RESUMEN
Scientific interest in iron-oxides and in particular magnetite has been renewed due to the broad scope of their fascinating properties, which are finding applications in electronics and biomedicine. Specifically, iron oxide nanoparticles (IONPs) are gathering attraction in biomedicine. Their cores are usually constituted by a mixture of maghemite and magnetite phases. In view of this, to fine-tune the properties of an ensemble of IONPs towards their applications, it is essential to enhance mass fabrication processes towards the production of monodisperse IONPs with controlled size, shape, and stoichiometry. We exploit the vacancy sensitivity of the Verwey transition to detect the presence of magnetite. Here we provide direct evidence for the Verwey transition in an ensemble of IONPs through neutron diffraction. This transition is observed as a variation in the Fe magnetic moment at octahedral sites and, in turn, gives rise to a change of the net magnetic moment. Finally, we show this variation as the microscopic ingredient driving the characteristic kink that hallmarks the Verwey transition in thermal variation of magnetization.
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A series of GdCu 2 nanoparticles with controlled sizes ranging from 7 nm to 40 nm has been produced via high-energy inert-gas ball milling. Rietveld refinements on the X-ray diffraction measurements ensure that the bulk crystalline I m m a structure is retained within the nanoparticles, thanks to the employed low milling times ranging from t = 0.5 to t = 5 h. The analysis of the magnetic measurements shows a crossover from Superantiferromagnetism (SAF) to a Super Spin Glass state as the size decreases at NP size of ã D ã ≈ 18 nm. The microstrain contribution, which is always kept below 1%, together with the increasing surface-to-core ratio of the magnetic moments, trigger the magnetic disorder. Additionally, an extra contribution to the magnetic disorder is revealed within the SAF state, as the oscillating RKKY indirect exchange achieves to couple with the aforementioned contribution that emerges from the size reduction. The combination of both sources of disorder leads to a maximised frustration for ã D ã ≈ 25 nm sized NPs.
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Clustering of magnetic nanoparticles can drastically change their collective magnetic properties, which in turn may influence their performance in technological or biomedical applications. Here, we investigate a commercial colloidal dispersion (FeraSpinTMR), which contains dense clusters of iron oxide cores (mean size around 9 nm according to neutron diffraction) with varying cluster size (about 18-56 nm according to small angle x-ray diffraction), and its individual size fractions (FeraSpinTMXS, S, M, L, XL, XXL). The magnetic properties of the colloids were characterized by isothermal magnetization, as well as frequency-dependent optomagnetic and AC susceptibility measurements. From these measurements we derive the underlying moment and relaxation frequency distributions, respectively. Analysis of the distributions shows that the clustering of the initially superparamagnetic cores leads to remanent magnetic moments within the large clusters. At frequencies below 105 rad s-1, the relaxation of the clusters is dominated by Brownian (rotation) relaxation. At higher frequencies, where Brownian relaxation is inhibited due to viscous friction, the clusters still show an appreciable magnetic relaxation due to internal moment relaxation within the clusters. As a result of the internal moment relaxation, the colloids with the large clusters (FS-L, XL, XXL) excel in magnetic hyperthermia experiments.
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A change in the Kondo lattice behavior of bulk YbAl3 has been observed when the alloy is shaped into nanoparticles (≈12 nm). Measurements of the electrical resistivity show inhibited coherence effects and deviation from the standard Fermi liquid behavior (T 2-dependence). These results are interpreted as being due to the effect of the disruption of the periodicity of the array of Kondo ions provoked by the size reduction process. Additionally, the ensemble of randomly placed nanoparticles also triggers an extra source of electronic scattering at very low temperatures (≈15 K) due to quantum interference effects.
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The structural state and static and dynamic magnetic properties of TbCu2 nanoparticles are reported to be produced by mechanical milling under inert atmosphere. The randomly dispersed nanoparticles as detected by TEM retain the bulk symmetry with an orthorhombic Imma lattice and Tb and Cu in the 4e and 8h positions, respectively. Rietveld refinements confirm that the milling produces a controlled reduction of particle sizes reaching ≃6 nm and an increase of the microstrain up to ≃0.6%. The electrical resistivity indicates a metallic behavior and the presence of a magnetic contribution to the electronic scattering which decreases with milling times. The dc-susceptibility shows a reduction of the Néel transition (from 49 K to 43 K) and a progressive increase of a peak (from 9 K to 15 K) in the zero-field-cooled magnetization with size reduction. The exchange anisotropy is very weak (a bias field of ≃30 Oe) and is due to the presence of a disordered (thin) shell coupled to the antiferromagnetic core. The dynamic susceptibility evidences a critical slowing down in the spin-disordered state for the lowest temperature peak associated with a spin glass-like freezing with a tendency of zv and ß exponents to increase when the size becomes 6 nm (zv ≃ 6.6 and ß ≃ 0.85). A Rietveld analysis of the neutron diffraction patterns 1.8 ≤ T ≤ 60 K, including the magnetic structure determination, reveals that there is a reduction of the expected moment (≃80%), which must be connected to the presence of the disordered particle shell. The core magnetic structure retains the bulk antiferromagnetic arrangement. The overall interpretation is based on a superantiferromagnetic behavior which at low temperatures coexists with a canting of surface moments and a mismatch of the antiferromagnetic sublattices of the nanoparticles. We propose a novel magnetic phase diagram where changes are provoked by a combination of the decrease of size and the increase of microstrain.
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We report the revisited magnetic phase diagram for the Kondo (ferromagnetic and antiferromagnetic) CeNi1−xCux series based on acdc magnetization, heat capacity, neutron diffraction and muon spectroscopy down to very low temperatures (~100 mK). An evolution from antiferromagnetism, observed for Cu-rich alloys (0.8 ≤ x ≤ 1), to clustered-ferromagnetism, seen for samples with 0.3 ≤ x ≤ 0.6, and then to spin-glass for 0.1 ≤ x ≤ 0.2, has been observed. The clustered-ferromagnetic phase emerges from a cluster-glass state without any indication of Curie temperature. For the samples adjacent to the magneticnonmagnetic crossover 0.1 ≤ x ≤ 0.2, only the cluster-glass state is observed due to the weakening of the RKKY interactions. We discuss the emerging phenomena taking into account the cluster-percolative scenario proposed for this series and the role of the interactions involved along the whole series. The proximity to a T = 0 K spin-glass quantum phase transition in the phase diagram is discussed.
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We present evidence for the existence of magnetic clusters of approximately 20 A in the strongly correlated alloy system CeNi 1-x Cux (0.7
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The study of the magnetic properties depending upon mechanical milling of the ferromagnetic polycrystalline TbAl(2) material is reported. Rietveld analysis of the x-ray diffraction data reveals a decrease in the grain size down to 14 nm and a -0.15% variation in the lattice parameter, after 300 h of milling time. Irreversibility in the zero field cooled-field cooled (ZFC-FC) dc susceptibility and clear peaks in the ac susceptibility between 5 and 300 K show that the long-range ferromagnetic structure is inhibited in favour of a disordered spin arrangement below 45 K. This glassy behaviour is also deduced from the variation of the irreversibility transition with the field (H(2/3)) and frequency. The magnetization process of the bulk TbAl(2) is governed by domain-wall thermal activation processes. In contrast, in the milled samples, cluster-glass properties arise as a result of cooperative interactions due to the substitutional disorder. The interactions are also influenced by the nanograin structure of the milled alloys, showing a variation in coercivity with the grain size, below the crossover between the multi- and single-domain behaviours.
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We study the magnetic ground state in La(2/3)Ca(1/3)Mn(1-x)Ga x O3 manganites, where a quantum critical point (QCP) has been theoretically predicted. The metallic ferromagnetic ground state for low Ga doping breaks down for x > or = 0.11, an insulating state being established at low temperatures. Long-range ferromagnetism coexists with short-range magnetic correlations in the concentration range 0.11 < or = x < or = 0.145 while only the short-range correlations survive for x > or = 0.16. We discuss the implications of such a QCP to the physics of manganites and compare to other QCP systems.
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The lateral coherence length is of the order of 100 micron at the 'long' (145 m) ID19 beamline of the ESRF, which is mainly devoted to imaging. Most of the optical elements located along the X-ray path can thus act as ;phase objects', and lead to spurious contrast and/or to coherence degradation, which shows up as an enhanced effective angular size of the source. Both the spurious contrast and the coherence degradation are detrimental for the images (diffraction topographs, tomographs, phase-contrast images) produced at this beamline. The problems identified and the way they were solved during the commissioning of ID19 are reported. More particularly, the role of the protection foils located in the front end, the beryllium windows, the filters and the monochromator defects (scratches, dust, small vibrations) is discussed.
