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
Improved photocatalytic and antibacterial performance of Cr doped TiO2 nanoparticles
(Elsevier, 2021) Gómez Polo, Cristina; Larumbe Abuin, Silvia; Gil Bravo, Antonio; Muñoz Labiano, Delia; Rodríguez Fernández, L.; Fernández Barquín, Luis; García-Prieto, Ana; Fernández-Gubieda, María Luisa; Muela, Alicia; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2; Ciencias
The effect of Cr and N doping in the adsorption capacity, photocatalytic properties and antibacterial response of TiO2 anatase nanoparticles is analyzed. The nanoparticles (N-TiO2, Cr-TiO2 and Cr/N-TiO2) were prepared by the sol-gel method. The structural (X-ray diffraction and TEM) and magnetic (SQUID magnetometry) characterization confirms the nanosized nature of the anatase nanoparticles and the absence of secondary phases. The enhancement of the adsorption capacity of the dye (methyl orange) on the surface of the catalysts for the Cr and Cr/N doped samples, together with the redshift of the UV-Vis absorbance spectra promote a high photocatalytic performance under visible light in these nanocatalysts. The culturability and viability of the Escherichia coli DH5α in a medium supplemented with the nanoparticles was characterized and compared with the evolution under visible light (both without and with nanoparticles). The results show that Cr-TiO2 nanoparticles under visible light display antibacterial activity that cannot be accounted by the toxicity of the nanoparticles alone. However the antibacterial effect is not observed in N-TiO2 and Cr/N-TiO2. The differences in the electrostatic charge (isoelectric point) and the degree of nanoparticle dispersion are invoked as the main origins of the different antibacterial response in the Cr-TiO2 nanoparticles.
Open Access
Calibrating lower-middle Miocene mammal faunas and unravelling climate change during the Miocene Climate Optimum: the Bardenas Reales de Navarra record (Ebro basin, NE Iberian Peninsula)
(Springer, 2024-10-22) Larrasoaña, Juan Cruz; Suárez-Hernando, Oier; Beamud, Elisabet; Garcés, Miguel; Pérez de Landazábal Berganzo, José Ignacio; Gómez Polo, Cristina; Ruiz-Sánchez, Francisco Javier; Mata, María Pilar; Murelaga, Xabier; Ciencias; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2
The chronology of lower Miocene Iberian small mammal faunas is still poorly constrained given the scarcity of well dated sedimentary successions including small mammal fossil localities. Such scarcity has prevented also an accurate understanding of the response of European terrestrial ecosystem to global changes across the Miocene climate optimum (MCO), one of the best analogues of present-day global warming. Here we present an updated fossil small mammal record of the Bardenas Reales de Navarra (western Ebro basin, Spain), where an expanded lower to middle Miocene continental succession is superbly exposed. Previous and new magnetostratigraphic results from this succession have enabled us to propose, along with additional magnetostratigraphically-dated Iberian faunas, a new chronology for local zones Y to D (Mammal Neogene zones MN2 to MN5). In addition to that, the studied small mammal faunas point to a gradual increase in temperature and humidity conditions in SW Europe between 20 and 15.5 Ma, which appears to be coupled with the progressive shift towards warmer regional (Atlantic) and global conditions across the MCO, thereby pointing to gradual changes in oceanic circulation as the main driver of this period of global warmth. The evolution of sedimentary facies appears to indicate a threshold response of the Ebro basin hydrological balance to the MCO, whereas pedogenic formation of magnetic minerals seems to be linked to periods of enhanced climate variability. These results highlight the need of combining different paleoenvironmental indicators in order to obtain a reliable view of the response of continental ecosystems to global warming.
Open Access
Tailoring the structural and magnetic properties of Co-Zn nanosized ferrites for hyperthermia applications
(Elsevier, 2018) Gómez Polo, Cristina; Recarte Callado, Vicente; Cervera Gabalda, Laura María; Beato López, Juan Jesús; López García, Javier; Rodríguez Velamazán, José Alberto; Ugarte Martínez, María Dolores; Mendonça, E. C.; Duque, J. G. S.; Zientziak; Estatistika, Informatika eta Matematika; Institute for Advanced Materials and Mathematics - INAMAT2; Ciencias; Estadística, Informática y Matemáticas; Gobierno de Navarra / Nafarroako Gobernua
A comparative study of the magnetic properties (magnetic moment, magnetocrystalline anisotropy) and hyperthermia response in Co-Zn spinel nanoparticles is presented. The CoxZn1-xFe2O4 nanoparticles (x = 1, 0.5, 0.4, 0.3, 0.2 and 0.1) were synthesized by co-precipitated method and the morphology and mean crystallite size (around 10 nm) of the nanoparticles were analysed by TEM Microscopy. Regarding the magnetic characterization (SQUID magnetometry), Co-Zn nanoparticles display at room temperature anhysteretic magnetization curves, characteristic of the superparamagnetic behavior. A decrease in the blocking temperature, T-B, with Zn content is experimentally detected that can be ascribed to the reduction in the mean nanoparticle size as x decreases. Furthermore, the reduction in the magnetocrystalline anisotropy with Zn inclusion is confirmed through the analysis of TB versus the mean volume of the nanoparticles and the law of approach to saturation. Maximum magnetization is achieved for x = 0.5 as a result of the cation distribution between octahedral and tetrahedral spinel sites, analysed by neutron diffraction studies. The occurrence of a canted spin arrangement (Yafet-Kittel angle) is introduced to properly fit the magnetic spinel structures. Finally, the heating capacity of these spinel ferrites is analyzed under ac magnetic field (magnetic hyperthermia). Maximum SAR (Specific Absorption Rate) values are achieved for x = 0.5 that should be correlated to the maximum magnetic moment of this composition.
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
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 carbon Fe3O4 nanocomposites synthesized via magnetic induction heating
(Springer Nature, 2023) Cervera Gabalda, Laura María; Gómez Polo, Cristina; Ciencias; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2; Universidad Pública de Navarra/Nafarroako Unibertsitate Publikoa
Magnetic Induction Heating (MIH) of magnetite nanoparticles is employed as a novel synthesis procedure of carbon based magnetic nanocomposites. Magnetic nanoparticles (Fe3O4) and fructose (1:2 weight ratio) were mechanically mixed and submitted to a RF magnetic field (305 kHz). The heat generated by the nanoparticles leads to the decomposition of the sugar and to the formation of an amorphous carbon matrix. Two sets of nanoparticles, with mean diameter sizes of 20 and 100 nm, are comparatively analysed. Structural (X-ray diffraction, Raman spectroscopy, Transmission Electron Microscopy (TEM)), electrical and magnetic (resistivity, SQUID magnetometry) characterizations confirm the nanoparticle carbon coating through the MIH procedure. The percentage of the carbonaceous fraction is suitably increased controlling the magnetic heating capacity of the magnetic nanoparticles. The procedure enables the synthesis of multifunctional nanocomposites with optimized properties to be applied in different technological fields. Particularly, Cr (VI) removal from aqueous media is presented employing the carbon nanocomposite with 20 nm Fe3O4 nanoparticles.
Open Access
Antibacterial performance of Co-Zn ferrite nanoparticles under visible light irradiation
(Wiley, 2024-11-20) Gubieda, Alicia G.; Abad Díaz de Cerio, Ana; García-Prieto, Ana; Fernández-Gubieda, María Luisa; Cervera Gabalda, Laura María; Ordoqui Huesa, Eduardo; Cornejo Ibergallartu, Alfonso; Gómez Polo, Cristina; Ciencias; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2
BACKGROUND: To address water scarcity and promote sustainable resource management, more efficient and cost-effective water treatment solutions are necessary. Particularly, pathogens in drinking water are a topic of growing concern. One promising technology is the use of photocatalytic nanoparticles activated by visible light as antibacterial agents. This study focuses on the characterization and antibacterial properties of Co-Zn ferrite nanocatalysts, tested against Escherichia coli. RESULTS: The CoxZn1¿xFe2O4 (x = 0, 0.1, 0.4 and 0.6) ferrites were synthesized by the co-precipitation method. Structural, morphological and optical analyses confirmed that these nanoparticles have a cubic spinel structure, with sizes of around 10 nm, and band gap energies suitable for visible light activation (1.4¿1.7 eV). The antibacterial efficacy of the nanoparticles against E. coli was tested and compared with their photocatalytic performance employing phenol as organic pollutant model (highest phenol degradation for x = 0.6). Specifically, the antibacterial capacity of these nanoparticles was evaluated by comparing the ability of bacteria to grow after being incubated with the nanoparticles under visible light and in the dark. It was found that nanoparticles with lower cobalt content (x = 0 and 0.1) significantly reduced bacterial culturability under visible light. Transmission Electron Microscopy analysis revealed that nanoparticles with cobalt content caused bacteria to secrete biofilm, potentially offering some protection against the nanoparticles. CONCLUSION: ZnFe2O4 nanoparticles show the highest antibacterial effect amongst those tested. This is attributed to the combined action of Zn2+ ion release and the photocatalytic effect under visible light. Furthermore, Zn might inhibit protective biofilm secretion, leading to higher antibacterial effects.
Open Access
Effect of Cu substitution on the magnetic and magnetic induction heating response of CdFe₂O₄ spinel ferrite
(Elsevier, 2020) Ghasemi, R.; Echeverría Morrás, Jesús; Pérez de Landazábal Berganzo, José Ignacio; Beato López, Juan Jesús; Naseri, M.; Gómez Polo, Cristina; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2; Ciencias
In this work, a comparative study of the effect of Cu on the structural, magnetic and magnetic induction heating response in CdFe2O4 spinel is presented. The ceramic nanoparticles (Cu1−xCdxFe2O4; 0 ≤ x ≤ 1) were synthesized by co-precipitation from Cu(II), Cd(II) and Fe(III) salts. The samples, characterized by X-ray diffractometry, display the characteristic spinel cubic structure (space group Fm3m) where CdO is detected as main secondary phase (≈ 16% weight for x = 1). A high degree of nanoparticle agglomeration is inferred from the Transmission Electron Microscopy (TEM) images, as a consequence of the employed synthesis procedure. Regarding the magnetic properties, superparamagnetic behavior at room temperature can be disregarded according to the low field magnetization response (ZFC-FC curves). For 0.4 ≤ x ≤ 0.8 ratios, the samples display maximum values in the magnetic moment that should be correlated to the cation distribution between the octahedral and tetrahedral sites. Maximum magnetization values lead to an enhancement in the magnetic induction heating response characterized by highest heating temperatures under the action of an ac magnetic field. In particular, maximum SAR values are estimated for x = 0.8 as a combined effect of high magnetic moment, low dc coercive field (high susceptibility). Although these Cu-Cd ferrite nanoparticles display moderate SAR values (around 0.7 W/g), the control of the maximum heating temperatures through the cation distribution (composition) provides promising properties to be used as nanosized heating elements (i.e. hyperthermia agents).
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.

Gómez Polo, Cristina

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