We studied the behavior of dilute dispersions of nanoparticles of hematite, alumina, and titania in the presence of various concentrations of very pure sodium dodecyl-, tetradecyl-, and hexadecylsulfate. The concentrations studied were up to critical micelle concentration (CMC) for sodium dodecylsulfate, and up to the solubility limit in case of sodium tetradecyl- and hexadecylsulfate. The dispersions were adjusted to different pH (3–11), and 10−3 M NaCl was used as the supporting electrolyte. The solid-to-liquid ratio was strictly controlled in all dispersions, and the behavior of fresh dispersions was compared with dispersions aged for up to eight days. The presence of very low concentrations of ionic surfactants had rather insignificant effects on the ζ potentials of the particles. At sufficient concentrations of ionic surfactants the isoelectric point (IEP) of metal oxides shifted to low pH, and the long-chain surfactants were more efficient in shifting the IEP than their shorter-chain analogues. Once the surfactant concentration reached a critical value, the ζ potentials of the particles reached a pH-independent negative value, which did not change on further increase in the surfactant concentration and/or aging of the dispersion. This critical concentration increases with the solid-to-liquid ratio, and it is rather consistent (for certain oxides and certain surfactants) when it is expressed as the amount of surfactant per unit of surface area. Surprisingly, the surfactant-stabilized dispersions always showed a substantial degree of aggregation; that is, the particle size observed in dispersions by dynamic light scattering was higher than the size of particles observed in dry powders by electron microscopy. Apparently, in spite of relatively high ζ potentials (about 60 mV in absolute value), the surfactant-stabilized dispersions consist of aggregates rather than of primary particles, and in certain dispersions the high concentration of surfactant seems to induce aggregation rather than prevent it.
In this work, nanocrystalline powders of iron-doped zinc oxide ZnO (iron content 3, 5, and 10 at.%) were prepared utilizing co-precipitation method. X-ray diffraction, scanning electron microscopy, and the Mössbauer spectroscopy were used as complementary methods to investigate the structure and hyperfine interactions of the material. It was found that Fe dopant is incorporated into the ZnO würtzite structure. As confirmed by energydispersive X-ray spectroscopy the distribution of Fe dopant in the obtained samples is homogeneous up to 5 at.%. For 10 at.% of iron, spinel ZnFe2O4 phase was registered both by X-ray diffraction and the Mössbauer techniques. Paramagnetic behavior in Fe-doped ZnO was observed in the Mössbauer spectra at room temperature. Hyperfine interactions parameters indicate the presence of Fe 3+ ions substituting Zn 2+ ions at tetrahedral sites both in the crystallite interior and near the surface of grains.
Modification of SBA-15 with non-noble metal leads to functional materials, which can be applied as gas sensors, adsorbents, and catalysts of various reactions. The new materials contain up to four various metals, which are deposited consecutively or simultaneously at various concentrations ranging from a fraction of 1% to an amount that is comparable with the mass of silica-support. These materials contain metals at various oxidation levels, usually as oxides, which occur in crystalline form (a typical crystallite size of about 10 nm matches the width of the SBA-15 channels), but in a few other materials, crystalline metal compounds have not been detected. Many researchers have provided detailed physico- chemical characteristics of SBA-15 modified with non-noble metals by the means of various microscopic and spectroscopic techniques.
The chemical vapour deposition technique was applied to obtain Ti/SBA-15 composites. Titanium(IV) tetraisopropoxide (TTIP) and titanium(IV) tetrabutoxide (TNBT) as sources of TiO2 were deposited on mesoporous silica (SBA-15) from the gaseous phase at 180–200 °C and treated at 250 °C in air. X-ray diffraction, Fourier-transform infrared spectroscopy, and Raman spectroscopy were used for structural investigations. Moreover, energy-dispersive X-ray spectroscopy studies and electrophoretic mobility measurements were conducted. Investigations revealed that Ti ions were mainly deposited on the SBA-15 surface as a thin layer of amorphous TiO2. However, Ti ions were not detected in the composites synthesized using TNBT as the starting reagent. The thickness of the deposited titanium oxide layer was estimated as 6–7 nm, and the porous silica structure has not been damaged. Moreover, the Ti ions deposition on the SBA-15 surface did not significantly change the investigated Ti/SBA-15 composites’ thermal stability compared to pristine silica.
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