色计来测定。Cu球的氧化膜厚使用ULVAC PHI700的FE―AES测定装置来测定。测定装置的加速电压设为10kV，照射电流设为10nA。氧化膜厚(深度)由用离子(Ar)削去试样表面的速度(蚀刻速率)来求出，使用成为来自氧的强度的1/2峰值的蚀刻深度作为氧化膜厚近似值。蚀刻速率是以削去SiO2标准试样的速度换算的SiO2换算值。将所测定的各实施例1A、1B、1C、比较例1A的Cu芯球的亮度和黄色度与氧化膜厚的关系示于表2。表2中，氧化膜厚的单位为(nm)。
[表2]
如表2的实施例1A、1B、1C所示，作为洗涤条件，在搅拌洗涤的基础上进行超声波洗涤时，烘烤试验后的亮度达到62.5以上，Cu芯球的氧化膜厚达到4.9nm以下。由此，从Cu芯球的氧化膜厚与Cu芯球的洗涤条件具有相关关系的角度出发，可知：在选择(获得)满足加热保管后的亮度为62.5以上的条件的Cu芯球时，可以辨别、管理充分实施了洗涤、长期保管后也不易氧化的(氧化膜薄的)Cu芯球。
另一方面，如表2的比较例1A所示，作为洗涤条件仅进行搅拌洗涤时，烘烤试验后的Cu芯球的亮度小于62.5，Cu芯球的氧化膜厚超过4.9nm。由此可知，当选择满足加热保管后的亮度小于62.5的条件的Cu芯球时，洗涤不充分、软钎料镀覆液残渣量增多，其结果是，成为长期保管后容易氧化(氧化膜厚)的Cu芯球。
需要说明的是，对上述烘烤试验中使用表1所示的实施例1的Cu芯球的例子进行了说明，但并非仅限于此。使用表1所示的实施例2～10的Cu芯球的情况虽然未在表中示出，但我们获知能得到与使用实施例1的Cu芯球时同样的结果。具体而言，烘烤试验后的Cu芯球的亮度达到62.5以上，Cu芯球的氧化膜厚达到4.9nm以下。
然后，将加热、保管处理前的Cu芯球的刚洗涤后的Cu芯球的亮度和黄色度与氧化膜厚的关系示于表3。表3中，氧化膜厚的单位为(nm)。
[表3]
如表3的参考例1～4所示，进行烘烤试验前的Cu芯球的刚洗涤后的Cu芯球的亮度达到71.2以上、氧化膜厚达到1.2nm以下。由此确认：在刚洗涤后且进行烘烤试验前的状态下，未发生镀覆液残渣促进氧化膜的生长的情况，即使洗涤条件不同的情况下，氧化膜厚也未产生多大差异。
然后，将在温度150℃下进行5天(120小时)烘烤试验时的Cu芯球的亮度和黄色度与氧化膜厚的关系示于表4。表4中，氧化膜厚的单位为(nm)。
[表4]
如表4的参考例5～7所示，作为洗涤条件，在搅拌洗涤基础上进行超声波洗涤时，烘烤试验后的Cu芯球的亮度达到57.1以上，Cu芯球的氧化膜厚达到8.1nm以下。另一方面，如表4的参考例8所示，作为洗涤条件，仅进行搅拌洗涤的情况下，烘烤试验后的Cu芯球1的亮度小于57.1，Cu芯球的氧化膜厚超过8.1nm。
然后，将在温度150℃下进行7天(168小时)的烘烤试验时的Cu芯球的亮度和黄色度与氧化膜厚的关系示于表5。表5中，氧化膜厚的单位为(nm)。
[表5]
如表5的参考例9～11所示，作为洗涤条件，在搅拌洗涤基础上进行超声波洗涤时，烘烤试验后的Cu芯球的亮度达到53.9以上，Cu芯球的氧化膜厚达到11.5nm以下。另一方面，如表5的参考例12所示，作为洗涤条件，仅进行搅拌洗涤的情况下，烘烤试验后的Cu芯球1的亮度小于53.9，Cu芯球的氧化膜厚超过11.5nm。
上述本实施例、参考例中，从同一批处理的多个Cu芯球中抽取特定的Cu芯球使用。因此，用本实施例、参考例的Cu芯球得到的各结果也可以同样应用于未进行烘烤试验工序的同一批处理的其它Cu芯球。
需要说明的是，本发明不限于上述实施方式本身，在实施阶段，可以在不脱离其主旨的范围内使构成要素变形、具体化。此外，可以将上述实施方式中公开的多个构成要素适当组合来形成各种发明。
附图标记说明
1 Cu芯球(软钎料材料)
2 Cu球(芯)
3 软钎料层(被覆层)

Claims (17)

1.一种软钎料材料，其具备：
用于在接合物与被接合物之间确保间隔的芯；以及，
被覆所述芯的由Sn或以Sn为主要成分的软钎料合金构成的被覆层，
其特征在于，
在位于温度为25℃、湿度为40％的室内的150℃的恒温槽中的72小时的烘烤试验后，在L*a*b*表色系统中的亮度为62.5以上，
所述烘烤试验前的所述软钎料材料在L*a*b*表色系统中的亮度为65以上且在L*a*b*表色系统中的黄色度为7.0以下。
2.根据权利要求1所述的软钎料材料，其特征在于，
被覆有由选自Ni和Co中的1种以上元素形成的层的所述芯被所述被覆层被覆。
3.根据权利要求1或2所述的软钎料材料，其特征在于，
所述软钎料材料在所述烘烤试验后、在L*a*b*表色系统中的所述亮度为70.2以上。
4.根据权利要求1或2所述的软钎料材料，其特征在于，
所述芯由球状的选自由Cu、Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg组成的组中的至少1种元素或树脂材料构成。
5.根据权利要求3所述的软钎料材料，其特征在于，
所述芯由球状的选自由Cu、Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg组成的组中的至少1种元素或树脂材料构成。
6.根据权利要求1或2所述的软钎料材料，其特征在于，
所述芯由圆柱状的选自由Cu、Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg组成的组中的至少1种元素或树脂材料构成。
7.根据权利要求3所述的软钎料材料，其特征在于，
所述芯由圆柱状的选自由Cu、Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg组成的组中的至少1种元素或树脂材料构成。
8.一种焊接接头，其使用了权利要求1～7中的任一项所述的软钎料材料。
9.一种软钎料材料，其具备：
用于在接合物与被接合物之间确保间隔的芯；以及，
被覆所述芯的由Sn或以Sn为主要成分的软钎料合金构成的被覆层，
其特征在于，
在位于温度为25℃、湿度为40％的室内的150℃的恒温槽中的72小时的烘烤试验后，氧化膜厚为4.9nm以下。
10.根据权利要求9所述的软钎料材料，其特征在于，
被覆有由选自Ni和Co中的1种以上元素形成的层的所述芯被所述被覆层被覆。
11.根据权利要求9或10所述的软钎料材料，其特征在于，
所述烘烤试验后的所述氧化膜厚为3.1nm以下。
12.根据权利要求9或10所述的软钎料材料，其特征在于，
所述芯由球状的选自由Cu、Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg组成的组中的至少1种元素或树脂材料构成。
13.根据权利要求11所述的软钎料材料，其特征在于，
所述芯由球状的选自由Cu、Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg组成的组中的至少1种元素或树脂材料构成。
14.根据权利要求9或10所述的软钎料材料，其特征在于，
所述芯由圆柱状的选自由Cu、Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg组成的组中的至少1种元素或树脂材料构成。
15.根据权利要求11所述的软钎料材料，其特征在于，
所述芯由圆柱状的选自由Cu、Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg组成的组中的至少1种元素或树脂材料构成。
16.一种焊接接头，其使用了权利要求9～15中的任一项所述的软钎料材料。
17.一种软钎料材料的检查方法，其特征在于，具有如下工序：
将具备用于在接合物与被接合物之间确保间隔的芯、和被覆该芯的由Sn或以Sn为主要成分的软钎料合金构成的被覆层的软钎料材料在温度为25℃、湿度为40％的室内在设为150℃的恒温槽中加热72小时的工序；以及，
获得在所述工序中加热后的所述软钎料材料在L*a*b*表色系统中的亮度为62.5以上的软钎料材料的工序。
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JP5850199B1 (ja) 2016-02-03
US10888957B2 (en) 2021-01-12
EP3315245A1 (en) 2018-05-02
US20180281118A1 (en) 2018-10-04
JP2017013080A (ja) 2017-01-19

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