Powders, Volume 3, Issue 2 (June 2024) – 9 articles

The fractionation in microchannels is a promising approach for the delivery of microparticles in narrow property distributions. The underlying mechanisms of the channels are however often not completely understood and are therefore subject to current research. These investigations are done using different numerical and experimental methods. In this work, we present and evaluate our method of combining a numerical Discrete Element Method (DEM)-Lattice Boltzmann Method (LBM) approach with experimental long-exposure fluorescence microscopy, micro-Particle Image Velocimetry (µPIV) and Astigmatism Particle Tracking Velocimetry (APTV) measurements. The suitability of the single approaches and their synergies are evaluated using the exemplary investigation of multidimensional fractionation in different channel geometries. It shows that both, numerical and experimental method are well suited to evaluate particle dynamics in microchannels. As they furthermore show strengths canceling out weaknesses of the respective other method, the combined method is very well suited for the comprehensive analysis of particle dynamics in microchannels. 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

As nanoparticle syntheses on a large scale usually yield products with broad size and shape distributions, the properties of nanoparticle-based products need to be tuned after synthesis by narrowing the size and shape distributions or via the removal of undesired fractions. The development of property-selective classification processes requires a universal framework for the quantitative evaluation of multi-dimensional particle fractionation processes. This framework must be applicable to any property and any particle classification process. We extended the well-known one-dimensional methodology commonly used for describing particle size distributions and fractionation processes to the multi-dimensional case to account for the higher complexity of the property distribution and separation functions. In particular, multi-dimensional lognormal distributions are introduced and applied to diameter and length distributions of gold nanorods. The fractionation of nanorods via centrifugation and by orthogonal centrifugal and electric forces is modeled. Moreover, we demonstrate that analytical ultracentrifugation with a multi-wavelength detector (MWL-AUC) is a fast and very accurate method for the measurement of two-dimensional particle size distributions in suspension. The MWL-AUC method is widely applicable to any class of nanoparticles with size-, shape- or composition-dependent optical properties. In addition, we obtained distributions of the lateral diameter and the number of layers of molybdenum disulfide nanosheets via stepwise centrifugation and spectroscopic evaluation of the size fractions. Full article

The perpetual significance of the pharmaceutical industry in society necessitates ongoing research efforts to enhance the efficacy of its manufacturing processes. Given that drug product manufacturing typically involves powder processing, a thorough understanding of powder characterization is needed for optimal process performance. Powder rheology is commonly examined in pharmaceutical manufacturing to elucidate the relationship between powder properties and the performance of pharmaceutical processes. This paper provides a brief discussion of recent literature regarding the various powder properties and characterization techniques encompassed in powder rheology. The powder properties are categorized into particle size, particle morphology, friability, electrostatics, permeability, wettability, cohesion, bulk density, and agglomeration sections. A distinct focus is placed on the segment about powder wettability. This review informs readers about the fundamental properties of powders known to influence pharmaceutical processes. It discusses the interrelationships among these properties, powder characterization techniques, and ideal states of powder properties that lead to optimal process performance. Full article

Magnetic seeded filtration (MSF) is a multidimensional solid–liquid separation process capable of fractionating a multimaterial suspension based on particle size and surface properties. It relies on the selective hetero-agglomeration between nonmagnetic target and magnetic seed particles followed by a magnetic separation. Experimental investigations of multimaterial suspensions are challenging and limited. Therefore, a Monte Carlo model for the simulation of hetero-agglomeration processes is developed, validated, and compared to a discrete population balance model. The numerical investigation of both charge-based and hydrophobicity-based separation in an 11-material system, using synthetic agglomeration kernels based on real-world observations, yields results consistent with prior experimental studies and expectations: Although a multidimensional separation is indeed possible, unwanted hetero-agglomeration between target particles results in a reduced selectivity. This effect is more pronounced when separation is based on a dissimilarity rather than a similarity in the separation criterion and emphasizes the advantages of hydrophobicity-based systems. For the first time, 2D grade efficiency functions $T(\phi ,d)$ are presented for MSF. However, it is shown that these functions strongly depend on the initial state of the suspension, which casts doubt on their general definition for agglomeration-based processes and underlines the importance of a simulation tool like the developed MC model. Full article

The consumption of fiber in the human diet is a global recommendation to ensure a healthy diet. Quinoa (Chenopodium quinoa Willd.), a gluten-free grain, and chia (Salvia hispanica), a seed, contain a high fiber content, and both have the potential to be used in the development of nutraceutical and pharmaceutical formulations. An interesting characteristic of chia is its ability to form viscous mucilage when in contact with water, making it a potential binder in solid formulations. However, there are no studies on chia as a binder, and therefore, the objective of the present study was to evaluate the feasibility of using chia as a binder to produce quinoa granules and, subsequently, develop chewable tablet formulations. The quinoa and chia were in a powder form and then transformed into a wet mass with the help of mixer torque rheometer (MTR) equipment. In the wet granulation form, the following parameters were tested: multiple additions, 15 g of material, and 25 timepoints for the addition of 1 mL of water. An experimental design was carried out to evaluate the impact of the variables on the MTR results for subsequent granulation. The granulation point was possible for T1–T9, and most formulations gave satisfactory results, such as an acceptable resistance of the granules. In the end, a formulation was selected for the development of chewable tablets containing quinoa and chia fibers. Full article

Population balance models (PBMs) for milling processes are based on two fundamental concepts: specific breakage rate function and breakage distribution function, which vary with particle size as well as design–operation conditions. The solution of the inverse problem, i.e., the estimation of these two functions’ parameters, may cause falsified kinetics and breakage distribution mechanisms. This perspective article aims to expose and mitigate various aspects of potential falsification, thus enabling the development of a robust PBM. Through an in-depth analysis of historical approaches to the PBM inverse problem and experimental observations, as well as the author’s recent contributions to the inverse methodology within the context of back-calculation methods, six principles have been offered: (i) include the governing physical phenomena and reduce errors in model building; (ii) reduce the number of model parameters via size–operation-dependent functional forms, hybrid approaches for back-calculation, and combination with CFD–DEM and other mechanistic models; (iii) generate a dense particle size distribution data set obtained at various milling times and/or locations; (iv) ensure a grid-independent solution with a sufficient number of size classes; (v) use a global optimization-based back-calculation method for parameter estimation and provide standard errors of the estimates; and (vi) test the predictive capability of the PBM. This perspective article boosts awareness of various challenges involved in the solution of the inverse PBM problem as pertinent to milling processes and provides researchers with six principles to minimize falsified kinetics. Full article

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

Metal additive manufacturing technologies, such as Laser Powder-Bed Fusion, often rate as sustainable due to their high material efficiency. However, there are several drawbacks that reduce the overall sustainability and offer potential for improvement. One such drawback is waste emerging from the process. These smoulder particles form when the laser hits the powder-bed surface, are blown away from the part by the shielding gas stream and accumulate on the edge of the build chamber. Usually, smoulder does not contribute to the circular reuse of powder that was part of the powder-bed but was not integrated into a part. Instead, it marks an end-of-life state of powder. Significant amounts of smoulder accumulate depending on the irradiated area or the build volume in one job, respectively. This results in the waste of powder that was produced with low energy efficiency. This study investigates the question of whether smoulder can transform from waste to resource via common powder characterization methods and first build jobs using processed smoulder. The investigation of process-relevant powder properties like apparent density and flowability showed no significant difference between virgin powder and smoulder. Sample characterization indicated that neither porosity, surface quality nor mechanical properties deteriorate when samples contain about 50% smoulder. This allows for the reuse of smoulder in terms of powder characterization and part quality. Full article