RESUMEN
Magnetic refrigeration (MR) is a key technique for hydrogen liquefaction. Although the MR has ideally higher performance than the conventional gas compression technique around the hydrogen liquefaction temperature, the lack of MR materials with high magnetic entropy change in a wide temperature range required for the hydrogen liquefaction is a bottle-neck for practical applications of MR cooling systems. Here, we show a series of materials with a giant magnetocaloric effect (MCE) in magnetic entropy change (-∆Sm > 0.2 J cm-3K-1) in the Er(Ho)Co2-based compounds, suitable for operation in the full temperature range required for hydrogen liquefaction (20-77 K). We also demonstrate that the giant MCE becomes reversible, enabling sustainable use of the MR materials, by eliminating the magneto-structural phase transition that leads to deterioration of the MCE. This discovery can lead to the application of Er(Ho)Co2-based alloys for the hydrogen liquefaction using MR cooling technology for the future green fuel society.
RESUMEN
Materials that possess nontrivial topology and magnetism is known to exhibit exotic quantum phenomena such as the quantum anomalous Hall effect. Here, we fabricate a novel magnetic topological heterostructure Mn4Bi2Te7/Bi2Te3 where multiple magnetic layers are inserted into the topmost quintuple layer of the original topological insulator Bi2Te3. A massive Dirac cone (DC) with a gap of 40-75 meV at 16 K is observed. By tracing the temperature evolution, this gap is shown to gradually decrease with increasing temperature and a blunt transition from a massive to a massless DC occurs around 200-250 K. Structural analysis shows that the samples also contain MnBi2Te4/Bi2Te3. Magnetic measurements show that there are two distinct Mn components in the system that corresponds to the two heterostructures; MnBi2Te4/Bi2Te3 is paramagnetic at 6 K while Mn4Bi2Te7/Bi2Te3 is ferromagnetic with a negative hysteresis (critical temperature ~20 K). This novel heterostructure is potentially important for future device applications.
RESUMEN
The distribution of Mn in a Ga(0.963)Mn(0.037)As ferromagnetic semiconductor film has been characterized by the three-dimensional atom probe (3DAP) technique. Atom probe specimens were directly prepared from the (Ga,Mn)As film grown epitaxially on a p-type GaAs substrate by the lift-out technique using a scanning electron microscope/focused ion beam system. The atom probe elemental map revealed that the Mn atoms in the Ga(0.963)Mn(0.037)As are uniformly dissolved without forming any nanometer-sized clusters.
RESUMEN
Influence of femtosecond laser pulse condition on the performance of an energy-compensated optical tomographic atom probe has been investigated. The unstable oscillator makes the mass peaks significantly broadened. Double 80fs pulse train with 10ns interval makes the mass peaks slightly shifted to the higher mass side. The mass peak shift corresponds to the fight time of ions triggered by laser pulsing. Chirping ratio for the laser pulses ranging from 80fs to 10ps is controlled by the pulse compressor for the fragile specimens such as oxide dispersion strengthen steel or insulator materials. A first-principle calculation for optical dielectric breakdown in diamond has been successfully demonstrated. It is shown that effective conductive increase has appeared at the laser intensity around 10(13)W/cm(2).
RESUMEN
We have used a first-order reflectron lens in an optical tomographic atom probe in order to improve the mass resolution. Calculations have been performed to determine the effect of second-order errors in ion energy and incidence angle on the performance of the lens. By applying a correction procedure based on the results of these calculations, we have been able to improve experimental mass resolution by 30%.
RESUMEN
In order to improve properties of functional materials, it is important to understand the relation between the structure and the properties since the structure has large effect to the properties. This can be done by using multi-scale microstructure analysis from macro-scale to nano and atomic scale. Scanning electron microscope (SEM) equipped with focused ion beam (FIB), transmission electron microscope (TEM) and 3D atom probe (3DAP) are complementary analysis tools making it possible to know the structure and the chemistry from micron to atomic resolution. SEM gives us overall microstructural and chemical information by various kinds of detectors such as secondary electron, backscattered electron, EDS and EBSD detectors. Also, it is possible to analyze 3D structure and chemistry via FIB serial sectioning. In addition, using TEM we can focus on desired region to get more complementary information from HRTEM/STEM/Lorentz images, SAED/NBD patterns and EDS/EELS to see the detail micro or nano-structure and chemistry. Especially, combination of probe Cs corrector and split EDS detectors with large detector size enable us to analyze the atomic scale elemental distribution. Furthermore, if the specimen has a complicated 3D nanostructure, or we need to analyze light elements such as hydrogen, lithium or boron, 3DAP can be used as the only technique which can visualize and analyze distribution of all constituent atoms of our materials within a few hundreds nm area. Hence, site-specific sample preparation using FIB/SEM is necessary to get desired information from region of interest. Therefore, this complementary analysis combination works very well to understand the detail of materials.In this presentation, we will show the analysis results obtained from some of functional materials by Carl Zeiss CrossBeam 1540EsB FIB/SEM, FEI Tecnai G(2) F30, Titan G2 80-200 TEMs and locally build laser assisted 3DAP. As the one of the example, result of multi-scale characterization for ultra-fine grain Nd-Fe-B permanent magnet will be shown [1]. In order to improve the magnetic properties, especially to increase the coercivity (resistance against magnetization reversal) of the magnet, decreasing the grain size and isolating each grain by non-ferromagnetic grain boundary phase are quite important since the nucleation of magnetic reversal from grain boundary phase can be suppressed and pinning force of magnetic domain wall at the grain boundary phase can be strengthened. Therefore, micro and nano structure and chemistry analysis can shed a light do grain boundary engineering.Figure 1(a,b) shows SEM BSE images of ultrafine grain Nd-Fe-B sintered magnet and the reconstructed 3D tomography of Nd-rich phases obtained by FIB/SEM serial sectioning. This data can provide us information about the distribution of Nd-rich phase and its volume fraction. Moreover, the HRTEM image from the grain boundary phase, the 3DAP maps and the concentration depth profiles are shown in Fig. 1(c,d,e). This magnet shows high coercivity (1517kA/m), and by comparing these results with the microstructures of low coercivity specimen, importance of grain boundary formation was confirmed and it gives us hint to improve the coercivity further. We will show the detail and results from other materials.jmicro;63/suppl_1/i6/DFU046F1F1DFU046F1Fig. 1.(a) SEM BSE images of ultrafine grain Nd-Fe-B sintered magnet. (b) 3D FIB/SEM tomography of Nd-rich phases. (c) HRTEM image from the grain boundary phase. (d) 3DAP maps of Nd, Cu and Al. (e) Concentration depth profiles for Fe, Nd+Pr, B, Co, Cu and Al, determined from the selected box in (d)[1].
RESUMEN
The interplay of light and magnetism allowed light to be used as a probe of magnetic materials. Now the focus has shifted to use polarized light to alter or manipulate magnetism. Here, we demonstrate optical control of ferromagnetic materials ranging from magnetic thin films to multilayers and even granular films being explored for ultra-high-density magnetic recording. Our finding shows that optical control of magnetic materials is a much more general phenomenon than previously assumed and may have a major impact on data memory and storage industries through the integration of optical control of ferromagnetic bits.
RESUMEN
The Nd-rich phases in pressless processed fine grained Nd-Fe-B sintered magnets have been characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and three dimensional atom probe tomography (3DAP). The combination of the backscattered electron (BSE) and in-lens secondary electron (IL-SE) images in SEM led to an unambiguous identification of four types of Nd-rich phases, NdOx, Ia3 type phase, which is isostructural to Nd2O3, dhcp-Nd and Nd1Fe4B4. In addition, the 3DAP analysis of thin Nd-rich grain boundary layer indicate that the coercivity has a close correlation with the chemistry of the grain boundary phase.
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We demonstrate that the atom probe analyses of metallic thin films on insulating substrates are possible using laser assisted field evaporation. The tips with metallic thin film and insulating substrate (0.6-3 µm in thickness) were prepared by the lift-out and annular ion beam milling techniques on tungsten supports. In spite of the existence of thick insulating layer between the metallic film and the tungsten support, atom probe tomography with practical mass resolution, signal-to-noise ratio and spatial resolution was found to be possible using laser assisted field evaporation.
RESUMEN
We have investigated the laser assisted field evaporation phenomena of ZnO, and MgO to explore the feasibility of quantitative three dimensional atom probe analyses of insulating oxides. To assist the field evaporation of these oxides, the usage of short wavelength 343 nm ultraviolet (UV) laser was found to be more effective than 515 nm green laser. We observed field ion microscopy (FIM) image expansion and mass peak shifting when 343 nm laser was irradiated on MgO. This phenomenon can be attributed to the laser induced electron excitation which causes the reduction of the resistivity of the specimen.
RESUMEN
The influence of laser power, wave length, and specimen temperature on laser assisted atom probe analyses for Mg alloys was investigated. Higher laser power and lower specimen temperature led to improved mass and spatial resolutions. Background noise and mass resolutions were degraded with lower laser power and higher specimen temperature. By adjusting the conditions for laser assisted atom probe analyses, atom probe results with atomic layer resolutions were obtained from all the Mg alloys so far investigated. Laser assisted atom probe investigations revealed detailed chemical information on Guinier-Preston zones in Mg alloys.
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We have investigated the irradiation conditions of femtosecond laser pulses for quantitative atom probe analyses of rare-earth (RE) doped ceria. The influence of laser wavelength, power, pulse frequency, as well as specimen temperature on mass resolution and background noise of atom probe mass spectra were investigated. Furthermore, quantitative atom probe analysis of yttrium distribution in Y-doped ceria was carried out with the optimized evaporation conditions. The distribution of yttrium was found to be uniform within the grains, but they were confirmed to be segregated at grain boundaries.
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We report a successful atom probe tomography of hydrides in hydrogenation-disproportionated Nd-Fe-B powder using a green femtosecond laser. The atom probe specimens were prepared from one particle of powder using the focused ion beam lift-out method. The atom probe tomography taken from an α-Fe/NdH(2) structure suggested that B and Ga (trace added element) were partitioned in the NdH(2) phase. The hydrogen concentration of 64 at% determined from the atom probe analysis was in excellent agreement with the stoichiometry of the NdH(2) phase.
RESUMEN
To explain the recent successful three-dimensional atom probe (3DAP) analyses of insulating oxides by laser assisted field evaporation, we investigated the mechanism of the laser-induced field evaporation of oxides by ab initio calculations. The calculated potential energy surfaces (PESs) for the ground and excited states indicated that the activation barrier height for field evaporation is substantially reduced by the accumulation of holes near the tip apex. This would make the direct electronic excitation possible to promote field evaporation along with thermal excitation. These theoretical calculations are supported by experimental observations.
RESUMEN
Laser assisted field evaporation using ultraviolet (UV) wavelength gives rise to better mass resolution and signal-to-noise ratio in atom probe mass spectra of metals, semiconductors and insulators compared to infrared and green lasers. Combined with the site specific specimen preparation techniques using the lift-out and annular Ga ion milling in a focused ion beam machine, a wide variety of materials including insulating oxides can be quantitatively analyzed by the three-dimensional atom probe using UV laser assisted field evaporation. After discussing laser irradiation conditions for optimized atom probe analyses, recent atom probe tomography results on oxides, semiconductor devices and grain boundaries of sintered magnets are presented.
RESUMEN
Fermi level tuning has been successfully demonstrated in Co-based full-Heusler alloy Co(2)FeAl(0.5)Si(0.5) (CFAS). The half-metallic band gap of CFAS was proved by the behavior of differential conductance of CFAS/(MgAl(2))O(x)/CoFe magnetic tunneling junctions with an unexplored crystalline (MgAl(2))O(x) barrier. CFAS exhibits the highest effective spin polarization (P_{eff}) at 300 K and the weakest temperature dependence of P_{eff} among all known half metals. Further study shows that P_{eff} of CFAS decays with increasing temperature (T) following T;{3/2} law perfectly, which indicates that the depolarization of CFAS is determined by spin wave excitation only.