The sonochemical synthesis of stable palladium nanoparticles has been achieved by ultrasonic irradiation of palladium(II) nitrate solution. The starting solutions were prepared by the addition of different concentrations of palladium(II) nitrate in ethylene glycol and poly(vinylpyrrolidone) (PVP). The resulting mixtures were irradiated with ultrasonic 50 kHz waves in a glass vessel for 180 min. The UV-visible absorption spectroscopy and pH measurements revealed that the reduction of Pd(II) to metallic Pd has been successfully achieved and that the obtained suspensions have a long shelf life. The protective effect of PVP was studied using Fourier transform infrared (FT-IR) spectroscopy. It has been found that, in the presence of ethylene glycol, the stabilization of the nanoparticles results from the adsorption of the PVP chain on the palladium particle surface via the coordination of the PVP carbonyl group to the palladium atoms. The effect of the initial Pd(II) concentration on the Pd nanoparticle morphology has been investigated by transmission electron microscopy. It has been shown that the increase of the Pd(II)/PVP molar ratio from 0.13 x 10(-3) to 0.53 x 10(-3) decreases the number of palladium nanoparticles with a slight increase in particle size. For the highest Pd(II)/PVP value, 0.53 x 10(-3), the reduction reaction leads to the unexpected smallest nanoparticles in the form of aggregates.
Nanostructured Fe and Fe 50 Co 50 powders were prepared by high-energy ball milling. Microstructural and magnetic properties changes with milling time were followed by x-ray diffraction, differential scanning calorimetry and vibrating sample magnetometry. The nonequilibrium microstructure originates from a grain size reduction to about 12 nm and the introduction of internal strain up to 1.5% (root-mean-square strain). The occurrence of disorder in the ball-milled powders is evidenced by the broad exothermic reaction during the heating of ball-milled samples, the variation of lattice parameters and the increase of the saturation magnetization during the first 3 h of milling for Fe and continuously for the Fe 50 Co 50 powder mixture. According to both the reduction of Fe Curie temperature, T c , and the increase of the phase transformation T α→γ , the paramagnetic temperature domain of nanostructured bcc α-Fe is extended by about 50 • C. The Fe 50 Co 50 nanostructured powder behaves as a soft ferromagnet with low values of both the coercive field and the squareness ratio M r /M s .
Mullite-anorthite-albite porous ceramic materials were successfully prepared by a solid-state reaction between kaolin clay and two different additives (CaCO 3 and Na 2 CO 3 ). The starting raw material was characterized by X-ray fluorescence, X-ray diffraction (XRD) and dynamic light scattering techniques. The effect of CaCO 3 and Na 2 CO 3 concentration (10 to 70 wt%) on structure, morphology and thermal properties of the obtained ceramics was investigated by XRD, scanning electron microscopy and differential scanning calorimetry (DSC) techniques. The XRD patterns showed that mullite (3Al 2 O 3 .2SiO 2 ), anorthite (CaO.Al 2 O 3 .2SiO 2 ) and albite (Na 2 O.Al 2 O 3 .6SiO 2 ) were the main crystalline phases present in the materials. The morphology investigation revealed the porous texture of obtained ceramics characterized by the presence of sponge-like structure mainly due to the additive decomposition at high temperatures. The DSC results confirm the presence of four temperature regions related to the kaolin thermal transformations and the formation of minerals. The temperature and enthalpy of mineral formation are additive concentration dependent. As a result, the optimal content of additives which allowed the coexistence of the three phases, a spongelike morphology, and high porosity without cracks corresponded to 15 wt% CaCO 3 , 15 wt% Na 2 CO 3 , and 70 wt% kaolin.
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