Revistas
Autores:
Pérez-Cerrato, M.; Fraile, I.; Gómez-Cortes, J. F.; et al.
Revista:
MATERIALS
ISSN:
1996-1944
Año:
2022
Vol.:
15
N°:
18
Págs.:
6284
Shape memory alloys (SMAs) are functional materials that are being applied in practically all industries, from aerospace to biomedical sectors, and at present the scientific and technologic communities are looking to gain the advantages offered by the new processing technologies of additive manufacturing (AM). However, the use of AM to produce functional materials, like SMAs, constitutes a real challenge due to the particularly well controlled microstructure required to exhibit the functional property of shape memory. In the present work, the design of the complete AM processing route, from powder atomization to laser powder bed fusion for AM and hot isostatic pressing (HIP), is approached for Cu-Al-Ni SMAs. The microstructure of the different processing states is characterized in relationship with the processing parameters. The thermal martensitic transformation, responsible for the functional properties, is analyzed in a comparative way for each one of the different processed samples. The present results demonstrate that a final post-processing thermal treatment to control the microstructure is crucial to obtain the expected functional properties. Finally, it is demonstrated that using the designed processing route of laser powder bed fusion followed by a post-processing HIP and a final specific thermal treatment, a satisfactory shape memory behavior can be obtained in Cu-Al-Ni SMAs, paving the road for further applications.
Revista:
MATERIALS CHARACTERIZATION
ISSN:
1044-5803
Año:
2022
Vol.:
187
Págs.:
111824
Gas atomized Nd-Fe-B powders of several compositions were separated in different size fractions by sieving. These fractions were annealed between 1100 degrees C and 1150 degrees C for 24 and 96 h. The oxygen content of the powders was measured before and after annealing for the different size fractions. The oxygen concentration of the powders depends strongly on the particle size and increases significantly during annealing, particularly in the case of small particle sizes. The effect of particle size on the microstructural changes was analyzed in detail, particularly on grain growth, using high resolution scanning electron microscopy and transmission electron microscopy. Electron back scattering diffraction was used to measure grain size. When the particle size rises, the degree of sintering decreases and the higher solid/vapor surface area reduces the mobility of grain boundaries. Oxidation also reduces grain growth rate and its effect is more evident for particles sizes below 45-63 mu m and high Nd concentrations. Nb addition leads to the formation of intra- and intergranular precipitates. The size of these Nb-Fe-containing precipitates increases with the particle size for equivalent annealing conditions. At 1150 degrees C, Nb loses its effect as an inhibitor of grain growth in the particle size fractions larger than 45-63 mu m.
Autores:
Del-Río, L.; No, M. L.; Sota, A.; et al.
Revista:
JOURNAL OF ALLOYS AND COMPOUNDS
ISSN:
0925-8388
Año:
2022
Vol.:
919
Págs.:
165806
Among the different families of shape memory alloys (SMA), the Fe-Mn-Si-Cr-Ni alloys have attracted a renewed interest because of its low cost, high corrosion resistance and high recovery strength during the shape memory effect, and the new technologies of additive manufacturing offer unforeseen possibilities for this family of SMA. In the present work, the reversible gamma - epsilon martensitic transformation (MT), responsible for the shape memory effect, is studied in two Fe-Mn-Si-Cr-Ni alloys with high (20.2 wt%) and low (15.8 wt%) Mn content, produced by the conventional route of casting and rolling, in comparison with the MT in another similar alloy, with intermediate Mn content (19.4 wt%), which was produced by gas atomization and additive manufacturing through laser metal deposition. The forward and reverse gamma - epsilon MT is studied by mechanical spectroscopy through the internal friction spectra and the dynamic modulus variation, together with a parallel microstructural characterization including in-situ observation of the gamma - epsilon MT during cooling and heating at the scanning electron microscope. The evolution of the transformed fraction of epsilon martensite, evaluated through the integral area of the internal friction peak, was followed along thermal cycling in all three alloys. Both, the internal friction and the electron microscopy studies show that the epsilon martensite amount increases very fast during the first few cycles, and then decreases with a tendency towards its stabilization for many tens of cycles. The results show that the gamma - epsilon MT is more stable on cycling in the additive manufactured sample than in the conventionally processed samples, opening new avenues for designing shape memory steels to be specifically processed through additive manufacturing.
Revista:
MATERIALS CHARACTERIZATION
ISSN:
1044-5803
Año:
2021
Vol.:
172
Págs.:
110844
Nd-Fe-B powders of different compositions were produced by gas atomization. These powders were annealed between 1000 and 1150 degrees C for several times to study the microstructural evolution. Differential scanning calorimetry was used to determine the thermal transitions on the as-atomized powders and after slow solidification. The microstructure was studied by high resolution scanning electron microscopy at each stage. Electron back scattering diffraction was used to measure grain size and confirm that gas atomized powders are isotropic. It was observed the formation of necks between the particles, densification, and grain growth due to liquid phase sintering. Grain growth and densification occur in parallel by a dissolution-reprecipitation mechanism. The effect of Nd content and Nb addition on the microstructural changes was analyzed in detail, particularly on grain growth. The degree of sintering increases with Nd content, as this element enhances the formation of the liquid phase. Nb addition leads to the formation of precipitates that delay densification and grain growth at 1000 degrees C, but promote abnormal grain growth at 1100 degrees C.
Revista:
NANOMATERIALS
ISSN:
2079-4991
We present the evolution of magnetic anisotropy obtained from the magnetization curve of (Fe0.76Si0.09B0.10P0.05)(97.5)Nb2.0Cu0.5 amorphous and nanocrystalline alloy produced by a gas atomization process. The material obtained by this process is a powder exhibiting amorphous character in the as-atomized state. Heat treatment at 480 degrees C provokes structural relaxation, while annealing the powder at 530 degrees C for 30 and 60 min develops a fine nanocrystalline structure. Magnetic anisotropy distribution is explained by considering dipolar effects and the modified random anisotropy model.
Autores:
Alvarez, K. L. (Autor de correspondencia); Baghbaderani, H. A.; Martín, José Manuel; et al.
Revista:
JOURNAL OF MAGNETISM AND MAGNETIC MATERIALS
ISSN:
0304-8853
The present work demonstrates the high-frequency core loss performance of Fe-based amorphous and nanocrystalline powder cores, initially produced by gas atomised powder, consolidated using sieved particles <= 20 mu m, and isolated by a precise insulating layer of polymer to limit the inter- and intra-particle eddy currents to attain enhanced performance. The large glass forming ability (GFA) of the gas atomised powder, reflected by different glass forming instruments, such as the supercooled region (Delta T-x = 54 degrees C) and the reduced glass transition temperature (T-rg = 0.56), is consistent with the substantial amorphisation capability of the alloy. To the best of our knowledge, this is the first-ever report to reveal a large Delta T-x in the Finemet-type alloy powders, an essential parameter to gas-atomise the amorphous powders with significantly lower cooling rates compared to the melt-spun ribbons. Further, subsequent annealing of the amorphous powders, between the exothermic events guided by differential scanning calorimetry (DSC), lead to the growth of a fine nanocrystalline structure of grains <= 15 nm, thanks to the positive enthalpy of mixing of Cu with the constituents to act as a nucleation agent, to retain the excellent soft magnetic properties. The DC soft magnetic properties of the powders were significantly improved on thermal annealing, confirmed by hysteretic loops, quantified by reduced coercivity H-c < 1 Oe of annealed powders at < 575 degrees C, and attributed to the reduced magnetoelastic contribution due to zero/near-zero magnetostriction anisotropy, attained due to the homogenous nanocrystalline structure. The amorphous and nanocrystalline powder cores, consolidated by compression moulding, show ultra-high loss performance, due to the ultra-low coercivity attained on nanocrystallisation, and negligible eddy currents loss, owning to efficient insulation of small particles, for high-frequency power conversion applications, such as voltage regulator (VR), and resonant converters, in automotive industry and data storage centres.
Revista:
FUSION ENGINEERING AND DESIGN
ISSN:
0920-3796
Año:
2019
Vol.:
146
N°:
Part.B
Págs.:
1596 - 1599
Compared to pure tungsten, self-passivating tungsten based alloys for the first wall armor of future fusion reactors shall provide a major safety advantage in case of a loss-of-coolant accident with simultaneous air ingress, due to the formation of a stable protective scale at high temperatures in presence of oxygen preventing the formation of volatile and radioactive WO3. Recently developed W-Cr-Y alloys produced by mechanical alloying and hot isostatic pressing (HIP) exhibit a strong reduction of oxidation rate compared to pure W and high mechanical strength. A heat treatment after HIP at 1555°C results in a one-phase material with a high thermal shock resistance. Nevertheless, the microstructure is metastable and its thermal stability under operational conditions has to be assessed. In this work results of thermal stability tests on heat treated W-10Cr-0.5Y alloy subjected to temperatures of 650, 700, 800 and 1000°C for times ranging from 50 to 1000h are presented. After 1000h at 650°C and 100h at 700°C no visible change of the microstructure is detected. After 100h at 1000°C a complete decomposition takes place with the formation of a uniform, fine-scale mixture of W- and Cr-rich phases, typical for spinodal decomposition.
Autores:
Gabilondo, M.; Fraile, I. (Autor de correspondencia); Burgos, Nerea; et al.
Revista:
CERAMICS INTERNATIONAL
ISSN:
0272-8842
Año:
2019
Vol.:
45
N°:
17
Págs.:
23149 - 23156
Piezoelectric materials are used in several applications, including sensors and actuators. Perovskite type ferroelectrics, specially, lead zirconate titanate (PZT), due to its excellent dielectric, piezoelectric and ferroelectric properties are usually employed. In this work, a series of Spin Coated PZT thick films were deposited on alumina and stainless steel substrates. These PZT-based films were obtained using inks containing either pArtículos or a precursor that were synthesised using a chemical method. In order to consolidate the deposit as a thick film, a thermal treatment is required after deposition on a substrate. Under temperature exposure, the PZT pArtículos tend to sinter after the elimination of the organic vehicle. Moreover, the PZT precursor transforms to crystalline PZT. Films based on the PZT precursor exhibited many cracks after treatment, while those constituted by PZT pArtículos required sintering temperatures higher than 1000 degrees C which resulted in unstable PZT structures. As an alternative, slurries forming mixtures of PZT precursor and pArtículos, varying their relative proportions, were studied to improve the properties of the films. Films generated in this study were characterized by SEM and X-ray diffractometry.
Revista:
JOURNAL OF ALLOYS AND COMPOUNDS
ISSN:
0925-8388
Fe-Si-B-Nb-Cu alloy powders, with and without P additions, were produced by gas atomization. The particles smaller than 20 mm are fully amorphous, exhibiting good soft magnetic properties. The crystallization process was studied by differential scanning calorimetry, demonstrating that its kinetics changes dramatically with small variations in the composition. The (Fe0.76Si0.09B0.10P0.05)(97.5)Nb2.0Cu0.5 (at. %) alloy was annealed in the supercooled liquid region (480 degrees C) and at the first crystallization peak (530 degrees C). The structural characterization by means of differential scanning calorimetry, X-ray diffraction, and transmission electron microscopy provided information that explained the excellent soft magnetic properties. Annealing at 480 degrees C produced an amorphous relaxed structure with improved soft magnetic properties. At 530 degrees C, a two-phase material formed by nanocrystals with an average grain size of 16-17 nm embedded in an amorphous matrix was developed. Partial nanocrystallization increased the saturation magnetization from 139 to 144 emu/g and reduced the coercivity from 2.24 to 0.69 Oe. These results can be understood in terms of the algebraic contribution of both phases to the magnetization and the application of the random anisotropy model to nanocrystalline soft magnetic materials. (C) 2019 Elsevier B.V. All rights reserved.
Revista:
CERAMICS INTERNATIONAL
ISSN:
0272-8842
Año:
2018
Vol.:
44
N°:
13
Págs.:
15603 - 15610
Lead zirconate titanate (PZT) Pb(ZrxTi1-x)O-3 is one of the most studied perovskite type ferroelectric materials due to its excellent dielectric, piezoelectric and ferroelectric properties. PZT particles and a PZT precursor were synthesized using a chemical method. A vehicle was added to the synthesized particles and precursor for obtaining two inks with appropriate rheological properties to be printed by Inkjet Printing. The use of an 80 mu m diameter nozzle made necessary the utilization of an energetic ball milling for assuring the dispersion of small PZT particles in the ink. After ball milling nanoparticles of 150 nm diameter were obtained. These inks were deposited on alumina and steel substrates followed by sintering using a pulsed laser of 1064 nm wavelength. The work shows the effect laser sintering has on, both inks, the one containing PZT nanoparticles and that one based on the PZT precursor. Laser processing was optimized in order to generate suitable films to be subsequently poled. The effect of poling on these films was also studied and their piezoelectric properties were measured by a compression test. The microstructural characteristics of these films were obtained by SEM and X ray diffractometry.
Autores:
Sarasketa, E.; Otaegi, L.; Rodriguez, L.M.; et al.
Revista:
SOLID STATE IONICS
ISSN:
0167-2738
Año:
2012
Vol.:
222 - 223
Págs.:
16 - 22
Porous Crofer Fe22Cr stainless steel supports for tubular Solid Oxide Fuel Cells (SOFC) were developed and tested successfully under hydrogen fuel with 50% humidification at 800 degrees C. Corrosion resistance and stability as a function of operation lifetime, porosity and thermal cycling were studied through the investigation of oxide growth and microstructure. Oxidation reactions followed subparabolic kinetics and substrates with porosities between 25 and 40% showed long-term stability over 4500 h and suitable properties for metal-supported SOFC technology application. (C) 2012 Elsevier B.V. All rights reserved.
Autores:
Rodriguez-Martinez, L.; Rivas, M.; Otaegi, L.; et al.
Revista:
ECS TRANSACTIONS
ISSN:
1938-5862
Año:
2011
Vol.:
35
N°:
1
Págs.:
445 - 450
Tubular metal supported SOFC technology has successfully been developed over the past years with the aim at domestic CHP systems below 3 kWe. The basic cell structure consists of a metal porous support, a protective barrier layer, an anode and an electrolyte cofired at 1350ºC. Cathode and contacting layers are subsequently sintered at lower temperatures. The most significant results to date include successful thermal cycling of the cell and anodic connection during 450 cycles and 2000 hours, oxidation testing of the metal support for more than 2500 hours and a comparison of influence of porosity during 100 hours oxidation of metal porous substrates under high water vapour atmospheres.
Autores:
Antepara, I.; Rivas, M.; Villarreal, I.; et al.
Revista:
JOURNAL OF FUEL CELL SCIENCE AND TECHNOLOGY
ISSN:
1550-624X
Crofer can be considered as the reference interconnect material in solid oxide fuel cells (SOFCs) working under 800 degrees C. Thanks to its thermal expansion coefficient, it is suitable to replace ceramic components, such as the interconnect and the metal support, and it can be cost effective. Several research groups, including Ikerlan, have used porous substrates with the same composition as Crofer (PM from H. C. Starck GmbH, Goslar, Germany) as the metal support for their SOFC cells. The aim of this study is to determine the effect of certain variables (time, temperature, vapor content, cycling, porosity, and current flow), while other aspects are constant (sample composition and particle size and shape). [DOI: 10.1115/1.4001764]