Search results for "crystallization"
showing 10 items of 774 documents
New insights in the formation of silanol defects in silicalite-1 by water intrusion under high pressure.
2010
International audience; The "water-silicalite-1" system is known to act as a molecular spring. The successive intrusion-extrusion cycles of liquid water in small crystallites (6 × 3 × 0.5 μm(3)) of hydrophobic silicalite-1 were studied by volumetric and calorimetric techniques. The experiments displayed a decrease of the intrusion pressure between the first intrusion-extrusion cycle and the consecutive ones, whereas the extrusion pressures remained unchanged. However, neither XRD studies nor SEM observations revealed any structural and morphological modifications of silicalite-1 at the long-range order. Such a shift in the value of the intrusion pressure after the first water intrusion-extr…
Preparation, Characterization, and Photoactivity of Polycrystalline Nanostructured TiO2 Catalysts.
2004
Various preparations of nanostructured TiO2 starting from Ti(iso-OC3H7)4 or TiCl4 are reported. The samples were characterized by X-ray diffractometry, specific surface area and porosity determinations, scanning and transmission electron microscopy, and diffuse reflectance spectroscopy. 4-Nitrophenol photodegradation in aqueous medium was employed as a probe reaction to test the photoactivity of the catalysts. The photoactivity of some samples derived from Ti(iso-OC3H7)4 was found comparable with that of commercial powders. Calcination after the hydrolysis process was necessary to achieve crystallization of the particles before using them as photocatalysts for the reaction studied. The samp…
Recovery of Lithium Carbonate from Dilute Li-Rich Brine via Homogenous and Heterogeneous Precipitation
2022
An extensive experimental campaign on Li recovery from relatively dilute LiCl solutions (i.e., Li+ similar to 4000 ppm) is presented to identify the best operating conditions for a Li2CO3 crystallization unit. Lithium is currently mainly produced via solar evaporation, purification, and precipitation from highly concentrated Li brines located in a few world areas. The process requires large surfaces and long times (18-24 months) to concentrate Li` up to 20,000 ppm. The present work investigates two separation routes to extract Li+ from synthetic solutions, mimicking those obtained from low-content Li+ sources through selective Li+ separation and further concentration steps: (i) addition of …
New acridinium trifluoromethanesulfonate stacks induced in the presence of organotin(IV) complexes
2013
Abstract Three new crystalline architectures based on acridinium trifluoromethanesulfonate salts [C13H10N]+[CF3SO3]– have been isolated as single crystals from the reaction of the dimeric hydroxo di-n-butylstannane trifluoromethanesulfonato complex [n-Bu2Sn(OH)(H2O)(CF3SO3)]2 (1) with acridine (C13H9N, Acr), in dichloromethane at room temperature. When an equimolar mixture of anthracene (C14H10, Ant) and acridine is initially used, the crystallization of a sandwich-type arrangement occurs, leading to the intercalation of one molecule of anthracene between two acridium trifluoromethanesulfonate salt molecules. In the three X-ray structures reported, the crystal packing involves the contribut…
Organic solvent desorption from two tegafur polymorphs.
2013
Desorption behavior of 8 different solvents from α and β tegafur (5-fluoro-1-(tetrahydro-2-furyl)uracil) has been studied in this work. Solvent desorption from samples stored at 95% and 50% relative solvent vapor pressure was studied in isothermal conditions at 30 °C. The results of this study demonstrated that: solvent desorption rate did not differ significantly for both phases; solvent desorption in all cases occurred faster from samples with the largest particle size; and solvent desorption in most cases occurred in two steps. Structure differences and their surface properties were not of great importance on the solvent desorption rates because the main factor affecting desorption rate …
Low-temperature Zr mobility: An in-situ synchrotron-radiation XRF study of the effect of radiation damage in zircon on the element release in $H_{2}O…
2006
The release of Zr, U, and Pb from nearly metamict zircon and its recrystallized analog and of Zr from fully crystalline and slightly radiation-damaged zircon in H 2 O + HCl ± SiO 2 fluids was investigated in situ at temperatures between 200 and 500 °C using a hydrothermal diamond-anvil cell and time-resolved synchrotron-radiation XRF analyses. Dissolution of nearly metamict zircon proceeded much faster than that of zircon with little or no radiation damage and resulted in a 1.5 to 2 log units higher Zr molality in 6 to 7 m HCl fluids. Extensive recrystallization of the almost fully amorphous material started at 260 to 300 °C in H 2 O + HCl, and at about 360 °C if quartz was added, and was c…
On the Creeping of Saturated Salt Solutions
2013
Creeping is a well-known but annoying phenomenon in the preparation of crystals from solution, where growing crystallites gradually extend up the walls of the growth vessel. In this process, solution is transported toward the tip of the creeping crystallites, where solvent evaporation takes place and solid material is deposited. In this study, the growth of crystal aggregates extending from evaporating droplets of saturated aqueous solutions of ionic salts, placed on different substrate materials, has been investigated using optical microscopy. It is shown that the rate determining step of the crystallization process is the evaporation of solution, following Fick’s laws. Fresh solution, nec…
Role of Water During Crystallization of Amorphous Cobalt Phosphate Nanoparticles
2016
The transformation of amorphous precursors into crystalline solids and the associated mechanisms are still poorly understood. We illuminate the formation and reactivity of an amorphous cobalt phosphate hydrate precursor and the role of water for its crystallization process. Amorphous cobalt phosphate hydrate nanoparticles (ACP) with diameters of ∼20 nm were prepared in the absence of additives from aqueous solutions at low concentrations and with short reaction times. To avoid the kinetically controlled transformation of metastable ACP into crystalline Co3(PO4)2 × 8 H2O (CPO) its separation must be fast. The crystallinity of ACP could be controlled through the temperature during precipitati…
Anhydrous Amorphous Calcium Oxalate Nanoparticles from Ionic Liquids: Stable Crystallization Intermediates in the Formation of Whewellite
2015
The mechanisms by which amorphous intermediates transform into crystalline materials are not well understood. To test the viability and the limits of the classical crystallization, new model systems for crystallization are needed. With a view to elucidating the formation of an amorphous precursor and its subsequent crystallization, the crystallization of calcium oxalate, a biomineral widely occurring in plants, is investigated. Amorphous calcium oxalate (ACO) precipitated from an aqueous solution is described as a hydrated metastable phase, as often observed during low-temperature inorganic synthesis and biomineralization. In the presence of water, ACO rapidly transforms into hydrated whewe…
Crystallization of the CaCO3 mineral in the presence of the protein ovalbumin
2004
Abstract The kinetics of CaCO3 mineralization was studied by SANS in a 0.1 M aqueous CaCl2 solution in the presence of the protein ovalbumin found in chicken eggs. As the scattering from the protein and the mineral was observed within different Q regimes the evolution of the protein and mineral could be followed independently. It is observed that ovalbumin denaturates during the first 3 h and leads to a strong enhancement of mineralization.