SAXS study of gelation, aging and drying of silica-polypropyleneglycol hybrid materials

New silica-polypropyleneglycol ormosils (organically modified silicates) with covalent bends between the organic (polymer) and inorganic (silica) phases have been prepared by the sol-gel process. Their structural evolution during sol formation, sol-gel transition, gel aging and drying has been studied in situ by small-angle X-ray scattering (SAXS). The experimental SAXS curves corresponding to sols and gels exhibit features expected from fractal objects. Clusters of size around 55 Angstrom with an initial fractal dimension D = 2.4 are formed in the sol. They are constituted of small primary silica particles chemically crosslinked at the end of the polymer chains. A strong liquid-like spatial correlation between the silica particles develops during drying due to the shrinkage of the polymeric network induced by water and ethanol evaporation. The continuous increase in SAXS intensity during drying, while the interparticle distance remains constant, is a consequence of the progressive growth of the dry fraction of the total volume. After drying, the gel structure consists of a rather compact arrangement of silica particles embedded in the polypropyleneglycol matrix.

Structure of weakly bonded PPG-silica nanocomposites

The structure of silica-polypropyleneglycol (PPG) nanocomposites with weak physical bonds between the organic (PPG) and inorganic (silica) phase, prepared by the sol-gel process, was investigated by small angle X-ray scattering (SAXS). These nanocomposite materials are transparent, flexible, have good chemical stability and exhibit high ionic conductivity when doped with lithium salt. Their structure was studied as a function of silica weight fraction x (0.06 less than or equal to x less than or equal to 0.29) and [O]/[Li] ratio (oxygens being of ether-type). The shape of the experimental SAXS curves agrees with that expected for scattering intensity produced by fractal aggregates sized between 30 and 90 Angstrom. This result suggests that the structure of the studied hybrids consists of silica fractal aggregates embedded in a matrix of PPG. The correlation length of the fractal aggregates decreases and the fractal dimension increases for increasing silica content. The variations in structural parameters for increasing Li+ doping indicate that lithium ions favor the growth of fractal silica aggregates without modifying their internal structure and promote the densification of the oligomeric PPG matrix.

Structural properties of silica gels prepared from oxalic-acid-catalyzed tetraethoxysilane sonohydrolysis

About similar to 2.1 x 10(-3) Mol SiO2 cm(-3) and similar to 88%-volume liquid-phase silica wet gels were prepared from oxalic-acid-catalyzed tetraethoxysilane (TEOS) sonohydrolysis. Aerogels were obtained by supercritical CO2 extraction. The samples were analyzed by thermogravimetry, small-angle X-ray scattering and nitrogen adsorption. Wet gels can be described as mass fractal structures with fractal dimension D similar to 1.94 and structural characteristic length zeta changing between similar to 3.3 to similar to 3.0 nm in the studied range of the catalyst concentration. A fraction of the porosity is apparently eliminated in the supercritical process. The values of the BET specific surface S-BET, the total pore volume V-p and the mean pore size l(p) of the aerogels were found to change almost randomly around the mean values S-BET = 874 m(2) g(-1), V-p = 0.961 cm(3) g(-1) and l(p) = 4.4 nm with catalyst concentration variation. These values were not substantially different from those from an equivalent HCl-catalyzed aerogel. (c) 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Structural characteristics of silica sonogels prepared with additions of isopropyl alcohol

Wet silica gels with similar to 1.4 x 10(-3) mol SiO2/cm(3) and similar to 92 vol% liquid phase were obtained from sonohydrolysis of tetraethoxysilane (TEOS) with different additions of isopropyl alcohol ( IPA). The IPA/TEOS molar ratio R was changed from 0 to 4. Aerogels were obtained by supercritical CO2 extraction. The samples were analyzed by small-angle X-ray scattering (SAXS) and nitrogen adsorption. The wet gels exhibit mass fractal structure with fractal dimension increasing from D similar to 2.10 to D similar to 2.22, characteristic length xi decreasing from similar to 9.5 to similar to 6.9 nm, as R increases from 0 to 4, and an estimated characteristic length for the primary silica particles lower than similar to 0.3 nm. The supercritical process apparently eliminates a fraction of the porosity, increasing the mass fractal dimension and shortening the fractality domain in the mesopore region. The fundamental role of isopropyl alcohol on the structure of the resulting aerogels is to decrease the porosity and the pore mean size as R changes from pure TEOS to R = 4. A secondary structure appearing in the micropore region of the aerogels can be described as a mass/surface fractal structure, with correlated mass fractal dimension D-m similar to 2.7 and surface fractal dimension D-s similar to 2.3, as inferred from SAXS and nitrogen adsorption data.

Shape-based features for cat ganglion retinal cells classification

This article presents a quantitative and objective approach to cat ganglion cell characterization and classification. The combination of several biologically relevant features such as diameter, eccentricity, fractal dimension, influence histogram, influence area, convex hull area, and convex hull diameter are derived from geometrical transforms and then processed by three different clustering methods (Ward's hierarchical scheme, K-means and genetic algorithm), whose results are then combined by a voting strategy. These experiments indicate the superiority of some features and also suggest some possible biological implications.

Structural study of aged saturated silica gels obtained from tetramethoxysilane sonohydrolysis with different water/tetramethoxysilane molar ratio

The structural characteristics of saturated silica sonogels were studied by means of small-angle x-ray scattering (SAXS) and thermogravimetric analysis (TG), after a long time of aging in saturated conditions. The sonogels were obtained by a sol-gel routine from ultrasound stimulated tetramethoxysilane (TMOS) hydrolysis carried out with the initial water/TMOS molar ratio (r) ranging from 2 to 10. The saturated sonogel structure can be described as composed by mass fractal-like aggregates (clusters) of primary silica particles, all imbibed in a liquid phase. The values of the mass fractal dimension (D) of the clusters was found all around 2.5, while the characteristic size of the clusters (ξ) was found generally increasing with r, going from approximately 2.3 nm (r = 2) to 4.5 nm (r = 10). The volume fraction of the clusters was estimated from the SAXS data. The results were compared to the values of weight loss fraction at the inflection point that has been found in the derivative of the TG curve, which should accounts for the instant in which the meniscus of the liquid phase penetrates into the clusters under a rapid evaporation process as in a TG test.

Comparative study using small-angle x-ray scattering and nitrogen adsorption in the characterization of silica xerogels and aerogels

A comparative study using small-angle x-ray scattering (SAXS) and nitrogen adsorption has been carried out in the structural characterization of silica xerogels and aerogels, obtained from tetraethoxysilane sonohydrolysis. The specific surface and the mean pore size as measured by both the techniques were found to be in notable agreement in all cases for aerogels and xerogels. According to the SAXS data, aerogels at 500 °C exhibit a mass fractal structure with fractal dimension D∼2.4 in the range between the correlation length ξ∼5.3 nm and a∼0.75 nm. An experimental method to probe the mass fractal structure of aerogels from exclusively nitrogen adsorption isotherms has been presented. For aerogels at 500 °C, we have found D∼2.4 in the range between the pore width 2rξ∼33 nm and 2ra∼4.5 nm, which is in notable agreement with the SAXS results (D ∼2.4, ξ∼5.3 nm, a∼0.75 nm) if we assign the pore width 2r probed by the Kelvin equation in the adsorption method to the Bragg distance 2π/q associated to the correlation length 1/q probed by SAXS.

Characterization of texture in image of skin lesions by support vector machine

Due to the increased incidence of skin cancer, computational methods based on intelligent approaches have been developed to aid dermatologists in the diagnosis of skin lesions. This paper proposes a method to classify texture in images, since it is an important feature for the successfully identification of skin lesions. For this is defined a feature vector, with the fractal dimension of images through the box-counting method (BCM), which is used with a SVM to classify the texture of the lesions in to non-irregular or irregular. With the proposed solution, we could obtain an accuracy of 72.84%. © 2012 AISTI.

Aprendizado de máquina simbólico e técnicas fractais para caracterizar rejeição em biópsia miocárdica

This work combines symbolic machine learning and multiscale fractal techniques to generate models that characterize cellular rejection in myocardial biopsies and that can base a diagnosis support system. The models express the knowledge by the features threshold, fractal dimension, lacunarity, number of clusters, spatial percolation and percolation probability, all obtained with myocardial biopsies processing. Models were evaluated and the most significant was the one generated by the C4.5 algorithm for the features spatial percolation and number of clusters. The result is relevant and contributes to the specialized literature since it determines a standard diagnosis protocol. © 2013 Springer.

Local and regional ecological drivers of fish assemblages in Brazilian estuaries

Spatial patterns in assemblage structures are generated by ecological processes that occur on multiple scales. Identifying these processes is important for the prediction of impact, for restoration and for conservation of biodiversity. This study used a hierarchical sampling design to quantify variations in assemblage structures of Brazilian estuarine fish across 2 spatial scales and to reveal the ecological processes underlying the patterns observed. Eight areas separated by 0.7 to 25 km (local scale) were sampled in 5 estuaries separated by 970 to 6000 km (regional scale) along the coast, encompassing both tropical and subtropical regions. The assemblage structure varied significantly in terms of relative biomass and presence/absence of species on both scales, but the regional variation was greater than the local variation for either dataset. However, the 5 estuaries sampled segregated into 2 major groups largely congruent with the Brazilian and Argentinian biogeographic provinces. Three environmental variables (mean temperature of the coldest month, mangrove area and mean annual precipitation) and distance between estuaries explained 44.8 and 16.3%, respectively, of the regional-scale variability in the species relative biomass. At the local scale, the importance of environmental predictors for the spatial structure of the assemblages differed between estuarine systems. Overall, these results support the idea that on a regional scale, the composition of fish assemblages is simultaneously determined by environmental filters and species dispersal capacity, while on a local scale, the effect of environmental factors should vary depending on estuary-specific physical and hydrological characteristics © 2013 Inter-Research.

Structural characteristics of P123-modified supercritical drying and hydrophobic ambient pressure drying aerogels

Supercritical drying (SCD) and hydrophobic ambient pressure drying (APD) aerogels were prepared from hydrolysis of tetraethoxysilane in solutions of poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) (P123) in the range of composition below the threshold for the ordered mesoporous silica precipitation. APD was carried out after silylation of wet gels with trimethylchlorosilane (TMCS) or hexamethyldisilazane (HMDZ). The samples were analyzed by small-angle X-ray scattering and nitrogen adsorption. Wet gels are formed by mass-fractal domains, with fractal dimension close to 2, and larger pores superposing the pores belonging to the fractal structure in case of high P123 concentrations. Aerogels exhibit smaller-sized mass-fractal domains with larger mass-fractal dimension accounting for some porosity elimination on drying. The pore volume of the aerogels increases significantly with the P123 amount and it is even larger in the APD aerogels than in the SCD aerogels. © 2013 Elsevier B.V. All rights reserved.

Structure and kinetics of formation of APTS/GPTS-derived organic/inorganic hybrids

The structure and the kinetics of formation of APTS/GPTS-derived organic/inorganic hybrids were studied in situ by small-angle-X-ray scattering. The data were interpreted in terms of a process of primary particles formation and growth of mass-fractal clusters. At the very early stage, the population of the nonfractal primary particles (D = 3) increases with time. As the mass-fractal clusters appear (D < 3) as a result of the aggregation process, the radius of gyration, Rg, of the clusters increases on average. At advanced stages of aggregation, the clusters grow in a mechanism in which the number of particles per clusters increases while the number of clusters diminishes with time, in such a way that the correlation volume of the clusters, Vc, fulfills the relationship Vc â̂ R g D, in agreement with a mass-fractal character of the clusters. These results supporting a cluster-cluster aggregation process, together with the typically very low value found for the mass-fractal dimension D, are in favor of a diffusion-controlled cluster aggregation mechanism. © 2013 American Chemical Society.

Generalização cartográfica para um Sistema de Navegação e Guia de Rota em Automóvel áudio-dinâmico com múltiplas escalas

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Síntese e caracterização de partículas esféricas de poli(álcool vinílico) e poli(acetato vinílico) para utilização em embolização

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Segmentação morfológica aplicada à cartografia

Pós-graduação em Ciências Cartográficas - FCT