Mechanical improvement of hydroxyapatite by TiO<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript> nanoparticles deposition

Deposition of Ti was carried out by laser ablation onto hydroxyapatite porous discs in an Ar atmosphere. Ti nanoparticles were deposited onto HAp surface in order to modify its roughness and morphology as it is observed by scanning electron microscopy (SEM) and scanning probe microscopy (SPM). A homogeneous distribution of Ti over the disc surface was corroborated by elemental mapping. A comparison of the hydroxyapatite hardness before and after deposition was performed using SPM nanoindentation. Transmission Electron Microscopy (TEM) showed that the Ti nanoparticles obtained were covered by an oxygen shell. It is shown that surface modifications of the covered HAp by Ti result in better mechanical properties, reducing the possible damage to the HAp ceramic by friction or impacts as it often happens in meniscus, bone junctions and the inclusion of prosthesis for human treatments.     

Modern Applications of Electron Microscopy to Catalysis

The active sites of ultra-dispersed Pt/-Al₂O₃ catalysts are studied using high-resolution electron microscopy, Z-contrast and dark field. In addition we have calculated using a method based in density functional theory the electrostatic potential and charge distribution of the active sites. It is conclude that the most likely Pt clusters that are formed correspond to Pt₁₃ and Pt with icosahedral and decahedral structure. It is shown that this is consistent with the electron microscopy data.     

Transmission electron microscopy and theoretical analysis of AuCu nanoparticles: atomic distribution and dynamic behavior

Though the application of bimetallic nanoparticles is becoming increasingly important, the local atomistic structure of such alloyed particles, which is critical for tailoring their properties, is not yet very clearly understood. In this work, we present detailed study on the atomistic structure of Au-Cu nanoparticles so as to determine their most stable configurations and the conditions for obtaining clusters of different structural variants. The dynamic behavior of these nanoparticles upon local heating is investigated. AuCu nanoparticles are characterized by high resolution transmission electron microscopy (HRTEM) and energy filtering elemental composition mapping (EFECM), which allowed us to study the internal structure and the elemental distribution in the particles. Quantum mechanical approaches and classic molecular dynamics methods are applied to model the structure and to determine the lowest energy configurations, the corresponding electronic structures, and understand structural transition of clusters upon heating, supported by experimental evidences. Our theoretical results demonstrate only the core/shell bimetallic structure have negative heat of formation, both for decahedra and octahedral, and energetically favoring core/shell structure is with Au covering the core of Cu, whose reverse core/shell structure is not stable and may transform back at a certain temperature. Experimental evidences corroborate these structures and their structural changes upon heating, demonstrating the possibility to manipulate the structure of such bimetallic nanoparticles using extra stimulating energy, which is in accordance with the calculated coherence energy proportions between the different configurations.     

Observation of sulfur on the surface of giant aurothiol nanoclusters

We report the study of aurothiol nanoclusters using high-resolution electron microscopy, energy loss spectroscopy, X-ray photoelectron spectroscopy, Auger spectroscopy, and microscopy. It is concluded that the sulfur atoms are located on the surface of the gold nanoparticles in both (100) and (111) microfacets. The X-ray photoelectron spectroscopy data show that there is a Au-Au bond as well as a Au-S bond. Auger depth profile measurements made by sputtering of the nanoparticles corroborates that the sulfur is located on the surface of the nanoparticle. Quantitative Auger analysis indicates a ratio Au/S between approximately 1.79 and 1.98.     

Immunochemical properties of a 60 kDa cell surface-associated heat shock-protein (Hsp60) from Helicobacter pylori

Western blot analysis (immunoblotting) of cell surface-associated proteins from Helicobacter pylori confirmed our previous findings that binding of human IgG is a common property (among H. pylori strains). Purification of the IgG-binding proteins (IGBP) was achieved by two purification steps, affinity chromatography on IgG-Sepharose and nickel chelate affinity chromatography. SDS-PAGE and immunoblotting analysis revealed a 60 kDa protein with affinity for peroxidase labeled human IgG. Solid phase binding assays showed that IgG binds to an immobilized protein (IGBP). The 60 kDa IGBP binds human IgG1, IgG3 and IgM. Binding could be inhibited by the kappa chain of the human IgG, but not with its Fc fragment, nor with IgA or IgM. In addition, rabbit polyclonal antibodies raised against the 60 kDa IGBP blocked IgG binding. Monoclonal antibodies, specific to the Hsp60 heat shock protein of H. pylori recognized the 60 kDa IGBP as revealed by immunoblotting analysis, both in crude preparations and in the purified fractions.     

Synthesis and characterisation of YSZ-Al2O3 nanostructured materials

In this work a co-precipitation route was used to synthesise two yttria-stabilised-zirconia (YSZ) phases with different concentrations of alumina (Al2O3). A tetragonal, with 3 mol% yttria, and a cubic, with 8 mol% yttria, phases were added with alumina in different weight proportions, 90/10, 80/20, 70/30, and 60/40, respectively. After synthesised, products were sintered in a range 800-1100 degrees C for different intervals of time. Compounds were characterised by X-ray diffraction, transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), scanning electron microscopy (SEM), and atomic force microscopy (AFM). Rietveld refinements, using FULPROF-Suite software, were carried out to obtain the cell parameters and structural characterisation of products.     

Neodymium nanoparticles: biosynthesis and structural analysis

Small metallic nanoparticles of neodymium are obtained by a facile route based on the biosynthesis and the pH conditions that demonstrate the possibility of obtaining particles of 1-8 nm. The size is controlled by synthesis conditions. Smaller clusters were obtained with pH = 5, while for pH = 10 evidences of nanorods productions are found and this opens the perspective to use this rare-earth element for zero and one dimensional based applications. Using transmission electron microscopy techniques, the size distribution and structure are studied. Density functional theory-based calculations allow the determination of the lowest energy configuration, which is based on the hexagonal bulk symmetry. Theoretical models are used to simulate the high resolution transmission electron microscopy to identify the experimental image, determining that the synthesized nanoparticles reach the lowest energy hexagonal configurations.     

Preparation of AlFe nanoparticles by mechanical alloyed technique

Small metallic particles (1-3 nm) have been obtained using mechanical alloying techniques. Analytical techniques such as scanning electron microscopy have been used for the morphological and chemical characterization of the AlFe alloyed powders. B, Ni and Ti have been explored as reinforced elements to the initial AlFe mixture. X-ray diffraction patterns and transmission electron microscopy (TEM) techniques have been employed for the structural characterization of the small metallic particles. Theoretical simulations based on molecular dynamics have been used to interpret some of the experimental structural results. Furthermore, theoretical simulations of HREM images based on the dynamical theory of electron diffraction have also been obtained and comparisons with the experimental results have been carried out. The complementary analyses determined that the produced clusters are basically AlFe alloyed nanoparticles immersed in a matrix and with multiple defected structures.     

Structure, stability and catalytic activity of chemically synthesized Pt, Au, and Au-Pt nanoparticles

Small (1-5 nm) metallic nanoparticles of Pt, Au, and Au/Pt of different nominal compositions in colloidal form were synthesized by a chemical reduction method using polymer (PVP) as protecting agent. Analytical techniques like HREM and UV-vis spectroscopy have been used to characterize the morphology and structural properties of these small particles. Theoretical simulations based on molecular dynamical have been used to interpret the experimental structural results and analyze the macroscopic properties like stability and catalytic selectivity of these nanoparticles based on the morphology and atomic distribution in the clusters.