Powders

Simulative and experimental studies were carried out to address multi-dimensional particle fractionation of non-biological particles according to size, shape, and density inside a high-throughput DLD array. Density sensitive separation was achieved for melamine and polystyrene particles at a diameter of 5 µm at a Reynolds number (Re) of 82, corresponding to an overall flow rate of 11.3 mL/min. This process is very sensitive, as no fractionation occurred for Re = 85 (11.7 mL/min). For the first time, the fractionation of elliptical polystyrene particles (5 × 10 µm) at Re > 1 was investigated up to Re = 80 (11 mL/min). A separation of elliptical particles from spherical melamine particles (5 µm) was observed in single experiments at all investigated Reynolds numbers. However, the separation is not reliably repeatable due to partial clogging of ellipsoidal particles along the posts. In addition, higher concentrations of polydisperse silica suspensions were experimentally investigated by using polydisperse silica particles at concentrations up to 0.4% (m/V) up to Re = 80 (20 mL/min). The separation size generally decreased with increasing Reynolds number and increased with increasing concentration. Separation efficiency decreased with increasing concentration, independent of the Reynolds number. In order to investigate the material-dependent separation in a contactless dielectrophoresis system (cDEP), the resolved CFD-DEM software was extended to calculate dielectrophoretic forces on particles. With this, the second stage of a serial-combined DLD-DEP system was simulated, showing good separation at lower flow rates. For these systems, different fabrication methods to minimize the distance between the electrodes and the fluid as well as the requirement to withstand high-throughput applications, were investigated. Full article

This collection of studies, conducted within the framework of the DFG-funded Priority Program SPP 2045, explores the role of X-ray tomography in advancing the multidimensional characterization of particulate systems, with a strong focus on enhancing 3D particle-discrete data quality. It critically assesses the limitations of traditional particle characterization methods, particularly those reliant on imaging techniques, and demonstrates how advanced methodologies can overcome these constraints by providing highly detailed and accurate geometric and structural 3D data. The research further introduces innovative sample preparation techniques for particle collectives, aiming to reduce post-processing efforts in image analysis. Additionally, the development of a particle database, aligned with FAIR data principles (Findable, Accessible, Interoperable, and Reusable), supports data sharing and collaborative research. Ultimately, this collection underscores the transformative potential of 3D particle-discrete datasets acquired through X-ray tomography in advancing particle technology and improving particle system analyses across diverse scientific and industrial fields. Full article

To obtain a more comprehensive understanding of the specific properties of complex-shaped technical aerosols—such as partially sintered aggregates formed in combustion processes or structured particles resulting from complex synthesis processes—it is essential to measure more than a single equivalent size. This study examines a novel method for determining a two-dimensional distribution of two distinct particle properties within the size range from $50\mathrm{nm}$ to $1000\mathrm{nm}$: the Centrifugal Differential Mobility Analyzer (CDMA). The CDMA enables the simultaneous measurement of both mobility and Stokes equivalent diameters, providing a detailed two-dimensional particle property distribution. This, in turn, allows for the extraction of shape-related information, which is essential for characterizing particles in terms of their chemical composition, reactivity, and other physicochemical properties. This paper presents a detailed evaluation of a first CDMA prototype. First, CFD simulations of the flow field within the classifier are presented in order to assess and understand non-idealities arising from the exact geometry. Subsequently, the transfer function is evaluated by particle trajectory calculations based on the simulated flow field. It can be demonstrated that the simulated transfer functions agree quite well with transfer functions derived from streamlines of an ideal flow field, indicating that the non-idealities in the classifying region are almost negligible in their effect on the classification result. An experimental determination of the transfer function shows additional effects not covered by the previous simulations, like broadening by diffusion and losses due to diffusion and precipitation within the in- and outlet of the classifier. Finally, the determined transfer functions are used to determine the full two-dimensional distribution with regard to the mobility and Stokes equivalent diameter of real aerosols, like spherical particles and aggregates at different sintering stages, respectively. Full article

This study aims to investigate the suitability of earthen housing for refugees and establish a more efficient system for selecting and adjusting materials by quantitatively analyzing the influence of various factors affecting the mechanical performance of earthen housing. This paper examined the impact of dry unit weight, particle size distribution of soil solidification, clay minerals, and pH on the mechanical performance of soil solidification through compressive strength testing. Additionally, the tensile strength resulting from capillary forces between particles was estimated using a prediction equation, and the effects of capillary forces and cohesive forces due to clay minerals were quantitatively assessed by comparing them with the results of the compressive strength experiments. In an alkaline environment, conflicting results were obtained regarding the effect of the dispersion of particles on compressive strength, depending on the presence or absence of clay minerals in the soil. Based on these results, the implementation of earthen houses constructed in the target refugee camp was evaluated, and strategies for building houses more efficiently under given conditions were discussed. Full article

Controlling the stability of colloidal nanoparticles in multicomponent systems is crucial for advancing formulations and separation processes. This study investigates the selective agglomeration approach for binary colloidal mixtures, providing both fundamental insights into stability/agglomeration mechanisms and a scalable separation strategy. First, we established a binary model system comprising gold nanoparticles (Au NPs) and ZnS quantum dots (QDs) to assess interparticle interactions. UV-visible spectroscopy revealed that impurities released from ZnS QDs, particularly thiol-based ligands and unbound Zn ions, triggered the aggregation of Au NPs depending on their surface stabilizers. Functionalization of Au NPs with bis(p-sulfonatophenyl) phenylphosphine (BSPP) significantly enhanced colloidal stability, with unpurified BSPP-functionalized Au NPs exhibiting superior resistance to agglomeration. Building on these insights, we applied selective agglomeration to separate a complex colloidal system consisting of InP/ZnS core–shell QDs and ZnS byproducts, a critical challenge in QD synthesis that is particularly relevant for post-processing of samples that originate from large-scale flow synthesis. By systematically tuning the ethanol concentration as a poor solvent, we successfully achieved composition-dependent fractionation. Optical and spectroscopic analyses confirmed that coarse fractions were enriched in InP/ZnS QDs, while fines fractions mainly contained pure ZnS QDs, with absorption peaks at 605 nm and 290 nm, respectively. Photoluminescence spectra further demonstrated a redshift in the coarse fractions, correlating with an increase in particle size. These results underscore the potential of selective agglomeration as a scalable, post-synthesis classification method, offering a framework for controlling stability and advancing post-synthesis separation strategies in colloidal multicomponent systems. Full article

As part of the so-called interfacial separation techniques, selective particle agglomeration is one of the few options that are suitable for the separation of heterogeneous, multicomponent systems of particles smaller than 1 μm. In this regard, the component to be separated is exclusively transferred into a coarser size range, so that a material selective size separation by traditional mechanical methods can be achieved. In the presented study, this is demonstrated using heterogeneous suspensions of ceramic and organic particles, from which the separation of the inorganic material is pursued subsequent to the targeted control of the material-specific, electrostatic particle–particle interaction. Resulting from theoretical considerations on these interactions, favorable conditions for the selective agglomeration can be predicted. Experimental data reveal that for suitable parameters, resulting from variations in interfacial particle properties, particle size, and the composition of the dispersions, a separation efficiency of up to 97% can be obtained. Thereby, the importance of the particle-number fraction as an adjustable parameter needs to be clearly emphasized. Since a separation of the agglomerates can be achieved by simply using centrifugal forces, the shown technique is easy to apply and valuable for various industrial fields such as chemical and pharmaceutical engineering or recycling processes. In addition, no external additives are required for selective agglomeration, eliminating the risk of secondary contamination. Full article

The efficiency of froth flotation drastically drops towards ultrafine particles. Some improvements may be possible using smaller bubbles and high degrees of turbulence, however, reaching their limits in the nanometer particle range. Therefore, an approach is presented where the nanoparticles themselves produce nanobubbles that remain attached and allow, in combination with small bubbles, for the direct flotation of nanoparticles. Here, the formation and the fate of these surface nanobubbles are investigated directly in the dispersed systems for the first time. The required differentiation between free and attached nanobubbles is realized by combining light scattering and extinction measurements. With this combination, it was also possible to study the formation of the attached nanobubbles and the strength of their mechanical attachment to the particles. The successful formation of attached nanobubbles is also confirmed with measurements of the settling velocities. Surprisingly, stable surface nanobubbles can be formed even on hydrophilic particles if the surface contains enough concave sites. Full article

The increasing demand for highly specific particulate products in industrial processes is a driving factor in the development of novel particle separation processes. In this work, a multidimensional separation process for wet simultaneous separation by hydrodynamic diameter and electrophoretic mobility was developed. The hydrodynamic effects and electrophoretic influences within this process were experimentally investigated on different scales with three setups for batch and continuous operation. Flow rates were varied from a few mL∙min⁻¹ to several 100 L∙h⁻¹, and electric field strengths of up to 300 V∙cm⁻¹ were employed to analyze different spherical particles in the range of 1 to 100 µm. The investigations demonstrated the limitation of the separation process due to some of the resulting effects, such as electrolysis. A scale-up approach for hydrodynamic separation was developed based on CFD simulation, which can predict the operating range of the process with the high efficiency. Full article

The recent progress in the acoustic fractionation of particulate suspensions within microfluidic devices emphasizes the utility of the acoustic fractionation process also for gas-suspended particles as a significant advancement in the field of mechanical process engineering. In the literature, analytical and numerical studies have found the gas-based acoustic particle fractionation process to be suitable for particles in a size range below 10 µm. The viability remains experimentally unassessed. In this article, we present particle fractionation experiments conducted on gas-born particles suspended in high-intensity acoustic fields. A particle-size-dependent accumulation of particles in the acoustic sound velocity lobes and nodes could be observed, indicative of an acoustic fractionation process. Additionally, evidence of acoustic streaming and acoustic focusing has been found, both of which have the potential to impede the fractionation process. The experimental results align with the conclusions of numeric simulations. The in-process particle behavior is discussed in the context of the relevant literature and reinforces the notion of selective entrainment. Full article

The processing and preparation of particulate products is an important process in modern industry and science. The enormous potential for innovation in research and development is due to the complex interactions of solids with their environment. The aim of advanced particle production is to achieve high yields of narrowly distributed particle sizes, shapes or material compositions that provide advantageous product specifications. The integration of solid–liquid separation into these processes expands the process engineering scope in terms of product quality and efficiency. Designing these processes to accommodate a wide range of separation characteristics at small-particle-size scales is a major challenge. Taking these aspects into account, the present work aims to improve a dynamic simulation tool for tubular centrifuges that models the time- and space-dependent mass transport and thus, for the first time, can predict separation outcomes when processing both single- and multi-component systems. Utilizing an optical measurement technique, nanosuspension properties can be measured in real time during separation to support model validation. The simulation results align closely with experimental findings and offer plausible insights when addressing multi-dimensional property distributions of non-spherical particles. This study contributes to advanced modeling of separation experiments in tubular centrifuges in real time, taking into account multiple particle properties such as material density and particle form. Full article

Gel electrophoresis is a powerful method for the separation of nanoparticulate suspensions into several fractions with distinct particle properties. To monitor particle migration through the three-dimensional net structure of the gel and gain insights about the separation process, this study introduces a self-designed fiber-based UV-Vis measurement system equipped with five probes for the sequential in situ recording of absorption spectra. The system was employed to investigate the migration and separation of Au and Fe₃O₄ particles within hydrogels of varying agarose concentrations (0.15–0.50 wt.-%), revealing an increase in scattering with higher agarose content. The identification of specific particle fractions with a spherical or rod-shaped morphology was successfully achieved within the gels due to characteristic absorption peaks, allowing the real-time observation of particle separation. For the separation of a binary mixture, an adequate migration distance is needed according to the difference in the electrophoretic mobility of the two samples. The particle tracking and an additional mathematical deconvolution allowed the analysis of mixed particle samples within the gel so that their weight ratio could be determined. Finally, the system was calibrated for the determination of the particle concentration within the gel matrix, quantitatively revealing the particle concentration at a specific position in the gel. Full article

Lab-on-a-Chip devices based on tilted-angle standing surface acoustic waves (tasSAWs) emerged as a promising technology for multidimensional particle separation, highly selective in particle size and acoustic contrast factor. For this active separation method, a tailored acoustic field is used to focus and separate particles on stationary pressure nodes by means of the acoustic radiation force. However, additional non-linear acoustofluidic phenomena, such as the acoustically induced fluid flow or dielectrophoretic effects, are superimposed on the separation process. To obtain a particle separation of high quality, control parameters that can be adjusted during the separation process as well as design parameters are available. The latter are specified prior to the separation and span a high-dimensional parameter space, ranging from the acoustic wavelength to the dimensions and materials used for the microchannel. In this paper, the physical mechanisms to control and design tasSAW-based separation devices are reviewed. By combining experimental, semi-analytical, and numerical findings, a critical channel height and width are derived to suppress the influence of the acoustically induced fluid flow. Dealing with the three-dimensional nature of the separation process, particles are focused at different height levels of equal force balance by implementing a channel cover of high acoustic impedance while achieving an approx. three-times higher acoustic pressure. Using this improved channel design, the particle shape is identified as an additional separation criterion, rendering the continuous acoustofluidic particle separation as a multidimensional technology capable of selectively separating microparticles below 10 μm with regard to size, acoustic contrast, and shape. Full article

Separation functions, so-called Tromp functions, are often used to quantitatively analyze the separation behavior in particle processing with respect to individual particle descriptors. However, since the separation behavior of particles is typically influenced by multiple particle descriptors, multivariate Tromp functions are required. This study focuses on methods that allow for the computation of multivariate parametric Tromp functions by means of statistical image analysis and copula-based modeling. The computations are exemplarily performed for the magnetic separation of Li-bearing minerals, including quartz, topaz, zinnwaldite, and muscovite, based on micro-computed tomography images and scanning electron microscopy with energy-dispersive X-ray spectroscopy analysis. In particular, the volume equivalent diameter, zinnwaldite fraction, flatness, and sphericity are examined as possible influencing particle descriptors. Moreover, to compute the Tromp functions, the probability distributions of these descriptors for concentrate and tailing should be used. In this study, 3D image data depicting particles in feed, concentrate, and tailings is available for the computation of Tromp functions. However, concentrate particles tend to be elongated, plate-like, and densely packed, making segmentation for extracting individual particles from image data extremely difficult. Thus, information on the concentrate could not be obtained from the available database. To remedy this, an indirect optimization approach is used to estimate the distribution of particle descriptors of the concentrate. It turned out that this approach can be successfully applied to analyze the influence of size, shape, and composition of particles on their separation behavior. Full article

The creation of highly specific particle systems in the nano- and micrometer size range is a challenging task. The demand for particle systems with narrowly distributed properties is increasing in many applications, especially for use in high-tech products. Conventional separation techniques often reach their limits in the micrometer size range or become (labor-)intensive, which makes them economically or ecologically unsustainable. In addition, sorting based on several properties is rarely feasible in just one separator. Dielectrophoretic processes can be a viable option for complex sorting tasks like this, given their ability to address several particle properties and their high degree of selectivity. In this paper, we summarize the progress of a project in which the capability of dielectrophoretic methods for multidimensional sorting of microparticles was investigated. We were able to develop an operation mode for multidimensional sorting of microparticles using dielectrophoresis as well as a scalable electrically switchable filter. This creates a basis for high-throughput and multi-target sorting of technical microparticles using dielectrophoretic processes. Full article

In this study, a two-dimensional separation of microparticles based on their settling velocity and triboelectric charge ability is achieved using an air classifier for size fractionation and simultaneous charging, followed by an electrostatic separator. In the first part, considerations for enhancing particle classification with high sharpness and low-pressure drops are discussed through improvements in blade design investigated with CFD simulations and validated experimentally. Blades with extended lengths towards the center of the classifier prevent the formation of high-velocity vortices, thereby minimizing the back-mixing of particles and enhancing separation sharpness. This approach also reduces pressure drops associated with these flow vortices. In the second part of the study, the modified blades within the classifier are utilized for two-dimensional separation. Powders from two different materials are fed into the classification system, where particles become triboelectrically charged, mainly through collisions with the walls of the classification system components. Coarse particles are rejected at the wheel and exit the classifier, while differently charged fine particles of the two materials are directed into an electrostatic separator for material sorting. An enrichment of approximately 25–35% for both materials has been achieved on the electrodes of the separator. Full article

Chemical and physical properties of nanoparticles (NPs) are strongly influenced not only by the crystal structure of the respective material, including crystal structure defects but also by the NP size and shape. Contemporary transmission electron microscopy (TEM) can describe all these NP characteristics, however typically with a different statistical relevance. While the size and shape of NPs are frequently determined on a large ensemble of NPs and thus with good statistics, the characteristics on the atomic scale are usually quantified for a small number of individual NPs and thus with low statistical relevance. In this contribution, we present a TEM-based characterization technique, which can determine relevant characteristics of NPs in a scale-bridging way—from the crystal structure and crystal structure defects up to the NP size and morphology—with sufficient statistical relevance. This technique is based on a correlative multi-scale TEM approach that combines information on atomic scale obtained from the high-resolution imaging with the results of the low-resolution imaging assisted by a semi-automatic segmentation routine. The capability of the technique is illustrated in several examples, including Au NPs with different shapes, Au nanorods with different facet configurations, and multi-core iron oxide nanoparticles with a hierarchical structure. Full article

The homogenized lattice Boltzmann method (HLBM) has emerged as a flexible computational framework for studying particulate flows, providing a monolithic approach to modeling pure fluid flows and flows through porous media, including moving solid and porous particles, within a unified framework. This paper presents a thorough review of HLBM, elucidating its underlying principles and highlighting its diverse applications to particle-laden flows in various fields as reported in literature. These include studies leading to new fundamental knowledge on the settling of single arbitrarily shaped particles as well as application-oriented research on wall-flow filters, hindered settling, and evaluation of the damage potential during particle transport. Among the strengths of HLBM are its monolithic approach, which allows seamless simulation of different fluid-solid interactions, and its ability to handle arbitrary particle shapes, including irregular and concave geometries, while resolving surface interactions to capture local forces. In addition, its parallel scheme based on the lattice Boltzmann method (LBM) results in high computational efficiency, making it suitable for large-scale simulations, even though LBM requires small time steps. Important future development needs are identified, including the addition of a lubrication force correction model, performance enhancements, such as support for hybrid parallelization and GPU, and the extension of compatible contact models to accommodate concave shapes. These advances promise expanded capabilities for HLBM and broader applicability for solving complex real-world problems. Full article

Background: Precise continuous feeding of active pharmaceutical ingredients (APIs) and excipients is crucial in a continuous powder-to-tablet manufacturing setup, as any inconsistency can affect the final tablet quality. Method: This study investigated the impact of various materials on the performance of a continuous twin-screw loss-in-weight (LIW) feeder. The materials tested included spray-dried lactose, anhydrous lactose, granulated lactose, microcrystalline cellulose (MCC), an MCC–lactose preblend (50%:50% w/w ratio), and a co-processed excipient (lactose–lactitol at a 95%:5% w/w ratio). The feeding performance of these excipients was systematically assessed, focusing on powder densification and screw layering within the LIW feeder. Results: The results demonstrated densification for the spray-dried lactose and preblend. Densification was more pronounced during the initial feeding cycles for spray-dried lactose, but decreased gradually over time. In contrast, the densification remained relatively constant throughout the feeding process for the preblend. Notably, minor screw layering was observed for both spray-dried lactose and anhydrous lactose, with the extent of this issue reducing over time for the spray-dried lactose. Interestingly, granulated lactose grades did not show screw layering, making them preferable for blending with APIs prone to severe screw layering. The LIW feeder control system successfully managed powder densification and minor screw layering, maintaining the mass flow rate at the set point for all investigated materials. Conclusions: These findings inform the selection of optimal excipients, appropriate tooling for LIW feeders, and the enhancement of control strategies to shorten startup times. By addressing these factors, the precision and reliability of continuous feeding processes can be improved. Full article

Particle systems and their efficient and precise separation are becoming increasingly complex. Therefore, instead of focusing on a single separation feature, a multidimensional approach is needed where more than one particle property is considered. This, however, requires the precise characterization of the particle system, which is especially challenging for fine particles with sizes below 10 µm. This paper discusses the benefits and limitations of different characterization techniques, including optical contour analysis, inverse gas chromatography, flow cytometry, and SEM-based image analysis. The separation of ultrafine particles was investigated for a binary system using froth flotation, where a novel developed flotation apparatus is used. A special focus was placed on the multidimensional evaluation of the separation according to the particle properties of size, shape, and wettability, which was addressed via multivariate Tromp and entropy functions. The results emphasize the intricacy of the flotation process and the complex interaction of the individual particle properties and process parameters. The investigations contribute to the understanding of the characterization of particulate properties as well as the separation behavior of ultrafine particles via froth flotation, especially in the case of a multidimensional approach. Full article