锡银铜合金的电沉积工艺与沉积机制及其焊接性能的研究
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摘要
传统电子封装工艺广泛使用Sn-Pb合金镀层作为可焊性镀层,但是Pb有毒性,已被禁止在电子产品中使用。因此,电沉积无铅可焊性镀层是电子电镀领域的研究热点之一。目前,纯锡镀层的焊接可靠性差,锡基二元合金镀层有脆性大、润湿性差等方面的问题,贵金属镀层成本高。综合分析表明,Sn-Ag-Cu三元合金作为无铅可焊性镀层具有良好的应用前景。因此,开展电沉积Sn-Ag-Cu三元合金的研究具有重要的理论与实际意义。
基于强酸性镀液和碱性镀液存在的诸多问题,开发了弱酸性甲磺酸盐–碘化物镀液电沉积Sn-Ag-Cu合金工艺。采用直流电沉积方法在铁、铜基体上电镀Sn-Ag-Cu合金,采用扫描电子显微镜观察镀层微观形貌,采用X-射线荧光光谱仪分析镀层组成。通过系统的工艺研究,明确了镀液组成及工艺条件的影响规律,从而优化出了获得光亮平整、结晶致密,Sn、Ag和Cu的质量分数分别为92%~97%、2%~6%和0.5%~2%的Sn-Ag-Cu合金镀层的镀液组成和工艺条件。
镀液中同时使用自制的HT添加剂和三乙醇胺(TEA)时能够得到光亮的Sn-Ag-Cu合金镀层。通过研究二者对阴极极化、镀层形貌和镀层组成等的影响发现,HT能显著增大阴极极化,使镀层结晶细小;TEA虽然使阴极极化减小,但能使镀层结晶致密。据此可认为HT是电镀Sn-Ag-Cu合金的主光亮剂,TEA是光亮促进剂。动力学模拟计算发现,HT中的芳香醛分子在镀层表面的吸附能力较强,而TEA的吸附能力较弱。根据上述分析,建立了HT和TEA在阴极表面的协同作用模型,合理地阐述了光亮镀层形成的原因。
通过对电镀液进行循环伏安曲线、极化曲线、计时电流曲线和阻抗谱等的测试,研究了Sn-Ag-Cu合金的电沉积行为。确定Sn-Ag-Cu合金的沉积类型为正则共沉积。随着电极电势的负移,电沉积过程可分为三个阶段:从扩散步骤控制发展到扩散步骤与电化学步骤混合控制,最后是电化学步骤控制。提出了金属配合离子的竞争放电机制,认为在一定的阴极电势下,镀液中的多种配合离子都具有相近的析出电势,它们在阴极表面竞争放电还原,形成Sn-Ag-Cu合金镀层。
采用差示扫描量热法、Tafel曲线测试、拉伸实验、焊料铺展实验和高温高湿实验等方法评价了Sn-Ag-Cu合金镀层的焊接性能。实验结果表明,Sn-Ag-Cu合金镀层熔点在221~223℃之间,与Sn-3.0Ag-0.5Cu焊料兼容性良好,耐蚀性能与Sn-Pb合金镀层相当。当Sn-Ag-Cu合金镀层的微观形貌较好时,其润湿性也较好。在Cu基体上电镀的Sn-Ag-Cu合金镀层容易生长锡须,当使用氨基磺酸盐镀Ni层作为中间层时可有效地抑制Sn-Ag-Cu合金镀层表面锡须的生长。
本文研究表明,从弱酸性镀液中可电沉积得到新型无铅可焊性镀层——Sn-Ag-Cu三元合金镀层。该镀层的可焊性优良,可作为印刷电路板和元器件的表面镀层,从而实现电子封装的无铅化。建立的光亮剂协同作用模型可为锡基合金镀液中光亮剂的选择提供理论指导,提出的配合离子竞争放电机制,丰富了合金共沉积理论。
Sn-Pb alloy deposit was widely used as a solder coating in traditional electronic packaging technology. However, Pb has been banned to use in electronic products due to its toxicity. Therefore, electroplating of lead-free solder coating is one of investigation hotspots in electronic electroplating field. At present, pure tin deposit has a bad solder reliability, tin-based binary alloy deposits have big brittleness or bad wettability, and noble metal deposits have high price. A general analysis shows that, Sn-Ag-Cu ternary alloy that used as a lead-free solder coating has a nice application foreground. So, it has an important theoretic and practical meaning to study on electrodeposition of Sn-Ag-Cu ternary alloy.
Since acidic baths and alkaline baths have a lot of shortcomings, a weakly acidic bath containing methylsulfonic acid salts and iodide was developed to electrodeposit Sn-Ag-Cu alloy coating. Electrodeposition of Sn-Ag-Cu alloy on Fe or Cu substrate is employed on a direct current power supply. Scanning electron microscopy was used to observe morphologies of coatings and X-ray fluorescence was used to analyze compositions of coatings. On base of systemic studies, influencing rules of compositions of electrolyte and process conditions were determined, and optimized compositions of electrolyte and process conditions are determined for electrodeposit bright, smooth and compact Sn-Ag-Cu alloy with mass contents of Sn, Ag and Cu are 92%~97%, 2%~6% and 0.5%~2%, respectively.
A bright Sn-Ag-Cu alloy coating can be electrodeposited from the electrolyte modified by adding both HT additive that was self-made and triethanolamine (TEA). Effect of HT and TEA on cathodic polarization of baths and morphologies and compositions of Sn-Ag-Cu coatings was studied. The results show that, HT increases cathodic polarization and makes crystal of the coating finer, and TEA decreases cathodic polarization and makes crystal of the coating denser. So, HT is considered as main brightener and TEA is considered as brightening promoter for electrodeposition of Sn-Ag-Cu alloy coating. The compute results of molecular kinetics show that, aromatic aldehyde molecules in HT are strongly adsorbed on surface of cathodic electrode, however TEA molecules have weak adsorption. Based on above analysis, a brightener corporate action model is put forward, which explains the form reason of bright deposits well.
Electrodeposition behaviors of Sn-Ag-Cu alloy in electrolyte were studied by testing of cyclic voltammetry, linear sweet voltammetry, chronoamperometry, and electrochemical impedance spectrum. Co-deposition type of Sn-Ag-Cu alloy is determined as canonical. With cathodic potential towards to negative direction, electrodeposition process is parted to three periods, which were controlled by diffusion, both diffusion and electrochemical step, and electrochemical step, respectively. Competed discharge mechanism of metal complexing ions is put forward. Multiform metal complexing ions have nearly equal graining potential under a certain cathodic potential, and discharge on cathodic surface vies with each other and forms Sn-Ag-Cu alloy coating.
Solder properties of Sn-Ag-Cu alloy coating were evaluated by differential scanning calorimetry, Tafel plots, extending, spreading, and high temperature and humidity tests. The results show that, melt points of Sn-Ag-Cu alloy coatings are 221~223℃, Sn-Ag-Cu alloy coatings have good compatibility with Sn-3.0Ag-0.5Cu solder and its corrosion resistance is as good as Sn-Pb alloy. Sn-Ag-Cu alloy coating has good wettability while its morphology is smooth and fine. Tin whiskers easily grow on surface of Sn-Ag-Cu coating when Cu is used as substrate, while growth of tin whisker is inhibited effectively when Ni electrodeposited from sulfamate electrolyte is used as preplating.
Investigations in this paper show that, eutectic Sn-Ag-Cu ternary alloy deposit electrodeposited from weakly acidic bath is a new lead-free solder coating. The coating has excellent solder properties and can be used on the surfaces of printed circuit board and patch-like electronic apparatus in order to carry out lead-free electronic packing. The brightener corporate action model affords theory guidance on choosing brighteners used in bath for tin-based deposits, and the mechanism of competed discharge of complexing ions enriches theory of co-deposition of alloys.
基于强酸性镀液和碱性镀液存在的诸多问题,开发了弱酸性甲磺酸盐–碘化物镀液电沉积Sn-Ag-Cu合金工艺。采用直流电沉积方法在铁、铜基体上电镀Sn-Ag-Cu合金,采用扫描电子显微镜观察镀层微观形貌,采用X-射线荧光光谱仪分析镀层组成。通过系统的工艺研究,明确了镀液组成及工艺条件的影响规律,从而优化出了获得光亮平整、结晶致密,Sn、Ag和Cu的质量分数分别为92%~97%、2%~6%和0.5%~2%的Sn-Ag-Cu合金镀层的镀液组成和工艺条件。
镀液中同时使用自制的HT添加剂和三乙醇胺(TEA)时能够得到光亮的Sn-Ag-Cu合金镀层。通过研究二者对阴极极化、镀层形貌和镀层组成等的影响发现,HT能显著增大阴极极化,使镀层结晶细小;TEA虽然使阴极极化减小,但能使镀层结晶致密。据此可认为HT是电镀Sn-Ag-Cu合金的主光亮剂,TEA是光亮促进剂。动力学模拟计算发现,HT中的芳香醛分子在镀层表面的吸附能力较强,而TEA的吸附能力较弱。根据上述分析,建立了HT和TEA在阴极表面的协同作用模型,合理地阐述了光亮镀层形成的原因。
通过对电镀液进行循环伏安曲线、极化曲线、计时电流曲线和阻抗谱等的测试,研究了Sn-Ag-Cu合金的电沉积行为。确定Sn-Ag-Cu合金的沉积类型为正则共沉积。随着电极电势的负移,电沉积过程可分为三个阶段:从扩散步骤控制发展到扩散步骤与电化学步骤混合控制,最后是电化学步骤控制。提出了金属配合离子的竞争放电机制,认为在一定的阴极电势下,镀液中的多种配合离子都具有相近的析出电势,它们在阴极表面竞争放电还原,形成Sn-Ag-Cu合金镀层。
采用差示扫描量热法、Tafel曲线测试、拉伸实验、焊料铺展实验和高温高湿实验等方法评价了Sn-Ag-Cu合金镀层的焊接性能。实验结果表明,Sn-Ag-Cu合金镀层熔点在221~223℃之间,与Sn-3.0Ag-0.5Cu焊料兼容性良好,耐蚀性能与Sn-Pb合金镀层相当。当Sn-Ag-Cu合金镀层的微观形貌较好时,其润湿性也较好。在Cu基体上电镀的Sn-Ag-Cu合金镀层容易生长锡须,当使用氨基磺酸盐镀Ni层作为中间层时可有效地抑制Sn-Ag-Cu合金镀层表面锡须的生长。
本文研究表明,从弱酸性镀液中可电沉积得到新型无铅可焊性镀层——Sn-Ag-Cu三元合金镀层。该镀层的可焊性优良,可作为印刷电路板和元器件的表面镀层,从而实现电子封装的无铅化。建立的光亮剂协同作用模型可为锡基合金镀液中光亮剂的选择提供理论指导,提出的配合离子竞争放电机制,丰富了合金共沉积理论。
Sn-Pb alloy deposit was widely used as a solder coating in traditional electronic packaging technology. However, Pb has been banned to use in electronic products due to its toxicity. Therefore, electroplating of lead-free solder coating is one of investigation hotspots in electronic electroplating field. At present, pure tin deposit has a bad solder reliability, tin-based binary alloy deposits have big brittleness or bad wettability, and noble metal deposits have high price. A general analysis shows that, Sn-Ag-Cu ternary alloy that used as a lead-free solder coating has a nice application foreground. So, it has an important theoretic and practical meaning to study on electrodeposition of Sn-Ag-Cu ternary alloy.
Since acidic baths and alkaline baths have a lot of shortcomings, a weakly acidic bath containing methylsulfonic acid salts and iodide was developed to electrodeposit Sn-Ag-Cu alloy coating. Electrodeposition of Sn-Ag-Cu alloy on Fe or Cu substrate is employed on a direct current power supply. Scanning electron microscopy was used to observe morphologies of coatings and X-ray fluorescence was used to analyze compositions of coatings. On base of systemic studies, influencing rules of compositions of electrolyte and process conditions were determined, and optimized compositions of electrolyte and process conditions are determined for electrodeposit bright, smooth and compact Sn-Ag-Cu alloy with mass contents of Sn, Ag and Cu are 92%~97%, 2%~6% and 0.5%~2%, respectively.
A bright Sn-Ag-Cu alloy coating can be electrodeposited from the electrolyte modified by adding both HT additive that was self-made and triethanolamine (TEA). Effect of HT and TEA on cathodic polarization of baths and morphologies and compositions of Sn-Ag-Cu coatings was studied. The results show that, HT increases cathodic polarization and makes crystal of the coating finer, and TEA decreases cathodic polarization and makes crystal of the coating denser. So, HT is considered as main brightener and TEA is considered as brightening promoter for electrodeposition of Sn-Ag-Cu alloy coating. The compute results of molecular kinetics show that, aromatic aldehyde molecules in HT are strongly adsorbed on surface of cathodic electrode, however TEA molecules have weak adsorption. Based on above analysis, a brightener corporate action model is put forward, which explains the form reason of bright deposits well.
Electrodeposition behaviors of Sn-Ag-Cu alloy in electrolyte were studied by testing of cyclic voltammetry, linear sweet voltammetry, chronoamperometry, and electrochemical impedance spectrum. Co-deposition type of Sn-Ag-Cu alloy is determined as canonical. With cathodic potential towards to negative direction, electrodeposition process is parted to three periods, which were controlled by diffusion, both diffusion and electrochemical step, and electrochemical step, respectively. Competed discharge mechanism of metal complexing ions is put forward. Multiform metal complexing ions have nearly equal graining potential under a certain cathodic potential, and discharge on cathodic surface vies with each other and forms Sn-Ag-Cu alloy coating.
Solder properties of Sn-Ag-Cu alloy coating were evaluated by differential scanning calorimetry, Tafel plots, extending, spreading, and high temperature and humidity tests. The results show that, melt points of Sn-Ag-Cu alloy coatings are 221~223℃, Sn-Ag-Cu alloy coatings have good compatibility with Sn-3.0Ag-0.5Cu solder and its corrosion resistance is as good as Sn-Pb alloy. Sn-Ag-Cu alloy coating has good wettability while its morphology is smooth and fine. Tin whiskers easily grow on surface of Sn-Ag-Cu coating when Cu is used as substrate, while growth of tin whisker is inhibited effectively when Ni electrodeposited from sulfamate electrolyte is used as preplating.
Investigations in this paper show that, eutectic Sn-Ag-Cu ternary alloy deposit electrodeposited from weakly acidic bath is a new lead-free solder coating. The coating has excellent solder properties and can be used on the surfaces of printed circuit board and patch-like electronic apparatus in order to carry out lead-free electronic packing. The brightener corporate action model affords theory guidance on choosing brighteners used in bath for tin-based deposits, and the mechanism of competed discharge of complexing ions enriches theory of co-deposition of alloys.
引文
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