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Recently, we have developed an algorithm to quantitatively evaluate the roughness of spherical microparticles using scanning electron microscopy (SEM) images. The algorithm calculates the root-mean-squared profile roughness (RMS-RQ) of a single particle by analyzing the particle's boundary. The information extracted from a single SEM image yields however only two-dimensional (2D) profile roughness data from the horizontal plane of a particle. The present study offers a practical procedure and the necessary software tools to gain quasi three-dimensional (3D) information from 2D particle contours recorded at different particle inclinations by tilting the sample (stage). This new approach was tested on a set of polystyrene core-iron oxide shell-silica shell particles as few micrometer-sized beads with different (tailored) surface roughness, providing the proof of principle that validates the applicability of the proposed method. SEM images of these particles were analyzed by the latest version of the developed algorithm, which allows to determine the analysis of particles in terms of roughness both within a batch and across the batches as a routine quality control procedure. A separate set of particles has been analyzed by atomic force microscopy (AFM) as a powerful complementary surface analysis technique integrated into SEM, and the roughness results have been compared.

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Soft magnetic composite cores were produced by spark plasma sintering (SPS) from Ni3Fe@ZnFe2O4 and NiFeMo@ZnFe2O4 pseudo-core-shell powders. In the Fe-Ni alloys@ZnFe2O4 pseudo-core-shell composite powders, the core is a large nanocrystalline Permalloy or Supermalloy particle obtained by mechanical alloying, and the shell is a pseudo continuous layer of Zn ferrite particles. The pseudo-core-shell powders have been compacted by SPS at temperatures between 500-700 °C, with a holding time of 0 min. Several techniques were used for the characterisation of the powders and sintered compacts: X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, magnetic hysteresis measurements (DC and AC), and electrical resistivity. The electrical resistivity is stabilised at values of about 7 × 10-3 Ω·m for sintering temperatures between 600-700 °C and this value is three orders of magnitude higher than the electrical resistivity of sintered Fe compacts. The best relative initial permeability was obtained for the Supermalloy/ZnFe2O4 composite compacts sintered at 600 °C, which decreases linearly for the entire frequency range studied, from around 95 to 50. At a frequency of 2000 Hz, the power losses are smaller than 1.5 W/kg. At a frequency of 10 kHz, the power losses are larger, but they remain at a reduced level. In the case of Supermalloy/ZnFe2O4 composite compact SPS-ed at 700 °C, the specific power losses are even lower than 5 W/kg. The power losses' decomposition proved that intra-particle losses are the main type of losses.

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This study investigated the sustainable room-temperature synthesis of In3Sn/γ-Ga2O3 core-shell particles via an acoustic route using molten eutectic Ga-In-Sn alloy (EGaInSn). Sonication was used for the emulsification and oxidation steps. During the emulsification step, the sonication of molten EGaInSn in ethanol (EtOH) at 45 kHz facilitated the formation of the smallest EGaInSn particles (average diameter, Dav = 782 nm). In terms of EGaInSn particle size, 45 kHz sonication was suitable for emulsification of molten EGaInSn and ethanol system than 24 kHz sonication. During the oxidation step, the preferential oxidation of Ga in the EGaInSn particles occurred via sonication in a solution of EtOH and hydrazine monohydrate (N2H4·H2O). This selective oxidation of Ga on the surface of the EGaInSn particles resulted in the formation of In3Sn/γ-Ga2O3 core-shell particles via sonication at 45 kHz and room temperature. The entire process eliminated the need for dispersants and high-temperature treatments. Additionally, the process did not generate waste fluid containing counter anions, such as chloride anions. This sustainable sonochemical method offers a carbon-neutral approach for synthesizing functional nanocomposites with improved safety, simplicity, and energy efficiency.

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Due to the favorable features obtained through the incorporation of fluorine atom(s), fluorinated drugs are a group with emerging pharmaceutical importance. As their commercial availability is still very limited, to expand the range of possible candidates, new fluorinated tryptophan analogs were synthesized. Control of enantiopurity during the synthesis procedure requires that highly efficient enantioseparation methods be available. In this work, the enantioseparation of seven fluorinated tryptophans and tryptophan was studied and compared systematically to (i) develop analytical methods for enantioselective separations and (ii) explore the chromatographic features of the fluorotrytophans. For enantioresolution, macrocyclic glycopeptide-based selectors linked to core-shell particles were utilized, applying liquid chromatography-based methods. Application of the polar-ionic mode resulted in asymmetric and broadened peaks, while reversed-phase conditions, together with mobile-phase additives, resulted in baseline separation for all studied fluorinated tryptophans. The marked differences observed between the methanol and acetonitrile-containing eluent systems can be explained by the different solvation abilities of the bulk solvents of the applied mobile phases. Among the studied chiral selectors, teicoplanin and teicoplanin aglycone were found to work effectively. Under optimized conditions, baseline separations were achieved within 6 min. Ionic interactions were semi-quantitatively characterized and found to not influence enantiorecognition. Interestingly, fluorination of the analytes does not lead to marked changes in the chromatographic characteristics of the methanol-containing eluents, while larger differences were noticed when the polar but aprotic acetonitrile was applied. Experiments conducted on the influence of the separation temperature indicated that the separations are enthalpically driven, with only one exception. Enantiomeric elution order was found to be constant on both teicoplanin and teicoplanin aglycone-based chiral stationary phases (L < D) under all applied chromatographic conditions.

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The co-assembly of polyelectrolytes (PE) with proteins offers a promising approach for designing complex structures with customizable morphologies, charge distribution, and stability for targeted cargo delivery. However, the complexity of protein structure limits our ability to predict the properties of the formed nanoparticles, and our goal is to identify the key triggers of the morphological transition in protein/PE complexes and evaluate their ability to encapsulate multivalent ionic drugs. A positively charged PE can assemble with a protein at pH above isoelectric point due to the electrostatic attraction and disassemble at pH below isoelectric point due to the repulsion. The additional hydrophilic block of the polymer should stabilize the particles in solution and enable them to encapsulate a negatively charged drug in the presence of PE excess. We demonstrated that diblock copolymers, poly(ethylene oxide)-block-poly(N,N-dimethylaminoethyl methacrylate) and poly(ethylene oxide)-block-poly(N,N,N-trimethylammonioethyl methacrylate), consisting of a polycation block and a neutral hydrophilic block, reversibly co-assemble with insulin in pH range between 5 and 8. Using small-angle neutron and X-ray scattering (SANS, SAXS), we showed that insulin arrangement within formed particles is controlled by intermolecular electrostatic forces between protein molecules, and can be tuned by varying ionic strength. For the first time, we observed by fluorescence that formed protein/PE complexes with excess of positive charges exhibited potential for encapsulating and controlled release of negatively charged bivalent drugs, protoporphyrin-IX and zinc(II) protoporphyrin-IX, enabling the development of nanocarriers for combination therapies with adjustable charge, stability, internal structure, and size.

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The powder aerosol deposition (PAD) method is a process to manufacture ceramic films completely at room temperature. Since the first reports by Akedo in the late 1990s, much research has been conducted to reveal the exact mechanism of the deposition process. However, it is still not fully understood. This work tackles this challenge using core-shell particles. Two coated oxides, Al2 O3 core with a SiO2 shell and LiNi0.6 Mn0.2 Co0.2 O2 core with a LiNbO3 shell, are investigated. Initially, the element ratios Al:Si and Ni:Nb of the powder are determined by energy-dispersive X-ray spectroscopy (EDX). In a second step, the change in the element ratios of Al:Si and Ni:Nb after deposition is investigated. The element ratios from powder to film strongly shift toward the shell elements, indicating that the particles fracture and only the outer parts of the particles are deposited. In the last step, this work investigates cross-sections of the deposited films with scanning transmission electron microscopy (STEM combined with EDX and an energy-selective back-scattered electron (EsB) detector to unveil the element distribution within the film itself. Therefore, the following overall picture emerges: particles impact on the substrate or on previously deposited particle, fracture, and only a small part of the impacting particles that originate from the outer part of the impacting particle gets deposited.

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HYPOTHESIS: Calcium carbonate (CaCO3) nanoparticles could have great potential for contrast-enhanced ultrasound imaging (CEUS) due to their gas-generating properties and sensitivity to physiological conditions. However, the use of nano CaCO3 for biomedical applications requires the assistance of stabilizers to control the size and avoid the fast dissolution/recrystallization of the particles when exposed to aqueous conditions. EXPERIMENTS: Herein, we report the stabilization of nano CaCO3 using lignin, and synthesized core-shell amorphous CaCO3-lignin nanoparticles (LigCC NPs) with a diameter below 100 nm. We have then investigated the echogenicity of the LigCC NPs by monitoring the consequent generation of contrast in vitro for 90 min in linear and non-linear B-mode imaging. FINDINGS: This research explores how lignin type and structure affect stabilization efficiency, lignin structuration around CaCO3 cores, and particle echogenicity. Interestingly, by employing lignin as the stabilizer, it becomes possible to maintain the echogenic properties of CaCO3, whereas the use of lipid coatings prevents the production of signal generation in ultrasound imaging. This work opens new avenue for CEUS imaging of the vascular and extravascular space using CaCO3, as it highlights the potential to generate contrast for extended durations at physiological pH by utilizing the amorphous phase of CaCO3.

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The purpose of this study is to develop modified particles with different structures to improve the flowability and compactibility of Liuwei Dihuang (LWDH) powder using co-spray drying technology, and to investigate the preparation mechanism of modified particles and their modified direct compaction (DC) properties. Moreover, tablets with high drug loading contents were also prepared. Particles were designed using polyvinylpyrrolidone (PVP K30) and hydroxypropyl methylcellulose (HPMC E3) as shell materials, and sodium bicarbonate (NaHCO3) and ammonium bicarbonate (NH4HCO3) as pore-forming agents. The porous particles (Ps), core-shell particles (CPs), and porous core-shell particles (PCPs) were prepared by co-spray drying technology. The key DC properties and texture properties of all the particles were measured and compared. The properties of co-spray drying liquid were also determined and analyzed. According to the results, Ps showed the least improvement in DC properties, followed by CPs, and PCPs showed a significant improvement. The modifier, because of its low surface tension, was wrapped in the outer layer to form a shell, and the pore-forming agent was thermally decomposed to produce pores, forming core-shell, porous, and porous core-shell composite structures. The smooth surface of the shell structure enhances fluidity, while the porous structure allows for greater compaction space, thereby improving DC properties during the compaction process.

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SA/CS-coated TiO2NPs hybrid fibers with photocatalytic self-cleaning properties, UV resistance and enhanced tensile strength were successfully prepared by adding CS-coated TiO2NPs to SA matrix. The FTIR and TEM results demonstrate the successful preparation of CS-coated TiO2NPs core-shell structured composite particles. SEM and Tyndall effect results showed that the core-shell particles were uniformly dispersed in the SA matrix. When the content of Core-shell particles increased from 0.1 to 0.3 wt%, the tensile strength of SA/CS-coated TiO2NPs hybrid fibers increased from 26.89 to 64.45 % compared with SA/TiO2NPs hybrid fibers. The SA/CS-coated TiO2NPs hybrid fiber (0.3 wt%) exhibits excellent photocatalytic degradation performance, achieving a 90 % degradation rate for the RhB solution. And the fibers also exhibit outstanding photocatalytic degradation performance towards various dyes and stains commonly encountered in daily life, including methyl orange, malachite green, Congo red, coffee and mulberry juice. The UV transmittance of the SA/CS-coated TiO2NPs hybrid fibers decreased significantly from 90 % to 75 % with the increase in core-shell particle addition, and correspondingly, the UV absorption capacity increased. The SA/CS-coated TiO2NPs hybrid fibers prepared lay the groundwork for potential applications in various fields, including textiles, automotive engineering, electronics and medicine.

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Biomimetic apatites exhibit a high reactivity allowing ion substitutions to modulate their in vivo response. We developed a novel approach combining several bioactive ions in a spatially controlled way in view of subsequent releases to address the sequence of events occurring after implantation, including potential microorganisms' colonization. Innovative micron-sized core-shell particles were designed with an external shell enriched with an antibacterial ion and an internal core substituted with a pro-angiogenic or osteogenic ion. After developing the proof of concept, two ions were particularly considered, Ag+ in the outer shell and Cu2+ in the inner core. In vitro evaluations confirmed the cytocompatibility through Ag-/Cu-substituting and the antibacterial properties provided by Ag+. Then, these multifunctional "smart" particles were embedded in a polymeric matrix by freeze-casting to prepare 3D porous scaffolds for bone engineering. This approach envisions the development of a new generation of scaffolds with tailored sequential properties for optimal bone regeneration.

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Thick dielectric SiO2 shells on the surface of iron particles enhance the thermal and electrodynamic parameters of the iron. A technique to deposit thick, 500-nm, SiO2 shell to the surface of carbonyl iron (CI) particles was developed. The method consists of repeated deposition of SiO2 particles with air drying between iterations. This method allows to obtain thick dielectric shells up to 475 nm on individual CI particles. The paper shows that a thick SiO2 protective layer reduces the permittivity of the 'Fe-SiO2-paraffin' composite in accordance with the Maxwell Garnett medium theory. The protective shell increases the thermal stability of iron, when heated in air, by shifting the transition temperature to the higher oxide. The particle size, the thickness of the SiO2 shells, and the elemental analysis of the samples were studied using a scanning electron microscope. A coaxial waveguide and the Nicholson-Ross technique were used to measure microwave permeability and permittivity of the samples. A vibrating-sample magnetometer (VSM) was used to measure the magnetostatic data. A synchronous thermal analysis was applied to measure the thermal stability of the coated iron particles. The developed samples can be applied for electromagnetic compatibility problems, as well as the active material for various types of sensors.

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Soft magnetic composite (SMC) cores have been obtained by Spark Plasma Sintering (SPS) using pseudo core-shell powders. Pseudo core-shell powders are formed by a core of soft magnetic particle (nanocrystalline permalloy or supermalloy) surrounded by a thin layer (shell) of nanosized soft ferrite (Mn0.5Zn0.5Fe2O4). Three compositions of pseudo core-shell powders were prepared, with 1, 2 and 3 wt.% of manganese-zinc mixt ferrite. The pseudo core-shell powders were compacted by SPS at temperatures between 500 and 700 °C, with a holding time ranging from 0 to 10 min. Several techniques have been used for characterization of the samples, both, powders and compacts X-ray diffraction (XRD, scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), magnetic hysteresis measurements (DC and AC) and electrical resistivity. The electrical resistivity is in the order of 1 × 10-2 Ωm, 3-4 orders of magnitude higher than supermalloy electrical resistivity. The SPS at lower temperatures (500 °C) conserves the initial phases of the composite, but increasing the sintering temperature and/or sintering time produces a solid-state reaction between the alloy and ferrite phases, with negative consequence on the magnetic properties of the compacts. The initial relative permeability is around 40 and remains constant until to 2000 Hz. The power losses are lower than 2 W/kg until to 2000 Hz.

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This work addresses the functional properties of the core-shell resins Capto Core 400 and 700 for a broad range of proteins spanning 66.5 to 660 kDa in molecular mass, including bovine serum albumin (BSA) in monomer and dimer form, fibronectin, thyroglobulin, and BSA conjugates with 10 and 30 kDa poly(ethylene glycol) chains. Negatively charged latex nanoparticles (NPs) with nominal diameters of 20, 40, and 100 nm are also studied as surrogates for bioparticles. Protein binding and its trends with respect to salt concentration depend on the protein size and are different for the two agarose-based multimodal resins. For the smaller proteins, the amount of protein bound over practical time scales is limited by the resin surface area and is larger for Capto Core 400 compared with Capto Core 700. For the larger proteins, diffusion is severely restricted in Capto Core 400, resulting in lower binding capacities than those observed for Capto Core 700 despite the larger surface area. Adding 500 mM NaCl reduces the local bound protein concentration and diffusional hindrance resulting in higher binding capacities for the large proteins in Capto Core 400 compared with low ionic strength conditions. The NPs are essentially completely excluded from the Capto Core 400 pores. However, 20 and 40 nm NPs bind significantly to Capto Core 700, further hindering protein diffusion. A model is provided to predict the dynamic binding capacities as a function of residence time.

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Having fundamental insights in the properties of stationary phases and in the driving forces during the column packing process, is crucial to obtain highly efficient and robust packed-bed column technologies for use in separation science. Here we discuss the properties of the most commonly-used stationary-phases, i.e., silica particulate materials, including fully-porous and core-shell silica particles and provide an overview of the most commonly used column hardware and available frit technologies. The different packing approaches that are considered are dry packing, high-pressure slurry packing, electrokinetic packing, and packing using centrifugal forces. In particular, sedimentation of particles in slurries and particle interaction during the packing process affecting the resulting sphere packing are discussed.

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The present study discusses UHPLC method development allowing to establish ultra-high-resolution separations in gradient mode while operating at the kinetic performance limits, targeting the analysis of complex residual multi-class antibiotic samples in food products. The peak capacity and gradient occupation have been systematically assessed at different flow rates and gradient duration. The small particle size (1.5 µm core-shell particles) used in this study limits the mass-transfer contribution to band broadening when operating at high flow rate. As a result, for high-throughput analysis, high-pressure (1500 bar) operation leads to high resolving power where the gradient steepness dominates the peak capacity generation vs mass-transfer resistance. To reach the highest possible resolving power within a practically acceptable analysis time, one should use coupled-column systems at 1500 bar and adjust the gradient steepness correspondingly. Coupling four columns and applying a shallow gradient at 1500 bar led to a sample peak capacity of 379 in 140 min, allowing to resolve 71% of the analytes in a mixture composed of 61 milk antibiotics.

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The dissolution of a polymeric solid typically starts with the absorption of solvent molecules, followed by swelling and volume expansion. Only when the extent of swelling reaches a threshold can the polymer chains be disentangled and then dissolved into the solvent. When the polymeric solid is encapsulated in a rigid shell, the swelling process will be impeded. Despite the widespread use of this process, it is rarely discussed in the literature how the polymeric solid is dissolved from the core for the generation of colloidal hollow particles. Recent studies have started to shed light on the mechanistic details involved in the formation of hollow particles through a template-directed process. Depending on the nature of the material used for the template, the removal of the template may involve different mechanisms and pathways, leading to the formation of distinct products. Here, a number of examples are used to illustrate this important phenomenon that is largely neglected in the literature. This article also discusses how the swelling of a polymeric template encapsulated in a rigid shell can be leveraged to fabricate new types of functional colloidal particles.

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There has been very limited work on the control loading and release of the drugs aprepitant and sofosbuvir. These drugs need a significant material for the control of their loading and release phenomenon that can supply the drug at its target site. Magnetic nanoparticles have characteristics that enable them to be applied in biomedical fields and, more specifically, as a drug delivery system when they are incorporated with a biocompatible polymer. The coating with magnetic nanoparticles is performed to increase efficiency and reduce side effects. In this regard, attempts are made to search for suitable materials retaining biocompatibility and magnetic behavior. In the present study, silica-coated iron oxide nanoparticles were incorporated with core-shell particles made of poly(2-acrylamido-2-methylpropane sulfonic acid)@butyl methacrylate to produce a magnetic composite material (MCM-PA@B) through the free radical polymerization method. The as-prepared composite materials were characterized through Fourier-transform infrared (FTIR)spectroscopy, scanning electron microscopy (SEM), X-ray diffraction analysis (XRD), energy-dispersive X-Ray Analysis (EDX), and thermogravimetric analysis (TGA), and were further investigated for the loading and release of the drugs aprepitant and sofosbuvir. The maximum loading capacity of 305.76 mg/g for aprepitant and 307 mg/g for sofosbuvir was obtained at pH 4. Various adsorption kinetic models and isotherms were applied on the loading of both drugs. From all of the results obtained, it was found that MCM-PA@B can retain the drug for more than 24 h and release it slowly, due to which it can be applied for the controlled loading and targeted release of the drugs.

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To stabilize drugs physisorbed on the surface of hydroxyapatite (HAp) nanoparticles and prevent burst release, these nanoparticles are commonly coated with polymers. Bioactive HAp, however, becomes shielded from the surface of such core/shell entities, which partially defeats the purpose of using it. The goal of this study was to assess the biological and pharmacokinetic effects of inverting this classical core/shell structure by coating poly(lactic-co-glycolic acid) (PLGA) spheres with HAp nanoparticles. The HAp shell did not hinder the release of vancomycin; rather, it increased the release rate to a minor degree, compared to that from undecorated PLGA spheres. The decoration of PLGA spheres with HAp induced lesser mineral deposition and lesser upregulation of osteogenic markers compared to those induced by the composite particles where HAp nanoparticles were embedded inside the PLGA spheres. This was explained by homeostatic mechanisms governing the cell metabolism, which ensure than the sensation of a product of this metabolism in the cell interior or exterior is met with the reduction in the metabolic activity. The antagonistic relationship between proliferation and bone production was demonstrated by the higher proliferation rate of cells challenged with HAp-coated PLGA spheres than of those treated with PLGA-coated HAp. It is concluded that the overwhelmingly positive response of tissues to HAp-coated biomaterials for bone replacement is unlikely to be due to the direct induction of new bone growth in osteoblasts adhering to the HAp coating. Rather, these positive effects are consequential to more elementary aspects of cell attachment, mechanotransduction, and growth at the site of contact between the HAp-coated material and the tissue.

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In this study, green synthesis of modified Cu(OH)2 nanowires by Fe3O4@SiO2 core-shell nanospheres was easily performed via chemical reduction. In other words, the direct coating of Cu(OH)2 on Fe3O4@SiO2 was successfully realized without the extra complicated procedures. Various concentrations of synthesized nanocomposites were tested on pathogenic and nosocomial bacteria. In this study, the structural information and characterization of Fe3O4@SiO2/Cu(OH)2 nanowires (FSCNWs) were obtained using FE-SEM, FT-IR, EDX and X-ray diffraction. This nanocomposite can effectively kill important infectious bacteria, including Staphylococcus aureus, Escherichia coli, Staphylococcus saprophyticus, Pseudomonas aeruginosa and Klebsiella pneumoniae. Studies have shown that FSCNW nanocomposites affect common antibiotic-resistant bacteria. This result confirms the function of FSCNW as an effective, beneficial and environmentally friendly antibacterial agent that can used in a wide range of applications in medicine. FSCNWs can be separated conveniently from bacteria-containing solutions using a magnet. Compared with nanocomposites based on other metals such as silver and gold, the use of FSCNWs in water treatment has been recommended because of the precursor of copper for its low price and less toxicity. In addition to its special properties such as mild reaction conditions, green synthesis methods, admissible magnetic properties, easy separation, high antibacterial activity and beneficial efficiency.

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In this article, we report the preparation and structural features of Fe-Pd powder alloys formed by galvanic replacement, annealing and selective dissolution of iron via acid treatment. The alloys were studied by the X-ray diffraction phase analysis, Mössbauer spectroscopy, scanning electron microscopy, and energy-dispersive spectroscopy. The Fe@Pd core-shell particles were obtained by a galvanic replacement reaction occurring upon treatment of a body-centered cubic (bcc) iron powder by a solution containing PdCl42- ions. It was found that the shells are a face-centered cubic (fcc) Pd(Fe) solid solution. HCl acid treatment of the Fe@Pd core-shell particles resulted in the formation of hollow Pd-based particles, as the bcc phase was selectively dissolved from the cores. Annealing of the Fe@Pd core-shell particles at 800 °C led to the formation of fcc Fe-Pd solid solution. Acid treatment of the Fe-Pd alloys formed by annealing of the core-shell particles allowed selectively dissolving iron from the bcc Fe-based phase (Fe(Pd) solid solution), while the fcc Fe-rich Fe-Pd solid solution remained stable (resistant to acid corrosion). It was demonstrated that the phase composition and the Fe/Pd ratio in the alloys (phases) can be tailored by applying annealing and/or acid treatment to the as-synthesized Fe@Pd core-shell particles.