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Register a new userBiological activity of a SiO2-CaO-P2O5 sol-gel glass highlighted by PIXE-RBS methods
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J. Lao
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It is proposed in this study to observe the influence of P2O5 on the formation of the apatite-like layer in a bioactive glass via a complete PIXE characterization. A glass in the SiO2-CaO-P2O5 ternary system was elaborated by sol-gel processing. Glass samples were soaked in biological fluids for periods up to 10 days. The surface changes were characterized using Particle Induced X-ray Emission (PIXE) associated to Rutherford Backscattering Spectroscopy (RBS), which are efficient methods for multielemental analysis. Elemental maps of major and trace elements were obtained at a micrometer scale and revealed the bone bonding ability of the material. The formation of a calcium phosphate-rich layer containing magnesium occurs after a few days of interaction. We demonstrate that the presence of phosphorus in the material has an impact on the development and the formation rate of the bone-like apatite layer. Indeed, the Ca/P atomic ratio at the glass/biological fluids interface is closer to the nominal value of pure apatite compared to P2O5 free glasses. It would permit, in vivo, an improved chemical bond between the biomaterials and bone.
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For a long time, RBS and PIXE techniques have been used in the field of cultural heritage. Although the complementarity of both techniques has long been acknowledged, its full potential has not been yet developed due to the lack of general purpose software tools for analysing the data from both techniques in a coherent way. In this work we provide an example of how the recent addition of PIXE to the set of techniques supported by the DataFurnace code can significantly change this situation. We present a case in which a non homogeneous sample (an oxidized metal from a photographic plate -heliography- made by Niepce in 1827) is analysed using RBS and PIXE in a straightforward and powerful way that can only be performed with a code that treats both techniques simultaneously as a part of one single and coherent analysis. The optimization capabilities of DataFurnace, allowed us to obtain the composition profiles for these samples in a very simple way.
The evolution of viscoelastic properties near the sol-gel transition is studied by performing oscillatory rheological measurements on two different types of systems: a colloidal dispersion and a thermo-responsive polymer solution under isothermal and non-isothermal conditions. While undergoing sol-gel transition, both the systems pass through a critical point. An approach to the critical point is characterized in terms of divergence of zero shear viscosity and the subsequent appearance of the low frequency modulus. In the vicinity of the critical gel state, both the viscosity and the modulus show a power-law dependence on relative distance from the critical point. Interestingly, the longest relaxation time has been observed to diverge symmetrically on both the sides of the critical point and also shows a power-law dependence on relative distance from the critical point. The critical (power-law) exponents of the zero-shear viscosity and modulus are observed to be related to the exponents of the longest relaxation time by the hyper scaling laws. The dynamic critical exponent has also been calculated from the growth of the dynamic moduli. Remarkably, the critical relaxation exponent and dynamic critical exponent predicted from the scaling laws precisely agree with the experimental values from the isothermal as well as non-isothermal experiments. The associated critical exponents show remarkable internal consistency and universality for different kinds of systems undergoing the sol-gel transition.
Quaternary CaO-MgO-Al2O3-SiO2 glasses are important constituents of the Earths lower crust and mantle, and they also have important industrial applications such as in metallurgical processes, concrete production and emerging low-CO2 cement technologies. In particular, these applications rely heavily on the composition-structure-reactivity relationships for CMAS glasses, which are not yet well established. In this study, we developed a robust method that combines force-field molecular dynamics (MD) simulations and density functional theory (DFT) calculations with X-ray/neutron scattering experiments to resolve the atomic structure of a CMAS glass. The final structural representation generated using this method is not only thermodynamically favorable (according to DFT calculations) but also agrees with experiments (including X-ray/neutron scattering data as well as literature data). Detailed analysis of the final structure (including partial pair distribution functions, coordination number, oxygen environment) enabled existing discrepancies in the literature to be reconciled and has revealed new structural information on the CMAS glass, specifically, (i) the unambiguous assignment of medium-range atomic ordering, (ii) the preferential role of Ca atoms as charge compensators and Mg atoms as network modifiers, (iii) the proximity of Mg atoms to free oxygen sites, and (iv) clustering of Mg atoms. Overall, this new structural information will enhance our mechanistic understanding on CMAS glass dissolution behavior, including dissolution-related mechanisms occurring during the formation of low-CO2 cements.
In this contribution, the effect of P2O5 and SiO2 addition on the phase, microstructure, and electrical properties of KNbO3 was studied. Sample powders with the general formula (1-x)KNbO3.xP2O5 (x = 0.03, 0.05) and (1-x)KNbO3.xSiO2 (x = 0.1) were prepared via mixed-oxide route. The thermal behavior of the mixed-milled powder was investigated by TG/DTA which revealed an overall weight loss of 33.4 wt % in the temperature range of 30 < T < 1200 C and crystallization exotherm occurring at about 795 C. The present results indicated that P2O5 acted as a sintering aid and lowered the sintering temperature by about 30 C and promoted densification of KNbO3. Sample compositions at various stages of processing were characterized using X-ray diffraction. Samples sintered at T < 1020 C revealed mainly KNbO3 together with a couple of low-intensity K3NbO4 peaks as a secondary phase. The SEM images of (1-x)KNbO3.xSiO2 (x = 0.1) samples showed a slight increase in the average grain size from 3.76 um to 3.86 um with an increase in sintering temperature from 1000 C to 1020 C. Strong variations in dielectric constant and loss tangent were observed due to P2O5 and SiO2 addition as well as frequency of the applied AC signals.
Pt/Ti metallisation bilayers are used as bottom electrodes for ferroelectric thin films. During deposition of the ferroelectric films, these electrodes are exposed to elevated temperatures causing modifications of the Pt/Ti bottom electrode. Diffusion and oxidation of the Ti adhesion layer have been studied by the application of factor analysis to AES depth profile data and by RBS. Factor analysis was employed to extract the chemical information from the measured AES spectra and to derive semiquantitative depth profiles of the identified material compounds. RBS was used to obtain the quantitative depth distribution of the elements. By the combination of both methods, diffusion and oxidation processes were observed and could be precisely describe.
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