Feature Papers in Powders 2023

Epoxy powders offer a low-cost way of manufacturing thick-section composite parts, such as those found in wind and tidal turbines. Currently, their processing cycle includes a lengthy drying stage (≥15 h) to remove ambient moisture. This drying stage prevents void defect formation and, thereby, a reduction in mechanical properties; however, it constitutes up to 60% of the processing time. Little research has been published which studies the drying stage or its optimisation. In the present work, experimental and simulated analyses are used to investigate the effects of hygroscopicity in epoxy powder composites. Tests are performed to quantify the void content of dried and undried laminates and to measure its impact on transverse flexural strength. Dynamic vapour sorption analysis is used to study the sorption behaviour of the epoxy powder. It is shown that the epoxy powder is slightly hygroscopic (1.36 wt%) and exhibits sorption behaviour that is characteristic of glassy polymers. This results in up to 4.8% voids (by volume) if processed in an undried state, leading to a 43% reduction in transverse flexural strength. A modified linear driving force model is fitted to the desorption data and then implemented in existing process-simulation tools. The drying of a thick epoxy powder composite section is simulated to investigate the influence of powder sintering on the duration of the drying stage. Process simulations reveal that a standard drying cycle prematurely sinters the powder, which inhibits moisture release. By maintaining the powder state, simulations show that the drying cycle can be reduced to 5 h. Full article

Based on the generalization of M. Yu. Balshin’s well-known equations in the framework of a discrete model of powder compaction process (PCP), two new die-compaction equations for powders have been derived that show the dependence of the compaction pressure p on the relative density ρ of the powder sample. The first equation, $p=\frac{w}{{(1-{\rho }_0)}^{(n-m)}}·\frac{{(\rho -{\rho }_0)}^n}{{(1-\rho )}^m}$, contains, in addition to the initial density ρ₀ of the powder in die, three constant parameters—w, n and m. The second equation in the form $p=\frac{H}{{\left(1-{\rho }_0\right)}^{\left(b-c\right)}}·\frac{{\left(\rho -{\rho }_0\right)}^b}{\left[{\left(1-{\rho }_0\right)}^c-a{\left(\rho -{\rho }_0\right)}^c\right]}$ also takes into account the initial density of the powder and contains four constant parameters H, a, b, and c. The values of the constant parameters in both equations are determined by fitting the theoretical curve according to these equations to the experimental powder compaction curve. The adequacy of the PCP description with these equations has been verified by approximating experimental data on the compaction of various powders, including usual metal powders such as iron, copper, and nickel, highly plastic powders such as tin and lead, a mixture of plastic powder (Ni) with non-plastic powder (Al₂O₃), nickel-plated alumina powder, as well as powder of a brittle compound, in particular titanium carbide TiC. The proposed equations make it possible to describe PCP with high accuracy, at which the coefficient of determination R² reaches values from 0.9900 to 0.9999. The four-constant equation provides a very accurate description of PCP from start to finish when the density of the samples stops increasing once the pressure increases to an extremely high level, despite the presence of porosity. Full article

The low deposition efficiency in directed energy deposition (DED) has prompted the reuse of powders that do not fuse to the builds to make additive manufacturing more sustainable. It is unknown, however, how the properties of the powder and deposited parts change as powders are continuously reused. In this study, AlSi10Mg was investigated for five deposition cycles in DED. Exposing AlSi10Mg powder to DED conditions changes the morphology, size, and flowability. The mechanical properties of AlSi10Mg DED parts decreased after the feedstock powder was reused one time. Notably, no additional significant changes were observed when the powder was further reused. Full article

Boron carbide (B₄C) powders with defined stoichiometry, high crystallinity, minimal impurity content, and a fine particle size are imperative for realizing the exceptional properties of this compound in advanced high-technology applications. Nevertheless, achieving the desired stoichiometry and particle size using traditional synthesis methods, which rely on prolonged high-temperature processes, can be challenging. The primary objective of this study is to synthesize fine B₄C powders characterized by high crystallinity and a sub-micron particle size, employing a fast and energy-efficient method. B₄C powders are synthesized from elemental boron and carbon in a high-frequency induction heating furnace using the electromagnetic induction synthesis (EMIS) method. The rapid heating rate achieved through contactless heating promotes the ignition and propagation of the exothermic chemical reaction between boron and carbon. Additionally, electromagnetic effects accelerate atomic diffusion, allowing the reaction to be completed in an exceptionally short timeframe. The grain size and crystallinity of B₄C can be finely tuned by adjusting various process parameters, including the post-ignition holding temperature and the duration of heating. As a result, fine B₄C powders can be synthesized in under 10 min. Moreover, these synthesized B₄C powders exhibit oxidation onset temperatures higher than 500 °C when exposed to air. Full article

In this work, the consolidation of calcium carbonate (CaCO₃) by polyacrylamide (PAM) of different molecular weights, charge densities, and functional groups was investigated via oscillatory rheology and unconfined compressive strength (UCS) analysis. Oscillatory rheology showed that the storage modulus G′ was approximately 10 times higher than the loss modulus G″, indicating a highly elastic CaCO₃ sample upon consolidation via PAM. Both oscillatory rheology and UCS analysis exhibited similar trends, wherein the mechanical values (G′, G″, and UCS) first increased with increasing polymer dosage, until they reached a peak value (typically at 3 mgpol/gCaCO₃), followed by a decrease in the mechanical values. This indicates that there is an optimum polymer dosage for the different PAM-CaCO₃ colloidal systems, and that exceeding this value induces the re-stabilisation of the colloidal system, leading to a decreased degree of consolidation. Regarding the effect of the PAM molecular weight, the peak G′ and UCS values of CaCO₃ consolidated by hydrolysed PAM (HPAM) of different molecular weights are very similar. This is likely due to the contour length of the HPAMs being either almost the same or longer than the average distance between two CaCO₃ particles. The effect of the PAM charge density revealed that the peak G′ and UCS values decreased as the charge density of the PAM increased, while the optimum PAM dosage increased with decreasing PAM charge density. The higher likelihood of lower-charge PAM bridging between the particles contributes to higher elastic energy and mechanical strength. Finally, regarding the PAM functional group, CaCO₃ consolidated by sulfonated polyacrylamide (SPAM) typically offers lower mechanical strength than that consolidated with HPAM. The bulky sulfonate side groups of SPAM interfere with the surface packing, reducing the number of polymers able to adsorb onto the surface and, eventually, reducing the degree of consolidation of CaCO₃. The zeta potential of the PAM-CaCO₃ samples became more negative with increasing PAM concentration due to the saturation of the particle surface. Good agreement between oscillatory rheology and UCS analysis could accelerate PAM screening for optimum CaCO₃ consolidation. Full article

A novel method has been proposed to induce rapid upward movement of colloidal particles with a density lower than water by applying an electric field of several V/mm in water. This phenomenon, known as the Electrically Induced Rapid Sedimentation (ERS) effect, marks the first occurrence of ‘rapid upward movement of colloidal particles’ within the scope of this phenomenon. Focusing on hollow particles, an investigation of the ERS effect was conducted through transmittance measurement. The hollow particles in water showed a drastic increase in ascending velocity through the application of an electric field. The ascending velocity raised when increasing the electric field strength. Utilizing a quasi-DC electric field (an extremely low-frequency AC electric field), aggregate structures were captured for the first time. 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

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

A novel method of the hot consolidation metal powders with shear deformation is proposed. The powders were encapsulated into tight containers and compacted after short-term heating in a furnace preheated to 900 °C. The method prevents powder oxidation, peripheral spalling and ensures the removal of the oxide films from the powder surfaces. Commercial titanium powders of different dispersivities and impurity concentrations were hot-compacted. The microstructure, hardness and bending strength of the compacts were investigated. The compacts from fine PTOM-1 powder, containing 0.32% of hydrogen, reveal the greatest values of the hardness and bending strength. Additional annealing results in 60% increase in the bending strength. Full article

This review, complemented by empirical investigations, delves into the intricate world of industrial powders, examining their elastic properties through diverse methodologies. The study critically assesses Young’s modulus (E) across eight different powder samples from various industries, including joint filler, wheat flour, wheat starch, gluten, glass beads, and sericite. Employing a multidisciplinary approach, integrating uniaxial compression methodologies—both single and cyclic—with vibration techniques, has revealed surprising insights. Particularly notable is the relationship between porosity and Young’s modulus, linking loose powders to the compacts generated under compression methods. Depending on the porosity of the powder bed, Young’s modulus can vary from a few MPa (loose powder) to several GPa (tablet), following an exponential trend. The discussion emphasizes the necessity of integrating various techniques, with a specific focus on the consolidation state of the powder bed, to achieve a comprehensive understanding of bulk elasticity. This underscores the need for low-consolidation methodologies that align more closely with powder technologies and unit operations such as conveying, transport, storage, and feeding. In conclusion, the study suggests avenues for further research, highlighting the importance of exploring bulk elastic properties in loose packing conditions, their relation with flowability, alongside the significance of powder conditioning. Full article

The well-known equations for the powder compaction process (PCP) in a rigid die published from the beginning of the last century until today were considered in this review. Most of the considered equations are converted into the dependences of densification pressure on the powder’s relative density. The equations were analyzed and their ability to describe PCP was assessed by defining the coefficient of determination when approximating experimental data on the compaction of various powders. It was shown that most of the equations contain two constants the values of which are determined by fitting the mathematical dependence to the experimental curve. Such equations are able to describe PCP with high accuracy for the compaction of powders up to a relative density of 0.9–0.95. It was also shown that different equations can describe PCP in the density range from the initial density to 0.9 with the same high accuracy, but when the process of compaction is extrapolated to higher values of density, the curves diverge. This indicates the importance of equations that can unambiguously describe PCP to a relative density equal to or close to 1.0. For an adequate description of PCP for relative density greater than 0.95, equations containing three or four constants have proven useful. Full article

The flowability of food powders is a critical determinant of their processing efficiency, product quality, and overall operational success. This review delves into the intricacies of powder flowability, elucidating the factors that govern it and exploring various methods for its evaluation and enhancement. Particle size and distribution, particle shape, surface properties, moisture content, and storage conditions stand as the key determinants of powder flowability. Finer powders, with their increased interparticle cohesive forces, tend to exhibit poorer flowability. Particle shape also plays a role, with irregular or elongated particles flowing less readily than spherical ones. Surface properties influence interparticle friction, thereby impacting flow behavior. Moisture content significantly affects flowability, as increased moisture can lead to liquid bridge formation, hindering powder movement. Storage temperature, on the other hand, generally enhances powder flow due to reduced interparticle cohesive forces at higher temperatures. This highlights the need to understand the factors influencing food powder flowability and to employ appropriate evaluation strategies for optimizing food powder processing efficiency, product quality, and overall production success. Full article

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