Geopolymer Composites-In Environmentally Friendly Aspects.

In the present work, a new, low energy consumption sol-gel synthesis route has been developed for geopolymer composites. Instead of the typically published 0.1-1.0 Al/Si molar ratios, the efforts of this study concentrated on the realization of >2.5 Al/Si molar ratios in the composite systems. The higher Al molar ratio significantly improves the mechanical properties. A very important aim was also the recycling of industrial waste materials with attention to environmentally friendly requirements. The very dangerous, toxic red mud as a waste product of aluminum industrial fabrication was selected for reclamation. The structural investigation was carried out by 27Al MAS NMR, XRD, and thermal analysis. The structural examination has unambiguously proven the composite phases in both gel and solid systems. The characterization of composites was performed with mechanical strength and water solubility measurements.

Hierarchical Porous SiO2 Cryogel via Sol-Gel Process.

The aim of this research work was to develop a new, low-cost and low-energy-consuming preparation route for highly porous silica systems. The precursor gel systems were synthesized by sol-gel chemistry. The starting materials were TEOS and water glass in the sol-gel syntheses. The effect of the chemical composition, the catalysis, the pH, and the additives were investigated on the structure and porosity of the cryogels. The gel systems were treated by freeze-drying process to obtain porous cryogel silica products. The cryogel systems possess hierarchical structures. The conditions of the freeze-drying process were also studied to increase the porosity. Small angle X-ray measurements, scanning electron microscope technique, and infrared spectroscopy were applied for the investigation of gel and cryogel systems.

Effect of phosphorus precursors on the structure of bioactive calcium phosphate silicate systems.

The main aim of this work was to synthesize calcium phosphate silicate bioceramics by a low energy-consuming sol-gel method applying various phosphorous precursors (triethyl phosphate, phosphoric acid, and ammonium hydrogen phosphate). The investigations concentrated on the influence of phosphorous initial compounds on the bond and crystalline structures and the material quality. The application of the alkoxide and inorganic P-precursors results in considerably different textures. The inorganic PO4-containing precursors lead to sol formations. The sol systems can be characterized by a randomly bonded aggregate structure. Monolith gel systems can only be prepared by using TEP. The alkoxide P-precursor more effectively furthers the connection between the phosphorous and silicon tetrahedra than the inorganic phosphate compounds. Over the P-precursors, the catalyst also affects the structure and properties. In the present work, a special attention was paid to identify the POSi bonds in the FTIR and 31P NMR spectra. The bond systems were investigated by FTIR, 31P and 29Si MAS NMR spectroscopies, the morphology by SEM, WAXS, and XRD measurements, and the water solubility of the ceramic systems also was tested.

Various three-dimensional structures connected by Al-O/OH/acetate-Al bonds.

In the present work, significantly various structures connected by Al-O/OH/acetate-Al bonds were synthesized in a versatile sol-gel route. The various bond systems result in several three-dimensional (e.g., fibrous, highly porous, and compact) macrostructures. The shared acetate and OH ions provide the fibrous character; the shared OH ions and oxygen-bridges between octahedral Al(III) ions assist in the formation of a porous network; and the oxygen-bridges between differently (octa-, tetra-, and pentahedrally) coordinated Al(III) ions characterize the compact structures. The newly developed synthesis route is a fast and low-energy consumption sol-gel technique. This method applies only two starting materials and does not adopt any basic agent or catalyst. The synthesis is fast because it does not require any time-consuming peptization; a 3-D network forms directly from the initial solution. The low energy consumption arises from the low temperature of reactions (80 °C) and heat treatment (400-600 °C).

Catalysis, nanostructure and macroscopic property triangle in bioactive calcium-containing ceramic systems.

Calcium silicate ceramics are intended for application as long-term implant materials. In the present work, attention was paid to understand the correlations between the nanostructure (aggregate size, crystallinity, porosity) and the macroscopic properties (solubility in water and simulated body fluids, SBF; hardness) varying the chemical composition. Varying the catalyst (from a base to various acids) during the chemical synthesis was shown to significantly impact on the pore size, crystallinity and mechanical properties. The basic catalyst yields the ceramics with the highest mechanical strength. Ammonia used in 1.0 or 10.0 molar ratio results in bulk ceramics with parameters required for a biomedical application, good hardness (180-200 HV) and low solubility (1-3%) in water and in SBF. The fine porosity (~50 nm) and homogeneous amorphous structure induce good mechanical character.

Liquid-phase synthesis of cobalt oxide nanoparticles.

Various liquid-phase syntheses of CoO and Co3O4 nanoparticles have been studied. The experiments focus on two synthesis routes: the coprecipitation and the sol-gel methods combined with thermal decomposition. The effect of synthesis route, the type of precursors (cobalt nitrate/chloride) and precipitation agent (carbonate, hydroxide, oxalic acid, and ammonia), the chemical compositions, pH, application of surfactants (PDMS, Triton X-100, NaDS, NaDBS, TTAB, ethyl acetate, citric acid), and the heat treatments on the properties of particles were investigated. The particle size and distribution have been determined by dynamic light scattering (DLS). The phases and the morphology of products have been analysed by XRD and SEM. The coprecipitation technique is less able to shape the particles than sol-gel technique. PDMS can be applied efficiently as surfactant in preparation methods. The finest particles (around 85 nm) with narrow polydispersity (70-100 nm) and spherical shape could be achieved by using sol-gel technique in medium of 1-propanol and ethyl acetate.

Structural characterization of gel-derived calcium silicate systems.

The main aim of this study is to synthesize calcium silicate ceramics that exhibit suitable properties to be used for biomedical applications. In the present work, attention was paid to the understanding of processing-structure relationships. A particular effort was made to clarify the identification of Ca-O-Si bonds by means of spectroscopy. The calcium silicate systems were prepared via a sol-gel route, varying the chemical compositions, the catalyst concentration, and the temperature and time of aging and heat treatment. The processes and the phases evolved during the sol-gel procedure were determined. The bond systems were investigated by Fourier transform infrared (FTIR) and (29)Si magic angle spinning nuclear magnetic resonance (MAS NMR) spectroscopy and the aggregate structures by scanning electron microscopy (SEM), small-angle neutron scattering (SANS), small-angle X-ray scattering (SAXS), wide-angle X-ray scattering (WAXS), and X-ray diffraction (XRD) measurements.

Nanostructure of gel-derived aluminosilicate materials.

In the present work, aluminosilicate aerogels prepared under various conditions were compared with respect to their nanostructures and porosity. The purpose of this investigation was to find a suitable way to predict the final product structure and to tailor a required texture. Several Al and Si precursors (Al nitrate, Al isopropoxide, Al acetate, tetraethoxysilane (TEOS), and sodium silicate) were used in our examinations; the solvent content (water and alcohols), surfactants, as well as the catalysts were varied. In addition, the aerogels were subjected to various heat treatments. Hybrid aerogels were synthesized by the addition of different polymers (poly(acrylic acid), polyvinyl acetate, and polydimethylsiloxane). Aluminosilicate and hybrid aerogel structures were investigated by 27Al MAS NMR, SAXS, SEM, and porosity measurements. Loose fractal structures with a good porosity and high Al incorporation can be achieved from TEOS and Al nitrate or isopropoxide via a sol-gel preparation route. The use of Al acetate led to compact aerogel structures independently of the Si precursor, the pH, and the catalyst.