Desarrollo de procesos termoquímicos para el tratamiento simultáneo de envejecimiento y nitruración en plasma de aceros maraging

El trabajo de investigación que se describe en esta tesis persigue un objetivo fundamental, que es el desarrollo de procesos de nitruración en plasma activados por arco eléctrico, susceptibles de ser trasladados a escala industrial, que permitan simultanear la propia nitruración con el tratamiento térmico específico de envejecimiento por precipitación de los aceros maraging. El trabajo identificó las condiciones de tratamiento ideales para el tratamiento del acero maraging, estudiando la influencia de la temperatura en los procesos de nitruración y envejecimiento, la presión del proceso, el potencial aplicado sobre las muestras (vías), así como la adición de hidrógeno al plasma. La principal conclusión de la tesis es que es posible la ejecución de los tratamientos simultáneos de envejecimiento y nitruración de los aceros maraging, habiéndose obtenido propiedades comparables, e incluso en algunos casos superiores, respecto al material tratado en dos etapas. En particular, los tratamientos termoquímicos desarrollados han conseguido una mejora muy notable de las propiedades superficiales de estos materiales en relación a su dureza superficial, resistencia a la corrosión y especialmente de su resistencia al desgaste abrasivoProyectos FORMA0 –financiado por CDTI y el Ministerio de Ciencia e Innovación–, SUPERMARAGING –financiado por el Gobierno de Navarra– y CONSOLIDER-FUNCOAT –cofinanciado por el Ministerio de Ciencia e Innovación y el Gobierno de NavarraPrograma Oficial de Doctorado en Ingeniería de Materiales y Fabricación (RD 1393/2007)Materialen eta Fabrikazioaren Ingeniaritzako Doktoretza Programa Ofiziala (ED 1393/2007

Microstructure and indentation hardness study of CAE-PVD (Cr,Ti,Al)N solid solution coatings deposited using a combinatorial multitarget approach

In this study we have analysed the indentation hardness and modulus of cathodic arc deposited CrTiAlN coatings as a function of the stoichiometric variables Ti/Cr, Al content and cation mix. The coatings have been prepared using a combinatorial cathode composition approach, leading up to 14 different stoichiometries produced in 5 batches. The coatings have been inspected by glow discharge optical emission spectroscopy, scanning electron microscopy, X-ray diffraction and nanoindentation techniques. The coatings develop crystalline structures compatible with solid solutions of face-centered cubic unit cells for all the compositions produced. Such unit cells exhibited a downwards lattice parameter dependency on the aluminum concentration of the coatings (from 0.417 nm down to 0.413 nm). The indentation hardness as a function of the Ti/Cr is compatible with other previous studies reported. The films hardnesses and moduli also increase as the aluminum concentration increases (21 GPa up to 34 GPa). Both indentation responses upon Ti/Cr and Al are attributed to solid solution strengthening. However in order to prove this statement, the indentation hardness and modulus were studied as a function of the mixing term of the cations, as this term is well representative of the solid solution compositional map. The observed results unambiguously evidence that the solid solution strengthening effect is confirmed on the basis of the dependency between the indentation hardness and the so called degree of mixing.This work has been funded by the Spanish Ministry of Science and Innovation of Spain through the project PGC2018-096855-A-C44. The authors also acknowledge the Centro para el Desarrollo Tecnológico e Industrial (CDTI) for the support of the excellence program CERVERA through the project CER2019-1003

Mechanical performance of AlCrSiN and AlTiSiN coatings on inconel and steel substrates after thermal treatments

The objective of this study was to explore the mechanical properties of AlCrSiN and AlTiSiN coatings deposited on Inconel and steel substrates after thermal treatments of 500 °C and 800 °C. Nanoindentation was used to measure the hardness and elastic modulus of the coatings, and microindentation was used for observing the contact damage with Hertzian contact loadings. Microscratch and Mercedes tests were used to evaluate the adhesive strength between coating and substrate with both progressive and static loads, respectively. The surface damage was inspected by optical microscopy and scanning electron microscopy (SEM). Focus ion beams (FIB) were used to mill the cross-sections in order to detect the extent and mode of failure. The results show that AlCrSiN coatings and Inconel substrates exhibit better mechanical performance, even after thermal treatments.Peer ReviewedPostprint (published version

Improved adhesion of cathodic arc PVD AlCrSiN coating on ion-implanted WC-Co substrates

Ion implantation has been shown to improve adhesion strength of AlCrSiN coatings due to a synergic enhancement on fracture toughness and load bearing capability of the substrate that can potentially increase the in-service efficiency of coated cutting tools. In this work, AlCrSiN coatings deposited by PVD on WC-Co substrates implanted with Ti, Cr and N ion species have been processed. The mechanical properties and adhesion have been characterized by contact techniques and the residual stress of the coatings and substrates have been evaluated using FIB-DIC technique and Vickers indentation tests, respectively. An improvement of adhesion strength is obtained for treated substrates, especially for those implanted with titanium and chromium ions. This improvement is attributed to the introduction of residual stresses in the substrate, which increases its fracture toughness and enhances its load bearing capability.Work funded through The Spanish Ministry of Science, Innovation and Universities through grants PGC-2018-096855-B-C41, PGC-2018-096855-B-C42 and PGC-2018-096855-A-C4

Improved adhesion and tribological properties of altin-tisin coatings deposited by dcms and hipims on nitrided tool steels

Hard coatings, such as AlTiN-TiSiN, deposited by Physical Vapor Deposition (PVD) techniques are widely used in industrial applications to protect and increase the lifetime of industrial components, such as cutting tools, dies, and forming tools. Despite their great properties, such as high hardness and wear and oxidation resistance, they are limited in cases of severe conditions due to the poor adhesion between the coating and the substrate. Duplex treatments have commonly been used to improve the adhesive properties of PVD coatings, especially those of the cathodic arc evaporation type. The purpose of this study is to achieve coatings with the good properties of the Magnetron Sputtering processes but with higher adhesion than that achieved with these techniques, thus achieving coatings that can be used under the most severe conditions. In this work, an AlTiN-TiSiN coating was deposited by a combination of DC Magnetron Sputtering (DCMS) and High-Power Impulse Magnetron Sputtering (HiPIMS) after a gas nitriding pretreatment on 1.2379 and Vanadis 4 tool steels. Mechanical (ultra-microhardness and scratch tests) and tribological tests were carried out to study the improvement in the properties of the coating. Duplex-treated samples showed improved adhesion between the coating and the substrate, with second critical load (Lc2) values greater than 100 N. Furthermore, they showed great toughness and wear resistance. These results show that this type of coating technique could be used in the most extreme applications and that they can compete with other techniques and coatings that to date they have not been able to compete with.This research was funded in part by the Spanish Ministry of Science, Innovation and Universities through grants PGC2018-096855-B-C43 and PGC2018-096855-A-C44

CrAlON CAE-PVD coatings for oxidation and wear protection of TZM alloys in FAST sintering applications

CrAlO and CrAlO/CrAlN multilayers deposited by cathodic arc evaporation were developed as protective films in metal and ceramic powder FAST sintering tool dies fabricated in titanium-zirconium-molybdenum (TZM). The films have been characterised in terms of their composition, microstructure, mechanical properties and thermal stability in air at high temperatures between 800 C and 1100 C; in addition the tribological performance has been analysed at room temperature and at 400 C. The crystalline structure and composition of the CrAlO based coatings are compatible with the formation of a mixture of a-corundum and a cubic fcc (Cr,Al)2O3. The crystalline structure of the multilayer is, on the other hand, dominated by the cubic fcc lattice plane reflections of the CrAlN. The deposited specimens have high hardness, between 25 and 30 GPa, which are stable even after annealing at 1000 C. Even more, the multilayer coating also exhibited good mechanical stability at 1100 C. The multilayer coating also exhibited an excellent behaviour against wear at 400 C. Sintering trials using coated TZM dies have been carried out using Ti90Sn10 and Al2O3 high energy ball milled powders. The experimental results show that the oxide based coating formulations are potentially able to protect the tools from wear, sticking and oxidation of their surfaces. This may allow for the use of TZM material as an alternative to other substrates such as graphite for high-temperature dies

The bii4africa dataset of faunal and floral population intactness estimates across Africa’s major land uses

Sub-Saharan Africa is under-represented in global biodiversity datasets, particularly regarding the impact of land use on species’ population abundances. Drawing on recent advances in expert elicitation to ensure data consistency, 200 experts were convened using a modified-Delphi process to estimate ‘intactness scores’: the remaining proportion of an ‘intact’ reference population of a species group in a particular land use, on a scale from 0 (no remaining individuals) to 1 (same abundance as the reference) and, in rare cases, to 2 (populations that thrive in human-modified landscapes). The resulting bii4africa dataset contains intactness scores representing terrestrial vertebrates (tetrapods: ±5,400 amphibians, reptiles, birds, mammals) and vascular plants (±45,000 forbs, graminoids, trees, shrubs) in sub-Saharan Africa across the region’s major land uses (urban, cropland, rangeland, plantation, protected, etc.) and intensities (e.g., large-scale vs smallholder cropland). This dataset was co-produced as part of the Biodiversity Intactness Index for Africa Project. Additional uses include assessing ecosystem condition; rectifying geographic/ taxonomic biases in global biodiversity indicators and maps; and informing the Red List of Ecosystems