Powders

The separation of particles smaller than 1 µm either by composition or by size is still a challenge. For the separation of SiO₂ and SnO₂, the creation of a selective separation feature and the specific adsorption of salts and surfactants were investigated. The adsorption of various salts, e.g., AlCl₃, ZnCl₂, MnCl₂ and MgCl₂ were therefore analyzed, and the necessary concentration for the charge reversal of the material was determined. It was noticed that the investigated materials differ in their isoelectric point (IEP) and therefore in their adsorption behavior because only ZnCl₂ and MgCl₂ are suitable for a charge reversal of both metal oxides. The phase transfer of the pure material at different pH values with ZnCl₂ or MgCl₂ and sodium dodecyl sulfate (SDS) revealed that the adsorption behavior of the particle has an influence on the phase transfer. As a result, the phase transfer of SiO₂ is pH dependent, whereas the phase transfer of SnO₂ operates over a wider pH range. This allowed the separation of SiO₂ and SnO₂ to be controlled by the salt and surfactant concentration as well as pH. The separation of SiO₂ and SnO₂ was investigated for various parameters such as salt and surfactant concentration, particle concentration and composition of the mixture. Also, pH 8, where a selective phase transfer for SiO₂ occurs, and pH 6, where the greatest difference between the materials exists, were also investigated. By comparing the parameters, it was found that the combination of ZnCl₂/SDS and MgCl₂/SDS enables a selective separation of the materials. Furthermore, it was also found that the concentration of SDS has a significant effect on the separation, as the formation of a bilayer structure is important for the separation, and therefore, higher SDS concentrations are required at higher particle concentrations to increase the separation efficiency. Full article

The effect of induction heating on alumina ceramics and alumina ceramic composites based on α-Al₂O₃ nanopowders (additives: SiC, Si₃N₄, SiO₂, ZrO₂) has been examined. Various factors such as the structure, grain size, distribution of elements, hardness, fracture toughness, and wear rate of hot-pressed ceramic materials were assessed. Despite achieving improved densification of alumina ceramics at a higher temperature of 1720 °C, there is a consistent trend toward a decline in hardness and fracture toughness. Heating at lower temperatures of 1300–1500 °C results in the development of a strengthened surface layer with a fine-grained structure enriched with carbon. Therefore, the wear rate behavior of such ceramics differs from the behavior of samples made at higher temperatures of 1600–1720 °C. This fact indicates the presence of a non-thermal microwave effect of induction heating. The incorporation of additives to alumina leads to the formation of novel structures with altered crack propagation patterns. The optimal ceramic composite, containing 5 wt. % SiC, displayed superior hardness and the lowest wear rate when compared to pure alumina ceramics. Across all investigated composites, a short dwell time at 1700 °C results in an enhancement of the mechanical properties. Full article

The drying structures of droplets of colloidal aqueous dispersions exhibit a wide variety of patterns depending on experimental conditions. It has been established by previous researchers that capillary flows and Marangoni convection significantly influence the macroscopic pattern formation. To the best of our knowledge, this study is the first to focus on sessile droplets of aqueous dispersions containing hollow particles. These hollow particles have a lower density than water and thus float in the medium. The drying pattern of these droplets was markedly different from the well-known ring pattern. Instead, a bump-shaped structure—often referred to as a “coffee-eye”—was formed due to the accumulation of particles at the center of the dried film. While a ring pattern was still present, it was extremely narrow and barely noticeable. This behavior is attributed to the dominance of the buoyant motion of the hollow particles, which prevented their transport by capillary flow. The findings of this study provide fundamental and important insights into the drying structures of various types of colloidal droplets. Full article

The drying process of microcrystalline cellulose and adipic acid particles in a cylindrical fluidized bed was investigated using the Gaussian spectral technique to monitor fluid–dynamic regime transitions associated with surface moisture loss. Pressure fluctuation signals were recorded and analyzed to assess hydrodynamic behavior. Excess moisture significantly alters the bubbling characteristics of the bed, leading to instability in the fluidization regime. The results demonstrated that the Gaussian spectral technique effectively captured these hydrodynamic changes, particularly at the critical moisture content threshold, when compared with the drying rate curves of the materials. For microcrystalline cellulose and adipic acid particles, it is reasonable to conclude that a mean central frequency above 5.75–6.0 Hz and a standard deviation exceeding 3.7–3.8 Hz correspond to a bubbling regime, indicating that the critical drying point has been reached. This approach provides a non-intrusive and sensitive method for identifying transitions in the drying process, offering a valuable tool for real-time monitoring and control. The ability to track fluidization regime changes with high precision reinforces the potential of this technique for optimizing drying operations in the pharmaceutical, food, and chemical industries. Full article

Characterizing powder feedstock is crucial for ensuring the quality and reliability of parts produced through metal additive manufacturing (AM). The morphology of particles impacts the flowability, packing density, and spreadability of powders, affecting productivity and part quality. A new methodology has been developed to classify particle morphological features in AM powder feedstocks, such as spherical or elongated shapes, and the presence of satellites and facets. This approach uses multiple descriptors for quantitative evaluation. The results from shape descriptors can vary based on image resolution, gray/color thresholding, and software algorithms. There are various commercial systems available for characterizing particle shape, some of which use images taken of static particles, while others use images of particles in motion. This diversity can lead to differences in powder characterization across laboratories with different equipment and methods. This paper compares results from a particle classification approach using two software programs that work with metallographic images with those from an automated static particle analyzer. While traditional methods offer higher resolution and precision, this study shows that automated systems can achieve similar particle shape classification using different shape descriptors and thresholds. Full article

Plant by-products are undervalued as they are an important source of nutrients and bioactive compounds with potential health benefits, which also contribute to aroma and color. Therefore, their use in human food is a challenging field of study that deserves to be explored. This study proposes the conversion of fava bean pods into a powdered product as a high-quality, stable, and easy-to-handle food ingredient, thus contributing to the sustainability of the food industry within the framework of the circular economy. The powdered product was obtained by freeze-drying and grinding. As the particle size of powders is a determinant of their quality and functionality, some properties of two bean pod powder samples with mean particle sizes of 102.9 and 45.3 μm, obtained by sieving at 200 and 45 μm, respectively, are compared. The results obtained indicate good flowability of both powders. However, the sample with the largest size showed, in addition to a greener tone, lower interparticle porosity related to a better packing capacity, lower hygroscopicity, and much better wettability, along with its higher swelling capacity and water and oil retention capacity. Nevertheless, in this case, the extraction of proteins and phenols decreased by 18% and 25%, respectively, without compromising the total fiber content. Considering the use of fava bean pod powder as a versatile food ingredient, the largest size of those studied, 102.9 μm, is recommended. Only if the objective is to obtain a healthy food supplement would it be more desirable to grind it to a smaller particle size. Full article

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