Metallurgical analyses and chemical characterizations were carried out on historical cannonballs from the Fortress of San Juan de Ulúa, Veracruz, México. Cannonballs dating from the 18th and 19th centuries share metallurgical characteristics similar to those of material coming from a shipment of ammunition found in the wreck of a sunken French ship from the battle of Trafalgar. The analyses show that the base material is grey cast iron with a carbon equivalent of 4.94 and a ferritic–perlitic matrix, in which the high phosphorus content has led to the formation of iron phosphide compounds in conjunction with a homogeneous distribution of carbon graphite flakes of Type C. In addition, corrosion products from samples revealed the presence of various crystalline iron compounds (X‐ray diffraction), mostly highly chlorinated iron compounds identified as akaganeite. X‐ray fluorescence identified various characteristics of the corrosion products as a function of the sampling depth. FT–IR spectroscopy revealed that the main difference between the corrosion products (internal and external) is determined by the number of organic species. Differential scanning calorimetry corroborated that these corrosion products are thermally stable compounds at elevated temperatures.
This study proposes an electrochemical conservation routine applicable to iron archaeological artifacts extracted from their archaeological context and later exposed to a marine atmosphere. The case of study consisted of a Nineteenth Century anchor safeguarded in the Mexican City of Campeche. Metallurgical characterization and electrochemical studies were used to evaluate and assess the conservation process (electrochemical free chloride removal and species reduction, passivation and coating treatment evaluation) and to quantify their effectiveness. Additionally, archaeological information regarding the manufacture process was obtained. The techniques used include potential measurement, potentiodynamic polarization (polarization curves), potentiostatic measurements, electrochemical impedance spectroscopy, electrochemical noise measurements, as well as metallography studies. The method here proposed can then be used in analogous set up as a guideline example for evaluation and assessment purposes during similar procedures.
Nanofibers have very well known applications in several fields like medicine, textile industry and energy systems. They can be produced by different techniques including electrospinning. In this work, a process for obtaining TiO2 cerium and iron TiO2 nanofibers with a mesoporous structure was performed in order to produce coatings and evaluate their properties. The formation of porous structures using titania, mixed titania/ceria and mixed titania/iron oxides precursor solutions was achieved with a polymer gel templating technique. The nanofibers were prepared with a sol–gel solution containing a mixture of poly (vinyl pyrrolidone) [PVP, Mw 1 300 000], titanium tetraisopropoxide [Ti(O-i-Pr)4], a triblock copolymer Pluronic F127, cerium(III) nitrate hexahydrate [Ce(NO3)3∙6H2O] and iron oxides using the electrospinning technique. The synthesis process was carried out afterward to promote the crystallization and phase transformation to anatase, as well as to remove the polymer via calcination in air at 500 °C. Scanning electron microscopy (SEM) revealed the average diameters of the resulting nanofibers were in the 70 nm to 200 nm range, depending on the preparation conditions. The aim of this work was to evaluate the electrochemical behavior of TiO2, cerium and iron TiO2based nanofibers coatings applied to copper and copper alloys surfaces. In order to achieve this goal, an experimental procedure was designed which allowed to simulate the degradation of the coatings in corrosive environments. The techniques used included electrochemical noise measurement, electrochemical impedance spectroscopy and potentiodynamic polarization.
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