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Water is an essential compound on earth and necessary for life. The presence of highly toxic contaminants such as arsenic and others, in many cases, represents one of the biggest problems facing the earth´s population. Treatment of contaminated water with magnetite (Fe

P-type and n-type metal oxide semiconductors are widely used in the manufacture of gas sensing materials, due to their excellent electronic, electrical and electrocatalytic properties. Hematite (

P-type and n-type metal oxide semiconductors are widely used in the manufacture of gas sensing materials, due to their excellent electronic, electrical and electrocatalytic properties. Hematite (α-Fe2O3) compound has been reported as a promising material for sensing broad types of gases, due to its affordability, good stability and semiconducting properties. In the present work, the efficient and easy-to-implement sol-gel method has been used to synthesize α-Fe2O3 nanoparticles (NPs). The TGA-DSC characterizations of the precursor gel provided information about the phase transformation temperature and the mass percentage of the hematite NPs. X-ray diffraction, transmission electron microscopy and x-ray photoelectron spectroscopy data analyses indicated the formation of two iron oxide phases (hematite and magnetite) when the NPs are subjected to thermal treatment at 400 °C. Meanwhile, only the hematite phase was determined for thermal annealing above 500 °C up to 800 °C. Besides, the crystallite size shows an increasing trend with the thermal annealing and no defined morphology. A clear reduction of surface defects, associated with oxygen vacancies was also evidenced when the annealing temperature was increased, resulting in changes on the electrical properties of hematite NPs. Resistive gas-sensing tests were carried out using hematite NPs + glycerin paste, to detect quaternary ammonium compounds. Room-temperature high sensitivity values (Sr ∼ 4) have been obtained during the detection of ∼1 mM quaternary ammonium compounds vapor. The dependence of the sensitivity on the particle size, the mass ratio of NPs with respect to the organic ligand, changes in the dielectric properties, and the electrical conduction mechanism of gas sensing was discussed., This research work was carried out with the financial support provided by CONCYTEC-PROCIENCIA within the framework of the call E038-01 [Contract N°07-2019-FONDECYT-BM-INC.INV]. JAHC wants to thank the Brazilian agencies CNPq (Grants number 443652/2018–0, 303182/2020–2) and FAPDF (grant number 00193.0000151/2019–20) for the financial support.

Nanosized nickel ferrite (NiFe2O4) is successfully synthesized by the sol-gel method using citric acid (C6H8O7) as fuel. The X-ray diffraction pattern of the as-synthesized sample shows formation of NiFe2O4 nanoparticles (NPs) as the main phase, with mean crystalline size ∼50 nm. While transmission electron microscopy (TEM) reveals nearly spherical morphology with mean particle diameter of 41 ± 5 nm, high-resolution TEM shows inter-planar distance (2.55 A) corresponding to the (1 1 3) plane of the spinel structure. Additionally, the Raman spectrum exhibits five Raman active modes (two A1g at 575 cm−1 and 710 cm−1; two Eg at 345 cm−1 and 670 cm−1; and one T2g at 497 cm−1) typical of NiFe2O4. X-band magnetic resonance (MR) data reveal a single broad resonance line in the whole temperature range (3.8 K ≤ T ≤ 300 K), with g-value decreasing monotonically from 3.10 ± 0.01 at 3.8 K to 2.77 ± 0.01 at 300 K. The temperature dependence of both resonance field and resonance linewidth show a remarkable change in the range of 60–70 K, herein credited to surface spin-glass behavior. The model picture used to explain the MR data assumes NPs with a core-shell structure. Below about 60–70 K the shell’s spin system progressively reveals a paramagnetic to spin-glass-like transition upon cooling, with a freezing temperature estimated at 2.1 ± 0.1 K. However, above about 60–70 K spins in the paramagnetic shell align along the NP’s core dipolar field, resulting in an effective enlarged nanoparticle size.

We describe a simple method for the preparation of gold-decorated silica (SiO₂) nanoparticles (NPs) by the in situ precipitation method using simple BH₄⁻ ions reduction as a procedure, where BH₄⁻ ions are adsorbed onto PEI-functionalized SiO₂ NPs for stabilizing and reducing gold ions onto PEI-SiO₂ surface in water under ambient conditions. The result was 3-nm gold nanoshell NPs attached to SiO₂ core (~ 75 nm) with a surface plasmon resonance (SPR) at ~ 680 nm. SPR band is associated with Au NP aggregates that arise from strong interparticle interaction. This is an alternative to the gold-seeding methods and the use of anionic gold species for the obtention of gold-decorated SiO₂ NPs with an important red-shift in UV–Vis absorption and with potential applications in biosensors and photothermal therapy., Facultad de Ciencias Exactas, Instituto de Investigaciones Fisicoquímicas Teóricas y Aplicadas

Magnetic nanoparticles (NPs) are especially interesting for several biomedical applications due to their chemical surface, especially for targeted cancer imaging and therapeutics. In order to realize these applications, it is important to know their magnetic properties among other complementary properties that help to improve the understanding of the synthesis process. In this work, we report the magnetic properties of polyethyleneimine-coated magnetite (PEI-Fe3O4) NPs synthesized by a one-step method via the co-precipitation method and using PEI as a stabilizer. Transmission electron microscopy (TEM) images revealed agglomerated magnetic nanoparticles with an average size of ∼10 nm; meanwhile, the X-ray diffraction (DRX) analysis confirmed a pure magnetite phase. The study of magnetic properties shows a superparamagnetic system with coexistence of non-interacting single NPs with a low blocking temperature (∼35 K) and interacting NPs in the aggregates with a higher blocking temperature (>150 K), in which the interparticle interactions of magnetic cores dominate over surface spin disorder. The interaction between the surface spin-disorder layer and NP core was found to be weak, related to a weak exchange bias effect. A maximum specific loss power (SLP) value of 70 W g−1 was obtained (f = 571 kHz and H = 23.87 kA m−1) indicating that the magnetic response plays a crucial role in determining the heating efficiency for future applications.

This study reports on the synthesis and characterization of oleic acid (OA)-coated Fe3O4 nanoparticles (Fe3O4@OA) and AO plus essential oil (EO)-coated Fe3O4 nanoparticles (Fe3O4@OA/EO). The EO was extracted from Croton cajucara Benth (CCB) leaves; a plant from the Brazilian Amazon region. Structural and morphological characterizations were carried out using X-ray diffraction (XRD) and transmission electron microscopy (TEM) images, respectively. Additionally, thermogravimetric analysis and magnetization measurements (hysteresis cycle, zero field-cooled-ZFC, field-cooled-FC, and AC susceptibility) were used to assess thermal and magnetic properties of the as-fabricated samples. Rietveld refinement of XRD pattern confirmed the formation of magnetite phase with no extra phases, whereas TEM images revealed spherically-shaped nanoparticles in the Fe3O4@OA and (Fe3O4@OA/EO) samples with a mean physical size of 8.5 nm and 10.1 nm, respectively. ZFC and FC curves revealed the occurrence of blocked/frozen state below the maximum peak (Tmax) at ∼81 K and ∼40 K for the Fe3O4@OA and (Fe3O4@OA/EO) samples, respectively. Moreover, low-temperature AC susceptibility vs. T curves recorded in the range of 0.2–1000 Hz showed that the OA coating of the Fe3O4 nanoparticles leads to a spin-glass-like behavior credited to the strong particle-particle interactions; meanwhile, the double layer (AO + EO) coating of the Fe3O4 nanoparticles remarkably quenches the particle-particle interaction leading to a superparamagnetic-like behavior.

NiFe2O4 nanocrystalline samples were synthesized by the sol-gel method. The X-ray diffraction patterns of the as-synthesized samples (S- NiFe2O4) showed the formation of main spinel ferrite structure, with an average crystalline size of ∼50 nm. After a washing process with magnetic separation two sets of NiFe2O4 particles was observed, one with ∼36 nm and other with very small size (∼2–3 nm). X-ray photoelectron spectroscopy (XPS) indicated the presence of Fe3+ and Ni2+ ions on the sample surface. Mossbauer spectra were recorded at 77 K and room temperature and were least square fitted for two sextets which have been assigned to the iron ions occupying the two symmetry sites of the ferrite structure. Magnetic measurements are consistent with the magnetic moment of Ni2+ ions suggesting the formation of an ideal inverse spinel structure in the sample S-NiFe2O4. Moreover, after the washing process with magnetic separation (sample P- NiFe2O4), when the formation of extremely small particles was determined, the Mossbauer and magnetic measurements indicated the reorganization of Ni2+/Fe3+ ions in the tetragonal and octahedral sites of the spinel structure and some features related to thermal relaxations of the small particles are determined.

Surface coating magnetic nanoparticles can be realized using organic moieties, such as essential oil (EO) extracted from Croton cajucara Benth leaves, a common plant from the Brazilian Amazon region successfully used for infusion in popular medicine. Although, there are reports in the literature indicating the protective and healing actions of the EO on gastric lesions, the inclusion of the magnetic core to control (targeting and retaining) the MNPs in specific sites can improve the performance of the EO molecules for the treatment of gastric disorders. Therefore, in this work, we report on fabrication and characterization of surface-coated magnetite nanoparticles (MNPs), aiming thermal-assisted site delivering EO. Firstly, oleic acid (OA) coated MNPs (sample M1) were fabricated using a thermal decomposition route. Secondly, the OA-coated MNPs were dressed with EO (sample M2). Meanwhile, x-ray diffraction and transmission electron microscopy data confirmed formation of spherically-shaped magnetite core while successful single OA coating and double OA + EO coating of MNPs was confirmed by infrared spectroscopy and thermogravimetric analysis (TGA). TGA results indicated release of the EO at ∼50 °C, whereas the OA is released only above ∼380 °C. Blocking (TB) and irreversible (TIRR) temperatures of samples M1 (TB = 210 K; TIRR = 210 K) and M2 (TB = 35 K; TIRR = 215 K) were assessed from magnetic measurements data analysis. In sample M2, the difference TB-TIRR (180 K) was related to inhomogeneous partial shifting of OA molecules by EO molecules whereas the remarkable reduction of MS with respect to sample M1 was assigned to a dead surface layer dominated by ferrous ions in low-spin state. Moreover, the lower TB value we have found in sample M2 (∼35 K) indicates negligible particle-particle interactions due to the successful double coating (OA plus EO) of the MNPs, in contrast to that obtained in sample M1. In sample M2 weakening of particle-particle interaction warrants superparamagnetic properties which can be used to obtain magnetic resonance image and for guiding the MNPs to targeting sites using gradients of external magnetic field. Therefore, the combination of the improved magnetic properties plus the detachment of EO at ∼50 °C (while keeping stable the OA coating) via magnetohyperthermia makes the double coated system (sample M2) a very promising candidate for site delivering of EO to treat gastrointestinal disorders.

In this work, we characterize the hollow hematite (α-Fe2O3) micro spheres obtained by two non-template techniques: i) sol gel and ii) spray roasting process. Both techniques allow the production of high yield hollow hematite spheres up to 100 g for the case of sol gel and up to 500 kg for the case of spray roaster process. The samples were characterized by X-ray diffraction, scanning electron microscopy and Mössbauer spectroscopy. The results indicate nearly uniform hollow spheres with diameters of around 1–1.5 μm and consisting of polycrystalline hematite. The Mӧssbauer spectroscopy reveals the signal change of quadrupole shift values evidencing the occurrence of the Morin transition and that the samples show an antiferromagnetic order at 77 K as in bulk hematite. The Morin temperature (TM) for both samples was obtained from the measurements of the magnetic moments as a function of the temperature in zero field cooling (ZFC) and field cooling (FC) modes. The values of TM for both samples are lower than that reported for bulk hematite (TM(bulk) = 263 K). Remarkably, the ZFC and FC loops do not overlap in both samples, revealing irreversible Morin transition. However, the sample obtained by sol gel presents thermal hysteresis with TM values of 260 K (in ZFC) and 248 K (FC). Whereas, the sample obtained by spray roaster process presents complete irreversibility and TM values of 252 K (in ZFC) and 242 K (in FC). Keywords: Hollow spheres, Hematite, Morin transition, Thermal hysteresis

The integration of noble metal and magnetic nanoparticles with controlled structures that can couple various specific effects to the different nanocomposite in multifunctional nanosystems have been found interesting in the field of medicine. In this work, we show synthesis route to prepare small Au nanoparticles of sizes = 3.9 ± 0.2 nm attached to Fe 3 O 4 nanoparticle cores ( = 49.2 ± 3.5 nm) in aqueous medium for potential application as a nano-heater. Remarkably, the resulted Au decorated PEI-Fe 3 O 4 (Au@PEI-Fe 3 O 4 ) nanoparticles are able to retain bulk magnetic moment M S = 82–84 Am 2 /kg Fe3O4 , with the Verwey transition observed at T V = 98 K. In addition, the in vitro cytotoxicity analysis of the nanosystem microglial BV2 cells showed high viability (>97.5%) to concentrate up to 100 µg/mL in comparison to the control samples. In vitro heating experiments on microglial BV2 cells under an ac magnetic field (H 0 = 23.87 kA/m; f = 571 kHz) yielded specific power absorption (SPA) values of SPA = 43 ± 3 and 49 ± 1 μW/cell for PEI-Fe 3 O 4 and Au@PEI-Fe 3 O 4 NPs, respectively. These similar intracellular SPA values imply that functionalization of the magnetic particles with Au did not change the heating efficiency, providing at the same time a more flexible platform for multifunctional functionalization. Fil: León Félix, L.. Universidade do Brasília; Brasil. Universidad de Zaragoza; España Fil: Sanz, B.. Nb Nanoscale Biomagnetics S.l.; España Fil: Sebastián, V.. Universidad de Zaragoza; España. Centro de Investigación en Red en Bioingeniería; España Fil: Torres Molina, Teobaldo Enrique. Universidad de Zaragoza; España. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Patagonia Norte; Argentina Fil: Sousa, Marcelo Henrique. Universidade do Brasília; Brasil Fil: Coaquira, J. A. H.. Universidade do Brasília; Brasil Fil: Ibarra, M.R.. Universidad de Zaragoza; España Fil: Goya, Gerardo Fabian. Universidad de Zaragoza; España

Magnetite (Fe3O4) nanoparticles coated with organic material are of considerable importance in various areas of engineering, as well as in biomedicine. Several papers show drastic changes in the magnetic properties related to the surface effects and the particle-particle interactions strength. However, there is no consensus about the origin or mechanisms that produce these changes, which could be different depending on the particle size and shape, coating efficiency and particle-particle interaction strength. Aiming to shed light on these issues, oleic acid (OA) coated Fe3O4 nanoparticles with different sizes were synthesized by a thermal decomposition method. Structural and microscopic results revealed Fe3O4 nanoparticles with good crystallinity and almost-spherical or polyhedral shapes depending on the solvent used for the synthesis. Infrared (FTIR) spectroscopy indicated OA molecules attached to the surface of Fe3O4 NPs via bidentate (chelating and/or bridging) bonds; meanwhile, thermogravimetric analysis confirmed the presence of weakly and strongly bonded OA molecules, suggesting a successful coating of Fe3O4 NPs. Magnetization (M) vs. magnetic field (H) curves are consistent with a core/shell structure formed by magnetite/defective magnetite (maghemite) phases, in consistency with FTIR spectroscopy. It was determined lower saturation magnetization values than that expected for bulk magnetite, which was assigned to the likely presence of a fraction of iron ions in low-spin (LS) states in the defective magnetite (maghemite) layer at the particles surface. The magnetic results evidence that depending on the amount of OA coating, it is possible to tune the particle-particle separation distance, avoid particles agglomeration and particle-particle interactions. The temperature dependence of magnetization reveals the presence of non-interacting and interacting NPs. Meanwhile, AC magnetic susceptibility measurements are consistent with those results and provide features related to superparamagnetic (SPM) behavior, assigned to the non-interacting NPs, and interacting SPM behavior, assigned to the interacting NPs, whose interaction strength is not enough to lead to a spin-glass like behavior.

We report the fabrication and characterization of copper microelectrodes obtained by a homemade lithography technique and after gold electroless deposition. For the fabrication, planes consisting of arrays of electrodes (black in color) with bow tie shape were designed and printed on a transparent paper (Canson ltd.). Using an embroidery frame with a silk fabric, a photographic emulsion was spread on the silk and simultaneously pressing the Canson paper on it. The system was introduced into a closed box and exposed with a UV light. The designed electrode templates prevented direct exposition of the UV light over copper films and indelible ink was spread over it. After the ink was dried, the copper film is immersed into ferric acid to attack the uncovered copper parts (where there is no ink). In this way, we obtained copper electrodes with initial gap separation of ~142μm and subsequently, they followed electroless deposition of gold to make the copper electrodes to contact. For the characterization, electrical measurements were performed. They present ohmic resistance values in the order of 106 Ω produced by surface scattering of the electrons within the gold microwire and enhanced by oxidation of the copper electrodes.

In this work we report the formation of hollow α-Fe2O3 (hematite) microspheres by the gas-bubble template method. This technique is simple and it does not require hard templates, surfactants, special conditions of atmosphere or complex steps. After reacting Fe(NO3)3.9H2O and citric acid in water by sol–gel, the precursor was annealed in air at different temperatures between 180 and 600 °C. Annealing at 550 and 600 °C generates bubbles on the melt which crystallize and oxidizes to form hematite hollow spheres after quenching. The morphology and crystal evolution are studied by means of X-ray diffraction and scanning electron microscopy. We found that after annealing at 250–400 °C, the sample consist of a mixture of magnetite, maghemite and hematite. Single hematite phase in the form of hollow microspheres is obtained after annealing at 550 and 600 °C. The crystallization and crystal size of the hematite shells increase with annealing temperature. A possible mechanism for hollow sphere formation is presented.

The structural and hyperfine properties of bulk TiFe0.5Ni0.5 intermetallic and ball-milled TiFe0.5Ni0.5/graphite compounds and their hydrides have been studied. The bulk and nanostructured TiFe0.5Ni0.5 compounds crystallize in the cubic crystal structure of CsCl (B2). After hydrogenation, the formation of hydrogen-poor phase (∝-phase) and hydride phase (β-phase) have been determined for the bulk compound. However, the formation of the ∝-phase and the hydrogen-richest phase (γ-phase) and other secondary phases have been determined for the ball-milled TiFe0.5Ni0.5/graphite sample. It has been determined that the ball-milled TiFe0.5Ni0.5/graphite sample presents a large amount of the γ-phase which indicates that the presence of graphite nearby nanostructured intermetallic grains enhances the absorption of hydrogen. Mossbauer results are consistent with the structural results. Meanwhile, no significant changes in the isomer shift (IS) value has been determined for the α-phase with respect to the intermetallic compound, a strong increase in the IS value has been determined for the β- and γ-phases with respect to the ∝-phase. That increase indicates a decrease of the s-electron density at the Fe nuclei due to the charge transfer from the metal to the nearby hydrogen atoms.

We present a systematic study of core-shell Au/Fe_3O_4 nanoparticles produced by thermal decomposition under mild conditions. The morphology and crystal structure of the nanoparticles revealed the presence of Au core of = (6.9\pm 1.0) nm surrounded by Fe_3O_4 shell with a thickness of ~3.5 nm, epitaxially grown onto the Au core surface. The Au/Fe_3O_4 core-shell structure was demonstrated by high angle annular dark field scanning transmission electron microscopy analysis. The magnetite shell grown on top of the Au nanoparticle displayed a thermal blocking state at temperatures below T_B = 59 K and a relaxed state well above T_B. Remarkably, an exchange bias effect was observed when cooling down the samples below room temperature under an external magnetic field. Moreover, the exchange bias field (H_{EX}) started to appear at T~40 K and its value increased by decreasing the temperature. This effect has been assigned to the interaction of spins located in the magnetically disordered regions (in the inner and outer surface of the Fe_3O_4 shell) and spins located in the ordered region of the Fe_3O_4 shell., Comment: 12 pages, 4 figures

Structural and magnetic studies of monophasic maghemite (γ-Fe2O3) magnetic nanocrystallites (MNCs) synthesized by the co-precipitation chemical route are reported in this paper. For the synthesis, a starting precursor of magnetite (Fe3O4) in basic medium was oxidized at room temperature by adjusting the pH = 3.5 at 80°C in an acidic medium without surfactants. X-ray diffraction (XRD) pattern shows widened peaks indicating nanometric size and Rietveld Refinement confirms only one single-phase assigned to γ-Fe2O3 MNCs. High Resolution Transmission Electron Microscopy (HR-TEM) demonstrates the formation of nanoparticles with diameter around D ≈ 6.8 ± 0.1 nm which is in good agreement with Rietveld Refinement (6.4 ± 1 nm). A selected area electron diffraction pattern was carried out to complement the study of the crystalline structure of the γ-Fe2O3 MNCs. M(H) measurements taken at different temperatures show almost zero coercivity and remanence indicating superparamagnetic domain and high magnetic saturation.

We report on the synthesis and characterization of uncoated and gold coated magnetite nanoparticles. Structural characterizations, carried out using X-ray diffraction, confirm the formation of magnetite phase with a mean size of ~7 and ~8 nm for the uncoated and gold covered magnetite nanoparticles, respectively. The value of the gold coated Fe3O4 nanoparticles is consistent with the mean physical size determined from transmission electron microscopy images. Mossbauer spectra at room temperature are consistent with the thermal relaxation of magnetic moments mediated by particle-particle interactions. The 77 K Mossbauer spectra are modeled with four sextets. Those sextets are assigned to the signal of iron ions occupying the tetrahedral and octahedral sites in the core and shell parts of the particle. The room-temperature saturation magnetization value determined for the uncoated Fe3O4 nanoparticles is roughly ~60 emu/g and suggests the occurrence of surface effects such as magnetic disorder or the partial surface oxidation. These surface effects are reduced in the gold-coated Fe3O4 nanoparticles. Zero-field–cooled and field-cooled curves of both samples show irreversibilities which are consistent with a superparamagnetic behavior of interacting nanoparticles.

In this work we present the study of hematite (α-Fe2O3) nanostructures synthesized by the ball milling technique. The structural characterization and the crystallite size estimation have been carried out using the X-ray diffraction (XRD) technique. Data analyses indicate that the hematite phase (space group, R-3C) is preserved after the milling process. As the milling time is increased, a second phase (α-Fe) appears. The mean crystallite size shows a decreasing tendency as the milling time is increased. High-resolution transmission electron microscopy (HRTEM) images show the formation of grains composed of crystallites with irregular shapes. Mossbauer spectra of milled powders carried out at 297 and 77 K are well modeled with a histogram distribution of hyperfine fields. The presence of one additional sextet which corresponds to the ∝-Fe phase is also determined in agreement with XRD data analysis. Magnetic measurements suggest the suppression of the Morin transition in the milled samples and the absence of thermal relaxation effects in agreement with the Mossbauer spectroscopy results.

Due to the current necessity to obtain epitaxial superconductor films at low cost, we report the growth of YBa2Cu3O7 (Y123) films by chemical deposition. The procedure involved simple steps such as precipitation of stoichiometric amounts of yttrium, barium and copper acetates in oxalic acid (H2C2O4). The precursor solution was dripped onto LaAlO3 (100) substrates with the help of a Fisher pipette. The films were annealed in oxygen atmosphere during 12 h at three different temperatures: 820 °C, 840 °C and 860 °C. After 820 °C and 860 °C annealing, X-ray diffraction (XRD) analysis revealed high intensity of the ( 00l ) reflections denoting that most of the Y123 grains were c-axis oriented. In addition, we also observed a-axis oriented grains (( h00 ) reflexion), minor randomly oriented grains and other phases (such as Y2BaCuO5 and CuO). In contrast, the sample treated at 840 °C, we noticed c – and a-axis oriented grains, very small amounts of randomly oriented grains without formation of other phases. From the magnetization versus temperature measurements, the critical temperatures were estimated at 70K and 90K for the samples annealed at 820 °C and 860 °C respectively.

En este trabajo se estudia la morfología y cristalización de la superficie de películas delgadas de Cu (expuestos al medio ambiente) sobre sustratos de SiO2/Si. Las muestras fueron sometidas a tratamientos térmicos mediante el uso de un horno tubular, en un rango de temperaturas comprendidas entre 250ºC y 1000ºC durante 3 horas para luego ser enfriadas a razón de 1.4ºC/min. La cristalización de las muestras luego de los tratamientos térmicos fueron caracterizadas mediante difracción de Rayos X (DRX), mientras que la morfología de la superficie se analizo usando Microscopia Electrónica de Barrido (MEB). Los resultados obtenidos fueron analizados y encontramos que la temperatura de recocido mas optima que mejor la dirección (111) en la pelicula de cobre y que permite conocer la dinámica de los átomos de la superficie del sistema Cu/SiO2 con respecto a la temperatura, está comprendida en el rango de 400 y 500ºC. Durante todo el proceso de recocido las superficies de las muestras se oxidan y notamos la presencia de siliciuros de cobre

We report the fabrication of nickel nanospaced electrodes by electroplating and electromigration for nanoelectronic devices. Using a conventional electrochemical cell, nanogaps can be obtained by controlling the plating time alone and after a careful optimization of electrodeposition parameters such as electrolyte bath, applied potential, cleaning, etc. During the process, the gap width decreases exponentially with time until the electrode gaps are completely bridged. Once the bridge is formed, the ex situ electromigration technique can reopen the nanogap. When the gap is ∼1 nm, tunneling current–voltage characterization shows asymmetry which can be corrected by an external magnetic field. This suggests that charge transfer in the nickel electrodes depends on the orientation of magnetic moments. (Some figures in this article are in colour only in the electronic version)