José Fernando Gómez-Cortés

Shape memory alloys (SMAs) are functional materials with a wide range of applications, from the aerospace sector to the biomedical field. Nowadays, there is a worldwide interest in developing SMAs through powder metallurgy like additive manufacturing (AM), which allows innovative building processes. However, producing SMAs using AM techniques is particularly challenging because of the microstructure required to obtain optimal functional properties. This aspect is critical in the case of Cu–Al–based SMAs, due to their high elastic anisotropy, making them brittle in polycrystalline form. In this work, we approached the processing of a Cu–Al–Ni SMA following a specific powder metallurgy route: gas atomization of a pre-alloyed melt; compaction of the atomized powders through hot isostatic pressing; and a final hot rolling plus thermal treatments. Then, the microstructure of the material was characterized by electron microscopy showing a specific [001] texture in the rolling direction that improved the functional behavior. The successive processing steps produce an increase of about 40 °C in the martensitic transformation temperatures, which can be well controlled and reproduced through the developed methodology. The thermomechanical functional properties of superelasticity and shape memory were evaluated on the final SMA. Outstanding, fully recoverable superelastic behavior of 4.5% in tension, as well as a ±5% full shape memory recovery in bending, were reported for many cycles. These experiments demonstrate the enhanced mechanical and functional properties obtained in polycrystalline Cu–Al–Ni SMAs by powder metallurgy. The present results pave the road for producing this kind of SMA with the new AM technologies, which always produce polycrystalline components and can improve their processes taking the powder metallurgy SMA, here produced, as reference material.

Nowadays, in-situ experiments using scanning electron microscopes (SEM) become extremely useful to explore the behavior of the materials at micro/nano scale in real time. This protocol presents a new methodology to perform in-situ nano-tensile tests inside the SEM. The first part of the protocol describes the sample preparation by FIB, starting from the extraction of the sample from the bulk material. Then, a dog-bone shape sample is milled and transferred to the push-to-pull (PTP) device, from the Bruker-Hysitron company, which allows making a nano-tensile test using a nano-indenter. The PTP device is also milled to receive the micro sample, which is finally thinned and finished on the device. In the second part, the PTP device with the sample is transferred to the SEM nano testing holders; the nano-tensile tests are performed following the procedures of the nano-indenters software and are not described here. Finally, in the third part, the protocol describes the different calibrations and corrections that must be applied to the raw data to properly analyze the nano-tensile test and get the true stress-strain curve of the material.

Cu-Al-Ni is a high-temperature shape memory alloy (HTSMA) with exceptional thermomechanical properties, making it an ideal active material for engineering new technologies able to operate at temperatures up to 200 °C. Recent studies revealed that these alloys exhibit a robust superelastic behavior at the nanometer scale, making them excellent candidates for developing a new generation of micro-/nano-electromechanical systems (MEMS/NEMS). The very large-scale integration (VLSI) technologies used in microelectronics are based on thin films. In the present work, 1 μm thickness thin films of 84.1Cu-12.4 Al-3.5Ni (wt.%) were obtained by solid-state diffusion from a multilayer system deposited on SiNx (200 nm)/Si substrates by e-beam evaporation. With the aim of evaluating the thermal stability of such HTSMA thin films, heating experiments were performed in situ inside the transmission electron microscope to identify the temperature at which the material was decomposed by precipitation. Their microstructure, compositional analysis, and phase identification were characterized by scanning and transmission electron microscopy equipped with energy dispersive X-ray spectrometers. The nucleation and growth of two stable phases, Cu-Al-rich alpha phase and Ni-Al-rich intermetallic, were identified during in situ heating TEM experiments between 280 and 450 °C. These findings show that the used production method produces an HTSMA with high thermal stability and paves the road for developing high-temperature MEMS/NEMS using shape memory and superelastic technologies.

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.

Shape‐memory alloys (SMAs) are the most stretchable metallic materials thanks to their superelastic behavior associated with the stress‐induced martensitic transformation. This property makes SMAs of potential interest for flexible and wearable electronic technologies, provided that their properties will be retained at small scale. Nanocompression experiments on Cu‐Al‐Be SMA single crystals demonstrate that micro‐ and nanopillars, between 2 µm and 260 nm in diameter, exhibit a reproducible superelastic behavior fully recoverable up to 8% strain, even at the nanoscale. Additionally, these micro‐/nanopillars exhibit a size effect on the critical stress for superelasticity, which dramatically increases for pillars smaller than ≈1 µm in diameter, scaling with a power law of exponent n = −2. The observed size effect agrees with a theoretical model of homogeneous nucleation of martensite at small scale and the universality of this scaling power law for Cu‐based SMAs is proposed. These results open new directions for using SMAs as stretchable conductors and actuating devices in flexible and wearable technologies.

In situ neutron diffraction is used to study the strain relaxation on a single crystal and other powdered Cu-Al-Ni shape memory alloys (SMAs) around martensitic transformation temperatures. This work is focused on the analysis of the strain evolution along the temperature memory effect appearing in these alloys after partial thermal transformations. A careful study of the influence of partial cycling on the neutron diffraction spectra in the martensitic phase is presented. Two different effects are observed, the d-spacing position shift and the narrowing of various diffraction peaks, along uncompleted transformation cycles during the thermal reverse martensitic transformation. These changes are associated with the relaxation of the mechanical stresses elastically stored around the martensitic variants, due to the different self-accommodating conditions after uncompleted transformations. The evolution of the stresses is measured through the strain relaxation, which is accessible by neutron diffraction. The observed effects and the measured strain relaxations are in agreement with the predictions of the model proposed to explain this behavior in previous calorimetric studies. In addition, the thermal expansion coefficients of both martensite and austenite phases were measured. The neutron experiments have allowed a complete description of the strains during martensitic transformation, and the obtained conclusions can be extrapolated to other SMA systems.