Renato Altobelli Antunes

Characterization of corrosion products formed on steels in the first months of atmospheric exposure

The corrosion products of carbon steel and weathering steel exposed to three different types of atmospheres, at times ranging from one to three months, have been identified. The steels were exposed in an industrial site, an urban site (Sao Paulo City, Brazil), and a humid site. The effect of the steel type on the corrosion products formed in the early stages of atmospheric corrosion has been evaluated. The corrosion products formed at the various exposure locations were characterized by Raman microscopy, X-Ray diffraction (XRD) and their morphology was observed by Scanning Electron Microscopy (SEM). Three regions of different colours (yellow, black and red) have been identified over the steel coupons by Raman microscopy. Analysis carried out on each of these areas led to the characterization of the correspondent oxide/hydroxide phases. The main phases present were lepidocrocite (g-FeOOH) and goethite (a-FeOOH). Small amounts of magnetite (Fe3O4) were also eventually encountered.

Corrosion fatigue of biomedical metallic alloys: mechanisms and mitigation.

Cyclic stresses are often related to the premature mechanical failure of metallic biomaterials. The complex interaction between fatigue and corrosion in the physiological environment has been subject of many investigations. In this context, microstructure, heat treatments, plastic deformation, surface finishing and coatings have decisive influence on the mechanisms of fatigue crack nucleation and growth. Furthermore, wear is frequently present and contributes to the process. However, despite all the effort at elucidating the mechanisms that govern corrosion fatigue of biomedical alloys, failures continue to occur. This work reviews the literature on corrosion-fatigue-related phenomena of Ti alloys, surgical stainless steels, Co-Cr-Mo and Mg alloys. The aim was to discuss the correlation between structural and surface aspects of these materials and the onset of fatigue in the highly saline environment of the human body. By understanding such correlation, mitigation of corrosion fatigue failure may be achieved in a reliable scientific-based manner. Different mitigation methods are also reviewed and discussed throughout the text. It is intended that the information condensed in this article should be a valuable tool in the development of increasingly successful designs against the corrosion fatigue of metallic implants.

Characterization of Corrosion Products on Carbon Steel Exposed to Natural Weathering and to Accelerated Corrosion Tests

The aim of this work was to compare the corrosion products formed on carbon steel plates submitted to atmospheric corrosion in urban and industrial atmospheres with those formed after accelerated corrosion tests. The corrosion products were characterized by X-ray diffraction, Mossbauer spectroscopy, and Raman spectroscopy. The specimens were exposed to natural weathering in both atmospheres for nine months. The morphologies of the corrosion products were evaluated using scanning electron microscopy. The main product found was lepidocrocite. Goethite and magnetite were also found on the corroded specimens but in lower concentrations. The results showed that the accelerated test based on the ASTM B117 procedure presented poor correlation with the atmospheric corrosion tests whereas an alternated fog/dry cycle combined with UV radiation exposure provided better correlation.

Surface interactions of a W-DLC-coated biomedical AISI 316L stainless steel in physiological solution

The corrosion stability of a W-DLC coated surgical AISI 316L stainless steel in Hanks’ solution has been evaluated. Particle induced X-ray emission (PIXE) measurements were performed to evaluate the incorporation of potentially bioactive elements from the physiological solution. The film structure was analyzed by X-ray diffractometry and micro-Raman spectroscopy. The wear behavior was assessed using the sphere-on-disc geometry. The in vitro biocompatibility of the W-DLC film was evaluated by cytotoxicity tests. The corrosion resistance of the stainless steel substrate decreased in the presence of the PVD layer. EIS measurements suggest that this behavior was closely related to the corrosion attack through the coating pores. PIXE measurements revealed the presence of Ca and P in the W-DLC film after immersion in Hanks’ solution. This result shows that the PIXE technique can be applied to identify and evaluate the incorporation of bioactive elements by W-DLC films. The film showed good wear resistance and biocompatibility.

FCAW repair welding cycles, HAZ microstructure and corrosion resistance of 2304 duplex stainless steel

Flux-cored arc welding (FCAW) is an automatic welding process widely employed to join duplex stainless steel (DSS) structures in industrial plants because of its high productivity. However, when multiple passes are performed, this process can lead to the formation of non-metallic inclusions originating from the slag in the fusion zone. In this case, the welded joint can be repaired using the same welding process. Some regions next to the heat-affected zone are not removed during the repairing operation. Thus, these regions are subjected to repeated welding cycles and to a high heat input, which can cause microstructural alteration that impairs the corrosion resistance of the welded material. The aim of this work was to study the corrosion resistance of 2304 DSS plates joined using the FCAW process and repaired using the same process. The influence of the repair procedure on the corrosion resistance of the welded joints was evaluated using potentiodynamic polarisation and chronoamperometric curves, which allow the determination of the critical pitting temperature of the samples. The microstructure obtained after each repair cycle was evaluated using optical microscopy and scanning electron microscopy. The results showed that the corrosion resistance was depressed as the number of repair cycles increased.

Comparison of the corrosion resistance of DIN W. Nr. 1.4970 (15%Cr-15%Ni-1.2%Mo-Ti) and ASTM F-138 (17%Cr-13%Ni-2.5%Mo) austenitic stainless steels for biomedical applications

The resistance to localised corrosion of the full austenitic 15%Cr-15%Ni-1.2%Mo titanium stabilized stainless steel (DIN W. Nr. 1.4970) was investigated by electrochemical methods including electrochemical impedance spectroscopy (EIS), potentiodynamic polarization and potentiostatic polarization measurements in a phosphate-buffered solution (PBS). The low carbon and non-stabilized austenitic stainless steel, AISI 316L (ASTM F-138), widely used for surgical implants, was also tested for comparison. The tests were conducted at room temperature after a stable potential had been reached. After the electrochemical measurements, the surfaces of the specimens were observed using SEM to evaluate the presence of pits. Potentiodynamic polarization results showed that both steels are prone to localized corrosion. Larger pits were found on the surface of AISI 316L specimens after the electrochemical tests. EIS response has indicated the duplex structure of the passive oxides. The results showed that the electrochemical behaviour of the DIN W. Nr. 1.4970 is better than of AISI 316L steel. Therefore, their application as an implant material may be considered.

Study of the correlation between flexible food packaging peeling resistance and surface composition for aluminum-metallized BOPP films aged at 60°C

ABSTRACT This study investigated the correlation between surface composition and peeling resistance in food packaging films by studying the heat aging of fabricated films over varying periods of time. The films consisted of a layer of aluminum (Al) metallized, biaxially oriented polypropylene (BOPP) bonded with a polyurethane (PU) adhesive onto another polymeric layer of low-density polyethylene (LDPE). The Al metallized films were prepared by physical vapor deposition (PVD) and aged at 60°C for either 5 or 15 days. The resulting aluminum surfaces were analyzed using X-ray photoelectron spectroscopy (XPS) and found to contain aluminum oxide (Al2O3) and trihydroxide (Al(OH)3). The XPS characterization also revealed a 29% increase in the Al(OH)3 layer thickness of the aged sample relative to a non-aged sample. Atomic force microscopy (AFM) was applied on investigations of possible morphology changes. The aluminum and PU adhesive surface energies were also determined using contact angles measurements and the aluminum surface energy was found to increase by as much as 11.7% compared to the non-aged sample, while the PU adhesive surface energy was at least 65% higher than that of the metallic substrate. The peeling resistance of the laminated aluminum was determined by average peel strength measurements and it was found that the variation in peel strength was related to changes in the Al2O3 layer thickness. The delaminated samples were analyzed using scanning electron microscopy/energy dispersive X-ray spectrometry (SEM/EDS) and showed the cohesive failure of the aluminum film.

Investigation on the Corrosion Resistance of PIM 316L Stainless Steel in PEM Fuel Cell Simulated Environment

Bipolar plates play main functions in PEM fuel cells, accounting for the most part of the weight and cost of these devices. Powder metallurgy may be an interesting manufacturing process of these components owing to the production of large scale, complex near-net shape parts. However, corrosion processes are a major concern due to the increase of the passive film thickness on the metal surface, lowering the power output of the fuel cell. In this work, the corrosion resistance of PIM AISI 316L stainless steel specimens was evaluated in 1M H2SO4 + 2 ppm HF solution at room temperature during 30 days of immersion. The electrochemical measurements comprised potentiodynamic polarization and electrochemical impedance spectroscopy. The surface morphology of the specimens was observed before and after the corrosion tests through SEM images. The material presented low corrosion current density suggesting that it is suitable to operate in the PEM fuel cell environment.

Effect of Processing on Microstructure and Corrosion Mitigating Properties of Hydrotalcite Coatings on AA 6061 Alloy

Pitting corrosion of the aluminium cladding of spent nuclear fuels stored in light water pools has been observed. To prevent this, coating of the Al cladding with hydrotalcite (HTC) was proposed. This paper presents the effect of chemical bath and processing parameters on microstructure and corrosion behavior of HTC coatings on alloy AA 6061 specimens. The HTC coating from the high temperature nitrate bath was homogeneous, thicker and consisted of well-defined intersecting platelets than that formed from the room temperature carbonate bath. Electrochemical polarization tests carried out with HTC coated AA 6061 specimens in 0.01 M NaCl revealed that specimens coated with HTC from the nitrate bath and further treated in a cerium salt solution were the most resistant to corrosion. Field tests in which un-coated and coated AA 6061 alloy coupons as well as full-size plates were exposed to the IEA-R1 reactors spent fuel basin for duration of up to 14 months further corroborated the high corrosion resistance imparted by the high temperature HTC + Ce coating. The mechanism by which the HTC coating and cerium protect the Al alloy is discussed.

The peeling resistance of flexible laminated food packaging: Roles of the NCO:OH ratio and aluminum surface aging times

ABSTRACT This work investigated the relationship between the NCO:OH ratio of the polyurethane (PU) adhesive of thermally treated aluminum substrates and the peel resistance of the obtained flexible laminate. Bicomponent PU-based commercial adhesives were combined with three different proportions of an isocyanate prepolymer and a biopolyol to vary the NCO:OH ratio. The aluminum substrates studied were commercial aluminum films deposited onto a bioriented polypropylene (BOPP) film via vacuum evaporation. The aluminum substrates were thermally treated at 60°C under an atmosphere of air using a conventional laboratory oven for different aging times. The aluminum substrate surfaces were characterized using X-ray photoelectron spectroscopy to evaluate their composition. Atomic force microscopy was employed to evaluate their morphology and contact angle to calculate their surface energy. The adhesive was deposited onto the aluminum substrates and a polyethylene film via manual lamination. The resulting samples were subjected to peel tests. The results showed a reduction in peeling resistance with increasing aging times. Meanwhile, a decrease in the NCO:OH ratio led to a reduction in the peeling resistance for shorter aging times.