Powders, Volume 2, Issue 3 (September 2023) – 10 articles

Mechanochemical technology is developing rapidly, judging by the scientific information in both basic and applied studies. However, many issues and points of view remain to be discussed. This review presents some new key issues for the optimization of mechanochemical processes in terms of theoretical and practical aspects. Emphasis is placed on powder technology aspects, which are not always discussed compared to functional or microscopic viewpoints. The transfer of chemical species across the interparticle interface between dissimilar species during the mechanosynthesis of nanocomposites offers many new opportunities. Since almost all material transport is preceded by charge transfer, its driving force has been sought using terminology beyond the well-established electrochemical terms. In particular, the valence state of the cationic species involved is of importance. The role of organic compounds throughout the process is emphasized, regardless of their survival in the final product. The similarity with pharmaceutical phenomena is pointed out, although its mentality is very different from that of the synthesis of nanocomposites. The rational amorphization and stabilization of molecular dispersion states with the participation of excipients are discussed. The effects of liquids, either added or formed by mechanochemical auto-liquefaction, are presented with reference to the comparison between wet and dry grinding. The mechanisms of the apparent stabilization of the mechanically activated states of the products are elucidated to investigate the practical applicability of these mechanochemically synthesized products. Finally, the most important aspects for the optimization of the mechanochemical processes of functional nanocomposites are listed. Full article

The understanding of granule growth mechanisms and the effects of formulation and operating conditions over product quality and process performance in fluidized bed co-melt granulation is nowadays of great interest. In this sense, this work systematically studies the combined effects of binder content (W_PEG) and fluidization air flowrate (F_A) and temperature (T_A) on granules’ quality and process-related variables (product mass (M_P), elutriated fines (M_f), mass stuck on walls (M_W)) by using a Box–Behnken-type design of experiments (DoE), as it is a statistical tool suggested by the Quality by Design (QbD) initiative. It was found that the granules’ size and powder flowability are significantly affected by W_PEG (higher W_PEG, higher granule size and better flowability). Interestingly, T_A is the process variable that significantly affects M_P, enhancing process performance at high temperature values. Regarding F_A, it significantly affects d₁₀, promoting the formation of small particles due to breakage at high flowrates and the presence of non-elutriated powder at low flowrates. As a consequence, intermediate F_A is the optimum for obtaining higher M_P. Regarding regime map studies, most runs experienced a rapid growth regime, which is in accordance with the granules’ high pore saturation. This result agrees with the observed high increment in particle size and the morphology of the final granules, allowing researchers to validate and extend existing previous maps. Full article

The paper presents the results of experimental studies on the production of fine char powder from sunflower seed husks by a novel method of thermomechanical treatment with pulsed shock waves and supersonic jets of the mixture of ultra-superheated (above 2000 °C) steam and carbon dioxide, as well as the results of examination of the produced char powder in terms of its chemical, phase, and granulometric composition and structural, morphological, and texture characteristics. The objective of the research is to explore the possibility of using the resulting char powder as a sorption-active material for organic substances. It is shown that the obtained char particles and their agglomerates have an average size of 20–30 nm and 12–24 µm, respectively, have the shape of disks and ellipsoids, consist mainly of amorphous carbon (up to 56 wt%) and oxygen (up to 42 wt%), and have a specific surface area of 1.1–1.7 m²/g. It is concluded that such a char powder can be used as an absorbent for organic substances when dried and deagglomerated. Full article

The CFD simulation of cyclone separators has remarkably evolved over the past decades. Nowadays, computational models are essential for designing, analyzing, and optimizing these devices. Due to the intrinsic anisotropy of the flow inside these separators, the Reynolds stress model (RSM) has been mostly employed. However, RSM models fail to solve most time and space scales, including those relevant to particle behavior. Consequently, the prediction of the grade collection efficiency may be hindered, particularly for low-Stokes-number particles. For example, the precessing vortex core phenomenon (PVC), a well-known phenomenon that is relevant for particle motion, is not usually captured in Reynolds-averaged Navier–Stokes (RANS) simulations. Alternatively, the large-eddy simulation (LES) has been proven to be a superior approach since it captures many time and space scales that would have been otherwise dissipated, allowing for more accurate predictions of particle collection. However, this accuracy comes at a considerable computational cost. To combine the advantages of these two models, the main objective of this research was to evaluate a new hybrid RSM-LES model applied to the cyclone’s flow. The results were compared to experimental data and with RSM model results. It showed that, compared to a RANS model given by the RSM closure model, the grade collection efficiency curve obtained by the hybrid model is closer to the experimental one, even for the coarser mesh. Beyond that, the results showed that while the improvement in results was not proportional to mesh refinement for RANS modeling, the hybrid model showed significant improvement with mesh refinement. Full article

The current state of separation technology often neglects the multidimensional nature of real particle systems, which are distributed not only in terms of size, but also in terms of other properties, such as surface charge. Therefore, the aim of this study is to experimentally investigate the applicability of magnetic seeded filtration as a multidimensional separation process. Magnetic seed particles are added to a multisubstance suspension, and a selective heteroagglomeration with the nonmagnetic target particles is induced, allowing for an easy subsequent magnetic separation. The results show that high separation efficiencies can be achieved and that the parameters pH and ionic strength govern the agglomeration process. Selective separation based on surface charge was observed, but undesirable heteroagglomeration processes between the target particles lead to a loss of selectivity. Particle size was clearly identified as a second relevant separation feature, and its partially opposite influence on collision frequency and collision efficiency was discussed. Finally, experimental data of multidimensional separation are presented, in which a size-distributed two-substance suspension is separated into defined size and material fractions in a single process step. This study highlights the need for multidimensional evaluation in general and the potential of magnetic seeded filtration as a promising separation technique. Full article

Mechanochemically synthesized particles of two types of magnesium ferrites, one of which with structural distortions and an average size of 170 nm, and another that is highly crystalline with an average size of 900 nm, were introduced into a matrix of ultra-high-molecular-weight polyethylene via the milling processing. The final material has been formed by hot pressing mechanocomposites based on ultra-high-molecular-weight polyethylene and magnesium ferrite particles of various fineness and concentration. Structural characteristics were studied using scanning electron microscopy, differential scanning calorimetry and X-ray diffraction analysis. The dielectric properties of the obtained composites were analyzed by testing the frequency dependence of the permeability, dielectric losses, and conductivity. The effect of filler concentration and particle size, as well as the crystallinity of the polymer, on the dielectric properties of the composite material were studied. Full article

In the current work, nanocrystalline powders with different compositions, namely Li_0.98Pr_0.02NbO₃, Li_0.93Pr_0.02Mg_0.05NbO₃ and Li_0.98Pr_0.02TaO₃ were synthesized for the first time using the method of high-energy ball milling of the starting materials (Li₂CO₃, Nb₂O₅, Ta₂O₅, MgO, Pr₆O₁₁), followed by high-temperature annealing. XRD data analysis confirmed the absence of parasitic phases in the obtained nanocrystalline compounds. The estimated particle sizes ranged from 20 to 80 nm. From the obtained nanopowders, ceramic samples were prepared using specially developed equipment, which allowed for pressing at elevated temperatures with a simultaneous application of a constant electric field. The obtained photoluminescence spectra exhibit characteristic features of Pr³⁺ ions in the crystal structure of LiNbO₃ and LiTaO₃ and are most efficiently excited by UV light. Samples pressed with an electric field application show higher intensity of photoluminescence. Investigations of the temperature dependence of electrical conductivity of the Li_0.98Pr_0.02NbO₃ sample, pressed with the application of an electric field, indicate that the conductivity mechanism is similar to that of LiNbO₃ single crystals and, at high temperatures, is attributed to the lithium conduction mechanism. Full article

Nowadays, the search for the coupled polymer nanocomposite thermoelectrics that exhibit a high value of thermoelectric figure of merit (ZT) and similar behaviour of physical properties for the use as legs of thermoelectric cells is a current challenge. The direct current (DC) conductivity is one of the three important components of thermoelectric figure of merit. The aim of this study was to obtain PANI-based nanothermoelectrics with Te⁰ and Bi₂Te₃ nanoparticles and MWCNT by mechanochemical methodology and to investigate the dependency of their DC electrical conductivity on temperature in the 298–353 K range using the Arrhenius and Mott’s variable range hopping (VRH) models. Inorganic Te⁰ and Bi₂Te₃ nanoparticles were pre-synthesized by the available and environmentally friendly method using a commercial tellurium powder. The samples obtained were characterized by X-ray diffractometry (XRD), IR and UV-Vis spectroscopy. The XRD study of ES-PANI/Te⁰ (4.4 wt% Te⁰) and ES-PANI/Bi₂Te₃ (2.9 wt% Bi₂Te₃) nanocomposites found that the nanoparticle average size was 32 nm and 17 nm, respectively. The DC conductivity study of the samples with different nanophase content (2.1, 4.4, 10.2 wt% Te⁰, 1.5, 2.9, 7.3 wt% Bi₂Te₃, 1.5 wt% MWCNT) by the two points measurement method reveals the following: (a) the presence of inorganic nanophase reduces the conductivity compared to the matrix, (b) the addition of MWCNT in ES-PANI increases its electrical conductivity, (c) the conductivity of ES-PANI/Te⁰ as well as ES-PANI/Bi₂Te₃ nanocomposite rises with the increasing inorganic nanophase content, (d) the observed increase in the electrical conductivity of MWCNT-based nanocomposites with increasing inorganic nanophase content is interrupted by a characteristic area of decrease in its value at average values of inorganic nanoparticles content (at Te⁰ content of 4.4 wt%, at Bi₂Te₃ content of 2.9 wt%), (e) a similar DC conductivity behaviour in ES-PANI/Te⁰—ES-PANI/Bi₂Te₃ and ES-PANI/Te⁰-MWCNT—ES-PANI/Bi₂Te₃-MWCNT nanocomposite pairs is observed. Full article

Quasicrystalline Al₉₃Fe₃Cr₂Ti₂ (at.%) gas-atomized powders, which exhibit a metastable composite microstructure, were used to produce coatings by cold spray additive manufacturing processing (CSAM) using different processing parameters. The metastable composite microstructure provides the Al₉₃Fe₃Cr₂Ti₂ alloy with excellent mechanical properties. At the same time, the metastability of its microstructure, achieved by the high cooling rates of the gas atomization process, limits the processability of the Al₉₃Fe₃Cr₂Ti₂ powder. The purpose of this study was to investigate the effect of process parameters on the CSAM of quasicrystalline Al₉₃Fe₃Cr₂Ti₂ powder. The powder was sieved and classified to a size range of −75 µm. Using N₂ carrier gas combined with different temperatures, pressures, nozzle apertures, and deposition substrate conditions, cold-sprayed coatings were produced. The porosity and thickness of the coatings were evaluated by image analyses. By SEM, XRD, DSC, and TEM, the microstructure was identified, and by Vickers microhardness, the mechanical properties of the coatings were investigated. Dense (≤0.50% porosity) and thick (~185.0 µm) coatings were obtained when the highest pressure (4.8 MPa), highest temperature (475 °C), and lowest nozzle aperture (A) were used in combination with an unblasted substrate. The SEM, XRD, and DSC data showed that the composite powder’s microstructure was retained in all coatings with no decomposition of the metastable i-phase into equilibrium crystalline phases. Supporting these microstructural results, all coatings presented a high and similar hardness of about 267 ± 8 HV. This study suggests that the CSAM process could, therefore. produce metastable quasicrystalline Al₉₃Fe₃Cr₂Ti₂ coatings with a composite microstructure and high hardness. Full article

Cu–Al bronzes are interesting metallic materials, demonstrating higher hardness, higher wear resistance, higher corrosion resistance and a lower friction coefficient as compared with unalloyed copper. The powder metallurgy approach to the fabrication of these alloys presents opportunities to tailor their phase composition and grain size. In the present work, the structural characteristics, phase composition and properties of Cu-10 wt.% Al alloys obtained by spark plasma sintering (SPS) of powder blends and a powder obtained by mechanical alloying (based on Cu(Al) solid solution) are reported. Alloys with different interaction degrees between the metals were obtained by SPS. The blends demonstrated better sinterability than the mechanically alloyed powder: a nearly fully dense alloy was obtained by SPS of the blend at 480 °C, whereas a temperature of 800 °C was necessary to consolidate the mechanically alloyed powder. The hardness and electrical conductivity of the sintered alloys were comparatively analyzed. It was shown that the Cu-10 wt.% Al alloys obtained without the mechanical alloying stage possess hardness and electrical conductivity comparable to those of the alloys obtained from the mechanically milled powder. Full article