Determination of surface coverage of iron-phosphate coatings on steel using the voltammetric anodic dissolution technique

Abstract

In this study, the effect of deposition time and concentration of NaNO2 in the phosphate bath on the surface morphology of iron-phosphate coatings on low carbon steel was investigated using scanning electron microscopy (SEM) and atomic force microscopy (AFM). The composition of ironphosphate coatings was determined using energy dispersive X-ray spectroscopy (EDS) and X-ray diffraction (XRD), while surface coverage was evaluated by the voltammetric anodic dissolution (VAD) technique in the borate solution. The addition of NaNO2 to the phosphate bath significantly increased the surface coverage since better packed crystals of smaller size, which favour the phosphate nucleation, were obtained. It was also shown that prolonged deposition time increased the surface coverage, coating roughness and crystal size in the lateral direction, altering also the crystal shape from large platelets non-uniformly distributed on the steel surface during the initial time to better packed laminated and needle-like structures during prolonged exposure.

U ovom radu je, primenom skenirajuće elektronske mikroskopije (SEM) i mikro- skopije međuatomskih sila (AFM), ispitivan uticaj vremena taloženja i koncentracije NaNO2 u rastvoru za fosfatiranje na morfologiju gvožđe-fosfatnih prevlaka na nisko-ugljeničnom čeliku. Sastav gvožđe–fosfatnih prevlaka je određen primenom energetske disperzione atomske analize (EDS) i difrakcijom H-zraka (XRD), dok je pokrivenost površine određivana anodnim rastvaranjem u boratnom rastvoru primenom linearne voltametrije (VAD). Pokazano je da dodatak NaNO2 u rastvoru za fosfatiranje značajno povećava pokrivenost površine čelika, jer se formiraju bolje pakovani kristali, manje veličine. Duže vreme taloženja takođe povećava pokrivenost površine, kao i hrapavost prevlake i širinu kristala. Oblik kristala se tokom dužeg vremena taloženja menja od kristala u obliku većih ploča neuniformno raspoređenih na površini čelika, ka bolje pakovanim laminarnim i igličastim kristalima.