0000000000060046
AUTHOR
José Miguel Calatayud
Improvement of boehmite nanoparticles' aqueous dispersability by controlling their size, shape and crystallinity
In this work, results on the control of size, shape, crystallinity and aqueous dispersability of boehmite prepared by a hydrothermal process are reported. The two step synthetic procedure entailed the precipitation of a xerogel by adding NaOH until pH 10 to a solution of aluminum nitrate at 100 °C without or with additives such as tartaric acid and maltitol, and a subsequent hydrothermal treatment at 150 and 200 °C for different periods of time. The final materials were characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD) and elemental analysis. The stability and other characteristics of the boehmite nanoparticle aqueous dispersions were determined by measuring t…
Cr- and Sb-containing TiO 2 inorganic orange nano-pigments prepared by a relative long hydrocarbon chain polyol
Abstract We report the preparation of a series of orange Cr- and Sb-containing TiO 2 nano-pigments by the polyol via using triethylenglycol (TEG). Poorly crystallized anatase nanopowders with nominal stoichiometric compositions Cr x Sb x Ti 1−2x O 2 , with 0 ≤ x ≤ 0.2, were obtained by heating at 180 °C a solution of antimony acetate, chromium acetylacetone and titanium butoxide in TEG. The transition temperature of the chromium- and antimonium-containing anatase nanoparticles into the rutile crystalline form occurred over the range of temperature between 500 and 650 °C, depending on the dopant amount. After annealing at 800 °C for short time the series of samples displaying the rutile stru…
Chromium oxide nanoparticles with controlled size prepared from hydrothermal chromium oxyhydroxide precursors
Abstract This work reports the preparation of morphologically well-defined chromium oxide nanoparticles with controlled sizes of 20–30 nm. The synthetic procedure encompass two stages, the first one refers to the preparation of chromium oxyhydroxide nanoparticles by a hydrothermal approach of previously precipitated xerogels, followed by a thermal transformation of CrOOH nanoparticles to Cr2O3. The series of chromium oxyhydroxide particles sized over the range 15–50 nm were prepared through the control of the pH of precipitation of the xerogels and the water/xerogel ratio of the hydrothermal aging. Results showed the formation of non-aggregated oxyhydroxide nanoparticles with two different …
Mesocrystalline Cr and Sb-codoped anatase visible-light-driven photocatalyst
Abstract We report on the synthesis, characterization and visible-light-driven photocatalytic activity of mesocrystalline Cr- and Sb-codoped anatase nanoparticles. Discrete and morphologically well-defined assemblies of anatase nanoparticles sized below 100 nm × 50 nm were prepared by hydrothermal aging of aqueous solutions containing titanium alkoxide, chromium acetylacetonate, antimony acetate and triethanolamine (TEOA) as stabilizer. The as-prepared and TEOA-free doped nanoparticles showed similar crystallographic parameters and spectroscopic features. The incorporation of Cr and Sb dopant cations into the anatase nanoparticles was evaluated by Rietveld refinement of X-ray diffraction pa…
Hydrothermal-mediated synthesis of orange Cr, Sb-containing TiO 2 nano-pigments with improved microstructure
Abstract A hydrothermal-mediated via was developed to prepare discrete, non-aggregated Cr,Sb-doped rutile nano-pigments. After annealing the Cr- and Sb-containing TiO2 anatase nanocrystals obtained by hydrothermal aging the nano-pigments Cr,Sb-TiO2 were characterized with the aid of X-ray diffraction (XRD) including lattice parameter and crystallite size determination, Raman spectroscopy, field emission scanning and transmission electron microscopies (FESEM and TEM, respectively) including energy-dispersive X-ray (FESEM/EDX) spectroscopy, high resolution transmission electron microscopy (HRTEM) including selected area electron diffraction (SAED), ultraviolet–visible diffuse reflectance (UV–…
Mesocrystalline anatase nanoparticles synthesized using a simple hydrothermal approach with enhanced light harvesting for gas-phase reaction
Mesocrystalline TiO2 nanoparticles were synthesized using a hydrothermal approach. A simple two-step procedure at low temperature (<140 °C) allowed the nucleation of primary particles sized 2–4 nm and their subsequent assembly as almost spherical aggregates sized ≈20 nm. X-ray powder diffraction (XRD), Raman and X-ray photoelectron spectroscopy (XPS) studies, and HRTEM studies confirmed anatase as the unique TiO2 crystalline phase. The mesocrystalline structure of the anatase aggregates was clearly evidenced by HRTEM and SAED results. The mesocrystalline nanopowders exhibit a mesoporous structure with a surface area and pore volume of 63.5 m2 g−1 and 0.22 cm3 g−1, respectively. Ultraviolet …
V-containing ZrO2 inorganic yellow nano-pigments
In this work we report new results on the preparation, characterization and color properties of the inorganic yellow nano-pigmenting system based on monoclinic V–ZrO2 solid solution nanoparticles. The series of solid solution nanopowders were obtained by a polyol technique where the precipitates, obtained after heating at 180 °C ethylene glycol solutions of vanadyl acetonate and zirconium n-propoxide, were annealed at different temperatures up to 1300 °C for a short duration, in order to improve their crystallinity and control the crystalline form of the final nanoparticles. On annealing at around 450 °C highly crystalline tetragonal V-containing zirconia particles were developed, which tra…
V-containing ZrO 2 inorganic yellow nano-pigments prepared by hydrothermal approach
Abstract Recent results on the preparation, characterization and color properties of the V-containing ZrO 2 inorganic yellow nano-pigment are reported. A series of monoclinic V-ZrO 2 solid solution nanocrystals (V x Zr 1-x O 2 , being x = 0, 0.1, 0.02, 0.03, 0.04, 0.05, 0.065, 0.08 and 0.1) were prepared straightforward by hydrothermal processing of mixtures of zirconyl nitrate and ammonium metavanadate in water. Interestingly, the crystalline precipitated obtained by hydrothermal processing at 140 °C for 3 d was almost entirely V-containing ZrO 2 nanocrystals with the structure of monoclinic zirconia for the whole range of compositions. Lattice parameters changes along the series of prepar…
Crystalline microstructure of boehmites studied by multi-peak analysis of powder X-ray diffraction patterns
Nanocrystalline boehmite (gamma-aluminium-oxyhydroxide) is a material of industrial importance, the functionality of which follows from its crystalline microstructure. A procedure for preparing boehmite nanoparticles, comprising the formation of a precipitate by the alkalization of an aqueous solution of aluminium nitrate and subsequent hydrothermal aging, was previously elaborated. The application of an additive (maltitol or tartaric acid) to control the sizes and shapes of crystallites in the produced polycrystalline powder of boehmite was developed. The aim of this work is a study of the effect of the hydrothermal treatment time on nanocrystalline characteristics of boehmite, both in abs…