Preparation of Fe@Fe3O4/ZnFe2O4 Powders and Their Consolidation via Hybrid Cold-Sintering/Spark Plasma-Sintering.

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.

Producing Soft Magnetic Composites by Spark Plasma Sintering of Pseudo Core-Shell Ni-Fe Alloy@Mn0.5Zn0.5Fe2O4 Powders.

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.

Structural, Microstructural and Compositional Changes of the AISI 314 Steel Used in the Sintering Furnace Belt Depending on the Operating Time.

The damage due to embrittlement of the sintering furnace belt and its replacement after a certain time of use represents a problem for the manufacturers of sintered parts. Finding out the reason for the damage could help to increase the duration of its operation. This research aimed to investigate the causes of embrittlement, considering both the temperatures and atmosphere of the sintering furnace to which the furnace belt is exposed during its operation. The furnace belt was made of AISI 314 stainless steel. Optical microscopy, scanning electron microscopy, combined with energy-dispersive X-ray analysis, X-ray diffraction and the Vickers hardness tests were used to analyze the microstructural, structural, compositional and hardness changes of the belt used for 45 weeks. Cr and Mn carbides, the oxides of Fe, Cr, Mn and Si were found to form at the edge of the furnace belt. The grains grew after 45 weeks of use, approximately 10 times, due to thermal cycles in an endothermic gas atmosphere to which the belt was exposed. Also, the hardness increased from 226 to 338 HV0.05, due to the formation of carbide and oxide-type compounds. All these results represent a starting point in optimizing the lifetime of the sintering furnace belt.

Morphological Analyses of W/Cu Functional Graded Materials Obtained by Conventional and Spark Plasma Sintering.

The paper presents the analysis of two compaction methods for obtaining W/Cu Functional Graded Materials (FGMs) consisting of three layers with the following compositions (% weight): first layer 80 W/20 Cu, second layer 75 W/25 Cu, and third layer 65 W/35 Cu. Each layer composition was obtained using powders obtained through mechanical milling. The two compaction methods were Spark Plasma Sintering (SPS) and Conventional Sintering (CS). The samples obtained after the SPS and CS were investigated from morphological (scanning electron microscopy-SEM) and compositional (energy dispersive X-ray spectroscopy-EDX) points of views. Additionally, the porosities and the densities of each layer in both cases were studied. It was found that the densities of the sample's layers obtained through SPS are superior to those obtained through CS. The research emphasizes that, from a morphological point of view, the SPS process is recommended for W/Cu-FGMs, having raw materials as fine-graded powders against the CS process.

Spark Plasma Sintered Soft Magnetic Composite Based on Fe-Si-Al Surface Oxidized Powders.

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.

Structural, Chemical and Magnetic Characterization of Quartz Sand from Cluj Area, Romania for Future Beneficiation in the Glass Industry.

For use in crystal glass production, quartz sand must contain less than 0.09% iron. If the sand contains more than 0.09% Fe, the iron must be removed. In the present study, quartz sand from tailings ponds near the Cluj area of Romania is analyzed for potential use in the glass industry, after magnetic separation. The particle size distribution of raw sand was determined, and mineralogical analyses was realized. Using scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX), morphology and elemental distribution maps on the particle was performed. The evolution of the iron content versus the particle size was analyzed. Using X-ray diffraction, the phases occurring in the sand were investigated in relation to the particle size. Magnetic separation with two magnets, having different energy, was performed for identifying the phases attached to the magnetic particles. Magnetic hysteresis measurements evidenced complex and multiple iron phase behavior.

Assessment of Limestone Waste Addition for Fired Clay Bricks.

Our aim was to investigate the feasibility of using limestone waste resulting from stone processing for the manufacturing of fired clay bricks. Waste materials were considered as a partial replacement for clays to reduce the exploitation of natural resources and as a response to the climate neutrality commitments. The samples were prepared to have a waste content of up to 15% and were fired at a temperature of 900 °C. The chemical and mineralogical composition and the physical analysis of raw materials were investigated by using SEM-EDS and XRD diffraction. The result showed an increase in CaO in the clay mixture due to the presence of limestone, which reduced the shrinkage of the products' compressive strength, up to 55% for samples with a higher content of limestone (15 wt.%), and influenced the samples' color by making them lighter than the reference sample.

Invar/WC Composite Compacts Obtained by Spark Plasma Sintering from Mechanically Alloyed Powders.

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.