Lucia Pedone

Synthesis, size control, and passivation of CdS nanoparticles in water/AOT/n-heptane microemulsions

Abstract CdS nanoparticles have been synthesised by adding tetrabutylammonium hydrogen sulphide to water/sodium bis(2-ethylhexyl) sulfosuccinate/ n -heptane microemulsions containing CdSO 4 . Analysis of UV–Vis absorption spectra recorded at various times indicates that an initial rapid formation of CdS nanoparticles is followed by a very slow growth process which can be well described by a power law. The growth process is totally inhibited by the addition of an appropriate amount of bis(2-ethylhexyl)amine (BEA) leading to the formation of stable nanosized CdS particles coated by an oriented monolayer of chemically bonded BEA molecules. Depending on the BEA addition time, the growth inhibition can be achieved at any moment of the process leading to an easy and fine size control. The main advantage of this procedure is that the BEA-coated CdS nanoparticles can be easily separated from the reaction medium and dispersed in nonpolar media such as heptane and in polar media such as an aqueous surfactant solution.

Luminescence Properties of Neodymium-Doped Yttrium Aluminium Garnet Obtained by the Co-Precipitation Method Combined with the Mechanical Process

Nanopowders of yttrium aluminium garnet Y3Al5O12 (YAG) doped with neodymium ions were obtained by the co-precipitation method from the reaction of aluminium and yttrium nitrate and neodymium oxide with ammonia. After washing and drying the hydroxide precursors were calcined at 500, 700, 800 and 900 °C for 1 hour and at 1000 °C for 3 hours. This product was treated by ball milling in a zirconia vial for 0.5, 1.5 and 10 h in order to achieve smaller nanoparticles. The structure, microstructure, morphology and optical properties were investigated by means of diffractometric, microscopic and spectroscopic techniques. The course of the amorphous-to-crystalline transformation was complete after calcining the powder for 1 hour at 900 °C. In the sample calcined for 3 hours at 1000 °C, the mean size of crystallite microdomains was reduced from 600 Å to 300, 250 and 160 Å after 0.5, 1.5 and 10 h of mechanical treatment respectively. The treated product was found to be contaminated with ZrO2. This contamination, from the vial and hardened ZrO2 balls reaches ca. 30 wt % after 10 h of mechanical treatment but causes only a slight reduction of the neodymium luminescence life-time, thus maintaining significant applicative properties.

Microwave Radiation Effect On The Synthesis Of Cadmium Sulphide Nanoparticles In Water In Oil Microemulsion: A Preliminary Study At Different Frequencies

Abstract Cadmium sulphide nanoparticles have been synthesised in water/sodium bis (2-ethylhexyl) sulfosuccinate (AOT)/n- heptane microemulsions kept at 30 °C by microwave irradiation coupled with water-cooling and in conventional thermostatic conditions at the same temperature. The study has been performed exposing the reaction media to microwave radiation at five different frequencies (2.45, 2.85, 8, 12 and 18 GHz). For each frequency, a suitable microwave exposure set-up has been assembled. During the growth process, the dimensions of the nanoparticles have been characterised by means of UV-Vis spectroscopy. At the end of the growth process, the surface morphology of the nanoparticles has been determined by using photoluminescence (PL) measurements. Results indicate that compared to conventional thermostatic conditions, microwave irradiation influences nanoparticle growth kinetics, affecting both the final size and surface morphology structure. The effect is microwave frequency dependent.

A novel radiation exposure control apparatus for microwave assisted chemical reactions

Abstract A radiation exposure control apparatus is used for microwave (2.45 GHz) treatment of chemical reactions in controlled and reproducible conditions. A spectrophotometer has been interfaced with the microwave set-up in order to monitor the reaction evolution in situ. Both numerical and experimental dosimetries are carried out in order to evaluate the field distribution within the sample. Finally, particular working conditions are suggested.

Structural effects of macrocyclic compounds and their partition in sodium dodecylsulphate aqueous solutions

The partition of 1,4,7,10,13,16-esaoxacyclooctadecane (18C6), 4,7,13,16-tetraoxa-1,10-diazacyclooctadecane (2.2), 2,5,8,11,14,17-esaoxabicyclo[16.4.0]dicosane (B18C6) and 2,5,8,15,18,21-esoxatricyclo[20.4.0.09.14]esacosane (Cy218C6) in sodium dodecyl sulfate (SDS) aqueous solutions and their effect on the structure of surfactant aggregates has been investigated by small-angle neutron scattering. Results from data analysis have shown that by increasing macrocycle concentration the SDS micelles dimensions reduce for all systems investigated. At the same time information on macrocycles partition between the micellar and the continuous phase have been obtained. It was found that an appreciable portion of macrocyclic compounds is located in micellar aggregates; in particular, the amount of B18C6 and Cy218C6 results larger than that of 18C6 and 2.2. It was found that 18C6 and 2.2 molecules interact with charged surface of SDS micelles only via complexes formation between the sodium ions and the macrocycles. B18C6 and Cy218C6 interact either via complexes formation with the charged surface or with hydrophobic region inside the micelle, as a consequence of the presence of hydrophobic substituents. It was concluded that Cy218C6 fraction present inside the micelles is located in the core, while the B18C6 fraction is located in the palisade.

Formation of α-ω(4,7,10,13-pentaoxa-16-azacyclooctadecane) hexadecane micelles in aqueous solution: effect of HCl addition

The structure of aggregates of a new bolaform surfactant [α-ω) (4,7,10,13-pentaoxa-16-azacyclooctadecane) hexadecane] in neat aqueous solution has been investigated by small-angle neutron scattering. Preliminary data analysis unequivocally indicates that globular micelles are formed. This finding has been confirmed by the analysis of data obtained upon addition of hydrochloric acid. The observed significant reduction of micelle aggregation number has been attributed to the peculiar complexing ability of the two aza-crown ether units in the surfactant molecule; this is in line with information inferred from the complexation of ions into the non alkylated azacrown ethers. As a consequence of hydrogen ion uptake into the aza-crown ether unit, the partial ionization of surfactant causes a decrease in the micelle dimension that follows the increased repulsion among head groups.