Persona: Gutiérrez del Olmo, Marcos
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Instituto Nacional de Técnica Aeroespacial
El Instituto Nacional de Técnica Aeroespacial es el Organismo Público de Investigación (OPI) dependiente del Ministerio de Defensa. Además de realizar actividades de investigación científica y de desarrollo de sistemas y prototipos en su ámbito de conocimiento, presta servicios tecnológicos a empresas, universidades e instituciones.
El INTA está especializado en la investigación y el desarrollo tecnológico, de carácter dual, en los ámbitos de la Aeronáutica, Espacio, Hidrodinámica, Seguridad y Defensa.
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Publicación Restringido Laboratory corrosion testing of coatings and substrates simulating coal combustion under a low NOx burner atmosphere(Wiley online library, 2013-07-02) Agüero, Alina; Gutiérrez del Olmo, Marcos; Muelas Gamo, Raúl; Plana, Daniel; Román, A.; Hernández, M.It is certainly a difficult task to evaluate new materials and coatings to be used for boilers in power plants, as conditions are extremely complex, comprising a highly erosive environment, high temperature, highly corrosive gases, and reactive deposits. In particular, early catastrophic failures, as well as higher degradation rates have been observed on different power plant boiler components when operating under atmospheres containing low levels of oxygen. These atmospheres are typical of low NOx burners, and can be more corrosive than normal oxidizing conditions. The presence of a sulfidizing atmosphere as well as ash deposits present in boilers, are in part responsible of this accelerated damage. In this work, testing under a low oxygen atmosphere has been carried out on T22 and P92 uncoated and coated specimens. The atmosphere was equal to that measured in a Spanish coal-fired power plant (ENDESA, Compostilla, León) and the test temperature was 580 °C. Tested coatings were slurry applied aluminides, as well as two HVOF sprayed coatings including a commercially deposited Cr2C3NiCr, and a newly developed Cr2O3-Cr composite coating. The specimens were covered with ash (taken from the plant) prior to testing. After testing, the uncoated substrates exhibited high thickness oxides with some sulfide inclusions whereas all tested coatings were very protective. Exposed samples of T22 tubes employed in the Compostilla power plants were analyzed and compared with the corresponding specimens tested in the laboratory. In both cases, the scales contained Fe3O4 and FeS but the sulfide content was significantly higher in the scale formed in the plant. Moreover, ash particles were found embedded in the both scales.Publicación Acceso Abierto Rapid α-Al2O3 Growth on an Iron Aluminide Coating at 600 °C in the Presence of O2, H2O, and KCl(ACS Publications, 2024-10-17) Agüero, Alina; Audigié, Pauline; Rodríguez Catela, Sergio; Gutiérrez del Olmo, Marcos; Pascual Ferreiro, Jon; Ssenteza, Vicent; Jonsson, Torbjörn; Johansson, Lars Gunnar; Agencia Estatal de Investigación (España); European CommissionIn this work, a slurry iron aluminide-coated ferritic steel SVM12 was subjected to a laboratory experiment mimicking superheater corrosion in a biomass-fired power boiler. The samples were exposed under model Cl-rich biomass conditions, in a KCl + O2 + H2O environment at 600 °C for 168, 2000, and 8000 h. The morphology of corrosion and the composition of the oxide scale and the coating were investigated by a combination of advanced analytical techniques such as FESEM/EDS, SEM/EBSD, and XRD. Even after short-term exposure, the coating developed a very fast-growing and up to 50 μm thick α-Al2O3 scale in contrast to the spontaneous formation of a protective, thin, dense, slow-growing, and very adhesive α-Al2O3 layer usually formed on metallic materials after high-temperature oxidation. In view of the literature on the formation of oxide scales on alloys and coatings, the formation of an α-Al2O3 scale at this relatively low temperature is very surprising in itself. The thick alumina scale was not protective as its formation resulted in fast degradation of the coating and rapid Fe2Al5 → FeAl phase transformation, which in turn generated porosity inside the coating. In all cases, the resulting thick Al2O3 scale was porous and consisted of both equiaxed α-Al2O3 grains and randomly oriented aggregated alumina whiskers. Potassium is concentrated in the outer part of the Al2O3 scale, while chlorine is concentrated close to the scale/aluminide interface. The unexpected formation of rapidly growing α-Al2O3 at relatively low temperature is attributed to the hydrolysis of aluminum chloride generated in the corrosion process.Publicación Restringido Deposition process of slurry iron aluminide coatings(Taylor and Francis online, 2008-10-04) Agüero, Alina; Gutiérrez del Olmo, Marcos; González, VanessaDiffusion iron aluminide coatings prevent steam oxidation of ferritic/austenitic steels at 650°C for at least 45,000 h. These coatings are deposited by applying Al slurries followed by a diffusion heat treatment at 650°C. The quality of the coatings is very sensitive to a number of factors such as surface preparation, slurry composition and diffusion treatment temperature. A study of the effect of the different processing parameters has been performed in order to optimize the process from an industrial perspective. Moreover, most commercially available Al slurries contain different levels of Cr6+, a highly carcinogenic species, and therefore Cr6+ free slurry formulations have been prepared. In addition, re-coating after exposure has also been developed since it is not clear yet if these coatings will last the 100,000 h which is the life limit for steam power plant design. Based on these studies, processes suitable for coating real size components and re-coating steam exposed components have been developed and are presented in this contribution.Publicación Restringido Low temperature MOCVD process for fast aluminium deposition on metallic substrates(Wiley, 2005-12-19) Agüero, Alina; Gutiérrez del Olmo, Marcos; García-Martínez, MaríaA CVD pilot plant, designed and built in INTA, is presently being used to deposit aluminium coatings with applications in the fields of industrial and aeronautic turbines, as well as on the protection of components employed in the chemical industry, waste incinerators, fuel cells, and for the replacement of Cd coatings in aeronautic components. The industrial process currently used to coat aeronautic and industrial turbine components employs AlCl3 as precursor at 700–1100 °C and requires more than 12 h per batch (including loading, heating, coating and cooling) due to the relatively low deposition rates and the long heating and cooling cycles. The new process carried out at INTA employs an organometallic precursor, which results in higher deposition rates, at 280–350 °C with a total processing time lower than 5 h per batch. As in any other CVD process, this one allows deposition of coatings in complex geometry components such as on the inner surfaces of turbine blades and heat exchangers tubes. Other important advantages of this particular process are the possibility of recovering and re-utilising the unreacted precursor as well as the high purity of the produced coatings in comparison with those produced by other commercially available technologies. It is well known that the higher the contamination degree, the lower the useful life of this type of coatings. The pilot plant has a deposition chamber with a useful coating zone of 30 cm in length and 18 cm in diameter, heated by a three zone furnace equipped with a pumping system that allows working pressures of 0.1–100 mbar. The system can be manually or automatically controlled and can be easily adapted to deposit other materials. By heat treating the pure Al coatings deposited on Ni base superalloys, Ni aluminide coatings have been obtained and excellent cyclic oxidation behaviour has been observed at 1000 °C. Al has also been deposited on ferritic steels (P91 and 92) and after a suitable heat treatment Fe aluminide coatings with excellent steam oxidation resistance have been obtained. Another potential important use of this process is the deposition of dense aluminium coatings for cadmium replacement in several industrial applications.Publicación Restringido Long term diffusion studies in Fe aluminide coatings deposited by slurry application on ferritic steel(Scientific.Net, 2009-04-22) Agüero, Alina; González, Vanessa; Gutiérrez del Olmo, MarcosDiffusion iron aluminide coatings have shown excellent resistance to high temperature oxidation in air, corrosive atmospheres and steam. A study of the diffusion behaviour of slurry applied diffusion aluminide coatings deposited on ferritic steel have been carried out under a 100% flowing steam atmosphere for up to 50,000 h at 650 °C. The results have shown that initially, the coating forms by outward growth possibly including the dissolution of the steel in molten aluminium. At later stages, during exposure to steam at 650 °C, aluminium diffuses inward and moreover, Fe also diffuses outward resulting in the progressive development of Kirkendall porosity. Results have also indicated that in order to form a pure protective Al2O3 scale the Al wt.% has to be > 4. Below this content Al-Fe mixed oxides develop exhibiting a less protective behaviour.Publicación Restringido Microstructural Evolution of Slurry Fe Aluminide Coatings during High Temperature Steam Oxidation(Trans Tech Publications, 2008-09-15) Agüero, Alina; Spiradek, Krystina; Höfinger, S; Gutiérrez del Olmo, Marcos; Muelas Gamo, RaúlSlurry iron aluminide coatings are very resistant to steam oxidation at 600-650º C. These coatings can be used to protect new generation Ultra Super Critical (USC) steam power plant ferritic/martensitic steel components. The microstructure of the initially deposited coating changes as a function of time, mainly due to coating-substrate interdiffusion, going from mostly Fe2Al5 to FeAl, causing the precipitation of AlN in those substrates containing a minimum content of N and moreover, developing Kirkendall porosity at the coating-substrate interface. Steam oxidation at 650º C causes the formation of a protective thin layer of hexagonal χ-Al2O3 phase along with some α- and γ-Al2O3 after the first few hours of exposure. However, despite the relatively low temperature, and after several thousands hours the protective layer was mostly composed of α-Al2O3. A study of the evolution of the microstructure of slurry aluminide coatings deposited on P92 and exposed to steam at 650º C has been carried out by scanning and transmission electron microscopy and X ray diffraction.Publicación Restringido Metal Dusting Protective Coatings. A Literature Review(Springer Nature Link, 2011-03-20) Agüero, Alina; Gutiérrez del Olmo, Marcos; Korcakova, L; Nguyen, T. T. M; Hinnemann, B; Saadi, SMetal dusting is a catastrophic form of carburization attack that takes place in carbon-supersaturated gaseous atmospheres, and is most commonly encountered in steam reforming processes such as the production of hydrogen or syngas for ammonia, Fischer–Tropsch and methanol applications. The consequence of metal dusting can be a severe loss of metal from the process units, leading to high-cost maintenance and serious safety issues. The present literature review discusses the latest developments within metal dusting protection of alloys with special emphasis on protective coatings. In the first part of the paper, an overview of the main theories for metal dusting of alloys as well as fundamental studies is provided. In the second part, the paper focuses on the different methods to prevent metal dusting, including surface poisoning, alloying, chemical, mechanical and laser treatments as well as coatings. Particular focus is given to coatings and their composition, and fabrication methods, and a critical analysis of the different materials’ behaviours and the suitability perspectives of deposition techniques are provided.Publicación Restringido Steam Oxidation Testing of Coatings for Next Generation Steam Power Plant Components(Scientific.Net, 2006-08-14) Agüero, Alina; Gutiérrez del Olmo, Marcos; Muelas Gamo, RaúlTo achieve higher power generation efficiency in steam turbines, operating temperatures are expected to rise from 550°C to 650°C. The use of oxidation resistant coatings on currently available materials, with high creep strength but inferior steam oxidation resistance, is being explored in order to accomplish this goal in the context of the European project “Coatings for Supercritical Steam Cycles” (SUPERCOAT). Coating techniques have been chosen on the basis of being potentially appropriate for coating steam turbine components: the application of metallic and ceramic slurries, pack cementation and the deposition of alloyed and cermet materials by thermal spray. The coatings were characterised by metallography, SEM-EDS and XRD and steam oxidation and thermal cycling laboratory testing was carried out at 650º C. In this presentation, the testing results of selected coatings will be shown including those which exhibit the most promising behaviour. For instance, slurry aluminides have been exposed to steam at 650°C for more than 38,000 h (test ongoing) without evidence of substrate attack. Some HVOF coatings such as FeAl, NiCr and FeCr also have shown excellent behaviour. The results have provided information regarding the mechanism of protection and degradation of these coatings as well as insight into new coating development.Publicación Restringido Oxidation under pure steam: Cr based protective oxides and coatings(Elsevier, 2013-09-20) Agüero, Alina; González, Vanessa; Gutiérrez del Olmo, Marcos; Muelas Gamo, RaúlAt temperatures of 900 °C and higher, the formation, transformation and failure of protective oxides in air have been deeply studied. However, there is significantly less available information of these processes when they take place under pure steam and in the lower temperature range pertinent to steam power plants. New designs for these plants are expected to operate at 625–700 °C, at which the candidate ferritic/martensitic steels exhibit very low steam oxidation resistance. In this paper, available knowledge of the behavior of Cr based protective oxides formed under steam at 650 °C will be presented. It is already known that on ferritic/martensitic steels with a Cr content lower than ~ 9 wt.% such as P92, a nonprotective, thick, dual layer composed of Fe3O4 and (Fe, Cr)3O4 forms. However, significantly higher steam oxidation resistance has been recently found when exposing NPM, a 9 wt.% Cr martensitic steel rich in W and Co, to pure steam at 650 °C. In this case a protective, very thin multilayer forms, with alternating Fe3O4 and (Fe, Cr, Mn)3O4 layers. Different oxides formed after 10,000 h of exposure to steam at 650 °C, on Cr containing coatings. In the case of Fe based, Cr rich coatings, both diffusion and overlay, a protective spinel was observed. However, Cr containing coatings based on Ni develop a very stable, protective thin Cr2O3 layer. Results show that along with the Cr content, other factors such as the grain size below the scale appear to determine the formation of thin protective scales. The steam pressure was also found to significantly and negatively affect the stability of protective Cr based oxides. Chromia former steels and coatings may not be the best solution for 650 °C new generation steam power plants.Publicación Acceso Abierto Modified high hardness steel coating for biomass corrosion protection(Springer Nature Link, 2025-09-13) Agüero, Alina; Gutiérrez del Olmo, Marcos; Audigié, Pauline; Rodríguez Catela, Sergio; Pascual Ferreiro, JonBiomass is a renewable and CO2-neutral energy source. However, the efficiency of biomass combustion plants remains lower than that of current fossil fuel-based systems. To minimize corrosion from aggressive species found in biomass combustion, these plants currently operate at a maximum temperature of 550 °C. The European project BELENUS explored new materials and coatings to raise the operating temperature to 600 °C, thereby improving plant efficiency. Among the coatings under investigation, a super high-hardness steel (SHS) modified with Al, applied by high velocity oxy-fuel (HVOF) thermal spray on ferritic steel SVM12, has demonstrated an improved performance in the laboratory, exposed to a model biomass environment containing KCl deposits for 8000 h at 600 °C. Microstructural analysis by field emission scanning electron microscopy (FESEM) and X-ray diffraction was conducted on the tested samples to examine the coating’s evolution in these environments, as well as the associated protection and degradation mechanisms. The presence of Al within the coating significantly enhanced its resistance to biomass corrosion when compared to uncoated SVM12 and the Al-free SHS coating. Possible reasons for the improved behaviour of the Al-modified coating are the reduction of porosity as well as the blocking effect of either intermetallic FeAl or Al oxide which forms at the splat boundaries prior to exposure to the corrosive atmosphere.
