Combined SANS and SAXS study of the action of ultrasound on the structure of amorphous zirconia gels

Abstract In the present work, we have studied for the first time the combined effect of both sonication and precipitation pH on the structure of amorphous zirconia gels synthesized from zirconium(IV) propoxide. The techniques of small-angle neutron and X-ray scattering (SANS and SAXS) and low temperature nitrogen adsorption provided the integral data on the changes in the microstructure and mesostructure of these materials caused by ultrasonic (US) treatment. Amorphous ZrO2·xH2O synthesized under ultrasonic treatment was found to possess a very structured surface, characterized by the surface fractal dimension 2.9–3.0, compared to 2.3–2.5 for the non US-assisted synthesis, and it was also found to possess a higher specific surface area, while the sizes of the primary particles remain unchanged

How xerogel carbonization conditions affect the reactivity of highly disperse SiO2–C composites in the sol–gel synthesis of nanocrystalline silicon carbide

A transparent silicon polymer gel was prepared by sol–gel technology to serve as the base in the preparation of highly disperse SiO2–C composites at various temperatures (400, 600, 800, and 1000°C) and various exposure times (1, 3, and 6 h) via pyrolysis under a dynamic vacuum (at residual pressures of ~1 × 10–1 to 1 × 10–2 mmHg). These composites were X-ray amorphous; their thermal behavior in flowing air in the range 20–1200°C was studied. The encapsulation of nascent carbon, which kept it from oxidizing in air and reduced the reactivity of the system in SiC synthesis, was enhanced as the carbonization temperature and exposure time increased. How xerogel carbonization conditions affect the micro- and mesostructure of the xerogel was studied by ultra-small-angle neutron scattering (USANS). Both the carbonization temperature and the exposure time were found to considerably influence structure formation in highly disperse SiO2–C composites. Dynamic DSC/DTA/TG experiments in an inert gas flow showed that the increasing xerogel pyrolysis temperatures significantly reduced silicon carbide yields upon subsequent heating of SiO2–C sys- tems to 1500°C, from 35–39 (400°C) to 10–21% (1000°C)

Microstructure of Zirconia-Based Sol-Gel Glasses Studied by SANS

Zirconia-based bulk glasses were prepared for the first time by sol-gel method. Such materials are very promising for application as photochromic devices, catalytic systems, chemical sensors, lasers and other nonlinear optics devices. Obtained transparent and semi-transparent materials were studied by small and ultra-small angle neutron scattering (SANS and USANS) methods. As evidenced by SANS, morphology of zirconia glasses is very sensitive to parameters of sol-gel synthesis, e.g. temperature and concentration of reactants. SANS data correlates rather well with surface porosity data. Increasing water concentration in reaction mixtures containing zirconium propylate leads to a significant increase in fractal cluster size, while decrease of the temperature results in an increase of the fractal dimension. The obtained results indicate that parameters of the microstructure and consequently physical properties of zirconia glasses can be effectively controlled by parameters of synthesis

Structural Analysis of Aluminum Oxyhydroxide Aerogel by Small Angle X-Ray Scattering

The work presents studies on the microstructure and mesostructure of nanostructured aluminum oxyhydroxide formed as a high porous monolithic material through the surface oxidation of aluminum liquidmetal solution in mercury in a temperature- and humidity-controlled air atmosphere. The methods of X-ray diffraction analysis, thermal analysis, the low temperature adsorption of nitrogen vapors, transmission electron microscopy, small-angle and very small-angle neutron scattering, and small-angle X-ray scattering are used for comprehensive investigation of the samples synthesized at 25°С as well as that annealed at temperatures up to 1150°C. It is found that the structure of the monolithic samples can be described within the framework of a three-level model involving primary heterogeneities (typical length scale of rc ≈ 9–19 Å), forming fibrils (cross-sectional radius R ≈ 36–43 Å and length L ≈ 3200–3300 Å) or lamellae (thickness T ≈ 110 Å and width W ≈ 3050 Å) which, in turn, are integrated into large-scale aggregates (typical size R c ≈ 1.25–1.4 μm) with an insignificant surface roughness. It is shown that a high specific surface (~200 m2/g) typical for the initial sample is maintained upon its thermal annealing up to 900°С, and it decreases to 100 m2/g after heat treatment at 1150°С due to fibrillary agglomeration

Combined SANS and SAXS study of the action of ultrasound on the structure of amorphous zirconia gels

In the present work, we have studied for the first time the combined effect of both sonication and precipitation pH on the structure of amorphous zirconia gels synthesized from zirconium(IV) propoxide. The techniques of small-angle neutron and X-ray scattering (SANS and SAXS) and low temperature nitrogen adsorption provided the integral data on the changes in the microstructure and mesostructure of these materials caused by ultrasonic (US) treatment. Amorphous ZrO2·xH2O synthesized under ultrasonic treatment was found to possess a very structured surface, characterized by the surface fractal dimension 2.9–3.0, compared to 2.3–2.5 for the non US-assisted synthesis, and it was also found to possess a higher specific surface area, while the sizes of the primary particles remain unchanged

Combined SANS and SAXS study of the action of ultrasound on the structure of amorphous zirconia gels

In the present work, we have studied for the first time the combined effect of both sonication and precipitation pH on the structure of amorphous zirconia gels synthesized from zirconium(IV) propoxide. The techniques of small-angle neutron and X-ray scattering (SANS and SAXS) and low temperature nitrogen adsorption provided the integral data on the changes in the microstructure and mesostructure of these materials caused by ultrasonic (US) treatment. Amorphous ZrO2·xH2O synthesized under ultrasonic treatment was found to possess a very structured surface, characterized by the surface fractal dimension 2.9–3.0, compared to 2.3–2.5 for the non US-assisted synthesis, and it was also found to possess a higher specific surface area, while the sizes of the primary particles remain unchanged

Magnetic Neutron Scattering in Reduced Graphene Oxide

The scale of magnetic correlations in materials based on reduced graphene oxide (RGO) has been estimated for the first time using the method of small-angle scattering of polarized neutrons. This information cannot be obtained by other methods. Experiments have demonstrated the presence of small-angle magnetic-nuclear interference scattering for both original RGO and an RGO-based composite in magnetized fields H about 1 T, which unequivocally indicates the presence of magnetized areas on the scale of 1000 Å in the studied materials

Structure of zirconium dioxide based porous glasses

This study is devoted to investigation of the micro- and mesostructure (including fractal properties) of porous zirconia glasses synthesized by precipitation from zirconium n-propoxide solutions in the presence of different hydrolyzing-agent (H2O) quantities at different temperatures. Analysis of small-angle neutron, ultra-small-angle neutron and X-ray scattering, scanning electron microscopy allows concluding that the synthesized glasses are complex systems with a three-level hierarchical fractal structure. It is revealed that both the temperature of synthesis and the H2O concentration in the initial solution significantly affect the structural characteristics of the glasses