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Master's Dissertation
DOI
10.11606/D.75.2010.tde-28042010-144335
Document
Author
Full name
Mariana Beatriz dos Reis Silva
Institute/School/College
Knowledge Area
Date of Defense
Published
São Carlos, 2010
Supervisor
Committee
Lima Neto, Benedito dos Santos (President)
Picon, Carlos Alberto
Polito, Wagner Luiz
Title in Portuguese
Aplicação de complexos de CuII, NiII, ZnII e NbV com ligantes carboxilatos em banhos de eletrodeposição
Keywords in Portuguese
Eletrodeposição
Ligantes carboxilatos
Nióbio
Abstract in Portuguese
Complexos de coordenação de Cu(II), Ni(II), Zn(II) e Nb(V) foram obtidos com os íons acetato, citrato e oxalato como ligantes (complexos ex-situ) para serem aplicados em banhos de eletrodeposição. O objetivo é usar estes complexos como fontes de metais sem adição de aditivos os quais são os ligantes que estão coordenados. Como estudos de referência, foram investigados banhos de eletrodeposição contendo sais de sulfatos dos íons metálicos na presença de ligantes nas razões metal:ligante de 10:1 e 1:5; assim, complexos de coordenações similares podem ser gerados em solução (complexos in-situ).
Os complexos ex-situ foram analisados por análise elementar, espectroscopias nas regiões do infravermelho e ultravioleta-visível e voltametria cíclica (em Pt). As eletrólises foram realizadas em substrato de aço 1020 com um ou dois complexos metálicos presentes no banho. Banhos de eletrodeposição de nióbio usando como substrato aço 1020 coberto com Cu e/ou Zn foram bem sucedidos. Os depósitos foram analisados por microscopia eletrônica de varredura (MEV), espectroscopia de dispersão de raios X (EDX), reflectância difusa, espectroscopia de difração de raios X (DRX) e por curvas de polarização anódica (estudos de corrosão).
Os banhos com complexos in-situ 10:1 fomeceram depósitos com aspectos morfológicos ruins em relação aos depósitos obtidos de banhos com complexos in-situ 1:5 e ex-situ. As morfologias dos depósitos obtidos dos banhos com acetato foram dendríticos e com baixa aderência. Os depósitos dos banhos com complexos citrato e oxalato foram lisos, compactos, com boa aderência e brilhantes.
Diferentes fases estruturais foram observadas nos depósitos e a maioria deles protege contra a corrosão.
Os estudos concluíram que os ligantes analisados influenciam diferentemente nos processos de eletrodeposição.
Title in English
Application of CuII, NiII, ZnII and NbV complexes with carboxilates ligands for electroplating baths
Keywords in English
Carboxilates ligands
Electrodeposition
Niobium
Abstract in English
Cu(II), Ni(II), Zn(II) and Nb(V) coordination complexes were obtained with acetate, citrate and oxalate ions as ligands (ex-situ complexes) to be applied in electrodeposition baths. The aim is to use these complexes as metal sources without further addition of additives which are the coordinated ligands. As reference study, electroplating baths with sulfate salts of the metal ions in presence of the ligands were investigated in the metal:ligand ratio of 1:5 and 10:1; then, similar coordination complexes can be generate in solution (in-situ complexes).
The ex-situ complexes were characterized by elemental analysis, infrared and UV-vis spectroscopies and cyclic voltammetry (in Pt). The electrolyses were performed in 1020 steel as substrate with one or two metal complexes present in the bath. Niobium electroplating baths with 1020 steel previously covered with Cu and/or Zn as substrates were also successfully performed. The deposits were analyzed by scanning electron microscopy (SEM), energy dispersive spectroscopy X-ray (EDS), diffuse reflectance, X-ray diffraction (XRD) and polarization curves (corrosion studies).
The bath with 10:1 in-situ complexes provided deposits with poor morphologic aspects in relation to the deposits obtained from bath with 1:5 in-situ and ex-situ complexes. The morphologies of the deposits obtained from bath with the acetate complexes were dendritics and with low adherence. The bath with both citrate- and oxalate-complexes were smoothes, compacts, with good adherence and brightness.
Different structural phases were observed in the deposits and the most of them provided protection against corrosion.
It was concluded that coordinated ligands influence differently in the electrodeposition processes.
 
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Publishing Date
2010-08-17
 
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