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
Interferometric vs wavelength selective optical fiber sensors for cryogenic temperature measurements
(SPIE, 2017) Miguel Soto, Verónica de; Leandro González, Daniel; López Aldaba, Aitor; Beato López, Juan Jesús; Pérez de Landazábal Berganzo, José Ignacio; Auguste, Jean-Louis; Jamier, Raphael; Roy, Philippe; López-Amo Sáinz, Manuel; Ingeniaritza Elektrikoa eta Elektronikoa; Fisika; Institute for Advanced Materials and Mathematics - INAMAT2; Ingeniería Eléctrica y Electrónica; Física
In this work, a preliminary study of the behavior of two different interferometric fiber optic sensors and two different wavelength selective fiber optic sensors is performed. A photonic cristal fiber Fabry-Pérot interferometer, a Sagnac interferometer, a commercial fiber Bragg grating (FBG) and a π-phase shifted fiber Bragg grating interrogated in a random distributed feedback fiber laser are analyzed. A comparison of their sensitivities and resolutions is carried out to analyze their performance as sensors for cryogenic temperatures, taking into account their advantages and drawbacks.
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
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
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
Routes for enhanced magnetism in Ni-Mn-In metamagnetic shape memory alloys
(Elsevier, 2019) López García, Javier; Sánchez-Alarcos Gómez, Vicente; Recarte Callado, Vicente; Pérez de Landazábal Berganzo, José Ignacio; Fabelo, O.; Cesari, Eduard; Rodríguez Velamazán, José Alberto; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2; Ciencias
The authors provide in-depth physical insight into the enhancement of the magnetic properties of metamagnetic shape memory alloys produced by thermal treatment and cobalt doping. They use neutron scattering to study the atomic order and magnetic structures in the austenitic phases of Ni50Mn34In16 and Ni45Co5Mn37In13 alloys in two different states induced by thermal treatments. The increase of the magnetization in the austenite phase, particularly by cobalt doping, is explained by the enhanced ferromagnetic coupling between the magnetic moments located in octahedral sites. The spin density maps obtained from polarized neutron diffraction reveal the magnetic interaction pathways responsible for this coupling scheme.
Open Access
Magnetocaloric effect enhancement driven by intrinsic defects in a Ni45Co5Mn35Sn15 alloy
(Elsevier, 2019) Sánchez-Alarcos Gómez, Vicente; López García, Javier; Unzueta, Iraultza; Pérez de Landazábal Berganzo, José Ignacio; Recarte Callado, Vicente; Beato López, Juan Jesús; García, José Ángel; Plazaola, Fernando; Rodríguez Velamazán, José Alberto; Fisika; Institute for Advanced Materials and Mathematics - INAMAT2; Física
The influence of mechanically-induced defects on the magnetostructural properties is analyzed in a Ni-Co-Mn-Sn alloy subjected to soft milling and subsequent annealing treatments. It is found that, opposite to what occurs in Ni-Mn-Sn ternary alloys, the annealing treatment affects the magnetic properties in a different way in martensite and in austenite. In particular, the saturation magnetization significantly increases in martensite after annealing whereas just a very slight variation is observed in austenite. This leads to the interesting fact that the presence of microstructural defects, far for worsening, makes the magnetocaloric effect to be higher in the as-milled state than after annealing. This behavior is explained as the result of the combination of the effect of defects on the Mn-Mn distance, the effect of Co on the magnetic exchange coupling between Mn atoms, and the effect of defects on the vibrational entropy change at the martensitic transformation.
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
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
119Sn Mössbauer spectroscopy for assessing the local stress and defect state towards the tuning of Ni-Mn-Sn alloys
(AIP Publishing, 2017) Unzueta, Iraultza; López García, Javier; Sánchez-Alarcos Gómez, Vicente; Recarte Callado, Vicente; Pérez de Landazábal Berganzo, José Ignacio; Fisika; Institute for Advanced Materials and Mathematics - INAMAT2; Física
The influence of defects and local stresses on the magnetic properties and martensitic transformation in Ni50Mn35Sn15 is studied at macroscopic and atomic scale levels. We show that both the structural and magnetic properties of the alloy are very sensitive to slight microstructural distortions. Even though no atomic disorder is induced by milling, the antiphase boundaries linked to dislocations promote the antiferromagnetic coupling of Mn, resulting in a significant decrease in the saturation magnetization. On the other hand, the temperature range of the transformation is considerably affected by the mechanically induced local stresses, which in turn does not affect the equilibrium temperature between the austenitic and martensitic phases. Finally, we demonstrate that the recovery of the martensitic transformation is directly related to the intensity of the non-magnetic component revealed by 119Sn Mössbauer spectroscopy. This result opens the possibility of quantifying the whole contribution of defects and the local stresses on the martensitic transformation in Ni-Mn-Sn alloys.