Obtaining Ca(H2PO4)(2)·H2O, monocalcium phosphate monohydrate, via monetite from brushite by using sonication.

Brushite was synthesized by precipitation of calcium chloride (CaCl(2)) and sodium phosphate monobasic (Na(2)HPO(4)) dried in vacuum and monetite was obtained from this brushite by sonication with a frequency of 90kHz at 500W for 90min. Monetite itself was also transformed in Ca(H(2)PO(4))(2)·H(2)O, monocalcium phosphate monohydrate (MCPM), by sonication with a frequency of 90kHz at 500W for 60min followed by lyophilization. The MCPM was sonicated and lyophilized by three times more until reach over 240min, but any other phase transformation was observed. All these phase transformations were analyzed by X-ray diffraction (XRD) and infrared spectroscopy (FTIR). Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) indicated a grain size of about 200nm in all the samples. The morphology observed was a corn-flake-like grain for brushite, a pseudo-needle-like grains for monetite, and lamellar-like grains for MCPM.

Crystallographic structure of human tooth enamel by electron microscopy and x-ray diffraction: hexagonal or monoclinic?

Recently reports on the major stability of the monoclinic phase of hydroxyapatite compared with the hexagonal phase have established it as the most observable structure of hydroxyapatite in natural materials, such as hard tissues. In this work, the structural and crystallographic analysis of the inorganic component of sound human tooth enamel was done by transmission electron microscopy, electron diffraction and X-ray diffraction techniques. The results indicated that its unit cell is hexagonal not monoclinic.

Interpretation of the nano-electron-diffraction patterns along the five-fold axis of decahedral gold nanoparticles.

The transition from 10-fold to 5-fold symmetry was observed during the analysis of nanodiffraction patterns of a gold decahedral multiple twinned nanoparticle of 15 nm in diameter. The analysis shows that as the convergence of the beam is increased, the rotational symmetry of the diffraction pattern shifts from 10- to 5-fold. The 10-fold symmetry predicted by Friedel's law is lost by the asymmetric shift of the diffraction spots, an effect that becomes more noticeable as the electron beam convergence increases. Dynamical and kinematical diffraction calculations indicate this decrease in symmetry is the result of a double refraction effect coupled with the variation of the dynamical diffraction conditions arising from a varying electron beam convergence.

On the interpretation of the forbidden spots observed in the electron diffraction patterns of flat Au triangular nanoparticles.

In many cases nanostructures present forbidden spots in their electron diffraction patterns when they are observed by transmission electron microscopy (TEM). To interpret their TEM and high resolution transmission electron microscopy (HRTEM) images properly, an understanding of the origin of these spots is necessary. In this work we comment on the origin of the forbidden spots observed in the [111] and [112] electron diffraction patterns of flat gold triangular nanoparticles. The forbidden spots were successfully indexed as corresponding to the first laue Zone (FOLZ) and the HRTEM images presented a contrast produced by the interference of the zero-order Laue zone (ZOLZ) and FOLZ spots. We discuss the use of the forbidden spots in the study of the structure of nanoparticles and show that they are related to the shape and incompleteness of layers in the very thin particles.

Structural characterization of SmMn2GeO7 single microcrystals by electron microscopy.

Single microcrystals of the new compound samarium dimanganese germanium oxide, SmMn2GeO7, were grown using the flux method in a double spherical mirror furnace (DSMF). The micrometric crystals were observed and chemically analysed with scanning electron microscopy (SEM) and X-ray energy dispersive spectroscopy (EDX). The structural characterization and chemical analysis of these crystals were also carried out using transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM), together with electron-energy-loss spectroscopy (EELS). We found that the new quaternary compound crystallizes in the orthorhombic system with the point group mmm (D2h), space group Immm (No. 71) and cell parameters a=8.30 (10), b=8.18 (10), c=8.22 (10) A and V=558.76 A3.

New model for the hydroxyapatite-octacalcium phosphate interface.

Some experimental results have indicated that hydroxyapatite (HA) and octacalcium phosphate (OCP) can form an epitaxic interface. Subsequently the OCP-HA interface has become of great biological interest in the context of mineralized tissue formation. In this work a new OCP-HA interface model based on Brown's proposed configuration [Brown (1962), Nature, 197, 1048-1050] and using the minimum interface free-energy optimization is presented. This new model is formed by half a unit cell of HA and one unit cell of OCP, as in Brown's model, but in our case [1-210] of HA is 'glued' with [010] of OCP. Therefore, the relationship found was: [000-1](HA) parallel to [001](OCP) and [1-210](HA) parallel to [010](OCP). Self-consistent field methods were used for the analysis of Brown's model and ours. It is shown that the atoms in our model have similar environments as in the HA and OCP unit cells and that, as a result of the differences between HA and OCP unit-cell parameters, this interface presents misfit-dislocation-like features. High-resolution transmission electron microscopy (HREM) simulated images for the new interface model have been included and, when they are compared with the experimental ones, the similarity is quite good.

Electron microscopy, micro-analysis, and X-ray diffraction characterization of the mineral-like tissue deposited by human cementum tumor-derived cells.

The nature and characteristics of the mineralized-like tissue deposited by cementoblasts are not well-known due to the difficulties in obtaining and culturing cells representing the cementum phenotype. We hypothesized that a putative cementoblastic cell line derived from a human cementoblastoma could serve as a suitable model to study the physical, chemical, and morphological features of the cementum-like tissue deposited in vitro. The cementoblastoma cell line was studied by transmission electron, high resolution, scanning, and atomic force microscopy and compared with human cellular cementum, human osteoblasts, and human alveolar bone. The analyses of the crystals and mineral-like tissue in the cell line were performed by x-ray diffraction microscopy and energy-dispersive x-ray micro-analysis. TEM examination of cementoblastoma cells revealed the presence of electron-dense intracellular vesicles surrounded by a membrane that contained filaments and needle-like structures. The diffraction patterns obtained from the intracellular material and human cellular cementum were similar, with D-spacings of 3.36 and 2.8, consistent with those of hydroxyapatite (3.440 and 2.814). The composition of the mineral-like tissue had a Ca/P ratio of 1.60 for cementoblastoma cells and 1.97 for human cellular cementum. Na (5.29%) and Cl (1.47%) were present in the composition of cementoblastoma cells. Human cellular cementum additionally contained Mg (4.95%). Osteoblastic cells showed a Ca/P ratio of 1.6280. Na represented 4.52% and Cl 1.22% of its composition. Human alveolar bone had a Ca/P ratio value of 2.01. Na (6.63%), Mg (2.10%), and Cl (0.84%) were also present. All samples examined represented biological-type hydroxyapatite. Based on the compositional and morphological features, these findings indicate that cementoblastoma-derived cells express the human cellular cementum phenotype.

Structural and Chemical Analysis of Micro-sized Particles Found in Aluminous Electrical Porcelains.

: Uncommon, micro-sized particles with different morphologies were found in sintered aluminous electrical porcelains. The presence of these particles seems to be relatively insensitive to changes in composition of the porcelain system as well as in firing temperatures. X-ray energy-dispersive spectrometry (EDS) microanalysis showed that some particles, those with very well-defined geometries, were composed of K, Si, Al, and O with empirical formula KAlSi(2)O(6)-that is, leucite particles. Other particles showed less well-defined geometries, including some composed of Na, Si, Al, and O, corresponding to a sodium aluminum silicate structure, and others of K, Si, Na, Al, and O, corresponding to the leucite composition, where some K has been substituted for Na. The well-defined geometry particles were detected most often, and diffraction analysis with backscattering electrons showed that their unit cell was cubic, with unit cell parameter a = 1.343 nm. The formation of these particles may be the result of the relatively high concentration of K(2)O and/or Na(2)O in some very localized zones of the glassy phase due to weak coupling (e.g., alkali-enriched or -depleted melts) during diffusion at a slow cooling rate in the presence of catalytic agents such as TiO(2).

Moiré patterns in high resolution electron microscopy images of MoS2.

The contrast observed in the (0001) HREM images of MoS2 are interpreted with a model based on rotational moiré patterns. Computer-simulated images show that rotations of two supercells by angles of 3, 5, 8, and 16 degrees around their centers reproduce the contrast observed in the experimental images. The calculations suggest that these rotations occur between the sulphur layers of the MoS2 structure.