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 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 Acceso Abierto Aluminide Coatings by Means of Slurry Application: A Low Cost, Versatile and Simple Technology(MPDI, 2024-09-29) Agüero, Alina; Audigié, Pauline; Lorente Sánchez, Cristina; Gutiérrez del Olmo, Marcos; Mora, Julio; Rodríguez Catela, Sergio; European Commission; Agencia Estatal de Investigación (España)The present study focused on demonstrating the versatility of the slurry deposition technique to produce aluminide coatings to protect components from high-temperature corrosion in a broad temperature range, from 400 to 1400 °C. This is a simpler and low-cost coating technology used as an alternative to CVD and pack cementation, which also allows the coating of complex geometries and offers improved and simple repairability for a lot of industrial applications, along with avoiding the use of non-hazardous components. Slurry aluminide coatings from a proprietary water-based-Cr6+ free slurry were produced onto four different substrates: A516 carbon steel, 310H AC austenitic steel, Ti6246 Ti-based alloy and TZM, a Mo-based alloy. The resulting coatings were thoroughly characterised by FESEM and XRD, mainly so that the identification of microstructures and appropriate phases was reported for each coating. The importance of surface preparation and heat treatment as key parameters for the coating final microstructures was also evidenced, and how those parameters can be optimised to obtain stable intermetallic phases rich in Al to sustain the formation of a protective Al2O3 oxide scale. These coating systems have applications in diverse industrial environments in which high-temperature corrosion limits the lifetime of the components.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 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.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 Restringido Comparison between field and laboratory steam oxidation testing on aluminide coatings on P92(Wiley online library, 2011-01-12) Agüero, Alina; González, V; Gutiérrez del Olmo, Marcos; Knödler, R; Straub, S; Muelas Gamo, Raúl; Centro de Astrobiología del Instituto Nacional de Técnica Aeroespacial y CSIC, MDM-2017-0737Steam oxidation has become an important issue for steam power plants as operating temperatures increase from the current 550 to 600–650 °C. For the last 10 years several groups have been carrying out steam oxidation testing of both uncoated substrates and coatings in the laboratory. On the other hand, field testing results are very scarce. In this paper, a comparison of laboratory steam oxidation testing with field test results carried out by Alstom at the Kraftwerk Westfalen power station located in Hamm, Germany will be presented. Both slurry deposited aluminide coatings and uncoated P92 steel have been included in the study. Under steam (atmospheric pressure) and isothermal conditions in the laboratory at 650 °C, spallation of oxides formed on ferritic steels occurs after significantly longer time when compared to exposure to real operating conditions. Oxide spallation results in serious damage in steam power plants by obstructing heat exchanger tubes, erosion of valves and turbine blades, etc. Moreover, the thickness of the oxide scales formed under field testing conditions is significantly higher after similar exposure. On the other hand, aluminide coated P92, which exhibit thickness through cracks, have shown to be stable in the laboratory for up to 60 000 h at 650 °C under steam, without evidence of crack propagation. However, field test results indicate that some degree of crack propagation occurs but without causing substrate attack up to 21 700 h of exposure. Moreover, the aluminium oxide observed in both laboratory and field tested specimens is different.Publicación Restringido Overview of steam oxidation behaviour of Al protective oxide precursor coatings on P92(Taylor and Francis online, 2016-03-04) Agüero, Alina; Gutiérrez del Olmo, Marcos; Muelas Gamo, Raúl; Spiradek Hahn, K.Future designs for steam power plants are expected to operate at 625–750°C, at which the candidate ferritic/martensitic steels exhibit insufficient steam oxidation resistance. Al-based coatings constitute an alternative to prevent or reduce oxidation. For over 50 years this type of coating has been applied on blades and vanes made of Ni- and Co-based alloys used in the hot section gas of turbines which operate at temperatures higher than 900°C. For these coatings, the mechanism of protection from high-temperature oxidation, is based on the formation and maintenance of a thin layer of dense α-Al2O3. Many articles have been written about the nature, formation and failure mechanism of oxide precursor coatings, under air, at over 900°C. [1–6] However, very little is known regarding alumina scales formed under pure steam at lower temperatures, which is the expected scenario for new steam power plants. This paper covers a recapitulation of the behaviour of Al-based protective oxides formed on coatings with various compositions under steam at 650°C, including new data relative to the formation of said oxides under steam and the microstructure of samples exposed to steam for 70 000 h. It has been shown that on Al containing coatings, such as diffusion Fe aluminides and FeCrAls, alumina forms under steam at 650°C. Provided that a critical content of Al is maintained underneath the scale, Al2O3 is very stable, surpassing 70 000 h under steam at 650°C, without evidence of spallation (testing is still ongoing). The industry target for coatings in this cases is 100 000 h. In turn, the critical Al content depends on the coating's Cr content, and if the oxidation takes place at temperatures of 900°C or higher, under air. However, under steam, alumina phases formation and transformations are different: at 650°C χ-Al2O3 forms initially, and appears to slowly transform unto α-Al2O3. General considerations regarding the stability of protective oxides formed under steam as a function of the composition of the subjacent material will be provided.
