Open Access
Giant direct and inverse magnetocaloric effect linked to the same forward martensitic transformation
(Springer Nature, 2017) Pérez de Landazábal Berganzo, José Ignacio; Recarte Callado, Vicente; Sánchez-Alarcos Gómez, Vicente; Beato López, Juan Jesús; Rodríguez Velamazán, José Alberto; Sánchez Marcos, J.; Gómez Polo, Cristina; Cesari, Eduard; Fisika; Institute for Advanced Materials and Mathematics - INAMAT2; Física
Metamagnetic shape memory alloys have aroused considerable attraction as potential magnetic refrigerants due to the large inverse magnetocaloric effect associated to the magnetic-field-induction of a reverse martensitic transformation (martensite to austenite). In some of these alloys, the austenite phase can be retained on cooling under high magnetic fields, being the retained phase metastable after field removing. Here, we report a giant direct magnetocaloric effect linked to the anomalous forward martensitic transformation (austenite to martensite) that the retained austenite undergoes on heating. Under moderate fields of 10 kOe, an estimated adiabatic temperature change of 9 K has been obtained, which is (in absolute value) almost twice that obtained in the conventional transformation under higher applied fields. The observation of a different sign on the temperature change associated to the same austenite to martensite transformation depending on whether it occurs on heating (retained) or on cooling is attributed to the predominance of the magnetic or the vibrational entropy terms, respectively.
Open Access
Entropy change caused by martensitic transformations of ferromagnetic shape memory alloys
(MDPI, 2017) L'vov, Victor A.; Cesari, Eduard; Kosogor, Anna; Torrens Serra, Joan; Recarte Callado, Vicente; Pérez de Landazábal Berganzo, José Ignacio; Física; Fisika
In this paper, our most recent findings on the influence of magnetic order on the main transformational caloric and elastic properties of shape memory alloys (SMAs) are reviewed. It is argued that ferromagnetic order has a strong influence on the temperature interval of martensitic transformation (MT), the characteristics of stress-induced MT, and the shear elastic modulus of SMA. The problem of separation of the magnetic contributions to the entropy change ΔS and heat Q exchanged in the course of martensitic transformation (MT) of SMA is considered in general terms, and theoretical formulas enabling the solution of the problem are presented. As an example, the ΔS and Q values, which were experimentally determined for Ni-Mn-Ga and Ni-Fe-Ga alloys with different Curie temperatures TC and MT temperatures TM, are theoretically analyzed. It is shown that for Ni-Mn-Ga martensites with TM < TC, the ratio of elastic and magnetic contributions to the entropy change may be greater or smaller than unity, depending on the temperature difference TC – TM.
Open Access
Long-range atomic order and entropy change at the martensitic transformation in a Ni-Mn-In-Co metamagnetic shape memory alloy
(MDPI, 2014) Sánchez-Alarcos Gómez, Vicente; Recarte Callado, Vicente; Pérez de Landazábal Berganzo, José Ignacio; Cesari, Eduard; Rodríguez Velamazán, José Alberto; Física; Fisika
The influence of the atomic order on the martensitic transformation entropy change has been studied in a Ni-Mn-In-Co metamagnetic shape memory alloy through the evolution of the transformation temperatures under high-temperature quenching and post-quench annealing thermal treatments. It is confirmed that the entropy change evolves as a consequence of the variations on the degree of L21 atomic order brought by thermal treatments, though, contrary to what occurs in ternary Ni-Mn-In, post-quench aging appears to be the most effective way to modify the transformation entropy in Ni-Mn-In-Co. It is also shown that any entropy change value between around 40 and 5 J/kgK can be achieved in a controllable way for a single alloy under the appropriate aging treatment, thus bringing out the possibility of properly tune the magnetocaloric effect.
Open Access
Outstanding role of the magnetic entropy in arrested austenite in an ordered Ni45Mn36.7In13.3Co5 metamagnetic shape memory alloy
(Elsevier, 2019) Pérez de Landazábal Berganzo, José Ignacio; Recarte Callado, Vicente; Sánchez-Alarcos Gómez, Vicente; Jiménez Ruiz, M.; Cesari, Eduard; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2; Ciencias
The relevance of the entropy and in particular the outstanding role of the magnetic contribution is analyzed in a non-equilibrium arrested austenite phase in a Ni 45 Mn 36.7 In 13.3 Co 5 metamagnetic shape memory alloy. The Debye and Bragg-Williams approximations have been used to analyze and quantify the vibrational and magnetic contributions respectively, to the total entropy change linked to the martensitic transformation. The sign on the entropy change associated to the forward austenite to martensite transformation is different depending on whether it occurs at low or at high temperature as a consequence of the different vibrational and magnetic contributions.
Open Access
Experimental observation of vacancy-assisted martensitic transformation shift in Ni-Fe-Ga alloys
(American Physical Society, 2019) Unzueta, Iraultza; Alonso de Robador Lorente, Daniel; Cesari, Eduard; Sánchez-Alarcos Gómez, Vicente; Recarte Callado, Vicente; Pérez de Landazábal Berganzo, José Ignacio; García, José Ángel; Plazaola, Fernando; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2; Ciencias
Positron annihilation lifetime spectroscopy is used to experimentally demonstrate the direct relationship between vacancies and the shift of the martensitic transformation temperature in a Ni55Fel7Ga28 alloy. The evolution of vacancies assisting the ordering enables shifts of the martensitic transformation up to 50 K. Our results confirm the role that both vacancy concentration and different vacancy dynamics play in samples quenched from the L2(1) and B2 phases, which dictate the martensitic transformation temperature and its subsequent evolution. Finally, by electron-positron density functional calculations V-Ni is identified as the most probable vacancy present in Ni55Fe17Ga28. This work evidences the capability of vacancies for the fine-tuning of the martensitic transformation temperature, paving the way for defect engineering of multifunctional properties.
Open Access
Changes in the crystalline degree in neutron irradiated EPDM viewed through infrared spectroscopy and inelastic neutron scattering
(Rede Latino-Americana de Materiais, 2018) Lambri, Osvaldo Agustín; Giordano, E. D.; Bonifacich, Federico Guillermo; Pérez de Landazábal Berganzo, José Ignacio; Recarte Callado, Vicente; Física; Fisika; Universidad Pública de Navarra / Nafarroako Unibertsitate Publikoa
The changes in the degree of crystallinity in commercial Ethylene Propylene Diene rubber-type M (EPDM) irradiated with neutrons at different doses has been studied by means of inelastic neutron scattering and infrared absorption spectroscopy experiments. EPDM samples were taken from the housing of non-ceramic electrical insulators which are used in outdoor transmission lines of 66 kV. Inelastic neutron scattering spectra were recorded at 5 K with an accessible energy-transfer range between 180 - 3500 cm-1. Infrared studies were performed at room temperature with an energy transfer between 4000 - 400 cm-1. Controlled neutron irradiation allows to obtain different volume fraction and size of crystalline zones in EPDM. The obtained results are discussed and correlated with studies of differential scanning calorimetry, dynamic mechanical analysis and positron annihilation lifetime spectroscopy from where the changes in crystallinity in EPDM were indirectly studied. Inelastic neutron scattering studies were not appropriate for determining the changes in the crystallinity degree in neutron irradiated commercial EPDM. In contrast, from infrared absorption spectroscopy the changes in crystallinity could be determined successfully.
Open Access
Thermal degradation of type I collagen from bones
(Tech Science Press, 2016) Lambri, Melania Lucila; Giordano, E. D.; Bozzano, P. B.; Pérez de Landazábal Berganzo, José Ignacio; Recarte Callado, Vicente; Fisika; Institute for Advanced Materials and Mathematics - INAMAT2; Física; Universidad Pública de Navarra / Nafarroako Unibertsitate Publikoa
The denaturation processes of collagen in the temperature range between 450 K and 670 K are revealed through studies performed on cow rib bones by means of mechanical spectroscopy, differential scanning calorimetry, thermogravimetry, scanning electron microscopy and infrared spectroscopy. The conformational change of the collagen molecules from a triple helix structure to a random coil was found at around 510 K. It was determined that the transformation is developed through the viscous movement of fibrils with an activation energy of (127 ± 8) kJ/mol. The second stage of massive bulk deterioration of the collagen was found at around 600 K, which leads to the loss of the mechanical integrity of the bulk collagen. In addition, an easy-to-handle viscoelastic procedure for obtaining the activation energy of the denaturation process from mechanical spectroscopy studies was also shown.
Open Access
Study of the martensitic transition in Ni-Mn-Sn-Ti ferromagnetic shape memory alloys
(Rede Latino-Americana de Materiais, 2018) Bonifacich, Federico Guillermo; Lambri, Osvaldo Agustín; Pérez de Landazábal Berganzo, José Ignacio; Recarte Callado, Vicente; Sánchez-Alarcos Gómez, Vicente; Fisika; Institute for Advanced Materials and Mathematics - INAMAT2; Física; Universidad Pública de Navarra / Nafarroako Unibertsitate Publikoa
In the present work, mechanical spectroscopy measurements as a function of temperature and strain have been performed in (at.%) Ni50Mn37Sn13-xTix (x=0, 0.5 and 2) ferromagnetic shape memory alloys in order both to study martensitic transition phenomenon and also to determine its temperature of appearance. For mechanical spectroscopy measurements, a five elements piezoelectric device recently developed has been used. In addition, other characterization techniques as, differential thermal analysis and superconducting quantum interference magnetic spectroscopy, were also used. Besides, relaxation processes near the martensitic transition temperature have been also observed.
Open Access
Influence of defects on the irreversible phase transition in the Fe-Pd doped with Co and Mn
(Rede Latino-Americana de Materiais, 2018) Bonifacich, Federico Guillermo; Lambri, Osvaldo Agustín; Pérez de Landazábal Berganzo, José Ignacio; Recarte Callado, Vicente; Sánchez-Alarcos Gómez, Vicente; Fisika; Institute for Advanced Materials and Mathematics - INAMAT2; Física; Universidad Pública de Navarra / Nafarroako Unibertsitate Publikoa
The appearance of BCT martensite in Fe-Pd-based ferromagnetic shape memory alloys, which develops at lower temperatures than the thermoelastic martensitic transition, deteriorates the shape memory properties. In a previous work performed in Fe70Pd30, it was shown that a reduction in defects density reduces the non thermoelastic FCT-BCT transformation temperature. In the present work, the influence of quenched-in-defects upon the intensity and temperature of the thermoelastic martensitic (FCC-FCT) and the non thermoelastic (FCT-BCT) transitions in Fe-Pd doped with Co and Mn is studied. Differential scanning calorimetric and mechanical spectroscopy studies demonstrate that a reduction in the dislocation density the stability range of the FCC-FCT reversible transformation in Fe67Pd30Co3 and Fe66.8Pd30.7Mn2.5 ferromagnetic shape memory alloys.
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.

Recarte Callado, Vicente

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