Here we report the synthesis of barium sulphate (BaSO4) nanoparticles from Ba(OH)2/BaCl2solutions by a combined method of precipitation and quenching in absence of polymer stabilizers. Transmission electron microscopy (HRTEM), Fourier transforms infrared spectroscopy (FTIR), and X-ray diffraction (XRD) were employed to characterize the particles. The Scherrer formula was applied to estimate the particle size using the width of the diffraction peaks. The obtained results indicate that the synthesized material is mainly composed of nanocrystalline barite, with nearly spherical morphology, and diameters ranging from 4 to 92 nm. The lattice images of nanoparticles were clearly observed by HRTEM, indicating a high degree of crystallinity and phase purity. In addition, agglomerates with diameters between 20 and 300 nm were observed in both lattice images and dynamic light scattering measurements. The latter allowed obtaining the particle size distribution, the evolution of the aggregate size in time of BaSO4in aqueous solutions, and the sedimentation rate of these solutions from turbidimetry measurements. A short discussion on the possible medical applications is presented.
A temperature-controlled X-ray powder diffraction experiment, complemented with TGA and DSC analysis, allowed us to follow changes in the molecular conformation and hydrogen-bond patterns of 4-piperidinecarboxylic acid. The presence of three phases is confirmed. Phase 1 represents the monohydrated form of 4-piperidinecarboxylic acid, which exists from room temperature to 359 K, where dehydration occurs. Phase 2 measured at 363 K corresponds to an anhydrous form of the acid. At ca 458 K the onset of a second, more gradual transition is observed, which ends at around 543 K. Phase 3 measured at 543 K is a high-temperature anhydrous form of the acid. The structures of phases 2 and 3 were solved from synchrotron powder diffraction data by simulated annealing using the DASH program and refined by the Rietveld method. The phase changes are accompanied by modification of the hydrogen-bond patterns and of the torsional orientation of the terminal carboxylate group. This group makes a 49 degrees rotation about the C1-C2 bond during the first transition.
Silver selenide (Ag2Se) is a promising nanomaterial due to its outstanding optoelectronic properties and countless bio-applications. To the best of our knowledge, we report, for the first time, a simple and easy method for the ultrasound-assisted synthesis of Ag2Se nanoparticles (NPs) by mixing aqueous solutions of silver nitrate (AgNO3) and selenous acid (H2SeO3) that act as Ag and Se sources, respectively, in the presence of dissolved fructose and starch that act as reducing and stabilizing agents, respectively. The concentrations of mono- and polysaccharides were screened to determine their effect on the size, shape and colloidal stability of the as-synthesized Ag2Se NPs which, in turn, impact the optical properties of these NPs. The morphology of the as-synthesized Ag2Se NPs was characterized by transmission electron microscopy (TEM) and both α- and β-phases of Ag2Se were determined by X-ray diffraction (XRD). The optical properties of Ag2Se were studied using UV–Vis spectroscopy and its elemental composition was determined non-destructively using scanning electron microscopy–energy-dispersive spectroscopy (SEM–EDS). The biological activity of the Ag2Se NPs was assessed using cytotoxic and bactericidal approaches. Our findings pave the way to the cost-effective, fast and scalable production of valuable Ag2Se NPs that may be utilized in numerous fields.
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