Small angle X-ray scattering study of surface modified tin oxide nanoparticles prepared by sol-gel route

The surface properties of SnO2 nanoparticles were modified by grafting ionic (Tiron (R). (OH)(2)C6H2(SO3Na)(2)(H2O)-H-.) or non-ionic (Catechol (R). C6H4-1,2-(OH)(2)) capping Molecules during aqueous sol-gel processing to improve the redispersibility of powdered xerogel. The effect of the amount of grafted organic molecules on the redispersibility of powders in aqueous solution at several basic pH values was Studied. The nanostructural features of the colloidal suspensions were analyzed by small angle X-ray scattering (SAXS) measurements. Irrespective of the nature and amount of grafted molecules, complete redispersion was obtained in aqueous solution at pH = 13. The redispersion at pH = 11 results in a mixture of dispersed primary particles and aggregates. The proportion of well dispersed nanoparticles and aggregates (and their average size) can be tuned by the quantity of grafted ionic molecules.

Synthesis and luminescence properties of water dispersible Eu3+-doped boehmite nanoparticles

Nanocrystallized boehmite gamma-AlOOH center dot nH(2)O had been synthesized by spray-drying (SD) of a solution of aluminium tri-sec-butoxide peptized by nitric acid. The sub-micronic spherical particles obtained had an average diameter of 500 nm and were built of 100 nm or less platelet-like sub-particles. The average crystallite size calculated from XRD was 1.6 nm following the b axis (i.e. one unit cell) and 3-4 nm perpendicular to b. As a result of the nanometric sizes of crystallites, there was a large surface free for water adsorption and it was found to be n = 1.18 +/- 0.24H(2)O per AlOOH. The SD spheres spontaneously dispersed in water at room temperature and formed stable-over months-suspensions with nanometre-size particles (25-85 nm). Luminescent europium-doped nanocrystallized boehmites AlOOH: Eu (Al0.98Eu0.02OOH center dot nH(2)O) were synthesized the same way by SD and demonstrated the same crystallization properties and morphologies as the undoped powders. It is inferred from the Eu3+ luminescence spectroscopy that partly hydrated europium species are immobilized on the boehmite nanocrystals where they are directly bonded to alpha(OH) groups of the AlOOH surface. The europium coordination is schematically written [Eu3+(OH)(alpha)(H2O)(7-alpha/2)]. The europium-doped boehmite from SD spontaneously dispersed in water: the luminescence spectroscopy proves that most of the Eu3+ ions were detached from the NPs during water dispersion. The AlOOH: Eu nanoparticles were modified by the amine acid asparagine (ASN). The modification aimed to render the NPs compatible for further bio-functionalization. After surface modification, the NPs easily dispersed in water; the luminescence spectra after dispersion prove that the Eu3+ ions were held at the boehmite surface.

Influence of silver additions on the Cu-13 wt pct Al alloy hardness.

The influence of silver additions on the Cu-13 wt. pot. Al alloy hardness was studied for additions in the range 0 to 16 wt. pot Ag. The results indicated a pronounced hardness increase with the silver content and an influence of the quenching temperature. Data obtained from scanning electron microscopy indicated that the formation of silver-rich precipitates, wich change with the quenching temperature, seems to produce the changes on alloys hardness.

Influence of silver additions on the thermal behavior of the Cu-8 mass% Al alloy

The influence of additions of 2, 4, 6, 8, 10 and 12 mass% Ag on the thermal behavior of the Cu-8 mass% Al alloy was studied using differential scanning calorimetry (DSC), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX) and X-ray diffractometry (XRD). The results indicate that the presence of silver introduces new thermal events, due to the formation of a silver-rich phase and, for additions of 10 and 12 mass% Ag, it is possible to verify the formation of the gamma (1) phase (Cu9Al4) and the metastable transitions which are only observed in alloys with a minimum of 9 mass% Al.

SAXS study of formation and growth of tin oxide nanoparticles in the presence of complexing ligands

The effect of acetylacetone (acac) complexing ligand on the formation and growth of tin oxide-based nanoparticles during thermohydrolysis at 70 degreesC of a tin precursor SnCl4-n(acac)(n) (0 less than or equal to n less than or equal to 2) solution was analyzed by in situ small-angle X-ray scattering. A. transparent and stable sol was obtained after 2 h of thermohydrolysis at 70 degreesC, allowing the quantitative determination of the particle volume distribution function and its variation with the reaction time. The number of colloidal particles for equivalent thermohydrolysis temperature and time decreases as the [acac]/[Sn] ratio in initial solution increases from 0.5 to 6. Instead, the amount of soluble species remaining in solution increases for increasing [acac]/[Sn] ratio within the same range. This indicates that increasing amounts of Sn-acetylacetone complexes partially prevent the hydrolysis and consequent formation of colloidal particles. The N-2 adsorption isotherm characterization of freeze-dried powders demonstrates that the average pore size is approximately equal to the average size (approximate to9 Angstrom) of the colloidal primary particles in the sol, and that the porosity and surface area (approximate to200 m(2) g(-1)) are independent of the acac content in the initial solution.

Indocyanine green nanoparticles useful for photomedicine

Objective: the aim of this study was to evaluate the potential application of biodegradable nanoparticles (NPs) containing indocyanine green (ICG) in photodynamic therapy (PDT). Methods: Important parameters, such as particle size and external morphology, were established by dynamic light scattering (DLS) and scanning electron microscopy (SEM). Also, drug encapsulation efficiency and in vitro release behavior were evaluated by spectroscopic methods. Results: the particles are spherical in shape, they exhibit an 817-nm diameter, and they have a low tendency to aggregate. The loading efficiency was 65%. ICG photophysical parameters showed a bathocromic shift in ICG-loaded nanoparticles (ICG-NP). Analysis of the cell P388-D1 in the presence of the ICG-NP by SEM showed that the majority of the nanoparticles were uptaken by phagocytic cells after 2 h of incubation. After laser irradiation photodamage was observed in P388-D1 cells where ICG-NPs had been uptaken by phagocytic cells. Conclusion: Polymeric NPs work as an efficient drug delivery system for PDT drugs, and this approach can be used in the administration of amphiphilic photosensitizers in the treatment of neoplasic cells.

Complete staining of nerve fiber and myoneural junctions with acetylthiocholine and silver

We describe a combined stain for simultaneous demonstration of the preterminal axons and cholinesterase activity at myoneural junctions of mammalian muscles. This technique employs acetylthiocholine iodide as the substrate for cholinesterase activity and silver nitrate impregnation of preterminal axons. The procedure is rapid, simple and uses fresh muscles. Intramuscular nerves, preterminal axons and myoneural junctions are stained simultaneously brown or black with minimal background staining of connective tissue and muscle fibers.

Solid-state and solution structural study of acetylacetone-modified tin(IV) chloride used as a precursor of SnO2 nanoparticles prepared by a sol-gel route

The effect of addition of different amounts of acetylacetone (acacH) on the species formed at room temperature and after thermohydrolysis at 70 degreesC for 30 and 120 min of ethanolic SnCl4.5H(2)O solutions is followed by EXAFS spectroscopy at the Sn K-edge. We show that thermohydrolyzed solutions are a mixture of SnO2 nanoparticles and soluble tin polynuclear species. The complexation of the tin molecular precursors by acetylacetonate ligands is evidenced by H-1, C-13, and Sn-119 NMR spectroscopy and EXAFS for a acacH/Sn ratio higher than 2. Single crystals are isolated from solution and the structure, determined by X-ray diffraction, is built up from monomeric Cl-3(H2O)Sn(acac)-H2O units bridged together by hydrogen bonding. The acacH/Sn ratio in solution controls the polycondensation of the hydrolyzed species but not the crystallite size of the SnO2 nanoparticles (similar to2 nm). Because of the major presence of chelated tin mono- and dimeric complexes in solution for acacH/Sn > 2, the condensation is almost inhibited, meanwhile the decrease of amount of chelated complexes for the acacH/Sn < 2 gives rise to an increase of the number of nanoparticles.

Wet-chemical synthesis of magnesium niobate nanoparticles powders

Nanosized and highly reactive magnesium mobate (MgNb2O6) powders were successfully synthesized by a new wet-chemical method by means of the dissolution of Nb2O5 center dot 5H(2)O and in a solution of oxalic acid followed by the addition of stoichiometric amounts of magnesium carbonate. The Nb-Mg-oxalic acid solution was evaporated resulting in a dry and amorphous powder that was calcined in the temperature range from 200 to 900 degrees C for 2 h. The crystallization process from the amorphous state to the crystalline MgNb2O6 was followed by thermal analysis. The calcined powders characterized by FT-Raman spectroscopy, X-ray diffraction (XRD) and their morphology examined by high resolution scanning electron microscopy (HR-SEM). Pure MgNb2O6, free from the second phases and obtained at 800 degrees C was confirmed by a combined analysis using XRD and FT-Raman. The average diameter of the particles was calculated from the HR-SEM image as 70 urn approximately. This technique allows a better mixing of the constituent elements and thus a better reactivity of the mixture to obtain pre-reaction products with high purity at lower temperatures and reducing cost. It can offer a great advantage in the PMN-PT formation with respect to the solid-state synthesis. (c) 2006 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Preparation of ceramic membranes from surface modified tin oxide nanoparticles

The preparation of crack-free SnO2 supported membranes requires the development of new strategies of synthesis capable to allow controlled changes of surface chemistry and to improve the processability of supported layers. In this way, the controlled modification of the SnO2 nanoparticle surface by adding capping molecules like Tiron(R) ((OH)(2)C6H2(SO3Na)(2)) during the sol-gel process was studied, aiming to obtain high performance membranes. Colloidal suspensions were prepared by hydrolyzing SnCl4.5H(2)O aqueous solution with NH4OH in presence of Tiron(R). The effect of the amount of Tiro(R) (from I to 20 wt.%) on the structural features of nanoparticles, powder redispersability and particle-solution interface properties was investigated by X-ray powder diffraction (XRPD), extended X-ray absorption fine structure (EXAFS), quasi-elastic light scattering and electrophoretic mobility measurements. XRPD and EXAFS results showed that the addition of Tiron(R) up to 20 wt.% to colloidal suspensions does not affect the crystallite size of SnO2 primary particles, determined around 2-3 nm. This value is comparable to the hydrodynamic size measured after redispersion of powder prepared with amount of Tiro(R) higher than 7.5 wt.%, indicating the absence of condensation reactions between primary particles after the initial precipitation step. As a consequence the powder with amount of Tiron(R) > 7.5 wt.%, can be fully redispersed in aqueous solution at pH greater than or equal to I I until a nanoparticle concentration of 6 vol.%. The electrophoresis measurements showed a decrease of the isoelectric point by increasing the amount of grafted Tiron(R) at the SnO2 nanoparticle surface, resulting in negatively charged particle-solution interface in all the studied pH range (2-11). These features govern the gelation process favoring the preparation of crack-free SnO2 supported membranes. The control exercised by Tiron(R) modifying agent in the aggregation process allows the fine-tuning of the porosity, from 0.124 to 0.065 cm(3) g(-1), and mean pore size, from 6.4 to 1.9 nm, as the amount of grafted molecules increases from 0 to 10 wt.%. In consequence, the membrane cut-off determined by filtration of polyethylene glycol standard solutions can be screened from 1500 to 3500 g mol(-1). (C) 2002 Elsevier B.V. B.V. All rights reserved.

Preparation of ZnO nanoparticles: Structural study of the molecular precursor

The structure of zinc acetate derived precursor currently used in the sol-gel synthesis of ZnO nanoparticles is described. The reaction products obtained before and after reflux of ethanolic zinc acetate solution have been studied by UV-Vis, photoluminescence, FTIR and EXAFS at the Zn K edge. EXAFS results evidence for both precursor solutions a change from the octahedral coordination sphere of oxygen atoms characteristic of the solid zinc acetate dihydrate compound into a four-fold environment. The EXAFS spectra of precursor solutions can be satisfactorily reproduced using the molecular structure reported for Zn4O(Ac)(6) (Ac = COOCH3). UV-Vis and FTIR measurements are also in agreement with the formation of this oligomeric precursor. The structural modification is more pronounced after reflux at 80degreesC, because the increase of the Zn4O(Ac)(6) amount and the formation of nearly 3.0 nm sized ZnO nanoparticle.

Potentiometric determination of saccharin in commercial artificial sweeteners using a silver electrode

A simple, precise, rapid and low-cost potentiometric method for saccharin determination in commercial artificial sweeteners is proposed. Saccharin present in several samples of artificial sweeteners is potentiometrically titrated with silver nitrate solution using a silver wire as the indicator electrode, coupled to a titroprocessor. The best pH range was from 3.0 to 3.5 and the detection limit of sodium saccharin was 2.5 mg/ml. Substances normally found along with saccharin in several commercial artificial sweeteners such as maltodextrin, glucose, sucrose, fructose, aspartame, cyclamate, caffeine, sorbitol, lactose, nitrate, methyl- and n-propyl-p-hydroxybenzoate, benzoic, citric and ascorbic acids do not interfere even in significant amounts (e.g. 20 excess relative to saccharin). Chloride ion interferes when present in concentrations larger than 10 mg l(-1); this interference is eliminated with previous extraction of the sweetener from the aqueous medium with ethyl acetate. The results obtained by applying the proposed method compared very favorably with those given by the HPLC method recommended by the FDA. (C) 2003 Elsevier Ltd. All rights reserved.

Evaluation of nanoparticles loaded with benzopsoralen in rat peritoneal exudate cells

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

X-ray powder diffraction analysis of a silver(I)-aspartame complex

Synchrotron X-ray powder diffraction (XRPD) data were collected for the silver(I)-aspartame complex [Ag(C14H17N2O5)]center dot 1/2 H2O. The complex was obtained from a stoichiometric mixture of aspartame (3-amino-N-(alpha-carboxyphenethyl)-succinamic acid N-methyl ester, C14H18N2O5), Na2CO3, and AgNO3. Indexing using Crysfire and Chekcell proposed an orthorhombic unit cell with space group P222(1). The lattice parameters are a = 12.4750(1) angstrom, b = 21.60614(14) angstrom, and c = 4.88888(9) angstrom. (C) 2006 International Centre for Diffraction Data.