RESUMO
A Ni2MnSn Heusler alloy was obtained as a single B2 phase after 12 h of mechanical milling. The influence of prolonged milling on the phase stability was analysed for milling times up to 50 h, related to mean crystallite size, lattice strain, and electrical resistivity. The nature of the powders in the milled range was found to be nanocrystalline, with a mean crystallite size of about 33 ± 2 nm. An evaluation of the internal stresses induced by milling was performed, a linear behaviour was found, and a coefficient of the internal stress increase with milling time was proposed. Particle size distributions of milled samples were analysed, and the morphology of the powders was visualised by scanning electron microscopy. The elemental distribution of milled samples was quantified by energy-dispersive X-ray spectroscopy. Electrical resistivity measurements were performed on compacted samples, and their behaviour with milling time was analysed.
RESUMO
Our study is focused on optimizing the synthesis conditions for the in situ oxidation of Fe particles to produce Fe@Fe3O4 core-shell powder and preparation via co-precipitation of ZnFe2O4 nanoparticles to produce Fe@Fe3O4/ZnFe2O4 soft magnetic composites (SMC) through a hybrid cold-sintering/spark plasma-sintering technique. XRD and FTIR measurements confirmed the formation of a nanocrystalline oxide layer on the surface of Fe powder and the nanosized nature of ZnFe2O4 nanoparticles. SEM-EDX investigations revealed that the oxidic phase of our composite was distributed on the surface of the Fe particles, forming a quasi-continuous matrix. The DC magnetic characteristics of the composite compact revealed a saturation induction of 0.8 T, coercivity of 590 A/m, and maximum relative permeability of 156. AC magnetic characterization indicated that for frequencies higher than 1 kHz and induction of 0.1 T, interparticle eddy current losses dominated due to ineffective electrical insulation between neighboring particles in the composite compact. Nevertheless, the magnetic characteristics obtained in both DC and AC magnetization regimes were comparable to those reported for cold-sintered Fe-based SMCs.
RESUMO
Soft magnetic composite (SMC) cores have been obtained by Spark Plasma Sintering (SPS) using pseudo core-shell powders. Pseudo core-shell powders are formed by a core of soft magnetic particle (nanocrystalline permalloy or supermalloy) surrounded by a thin layer (shell) of nanosized soft ferrite (Mn0.5Zn0.5Fe2O4). Three compositions of pseudo core-shell powders were prepared, with 1, 2 and 3 wt.% of manganese-zinc mixt ferrite. The pseudo core-shell powders were compacted by SPS at temperatures between 500 and 700 °C, with a holding time ranging from 0 to 10 min. Several techniques have been used for characterization of the samples, both, powders and compacts X-ray diffraction (XRD, scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), magnetic hysteresis measurements (DC and AC) and electrical resistivity. The electrical resistivity is in the order of 1 × 10-2 Ωm, 3-4 orders of magnitude higher than supermalloy electrical resistivity. The SPS at lower temperatures (500 °C) conserves the initial phases of the composite, but increasing the sintering temperature and/or sintering time produces a solid-state reaction between the alloy and ferrite phases, with negative consequence on the magnetic properties of the compacts. The initial relative permeability is around 40 and remains constant until to 2000 Hz. The power losses are lower than 2 W/kg until to 2000 Hz.
RESUMO
Nanocrystalline powders from the Permalloy family, Ni75Fe25, Ni79Fe16Mo5, and Ni77Fe14Cu5Mo4, were obtained by mechanical alloying starting from elemental powders. All compositions were milled for up to 24 h in a high-energy planetary ball mill. The powders were single phase and nanocrystalline as determined by X-ray diffraction studies, with larger flatted particle sizes for Ni75Fe25 (about 400 µm) and Ni77Fe14Cu5Mo4 (about 470 µm), and smaller particle sizes for Ni79Fe16Mo5 (about 170 µm). The homogeneity of the samples was verified by energy-dispersive X-ray spectroscopy (EDX). Soft magnetic composites were obtained by adding 3% of Araldite to the powders, followed by compaction at 700 MPa, and then polymerization. A very good powder covering by the polymer layer was proven by EDX elementals maps. The influence of composition change on the electrical resistivity of the compacts was studied. Hysteresis measurements in static and dynamic fields of up to 10 kHz were recorded, showing the influence of composition and particle size on the compact properties.
RESUMO
Soft magnetic composites (SMCs) need a stable matrix to apply heat treatments for enhancing their magnetic characteristics. A stable matrix can be offered by alumina, but the densification of the ferromagnetic particles covered by this oxide (by sintering) can be very difficult. This paper proposes a feasible synthesis route for obtaining alumina matrix SMCs. An Fe-Si-Al alloy with nominal composition Fe85Si9Al6 was obtained by mechanical alloying of elemental Fe, Si, and Al powders, and further, the as-milled powders were superficially oxidized by immersion in HCl solution. The oxide layer was composed of iron, silicon, and aluminum oxides, as the Fourier-transform infrared spectroscopy technique revealed. The Fe-Si-Al@oxide powder was densified by the spark plasma sintering technique-SPS. Upon sintering, a continuous matrix of oxide (mainly alumina) was formed by the reaction of the Fe-Si-Al powder coreswith their oxide layer. The main part of the composite compacts after sintering consisted of an Fe3Si-ordered phase dispersed in an oxide matrix. The DC and AC tests of magnetic composite compacts showed that upon increasing the sintering temperature, the density, magnetic induction, and magnetic permeability increased. The initial magnetic permeability was constant in the entire range of testing frequencies and the magnetic losses increased linearly. The stability of the magnetic characteristics in frequency is promising for developing further such types of magnetic composite.
RESUMO
The composite materials are used on an increasingly large scale in top fields, such as the automotive, aerospace, and nuclear industries, due to the combination of the specific properties of the composite components. Invar/WC nanocrystalline composite compacts were successfully obtained by spark plasma sintering from mechanical milled composite powder. The influence of the amount of tungsten carbide (WC) on sintering, coefficient of thermal expansion (CTE), and hardness has been investigated. The relative density and hardness of Invar/WC composite compacts increases with increasing the WC content up to 10 vol.%. At higher amount of WC (15% vol.), the relative density and hardness of the Invar/WC composite compacts decreases. The temperature up to which CTE remains at a low value (0.6-1) × 10-6 °C-1 is influenced by the WC content and decreases with the WC amount of increase.
