CN107653385A - 一种适用于铜丝的耐腐蚀改性方法 - Google Patents

一种适用于铜丝的耐腐蚀改性方法 Download PDF

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CN107653385A
CN107653385A CN201710863513.9A CN201710863513A CN107653385A CN 107653385 A CN107653385 A CN 107653385A CN 201710863513 A CN201710863513 A CN 201710863513A CN 107653385 A CN107653385 A CN 107653385A
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copper
copper wire
alloy
corrosion
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CN107653385B (zh
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邵光伟
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Jiangsu Luxin New Energy Technology Co., Ltd.
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Foshan Huichuang Zhengyuan New Mstar Technology Ltd
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Abstract

本发明公开了一种适用于铜丝的耐腐蚀改性方法，该改性方法先从原料铜中提取高纯铜，清洗、烘干后与镍、镓、磷钨酸钾、纳米氮化钽共同置于熔炼装置中熔化，经在线除气、脱氧、搅拌，用牵引机组离合式真空上引无氧合金铜杆，随后采用连续挤压机组生产合金铜带坯料，随后经粗拔、镀钯、精拔得到镀钯合金铜丝。利用该方法制备而成的镀钯合金铜丝具有良好的耐腐蚀性能，并且成本较低，能够满足行业的要求，具有良好的应用前景。同时，本发明还公开了该方法所制得的铜丝在集成电路中的应用。

Description

一种适用于铜丝的耐腐蚀改性方法
技术领域
本发明涉及金属材料加工技术领域，特别涉及一种抗氧化键合铜丝的制备方法及应用。
背景技术
铜具有优良的导电性、导热性以及化学稳定性而广泛应用于工业和日常生活中。键合铜线以其优良的力学性能、电学性能和低成本因素，在微电子封装上被逐步采用，现有的键合铜丝以高纯单晶铜为原材料，由于高纯单晶铜的氧化具有明显的取向性，非密排的晶面上界面能高、晶面原子堆垛相对疏松和原子尺度上粗糙，且氧化膜生长连续，氧化速率高于密排的晶面，单晶铜非密排的晶面氧化膜的致密性和附着性都较差，氧化速率大，耐腐蚀性差，不能满足高端微电子封装的要求。
镍是银白色金属，具有磁性和良好的可塑性。有好的耐腐蚀性，镍近似银白色、硬而有延展性并具有铁磁性的金属元素，它能够高度磨光和抗腐蚀。溶于硝酸后，呈绿色。主要用于合金(如镍钢和镍银)及用作催化剂(如兰尼镍，尤指用作氢化的催化剂)。因为镍的抗腐蚀性佳，常被用在电镀上，主要用来制造不锈钢和其他抗腐蚀合金，如镍钢、镍铬钢及各种有色金属合金，含镍成分较高的铜镍合金，就不易腐蚀。也作加氢催化剂和用于陶瓷制品、特种化学器皿、电子线路、玻璃着绿色以及镍化合物制备等。
镓是灰蓝色或银白色的金属。熔点很低，沸点很高。纯液态镓有显著的过冷的趋势，在空气中很稳定。常被用作制造半导体氮化镓、砷化镓、磷化镓、锗半导体掺杂元；纯镓及低熔合金可作核反应的热交换介质；高温温度计的填充料；有机反应中作二酯化的催化剂。
磷钨酸为无色、灰白色粉状固体或淡黄色的细小晶体。具有酸性，而且具有氧化还原性，是一种多功能的新型催化剂，具有很高的催化活性，稳定性好，可作均相及非均相反应，甚至可作相转移催化剂，对环境无污染，是绿色催化剂。略有风化性。能溶于醇、醚和水，溶于约0.5份水。
氮化钽，化工材料，用来制造精确片状电阻的材料,氮化钽电阻则可抵抗水汽的侵蚀。用作超硬质材料添加剂，可制备纯的五氯化钽：用于喷涂，增加变压器、集成线路、二极管的电稳定性。
基于目前常规键合铜丝存在容易被氧化(腐蚀)的缺陷，开发出一种新型铜丝以提高其耐腐蚀性能，从而促进复合铜丝在对材料要求较高的集成电路中的应用就显得尤为重要。
发明内容
为解决上述技术问题，本发明提供一种适用于铜丝的耐腐蚀改性方法，该改性方法先从原料铜中提取高纯铜，清洗、烘干后与镍、镓、磷钨酸钾、纳米氮化钽共同置于熔炼装置中熔化，经在线除气、脱氧、搅拌，用牵引机组离合式真空上引无氧合金铜杆，随后采用连续挤压机组生产合金铜带坯料，随后经粗拔、镀钯、精拔得到镀钯合金铜丝。利用该方法制备而成的镀钯合金铜丝具有良好的耐腐蚀性能，并且成本较低，能够满足行业的要求，具有良好的应用前景。
本发明的目的可以通过以下技术方案实现：
一种适用于铜丝的耐腐蚀改性方法，包括以下步骤：
(1)从原料铜中提取纯度大于99.999％的高纯铜，清洗、烘干后备用；
(2)将高纯铜以及占高纯铜质量5.5wt％的镍、3.8wt％的镓、1.2wt％的磷钨酸钾、0.5wt％的纳米氮化钽置于熔炼装置中熔化，采用木炭及石墨鳞片覆盖铜液表面保证熔化时的真空状态，并经在线除气、脱氧、搅拌，用牵引机组离合式真空上引无氧合金铜杆，随后采用连续挤压机组生产合金铜带坯料；
(3)将合金铜带坯料进行粗拔以制得直径为2mm的合金铜丝并退火；
(4)将退火后的按重量百分比计97.5wt％的合金铜丝作为铜芯，在所述铜芯的表面上电镀2.5wt％的纯钯；
(5)将完成步骤(4)的电镀有纯钯保护层的合金铜丝，精拔成直径为0.25mm的镀钯合金铜丝。
优选地，所述步骤(2)中，引杆速度550～650mm/min，引杆直径为25mm。
优选地，所述步骤(3)中，退火温度为350℃，退火时间为50min。
所述步骤(4)中，电镀用钯的纯度要求大于99.999％。
本发明的另一个目的是提供该改性方法所制得的镀钯合金铜丝在集成电路中的应用。
本发明与现有技术相比，其有益效果为：
(1)本发明将高纯铜与镍、镓、磷钨酸钾、纳米氮化钽共同熔炼，通过镍、镓、磷钨酸钾、纳米氮化钽与铜之间所产生的协同作用，可以大大提高铜丝自身的耐腐蚀性能，同时也提高了铜丝的机械强度。
(2)本发明的改性方法工艺简单，适于大规模工业化运用，实用性强。
具体实施方式
下面结合具体实施例对发明的技术方案进行详细说明。
实施例1
(1)从原料铜中提取纯度大于99.999％的高纯铜，清洗、烘干后备用；
(2)将高纯铜以及占高纯铜质量5.5wt％的镍、3.8wt％的镓、1.2wt％的磷钨酸钾、0.5wt％的纳米氮化钽置于熔炼装置中熔化，采用木炭及石墨鳞片覆盖铜液表面保证熔化时的真空状态，并经在线除气、脱氧、搅拌，用牵引机组离合式真空上引无氧合金铜杆，引杆速度600mm/min，引杆直径为25mm，随后采用连续挤压机组生产合金铜带坯料；
(3)将合金铜带坯料进行粗拔以制得直径为2mm的合金铜丝并退火，退火温度为350℃，退火时间为50min；
(4)将退火后的按重量百分比计97.5wt％的合金铜丝作为铜芯，在所述铜芯的表面上电镀2.5wt％的纯钯，其中钯的纯度要求大于99.999％；
(5)将完成步骤(4)的电镀有纯钯保护层的合金铜丝，精拔成直径为0.25mm的镀钯合金铜丝。
对比例1
(1)从原料铜中提取纯度大于99.999％的高纯铜，清洗、烘干后备用；
(2)将高纯铜以及占高纯铜质量3.8wt％的镓、1.2wt％的磷钨酸钾、0.5wt％的纳米氮化钽置于熔炼装置中熔化，采用木炭及石墨鳞片覆盖铜液表面保证熔化时的真空状态，并经在线除气、脱氧、搅拌，用牵引机组离合式真空上引无氧合金铜杆，引杆速度600mm/min，引杆直径为25mm，随后采用连续挤压机组生产合金铜带坯料；
(3)将合金铜带坯料进行粗拔以制得直径为2mm的合金铜丝并退火，退火温度为350℃，退火时间为50min；
(4)将退火后的按重量百分比计97.5wt％的合金铜丝作为铜芯，在所述铜芯的表面上电镀2.5wt％的纯钯，其中钯的纯度要求大于99.999％；
(5)将完成步骤(4)的电镀有纯钯保护层的合金铜丝，精拔成直径为0.25mm的镀钯合金铜丝。
对比例2
(1)从原料铜中提取纯度大于99.999％的高纯铜，清洗、烘干后备用；
(2)将高纯铜以及占高纯铜质量5.5wt％的镍、1.2wt％的磷钨酸钾、0.5wt％的纳米氮化钽置于熔炼装置中熔化，采用木炭及石墨鳞片覆盖铜液表面保证熔化时的真空状态，并经在线除气、脱氧、搅拌，用牵引机组离合式真空上引无氧合金铜杆，引杆速度600mm/min，引杆直径为25mm，随后采用连续挤压机组生产合金铜带坯料；
(3)将合金铜带坯料进行粗拔以制得直径为2mm的合金铜丝并退火，退火温度为350℃，退火时间为50min；
(4)将退火后的按重量百分比计97.5wt％的合金铜丝作为铜芯，在所述铜芯的表面上电镀2.5wt％的纯钯，其中钯的纯度要求大于99.999％；
(5)将完成步骤(4)的电镀有纯钯保护层的合金铜丝，精拔成直径为0.25mm的镀钯合金铜丝。
对比例3
(1)从原料铜中提取纯度大于99.999％的高纯铜，清洗、烘干后备用；
(2)将高纯铜以及占高纯铜质量5.5wt％的镍、3.8wt％的镓、0.5wt％的纳米氮化钽置于熔炼装置中熔化，采用木炭及石墨鳞片覆盖铜液表面保证熔化时的真空状态，并经在线除气、脱氧、搅拌，用牵引机组离合式真空上引无氧合金铜杆，引杆速度600mm/min，引杆直径为25mm，随后采用连续挤压机组生产合金铜带坯料；
(3)将合金铜带坯料进行粗拔以制得直径为2mm的合金铜丝并退火，退火温度为350℃，退火时间为50min；
(4)将退火后的按重量百分比计97.5wt％的合金铜丝作为铜芯，在所述铜芯的表面上电镀2.5wt％的纯钯，其中钯的纯度要求大于99.999％；
(5)将完成步骤(4)的电镀有纯钯保护层的合金铜丝，精拔成直径为0.25mm的镀钯合金铜丝。
对比例4
(1)从原料铜中提取纯度大于99.999％的高纯铜，清洗、烘干后备用；
(2)将高纯铜以及占高纯铜质量5.5wt％的镍、3.8wt％的镓、1.2wt％的磷钨酸钾置于熔炼装置中熔化，采用木炭及石墨鳞片覆盖铜液表面保证熔化时的真空状态，并经在线除气、脱氧、搅拌，用牵引机组离合式真空上引无氧合金铜杆，引杆速度600mm/min，引杆直径为25mm，随后采用连续挤压机组生产合金铜带坯料；
(3)将合金铜带坯料进行粗拔以制得直径为2mm的合金铜丝并退火，退火温度为350℃，退火时间为50min；
(4)将退火后的按重量百分比计97.5wt％的合金铜丝作为铜芯，在所述铜芯的表面上电镀2.5wt％的纯钯，其中钯的纯度要求大于99.999％；
(5)将完成步骤(4)的电镀有纯钯保护层的合金铜丝，精拔成直径为0.25mm的镀钯合金铜丝。
将通过实施例1和对比例1-4的改性方法制得的镀钯合金铜丝依据国家标准或行业标准的方法分别进行耐腐蚀性能(于温度25℃、湿度70％的环境下放置120h后测试)以及盐酸、多硫化物测试这两项性能测试，所得的测试结果见表1。
表1
氧化层厚度(nm) 盐酸、多硫化物测试
实施例1 6.3 无漏铜、无黑斑
对比例1 11.5 漏铜、黑斑
对比例2 10.9 漏铜、黑斑
对比例3 12.8 漏铜、黑斑
对比例4 10.6 漏铜、黑斑
本发明所涉及的适用于铜丝的耐腐蚀改性方法，先从原料铜中提取高纯铜，清洗、烘干后与镍、镓、磷钨酸钾、纳米氮化钽共同置于熔炼装置中熔化，经在线除气、脱氧、搅拌，用牵引机组离合式真空上引无氧合金铜杆，随后采用连续挤压机组生产合金铜带坯料，随后经粗拔、镀钯、精拔得到镀钯合金铜丝。利用该方法制备而成的镀钯合金铜丝具有良好的耐腐蚀性能，并且成本较低，能够满足行业的要求，具有良好的应用前景。
以上所述仅为本发明的实施例，并非因此限制本发明的专利范围，凡是利用本发明说明书内容所作的等效结构或等效流程变换，或直接或间接运用在其他相关的技术领域，均同理包括在本发明的专利保护范围内。

Claims (5)

1.一种适用于铜丝的耐腐蚀改性方法，其特征在于，包括以下步骤：
(1)从原料铜中提取纯度大于99.999％的高纯铜，清洗、烘干后备用；
(2)将高纯铜以及占高纯铜质量5.5wt％的镍、3.8wt％的镓、1.2wt％的磷钨酸钾、0.5wt％的纳米氮化钽置于熔炼装置中熔化，采用木炭及石墨鳞片覆盖铜液表面保证熔化时的真空状态，并经在线除气、脱氧、搅拌，用牵引机组离合式真空上引无氧合金铜杆，随后采用连续挤压机组生产合金铜带坯料；
(3)将合金铜带坯料进行粗拔以制得直径为2mm的合金铜丝并退火；
(4)将退火后的按重量百分比计97.5wt％的合金铜丝作为铜芯，在所述铜芯的表面上电镀2.5wt％的纯钯；
(5)将完成步骤(4)的电镀有纯钯保护层的合金铜丝，精拔成直径为0.25mm的镀钯合金铜丝。
2.根据权利要求1所述的适用于铜丝的耐腐蚀改性方法，其特征在于：所述步骤(2)中，引杆速度550～650mm/min，引杆直径为25mm。
3.根据权利要求1所述的适用于铜丝的耐腐蚀改性方法，其特征在于：所述步骤(3)中，退火温度为350℃，退火时间为50min。
4.根据权利要求1所述的适用于铜丝的耐腐蚀改性方法，其特征在于：所述步骤(4)中，电镀用钯的纯度要求大于99.999％。
5.权利要求1～4任一项所述的改性方法所制得的镀钯合金铜丝在集成电路中的应用。
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004193552A (ja) * 2002-10-17 2004-07-08 Mitsubishi Materials Corp 半導体装置配線シード層形成用銅合金スパッタリングターゲット
CN1856588A (zh) * 2003-09-19 2006-11-01 住友金属工业株式会社 铜合金及其制造方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004193552A (ja) * 2002-10-17 2004-07-08 Mitsubishi Materials Corp 半導体装置配線シード層形成用銅合金スパッタリングターゲット
CN1856588A (zh) * 2003-09-19 2006-11-01 住友金属工业株式会社 铜合金及其制造方法

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