伏安法在镀液分析中的应用

根据镀液中待测组份或杂质的电化学特性和添加剂对金属电沉积过程的阻化或活化效应,建立了测定某些镀液组份、一些杂质和常用添加剂的浓度的直接伏安法、间接伏安法和金属沉积层阳极溶出伏安法。这些方法测定步骤简单、快速,适合于电镀生产监控和电镀工艺研究。     

稀土对电沉积Ni-P合金镀液性能的影响

通过在电镀Ni P合金的镀液中加入一定量的镧和铈的氯化物 ,用赫尔槽实验、远近阴极实验等方法探讨了稀土元素对Ni P合金镀液性能的影响规律。结果表明 :CeCl3 ,LaCl3 以及它们的混合物的最佳添加量均为 2g·L- 1 。稀土元素的加入 ,能够显著增加Ni P合金镀液的光亮区范围 ,而且 ,这种作用在低电流密度范围内更显著。稀土元素加入到镀液中能够显著增大Ni P合金镀液的电流效率 ,并且导致电流效率随电流密度的变化趋势发生变化。实验结果还表明 ,稀土元素能够使镀液的分散能力有所提高。根据这一结果 ,从理论上推断稀土元素能够促进电沉积Ni P合金阴极过程的极化度。这一推断与阴极极化曲线的测量结果是一致的     

火焰原子吸收法测定造币镀液中微量铜

原子吸收光谱法测定铜的报道较多.但未见有关造币镀液中微量铜测定的报道.造币镀液样品中Ni~(2+)、SO_4~(2-)、Cl~-的含量均为50g·L~(-1)左右NH_4~+含量为1～10g·L~(-1)之间.极高量的Ni~(2+)、SO_4~(2-)、Cl~-等对铜的火焰原子吸收测定有一定的抑制作用.将作品适当稀释.控制Ni~(2+)、SO_4~(2-)、Cl~-等离子的含量在不影响测定的范围内,用塞曼效应扣背景-火焰原子吸收法测定造币镀液中的铜.结果满意.     

脉冲化学镀Ni—P合金镀液中磷酸盐含量分析

脉冲化学镀Ni-P合金是化学镀领域中的一种新兴技术.研究表明:脉冲化学镀的沉积速度远大于电沉积和化学沉积速度之和.本人通过对镀液成分的长期监控发现: 脉冲电流通过改变镀液组分(即改变镀液中亚磷酸和次磷酸的含量),进而影响化学镀的自催化过程.本文运用碘量法进行脉冲化学镀镀液中的磷酸盐含量分析.     

锌镀液中微量稀土元素的测定

新显色剂均三溴偶氮胂已被广泛应用于多种物料中稀土的测定.洛阳工学院有色研究室改进热镀锌的工艺,在原锌镀液中加入微量稀土元素,可使锌镀液的粘度降低,并使镀层减薄,在同等条件下,比原镀液镀出的镀件耐蚀性提高1.5倍,且粗糙度也得到改善。为研究稀土的适宜加入量及有关工艺条件,需对其稀土元素的含量作快速而准确的分析。本文对此进行了试验、探讨并确定了分析方法。     

火焰原子吸收光谱法连续测定陶瓷绝缘子镀液中的锌、铜、铁

采用火焰原子吸收光谱法进行镉镍电池陶瓷绝缘子镀液中锌、铜、铁含量的连续测定。在优化条件下．该方法灵敏度高，干扰小，选择性和重现性好，步骤简单，操作容易，分析周期短。测定结果的相对标准偏差均小于1．0％，加标回收率为97．0％～99．0％。该法适用于镉镍电池陶瓷绝缘子镀液中锌、铜、铁含量的现场控制分析和样品系统分析。     

离子色谱法检测酸性镀铜液中的微量氯离子

采用Na2CO3-NaHCO3为淋洗液和抑制电导检测,对酸性镀铜液中的微量氯离子进行检测。采用AgNO3作为沉淀剂使Cl-分离富集,再用Na2S2O3溶液溶解沉淀后进行检测,可以很好地消除酸性电镀液中高浓度SO4^2-的干扰。该方法线性良好,Cl^-的检出限为0.01μg/mL,回收率在98.6%-101.7%之间,由于该方法能够很好地消除大量SO4^2-的干扰,在电镀铜工业中对酸性镀铜液中氯离子的监控可发挥作用。     

钯银膜无电解镀共沉积的探讨

无电解镀共沉积钯银合金膜是纯化氢同位素最有发展前途的方法之一 .膜的制备技术有物理气相沉积法 [1 ]、化学气相沉积法 [2 ]、电镀 [3]和无电解镀法 [4]等 .无电解镀法使用设备简单、易于操作 ,而且可以均匀地沉积在形状复杂、硬度不同的基体上 .国内对电镀钯及有关钯银合金膜的研究 [5]较多 ,但无电解镀的研究甚少 .本文用无电解镀法制备含银量在摩尔分数2 3%～ 2 5 %的有支撑钯银膜 (膜厚为 3～ 5μm) .采用含有钯银两种离子的镀液制得的膜层 ,优于机械混合的均匀程度 .结果表明膜层没有合金化 .无电解镀条件为 :镀温 (5 0± 1 )℃ ,镀…     

电镀液中铜、铁、铅和锌等杂质元素的原子吸收光谱测定

电镀液中常见的有害杂质:铜、铁、铅和锌等的允许含量随镀液种类和杂质元素不同而异。例如,镀镍液中的铜、铁、铅和锌的允许范围在几个至几十个毫克/升内,而镀铬液中的铁的允许范围却在1—几克/升内。1964年Whittington报告用原子吸收加入法测镀镍液中的铜、铁、铅和锌。我们也用过此法。此法比较麻烦。虽然Parker报告把电镀液稀释后直接用原子吸收法测锌、铜、铬,但未报导具体条件。本文除测定镀镍液和镀钻液中低含量铁仍用加入法外,铜、铅、锌及镍、钴镀液中高于50毫克/升铁都用稀释法。实验表明:     

离子色谱法电导检测电镀液中的有机酸、S_2O_3~(2-)和SCN~-

电镀工业中,为了改善镀层性能,通常需要在电镀液中加入适量电镀添加剂,起到稳定镀液、细化结晶、提高分散能力与深镀能力、增加镀层光亮性等作用~([1]).添加剂的含量直接影响着电镀产品的质量,因而能否在生产过程中及时准确地监测其浓度变化是控制电镀过程的至关晕要的环节.常见组分采用化学滴定、高效液相~([2,3])等方法分类测定,相比而言,离子色谱法能同时完成的分析,优势更为明显~([4,5]).本研究建立了一种简单易行的离子色谱方法,同时测定了电镀液中弱保留组分和易极化离子S_2O_3~(2-)和SCN~-,使得电镀槽液的组分变化的监测更为精确且更加实时化.     

Revisiting the Electroplating Process for Lithium-Metal Anodes for Lithium-Metal Batteries

Electroplating has been studied for centuries, not only in the laboratory but also in industry for machinery, electronics, automobile, aviation, and other fields. The lithium-metal anode is the Holy Grail electrode because of its high energy density. But the recyclability of lithium-metal batteries remains quite challenging. The essence of both conventional electroplating and lithium plating is the same, reduction of metal cations. Thus, industrial electroplating knowledge can be applied to revisit the electroplating process for lithium-metal anodes. In conventional electroplating, some strategies like using additives, modifying substrates, applying pulse current, and agitating electrolyte have been explored to suppress dendrite growth. These methods are also effective in lithium-metal anodes. Inspired by that, we revisit the fundamental electroplating theory for lithium-metal anodes in this Minireview, mainly drawing attention to the theory of electroplating thermodynamics and kinetics. Analysis of essential differences between traditional electroplating and plating/stripping of lithium-metal anodes is also presented. Thus, industrial electroplating knowledge can be applied to the electroplating process of lithium-metal anodes to improve commercial lithium-metal batteries and the study of lithium plating/stripping can further enrich the classical electroplating technique.     

Revisiting the Electroplating Process for Lithium‐Metal Anodes for Lithium‐Metal Batteries

Electroplating has been studied for centuries, not only in the laboratory but also in industry for machinery, electronics, automobile, aviation, and other fields. The lithium‐metal anode is the Holy Grail electrode because of its high energy density. But the recyclability of lithium‐metal batteries remains quite challenging. The essence of both conventional electroplating and lithium plating is the same, reduction of metal cations. Thus, industrial electroplating knowledge can be applied to revisit the electroplating process for lithium‐metal anodes. In conventional electroplating, some strategies like using additives, modifying substrates, applying pulse current, and agitating electrolyte have been explored to suppress dendrite growth. These methods are also effective in lithium‐metal anodes. Inspired by that, we revisit the fundamental electroplating theory for lithium‐metal anodes in this Minireview, mainly drawing attention to the theory of electroplating thermodynamics and kinetics. Analysis of essential differences between traditional electroplating and plating/stripping of lithium‐metal anodes is also presented. Thus, industrial electroplating knowledge can be applied to the electroplating process of lithium‐metal anodes to improve commercial lithium‐metal batteries and the study of lithium plating/stripping can further enrich the classical electroplating technique.     

Electroplating of metal nanotubes and nanowires in a high aspect-ratio nanotemplate

Ordered metal (Co, Pt, and CoPt alloy) nanotube and nanowire structures were fabricated by a simple electroplating method in high aspect-ratio anodic aluminum oxide (AAO) membrane. The growth rate in pulse mode is always larger than that in constant-current mode, which represents that diffusion limitation exists in this electroplating condition. It is also found that the sputtered Au layer structure could influence the electroplating. Traditional nanowires could be fabricated in the template with a uniform Au layer as conducting contact. In case of unblocked AAO membrane, metal electroplating begins from the Au particles which were attached inside the holes during the sputtering step and produces metal nanotubes. Pt and CoPt nanotubes could be easily prepared by this method and might be applied as catalyst and magnetic material.     

高均匀性的铜柱凸块电镀

随着电子产品的小型化、多功能化和高性能化的发展,促使着2D集成封装向2.5D或3D集成封装发展。铜柱凸块电镀是晶圆级三维封装的关键基础技术之一。本文研究了铜柱凸块的电镀均匀性与添加剂浓度、 镀液对流、 电流密度和电镀设备之间的影响规律。研究结果表明, 添加剂浓度、 镀液对流以及电流密度对单个铜柱凸块的平整度影响较大,而对铜柱凸块高度的均一性影响较小。相反,电镀设备对铜柱凸块的高度均一性的影响较大, 而对铜柱凸块的平整度影响较小。在三种有机添加剂中, 整平剂对铜柱凸块的平整度影响最大, 随着镀液中整平剂浓度的增加,铜柱凸块顶部形状由凸起、变为平整、 再转变为凹陷。电镀液的单向对流会导致所沉积铜柱凸块形貌发生倾斜。 高的电流密度会导致凸顶的铜柱凸块形貌。精密设计的电镀设备可以提高晶圆上电流密度分布的均匀性, 继而大幅提高电镀铜柱凸块的共面性。本文的研究结果可为铜柱凸块的电镀优化提供指导。     

芯片铜互连研究及进展

本文详细介绍芯片制造中铜互连技术,综述酸性硫酸铜电镀工艺要点及常用添加剂作用机理,并概述国内外新型添加剂研究进展. 在此基础上,展望新型铜互连工艺替代酸性硫酸电镀铜工艺的可能性.     

荧光分析法测定痕量铬(Ⅵ)

拟定了一个测定痕量铬（Ⅵ）的新的荧光分析法。在硫酸介质中,铬能氧化吡咯红Y。使其荧光猝灭,方法的检出限为2．2μg/L,线性范围为8．0－88μg/L。本法用于电镀废液、电镀液、合金钢中痕量Cr(Ⅵ）的测定,结果满意。     

特殊整平剂甲基橙在通孔电镀铜的应用

甲基橙具有两种基团,可以同时起到加速和抑制作用,可作为特殊的整平剂应用与通孔电镀铜实验中。通过分子动力学模拟和量子化学计算来表征甲基橙在通孔电镀铜中的作用,结果表明甲基橙可以很好地吸附在阴极表面并抑制铜的电沉积。 通过恒电流测试和循环伏安测试结果显示, 甲基橙由于同时具有磺酸基的去极化和其分子结构部分的极化作用, 形成协同分子内对铜加速还原和阻碍传质的竞争效应, 所以几乎不影响电位。在板厚孔径为10:1的通孔电镀铜实验中, 仅以甲基橙和环氧乙烷和环氧丙烷嵌段共聚物作为添加剂, TP值可达到92.34%。     

复合镀膜在陶瓷颗粒透射电镜分析中的应用

本文介绍了一种对陶瓷颗粒进行透射电镜分析的样品制备方法。采用复合电沉积方法,将陶瓷颗粒均匀分散包埋在金属铜镀层中,得到复合镀层薄膜,再通过电解双喷将薄膜减薄,获得透射电镜样品,从而可以对陶瓷颗粒进行透射电镜观察分析,讨论了获得此种复合镀层薄膜所需的电流密度、镀液pH值、搅拌措施和电镀时间。透射电镜观察分析的结果显示此方法效果良好。     

碱熔-ICP-AES测定电镀废弃物中的镍

采用过氧化钠分解试样,盐酸浸取,通过仪器参数的优化、共存元素干扰等实验,建立了电感耦合等离子体原子发射光谱法测定电镀废弃物中镍含量的方法。方法的测定范围ω(Ni)1.00%~10.00%。经加标回收实验,镍元素的加标回收率为99.0%~107%(n=3),方法准确可靠,完全能够满足此类物料中镍含量的检验工作。     

Carbon nanofiber–copper composite powder prepared by electrodeposition

Carbon nanofiber–copper composite powder is prepared by an electrodeposition process using a copper plating bath containing homogeneously dispersed carbon nanofibers. Particles of the composite with a spiky ball structure are accumulated on the plating electrode during the initial stage of electroplating, and can be separated easily to give a powder carbon nanofiber–copper composite. The particle size can be controlled by selecting appropriate electroplating conditions.