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…

X-ray diffraction line broadening on vibrating dry-milled Two Crows sepiolite

A reference sample of sepiolite and products of its comminution by vibrating dry-milling have been studied using X-ray diffraction (XRD) line-broadening analysis, complementary field emission scanning electron microscopy (FESEM) images and surface area measurements. The apparent crystallite sizes determined via XRD are in agreement with observations on FESEM images. The sepiolite aggregates consist of lath-shaped agglutinations of prisms and pinacoids elongated along [001], each lath including several crystallites in that direction. The surface area magnitudes are in the range of previous experimental measurements of other sepiolites. The results obtained show the effectiveness of vibro-mil…

Crystalline microstructure of sepiolite influenced by grinding

The crystalline microstructure of ground sepiolite has been investigated. A reference sample of sepiolite and products of its comminution by dry grinding were studied through X-ray diffraction pattern analysis, specific surface measurements by nitrogen adsorption and complementary analysis of field emission scanning electron microscope images. A statistical model of polycrystals was applied to describe and determine the crystalline microstructure of the studied specimens. The model parameters characterizing the microstructure were prevalent crystallite shape, volume-weighted crystallite size distribution and second-order crystalline lattice strain distribution, and they were determined for …

X-ray diffraction line-broadening study on two vibrating, dry-milling procedures in kaolinites

Due to the great technological importance of the microstructure of kaolinite, characterizing its evolution during dry milling of kaolin and analyzing the microstructural information obtained from different methods were the main aims of this work. The microstructural alteration of kaolinite is evaluated by X-ray diffraction and electron microscopy methods, comparing the results obtained and analyzing the correlations between them. The Warren-Averbach and Voigt-function methods of X-ray diffraction microstructural analysis have been applied successfully to the study of the effects of two different, vibrating-cup dry-milling configurations in the microstructure of kaolinite from the reflection…

Crystallite size of kaolinites as indicator of different geochemical types of bauxite

A simple microstructural X-ray diffraction analysis using the Voigt function method reveals differences between bauxite deposits in the Iberian Range – Catalanides area (NE, Spain). The highest values of apparent crystallite sizes, measured by volume weighted Dv values from 001 kaolinite reflection, have been found in bauxites of type 1.

Crystalline Microstructure of Corundum Fillers Determined from Powder X-Ray Diffraction Patterns

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 …

Soil emissivity and reflectance spectra measurements

We present an analysis of the laboratory reflectance and emissivity spectra of 11 soil samples collected on different field campaigns carried out over a diverse suite of test sites in Europe, North Africa, and South America from 2002 to 2008. Hemispherical reflectance spectra were measured from 2.0 to 14 microm with a Fourier transform infrared spectrometer, and x-ray diffraction analysis (XRD) was used to determine the mineralogical phases of the soil samples. Emissivity spectra were obtained from the hemispherical reflectance measurements using Kirchhoff's law and compared with in situ radiance measurements obtained with a CIMEL Electronique CE312-2 thermal radiometer and converted to emi…

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 …

Tuning the size and shape of nano-boehmites by a free-additive hydrothermal method

A synthetic procedure allowing the control of boehmite micro and nanoparticles is presented. The proposed hydrothermal synthetic procedure is based on the control of three reaction parameters, the pH and temperature of precipitation of xerogels and the water/xerogel ratio for the hydrothermal process, carried out at 200 °C for 48 h. Results obtained by measurements on transmission electron microscopy (TEM) images indicate that at pH 5 micro or nanorods of controlled length between ca. 300 and 50 nm were obtained depending on the temperature of precipitation of the xerogel (25 or 100 °C) and the water/xerogel ratio used (1/1, 6/1, 15/1). On the contrary, at pH 10, nanoplatelets with major ba…

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…

Thermal stability of transition alumina nanocrystals with different microstructures

Abstract The preparation of well-crystallized boehmite nanoparticles with different morphologies, encompassing from aciculae or rods of 320, 150 and 70 nm of length to platelets of 50 nm in diameter, allowed a comparative study of their respective thermal evolutions as alumina precursors. Static thermal treatments of boehmite nanocrystals at 600, 1000 and 1200 °C and a dynamic, in situ synchrotron study between 100 and 1000 °C revealed that original boehmite microstructures, i.e. size and shape of the nanoparticles, were kept not only in γ-Al 2 O 3 but also in transitional aluminas up to 1000 °C. Specifically, at that temperature, acicular samples presented θ-Al 2 O 3 structure, while in pl…

Electrochemistry of Iron-Doped Zircon and Zirconia Materials and Electrocatalytic Effects on Nitrite Oxidation and Reduction

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…

A new FESEM procedure for assessment of XRD microstructural data of kaolinites

Abstract A sample preparation method for FESEM microstructural analysis of sheet silicates using oriented aggregates on metallic strips parallel to the electronic beam is described. The method allows the easy measurement of thickness of kaolinite crystallites. The results have been compared to the apparent crystallite size measured by XRD The performed measurements for a set of selected kaolinites are in the range 15–60 nm and show a good correlation with XRD crystallite thickness (in the range 11–48 nm) obtained by the Voigt function method.