Open Access
Martensitic transformation controlled by electromagnetic field: from experimental evidence to wireless actuator applications
(Elsevier, 2022) Garayo Urabayen, Eneko; La Roca, Paulo Matías; Gómez Polo, Cristina; Sánchez-Alarcos Gómez, Vicente; Recarte Callado, Vicente; Pérez de Landazábal Berganzo, José Ignacio; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2; Ciencias; Gobierno de Navarra / Nafarroako Gobernua
Mechanical actuators based on shape memory alloys (SMA) are becoming a key component in the development of novel soft robotic applications and surgically implantable devices. Their working principle relies in the temperature induced martensitic transformation (MT), which is responsible of the actuation mechanism. In this work, we found experimental evidence to show that the martensitic transformation can be controlled by electromagnetic field (EF) by a wireless process in ferromagnetic shape memory alloys. It is shown that the martensitic transformation can be driven by an external EF (frequency 45 kHz) while the specific absorption rate (SAR), which was determined through real-time dynamic magnetization measurements, allows the instantaneous monitoring of the transformation evolution. On the basis of the obtained results, we propose a strategy to achieve a battery-free wireless SMA actuator that can be remotely controlled. This concept can be applicable to other SMA material that exhibit a similar magneto-structural phase transition
Open Access
Magnetically activated 3D printable polylactic acid/polycaprolactone/magnetite composites for magnetic induction heating generation
(Springer, 2023) Galarreta Rodríguez, Itziar; López Ortega, Alberto; Garayo Urabayen, Eneko; Beato López, Juan Jesús; La Roca, Paulo Matías; Sánchez-Alarcos Gómez, Vicente; Recarte Callado, Vicente; Gómez Polo, Cristina; Pérez de Landazábal Berganzo, José Ignacio; Ciencias; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2; Universidad Pública de Navarra / Nafarroako Unibertsitate Publikoa
Additive manufacturing technology has attracted the attention of industrial and technological sectors due to the versatility of the design and the easy manufacture of structural and functional elements based on composite materials. The embedding of magnetic nanoparticles in the polymeric matrix enables the development of an easy manufacturing process of low-cost magnetically active novel polymeric composites. In this work, we report a series of magnetic composites prepared by solution casting method combining 5 to 60 wt.% of 140 ± 50 nm commercial Fe3O4 nanoparticles, with a semi-crystalline, biocompatible, and biodegradable polymeric blend made of polylactic acid (PLA) and polycaprolactone (PCL). The composites were extruded, obtaining 1.5 ± 0.2 mm diameter continuous and flexible filaments for fused deposition modelling 3D printing. The chemical, magnetic, and calorimetric properties of the obtained filaments were investigated by differential scanning calorimetry, thermogravimetric analysis, magnetometry, and scanning electron microscopy. Furthermore, taking advantage of the magnetic character of the filaments, their capability to generate heat under the application of low-frequency alternating magnetic fields (magnetic induction heating) was analyzed. The obtained results expose the versatility of these easy manufacturing and low-cost filaments, where selecting a desired composition, the heating capacity can be properly adjusted for those applications where magnetic induction plays a key role (i.e., magnetic hyperthermia, drug release, heterogeneous catalysis, water electrolysis, gas capture, or materials synthesis).
Open Access
Fe3O4-SiO2 mesoporous core/shell nanoparticles for magnetic field-induced ibuprofen-controlled release
(American Chemical Society, 2022-12-23) García Rodríguez, Lucía; Garayo Urabayen, Eneko; López Ortega, Alberto; Galarreta Rodríguez, Itziar; Cervera Gabalda, Laura María; Cruz Quesada, Guillermo; Cornejo Ibergallartu, Alfonso; Garrido Segovia, Julián José; Gómez Polo, Cristina; Pérez de Landazábal Berganzo, José Ignacio; Ciencias; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2; Universidad Pública de Navarra / Nafarroako Unibertsitate Publikoa, PJUPNA2020; Gobierno de Navarra / Nafarroako Gobernua
Hybrid magnetic nanoparticles made up of an iron oxide, Fe3O4, core and a mesoporous SiO2 shell with high magnetization and a large surface area were proposed as an efficient drug delivery platform. The core/shell structure was synthesized by two seed-mediated growth steps combining solvothermal and sol—gel approaches and using organic molecules as a porous scaffolding template. The system presents a mean particle diameter of 30(5) nm (9 nm magnetic core diameter and 10 nm silica shell thickness) with superparamagnetic behavior, saturation magnetization of 32 emu/g, and a significant AC magnetic-field-induced heating response (SAR = 63 W/gFe3O4, measured at an amplitude of 400 Oe and a frequency of 307 kHz). Using ibuprofen as a model drug, the specific surface area (231 m2/g) of the porous structure exhibits a high molecule loading capacity (10 wt %), and controlled drug release efficiency (67%) can be achieved using the external AC magnetic field for short time periods (5 min), showing faster and higher drug desorption compared to that of similar stimulus-responsive iron oxide-based nanocarriers. In addition, it is demonstrated that the magnetic field-induced drug release shows higher efficiency compared to that of the sustained release at fixed temperatures (47 and 53% for 37 and 42 °C, respectively), considering that the maximum temperature reached during the exposure to the magnetic field is well below (31 °C). Therefore, it can be hypothesized that short periods of exposure to the oscillating field induce much greater heating within the nanoparticles than in the external solution.
Open Access
Heatable magnetic nanocomposites with Fe3O4 nanocubes
(Elsevier, 2022-09-27) Larumbe Abuin, Silvia; Lecumberri, Cristina; Monteserín, María; Fernández, Lorea; Medrano Fernández, Ángel María; Garayo Urabayen, Eneko; Gómez Polo, Cristina; Ciencias; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2
The development of magnetic self-heating polymers is an area of great interest for many applications. The intrinsic magnetic properties of the magnetic fillers play a key role in the final heating capability of these nanocomposites. Thus, it has been already reported the improvement of the heating efficiency on Fe3O4 magnetic nanocubes with respect to spherical nanoparticles with the similar mean size1. This result is due to the contribution of the magnetic anisotropy giving rise to higher magnetic coercivity and as consequence, higher SAR (Specific Absorption Rate) values. In this work, well- defined Fe3O4 nanocubes were synthesized through thermal decomposition processes with a mean particle diameter around 70 nm (TEM) (Fig. 1). The SAR values were estimated through the measurement of the AC hysteresis loops, obtaining values of around 900 W/g for the dispersion of the nanocubes in water and values of 350 W/g for the nanocubes dispersed in agar (0.5% wt), with a frequency of 403 kHz and a field amplitude of 30kA/m . In this case, the decrease of the SAR values is due to the inmovilization of the particles in the medium and hence, the Brownian movement of the particles. The temperature increase was also characterized, where a clear enhancement of the heating properties was obtained for nanocubes comparing with spherical nanoparticles of similar mean diameter (Fig. 2). Finally, the heating capacity of the nanocomposites (30% weight of magnetic nanoparticles) was studied through the application of an external AC magnetic field with a Helmholtz coil (319 kHz, 400A, 200G approximately, induction equipment model EasyHeat Ambrell). The effect of the thickness of the polymeric discs on the final temperature achieved was studied (2 and 4 mm thickness and 30 mm diameter). Thus, temperatures of 100 °C or 250 °C were reached after 2 min for the nanocomposites with thicknesses of 2 and 4 mm respectively.
Open Access
Fast calculation methods for the magnetic field of particle lattices
(AIP Publishing, 2025-02-14) Royo Silvestre, Isaac; Gandía Aguado, David; Beato López, Juan Jesús; Garayo Urabayen, Eneko; Gómez Polo, Cristina; Ciencias; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2; Estadística, Informática y Matemáticas; Estatistika, Informatika eta Matematika
With the rise of 3D printing and composite materials, components comprising dispersed magnetic particles have become more interesting due to the possibility to design magnetic elements of any shape with varying amounts of the actual magnetic material. However, quick and easy calculation methods are needed to design these components enabling the selection of the optimum required percentage of magnetic particles (millimeter parts contain billions of micro-sized particles). This work proposes a semi-analytical iterative method for the estimation of the magnetic field generated by magnetic composites formed by embedded magnetic particles. The model is compared in terms of accuracy and calculation speed with finite element analysis and the average magnetization model of the magnetic composite. The results are finally supported by the comparison with experimental measurements of the weak magnetic field generated by a magnetic particle lattice.
Open Access
U-shape magnetostrictive harvester: design and experimental validation
(IEEE, 2024-07-05) Gandía Aguado, David; Garayo Urabayen, Eneko; Beato López, Juan Jesús; Royo Silvestre, Isaac; Gómez Polo, Cristina; Ciencias; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2
Electromagnetic vibrational harvesters stand out due to their high-power density, long-life robust structure and low-cost design. Moreover, they can be designed using magnetostrictive materials. The mechanical vibrations cause stress on the magnetostrictive material, leading to variations in its magnetization. This, in turn, induces an electromotive force (EMF) in a well-designed pick-up coil system, thereby transforming mechanical energy into electrical energy. In spite of the potentiality of these electromagnetic harvesters, their practical implementation is limited due to the difficulties in the design optimization in terms of the device dimensions, effective stresses on the magnetostrive material, distribution and magnetic field strength of the permanent magnets and pick-up coil characteristics. Finite Element Methods (FEM) enable the estimation of the induced voltage and thus the output power as a function of harvester design parameters, allowing us to experiment with different configurations and identify optimal parameters.
Open Access
Modulating photocatalytic activity of nitrogen doped TiO2 nanoparticles via magnetic field
(Elsevier, 2024-07-30) Gómez Polo, Cristina; Cervera Gabalda, Laura María; Garayo Urabayen, Eneko; Beato López, Juan Jesús; Pérez de Landazábal Berganzo, José Ignacio; Ciencias; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2; Universidad Pública de Navarra / Nafarroako Unibertsitate Publikoa
The effect of the magnetic field on the photocatalytic activity of TiO2-based nanoparticles is analyzed using a magnetically-assisted photoreactor with permanent magnets to generate a controlled uniform magnetic field, B (¿82 mT). Nitrogen doped TiO2 nanoparticles (sizes around 10 nm) were synthesized through a solvothermal method employing Ti(IV) butoxide and HNO3 (x = 0, 0.5, 1, 1.5 and 2 mL) as precursors and their structural, optical and magnetic properties were analyzed. Specifically, nitrogen doping is confirmed through Hard X-ray Photoelectron Spectroscopy (HAXPES) in those samples synthesized with low HNO3 concentrations (x = 0.5, 1). The correlation between spin polarization (magnetic susceptibility) and visible photocatalytic activity (methyl orange as a model organic pollutant) is particularly analyzed. Surprisingly, opposite effects of the magnetic field on the photocatalytic performance are found in the visible range (above 400 nm) or under UV-Vis irradiation (decrease and increase in the photocatalytic activity, respectively, under magnetic field). The Langmuir-Hinshelwood model allows us to conclude that the strong decrease in adsorption under the magnetic field (around 42 % for x = 0.5) masks the increase in the kinetic constant (close to 58 % for x = 0.5) related mainly to the effect of Lorentz forces on the reduction of the electron-hole recombination.
Open Access
Magnetic-field-assisted photocatalysis of N-TiO2 nanoparticles
(IEEE, 2023-09-04) Cervera Gabalda, Laura María; Garayo Urabayen, Eneko; Beato López, Juan Jesús; Pérez de Landazábal Berganzo, José Ignacio; Gómez Polo, Cristina; Ciencias; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2
Nitrogen doped TiO2 nanoparticles were synthesized through solvothermal method employing Ti (IV) butoxide and HNO3 as precursors. Structural and optical characterizations confirm their nanometer nature (sizes around 10 nm) and the band-gap energy values in the UV range (3.2 eV). Nitrogen doping enhances the occurrence of optical Urbach tails extending towards the visible region. Visible photocatalytic performance (degradation of methyl orange) is correlated with maximum values in the magnetic susceptibility linked to a magnetic polarization of the anatase structure via defects (oxygen vacancies). The application of magnetic field provides a positive effect (acceleration in reaction kinetics) within the UV-Vis range.
Open Access
Electromagnetic vibrational harvester based on U-shaped ferromagnetic cantilever: a novel two-magnet configuration
(Elsevier, 2024-09-07) Gandía Aguado, David; Garayo Urabayen, Eneko; Beato López, Juan Jesús; Royo Silvestre, Isaac; Cruz Blas, Carlos Aristóteles de la; Tainta Ausejo, Santiago; Gómez Polo, Cristina; Ciencias; Zientziak; Ingeniería Eléctrica, Electrónica y de Comunicación; Ingeniaritza Elektrikoa, Elektronikoa eta Telekomunikazio Ingeniaritza; Estadística, Informática y Matemáticas; Estatistika, Informatika eta Matematika; Institute for Advanced Materials and Mathematics - INAMAT2; Institute of Smart Cities - ISC
Electromagnetic vibrational harvesters are low-cost devices featuring high-power densities and robust structures, often used for capturing the energy of environmental vibrations (civil infrastructures, transportation, human motion, etc.,). Based on Faraday's law, energy generation relies on the modification of the magnetic field distribution within a magnetic element caused by mechanical vibrations inducing an electromotive force (EMF) in a pick-up coil. However, the practical implementation of this type of vibrational harvester is currently limited due to the reduced generated power under low-frequency vibrations. In this work, an electromagnetic vibrational harvester is experimentally characterized and analyzed employing magnetic circuit analysis. The harvester consists of a ferromagnetic U-shaped cantilever, a NdFeB magnet and a ferrite magnet used as ¿magnetic tip mass¿ to enhance the magnetic flux changes under vibrations of frequency < 100 Hz. For this configuration, an experimental voltage of ¿ 1.2 V peak-to-peak (open circuit) was obtained at a resonant frequency of 77 Hz, enabling the subsequent electronic rectification stage. Additionally, Finite Element Method (FEM) is used to explore different design possibilities including the modeling of complex geometries, mechanical properties and non-linear magnetic materials, enabling the tuning of the resonance frequency from 51 to 77 Hz, keeping constant the induced voltage.
Open Access
Steering the synthesis of Fe3O4 nanoparticles under sonication by using a fractional factorial design
(Elsevier, 2021) Echeverría Morrás, Jesús; Moriones Jiménez, Paula; Garrido Segovia, Julián José; Ugarte Martínez, María Dolores; Cervera Gabalda, Laura María; Garayo Urabayen, Eneko; Gómez Polo, Cristina; Pérez de Landazábal Berganzo, José Ignacio; Ciencias; Zientziak; Estadística, Informática y Matemáticas; Estatistika, Informatika eta Matematika; Institute for Advanced Materials and Mathematics - INAMAT2; Universidad Pública de Navarra / Nafarroako Unibertsitate Publikoa; Gobierno de Navarra / Nafarroako Gobernua
Superparamagnetic iron oxide nanoparticles (MNPs) have the potential to act as heat sources in magnetic hyperthermia. The key parameter for this application is the specific absorption rate (SAR), which must be as large as possible in order to optimize the hyperthermia treatment. We applied a Plackett-Burman fractional factorial design to investigate the effect of total iron concentration, ammonia concentration, reaction temperature, sonication time and percentage of ethanol in the aqueous media on the properties of iron oxide MNPs. Characterization techniques included total iron content, Fourier Transform Infrared Spectroscopy, X-Ray Diffraction, High Resolution Transmission Electron Microscopy, and Dynamic Magnetization. The reaction pathway in the coprecipitation reaction depended on the initial Fe concentration. Samples synthesized from 0.220 mol L−1 Fe yielded magnetite and metastable precipitates of iron oxyhydroxides. An initial solution made up of 0.110 mol L−1 total Fe and either 0.90 or 1.20 mol L−1 NH3(aq) led to the formation of magnetite nanoparticles. Sonication of the reaction media promoted a phase transformation of metastable oxyhydroxides to crystalline magnetite, the development of crystallinity, and the increase of specific absorption rate under dynamic magnetization.