Three silicon oxycarbide glasses (SiCO) with increasing C content were obtained through pyrolysis in inert atmosphere at 1000 °C of sol-gel derived siloxane networks containing Si-CH 3 and Si-H bonds. The glasses were further annealed at 1200, 1400, and 1500 °C to follow their evolution at high temperature. Quantitative information concerning the structure of glasses before and after annealing at high temperature was collected with a wide range of techniques (some of them used for the first time in this field) with the aim of probing the following: (i) the short-range order and chemical composition ( 29 Si and 1 H MAS NMR, RDF derived from X-ray and neutron scattering, inelastic neutron scattering, FT-IR, and elemental analysis), and (ii) the long-range order (X-ray and neutron diffraction) and microstructural features (HR-TEM combined with electron diffraction, Raman, porosity, and surface area measurements). This extensive collection of data, carried out on the same set of specimens, provided detailed and sound structural information on nearly-stoichiometric SiCO glasses and their high-temperature behavior.
Poly‐acrylic acid (PAAc) terminated silicon nanoparticles (SiNPs) have been synthesized and employed as a synchronous fluorescent signal indicator in a series of cultured mammalian cells: HHL5, HepG2 and 3T3‐L1. Their biological effects on cell growth and proliferation in both human and mouse cell lines have been studied. There was no evidence of in vitro cytotoxity in the cells exposed to PAAc terminated SiNPS when assessed by cell morphology, cell proliferation and viability, and DNA damage assays. The uptake of the nanocrystals by both HepG2 and 3T3‐L1 cells was investigated by confocal microscopy and flow cytometry, which showed a clear time‐dependence at higher concentrations. Reconstructed 3‐D confocal microscope images exhibited that the PAAc‐SiNPs were evenly distributed throughout the cytosol rather than attached to outer membrane. This study provides fundamental evidence for the safe application and further modification of silicon nanoparticles, which could broaden their application as cell markers in living systems and in micelle encapsulated drug delivery systems.
The influence of particle size on near-infra red (NIR) spectra is typically considered a 'nuisance factor' which many scatter correction methods attempt to eliminate, e.g., multiplicative scatter correction. However, particle size is a key issue in the formulation of many pharmaceutical products and has a profound effect on the behaviour of both raw materials and drug substances during formulation. NIR has already been demonstrated as a potential alternative particle sizing technique to current accepted methodology. This investigation assessed several chemometric approaches that model this information, using lactose monohydrate as the raw material. A variety of modelling techniques were applied to both zero order and second derivative spectra namely multiple linear regression, partial least squares, principal component regression and artificial neural networks. One further data transformation evaluated was polar coordinates, although no statistical data were generated. Typically, cross-validation root mean square errors of calibration and cross-validation root mean square errors of prediction of approximately 5 microns were calculated for all of the modelling techniques. These values are comparable to those associated with the reference technique (laser diffractometry). Correlation coefficients of approximately 0.98 for all techniques were also calculated. The predictive abilities for models generated using second derivative spectra were found to be comparable to those obtained using zero order spectra.
Gel to glass transformation of methyltriethoxysilane was investigated using infrared and Raman spectroscopies. The vibrational frequencies of the Si-O network are found to be a sensitive probe of the gel to glass transformation, which is measured to be at ca. 950°C for this system, under the experimental conditions used for the synthesis. Vibrational data are also compatible with an earlier suggestion of the presence of polyhedral silsesquioxanes type structures embedded in a 3-D network. Further evidence is presented for the formation of Si-CH 2 -Si and Si-C 2 H 4 -Si units during the pyrolysis process.
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