Passivated gold nanoparticles were synthesized through a microwave-assisted process in a two-phase system, in the presence of 1-dodecanethiol. An average particle size of 1.8 nm of the gold nanoparticles obtained and 0.35 S.D. was determined through HRTEM and STEM analysis. It was observed that these nanoparticles spontaneously self-assemble into self-supported superstructures of 1 μm in diameter avg and 400 nm thickness, yielding an off-white powder which can be handled as a simple powder. XRD analysis indicates that n-alkanethiol molecules used as a passivating compound, besides protecting against crystal growth, interact to form cubic ordered arrays between the nanoparticles. This interaction leads to the superstructure formation, with an average distance between nanoparticles in the array, of 3.56 nm. Theoretical calculations and molecular dynamics simulations were performed to analyze the resulting structure.
In this study, hydroxyapatite was synthesized using a microwave-assisted hydrothermal method. Calcium nitrate tetrahydrate (Ca(NO3)2·4H2O) and ammonium phosphate ((NH4)2HPO4) served as precursors in a pH 10 ammonium hydroxide (NH4OH) solution. Polyvinylpyrrolidone (PVP) was employed as a surfactant at varying concentrations of 0 (M0), 0.1% (M1), 0.2% (M2), and 0.3%wt (M3) to control particle size and morphology. The synthesized samples were characterized using Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FTIR). The addition of PVP during synthesis resulted in Ca/P ratios ranging from 0.93 to 1.37, and promoted predominantly rod-like morphologies. Samples M1 and M3 exhibited average diameters of 11.23–104.24 nm and lengths of 47.21–222.32 nm. XRD analysis confirmed the presence of both hexagonal and monoclinic phases, with crystallite sizes varying from 18.66 to 22.49 nm. FTIR spectra of sample M1 revealed an elongation at 3432 cm−1 corresponding to OH− groups, indicative of water absorption within the material structure. Vibrational bands at 2950–2300, 1090, and 975 cm−1, attributed to C–H bonds in PVP were also identified. These findings highlight the influence of PVP concentration on the structural and morphological properties of hydroxyapatite, providing insights into its potential applications in various fields.
24 April 2023 in Journal of Materials Engineering and Performance