Fatigue fracture analysis of amalgam by SEM-EDS.
Explore the source record for details and available documents.
Chemical Phenomena↗
SEARCH · Search PubMed
Results for “Electron Probe Microanalysis”
Search indexed PubMed citations on genomics, clinical trials, systematic reviews and public health. Explore titles, authors and supplied subject terms, then open the PubMed record.
Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.
Porcelain adherence to dental cast CP titanium: effects of surface modifications.
OBJECTIVES: A reaction layer forms on cast titanium surfaces due to the reaction of the molten titanium with the investment material. Such a layer prevents strong adhesion between titanium and porcelain. This study characterized the effects of surface modifications on cast titanium surfaces and titanium-ceramic adhesion. METHODS: ASTM grade II CP titanium was cast into an MgO-based mold. Castings were devested by sandblasting with alumina particles, and subjected to surface modification by immersion in one of the following solutions: (1) 35% HNO3-5% HF at room temperature for 1min; (2) 50% NaOH-10% CuSO4 x 5H2O at 105 degreesC for 10min; (3) the NaOH-CuSO4 solution followed by the HNO3-HF solution; (4) 50% NaOH-10% NaSO4 at 105 degreesC for 10 min; (5) the NaOH-NaSO4 solution followed by the HNO3-HF solution; and (6) 50% NaOH solution at 105 degreesC for 10min. Surfaces only sandblasted with alumina were used as controls. Specimen surfaces were characterized by XRD and SEM/EDS, and hardness-depth profiles were determined. All specimens were sandblasted with 110 microm alumina particles before porcelain firing. An ultra-low-fusing porcelain (Vita Titankeramik) was fused on the titanium surfaces. The titanium-ceramic adhesion was characterized by a biaxial flexure test, and area fraction of adherent porcelain (AFAP) was determined by X-ray spectroscopy. RESULTS: EDS analyses revealed a substantial amount (13-17 wt%) of Al on the control, and specimens modified with Methods 2, 4, and 6. XRD revealed residual stress in the titanium surfaces and corundum on the control, and Methods 2, 4, and 6 specimens. A new Ti(Cu, Al)2 phase was identified on the titanium surfaces modified by immersion in 50% NaOH-10% CuSO4 x 5H2O aqueous solution. Reduced residual stress was observed on Method 1, 3, and 5 specimens. No corundum peaks were detected on these specimens. Compared to the control, significantly lower (P < 0.05) hardness values were found for Methods 1-3 and Method 5 specimens at 20 microm below the surfaces and for Method 1-5 specimens at 50 microm below the surfaces. Significantly higher (P < 0.05) AFAP values were found for surfaces modified with Methods 2-6 compared to the control and Method 1, and no significant differences were found among Methods 1-6, and between control and Method 1. SIGNIFICANCE: Based on the results from the present study, porcelain adherence to cast CP titanium can be improved by the caustic baths used in the study.
Dental Casting Investment↗
Characteristics of the surface oxides on turned and electrochemically oxidized pure titanium implants up to dielectric breakdown: the oxide thickness, micropore configurations, surface roughness, crystal structure and chemical composition.
Titanium implants have been used widely and successfully for various types of bone-anchored reconstructions. It is believed that properties of oxide films covering titanium implant surfaces are of crucial importance for a successful osseointegration, in particular at compromized bone sites. The aim of the present study is to investigate the surface properties of anodic oxides formed on commercially pure (c.p.) titanium screw implants as well as to study 'native' oxides on turned c.p. titanium implants. Anodic oxides were prepared by galvanostatic mode in CH3COOH up to the high forming voltage of dielectric breakdown and spark formation. The oxide thicknesses, measured with Auger electron spectroscopy (AES), were in the range of about 200-1000 nm. Barrier and porous structures dominated the surface morphology of the anodic film. Quantitative morphometric analyses of the micropore structures were performed using an image analysis system on scanning electron microscopy (SEM) negatives. The pore sizes were < or = 8 microm in diameter and had 1.27-2.1 microm2 opening area. The porosity was in the range of 12.7-24.4%. The surface roughness was in the range of 0.96-1.03 microm (Sa), measured with TopScan 3D. The crystal structures of the titanium oxide were amorphous, anatase, and a mixtures of anatase and rutile type, as analyzed with thin-film X-ray diffractometry (TF-XRD) and Raman spectroscopy. The chemical compositions consisted mainly of TiO2, characterized with X-ray photoelectron spectroscopy (XPS). The native (thermal) oxide on turned implants was 17.4 nm (+/- 6.2) thick and amorphous. Its chemical composition was TiO2. The surface roughness had an average height deviation of 0.83 microm (Sa). The present results are needed to elucidate the influence of the oxide properties on the biological reaction. The results of animal studies using the presently characterized surface oxides on titanium implants will be published separately.
Crystallography, X-Ray↗
Effect of hydrothermally treated anodic oxide films on osteoblast attachment and proliferation.
In this study, the effect of anodization following hydrothermal treatments on osteoblast cell attachment and proliferation were evaluated. The anodic oxide films produced in this study was observed to exhibit overlapping microporous structures with microprojections. In addition, the anodic oxide surfaces were significantly rougher in comparison to control untreated titanium (Ti) surfaces. Following hydrothermal treatments for 2 and 4 h, hydroxyapatite (HA) crystals were observed on anodic surfaces. Using 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyl tetrazolium bromide (MTT) assay, no significant difference in the biocompatibility of the treated and untreated Ti surfaces was observed. However, scanning electron micrographs indicated rounded osteoblast cells on control and anodized Ti surfaces, with numerous microvilli after 6 h. In contract, cells cultured on hydrothermally treated surfaces after 6 h incubation were observed to exhibit polygonal shape, flattened, and fully spread. In addition, more cells were observed on Ti surfaces that were hydrothermally treated for 4 h as compared to Ti surfaces that were hydrothermally treated for 2 h. After culturing the cells for 24 h and 4 days, no significant difference was observed for cells cultured on all surfaces. It was concluded from this study that hydrothermally treated surfaces exhibited an effect on early osteoblast attachment.
Animals↗
Morphological evaluation of osteoblasts cultured on different calcium phosphate ceramics.
The objective of these investigations was to develop an in vitro test system for evaluating novel rapidly resorbable calcium phosphate ceramics of varying composition. Rat bone marrow cells were cultured on the disc-shaped test substrates for 14 days. Five calcium phosphates were examined: R1 CaNaPO4; R1/M2, composed of CaNaPO4 and MgNaPO4; R1/2, composed of CaNaPO4 and Mg2SiO4; R1 + 9% SiO2 consisting of CaNaPO4 and 9% SiO2 (wt%) and R17, Ca2KNa(PO4)2. Two studies were performed. In study I cultures were re-fed every two to three days. In study II the medium was changed daily, and calcium and phosphate concentrations of the medium were determined daily. Specimens were prepared for light microscopy and morphometric evaluation of the cell-covered substrate area, scanning electron microscopy and energy-dispersive X-ray analysis. With all materials tested except for R1/2, an increase of cellular growth was observed after changing the medium daily. Of the different calcium phosphate ceramics tested, R17 and R1/M2 facilitated osteoblast growth and elaboration of extracellular matrix to the highest degree. The inhibition of cell growth encountered with R1 in study I and R1/2 in both studies seemed to be related to a high phosphate-ion release from these materials.
Absorption↗
Lattice-resolution contrast from a focused coherent electron probe. Part I.
To develop a Bloch wave framework for lattice-resolution contrast derived from coherent or incoherent scattering of an electron probe focused onto a crystal, boundary conditions which influence the propagation of an arbitrarily distorted coherent electron probe are addressed. These boundary conditions are particularly relevant for a probe focused within a unit cell, and lead to a general theory which hinges on Bloch wave excitation amplitudes being written as a function of beam position and focus. Whereas antisymmetric Bloch states are not excited for an incident plane wave at an exact zone axis orientation, these states may be strongly excited depending on probe focus and position within the unit cell. Equations for both coherent and incoherent lattice image contrast in scanning transmission electron microscopy are derived for any detector configuration in the Bloch wave framework. An equivalent expression amenable to evaluation via multislice techniques is also described. It is shown explicitly how mixed dynamic form factors for incoherent scattering should be taken into account for annular dark field or backscattered electron detectors, as well as for characteristic losses detected by X-ray emissions or by electron energy loss spectroscopy. A background contribution from "absorbed" electrons is included in the theory. The contribution of cross-talk from neighbouring columns to incoherent contrast is examined within the context of this theoretical framework.
Algorithms↗
Synthesis and microstructural analysis of Si3N4 nanorods.
Alpha-Si3N4 nanorods with 20-80 nm width were synthesized by carbothermal reduction of SiO with amorphous activated carbon (AAC) as a reductant. Microstructural characterization of the synthesized nanorods was carried out by high resolution transmission electron microscopy (HRTEM) and energy dispersive X-ray analysis. Many Si3N4 nanorods were found to be twisted. Each twisted nanorod contained several straight Si3N4 parts. The straight parts had the rod axes orientated along the (1010) direction, which is the closest packing direction of alpha-Si3N4. There were two kinds of joints between the two adjacent straight Si3N4 parts. Formation mechanism of the Si3N4 nanorods is discussed.
Charcoal↗
The influence of tungsten on the chemical composition of a temporally evolving nanostructure of a model Ni-Al-Cr superalloy.
The influence of W on the temporal evolution of gamma' precipitation toward equilibrium in a model Ni-Al-Cr alloy is investigated by three-dimensional atom-probe (3DAP) microscopy and transmission electron microscopy (TEM). We report on the alloys Ni-10 Al-8.5 Cr (at.%) and Ni-10 Al-8.5 Cr-2 W (at.%), which were aged isothermally in the gamma + gamma' two-phase field at 1073 K, for times ranging from 0.25 to 264 h. Spheroidal-shaped gamma' precipitates, 5-15 nm diameter, form during quenching from above the solvus temperature in both alloys at a high number density (approximately 1023 m-3). As gamma' precipitates grow with aging at 1073 K, a transition from spheroidal- to cuboidal-shaped precipitates is observed in both alloys. The elemental partitioning and spatially resolved concentration profiles across the gamma' precipitates are obtained as a function of aging time from three-dimensional atom-by-atom reconstructions. Proximity histogram concentration profiles (Hellman et al., 2000) of the quaternary alloy demonstrate that W concentration gradients exist in gamma' precipitates in the as-quenched and 0.25-h aging states, which disappear after 1 h of aging. The diffusion coefficient of W in gamma' is estimated to be 6.2 x 10-20 m2 s-1 at 1073 K. The W addition decreases the coarsening rate constant, and leads to stronger partitioning of Al to gamma' and Cr to gamma.
Alloys↗
Preparation and characterization of copper-doped cobalt oxide electrodes.
Cobalt oxide (Co3O4) and copper-doped cobalt oxide (CuxCo(3-x)O4) films have been prepared onto titanium support by the thermal decomposition method. The electrodes have been characterized by different techniques such as cyclic voltammetry, scanning electron microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy (XPS). The effect on the electrochemical and crystallographic properties and surface morphology of the amount of copper in the oxide layer has been analyzed. The XPS spectra correspond to a characteristic monophasic Cu-Co spinel oxides when x is below 1. However, when the copper content exceeds that for the stoichiometric CuCo2O4 spinel, a new CuO phase segregates at the surface. The analysis of the surface cation distribution indicates that Cu(II) has preference for octahedral sites.
Cations, Divalent↗
Chitosan and chitosan/ethylene oxide-propylene oxide block copolymer nanoparticles as novel carriers for proteins and vaccines.
PURPOSE: The aim of this study was to investigate the interaction between the components of novel chitosan (CS) and CS/ethylene oxide-propylene oxide block copolymer (PEO-PPO) nanoparticles and to evaluate their potential for the association and controlled release of proteins and vaccines. METHODS: The presence of PEO-PPO on the surface of the nanoparticles and its interaction with the CS was identified by X-ray photoelectron spectroscopy (XPS). The mechanism of protein association was elucidated using several proteins, bovine serum albumin (BSA), and tetanus and diphtheria toxoids, and varying the formulation conditions (different pH values and concentrations of PEO-PPO), and the stage of protein incorporation into the nanoparticles formation medium. RESULTS: BSA and tetanus and diphtheria toxoids were highly associated with CS nanoparticles partly due to electrostatic interactions between the carboxyl groups of the protein and the amine groups of CS. PEO-PPO also interacted electrostatically with CS, thus competing with the proteins for association with CS nanoparticles. A visible amount of PEO-PPO was projected towards the outer phase of the nanoparticles. Proteins were released from the nanoparticles at an almost constant rate, the intensity of which was closely related to the protein loading. Furthermore, the tetanus vaccine was released in the active form for at least 15 days. CONCLUSIONS: CS and CS/PEO-PPO nanoparticles prepared by a very mild ionic crosslinking technique are novel and suitable systems for the entrapment and controlled release of proteins and vaccines.
Animals↗
The surface analysis of implant materials. 1. The surface composition of a titanium dental implant material.
The surfaces of titanium (Ti) plates, as models for Ti implants, have been characterized by X-ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectrometry (TOF SIMS). Plates were prepared with rough and smooth surface topographies--the rough being similar to that of an implant. The XPS data has been used to construct a model of the plates' surface chemical structure, from the gas-solid interface through to pure Ti metal. At the surface of as-received plates, which underwent the same preparative procedure as an implant, considerable surface contamination was detected. In particular, high levels of carbon (C) contaminants were detected; the nature of this C was elucidated by fitting the C 1s core line and from the secondary ion mass spectra. The oxygen (O) 1s core line could not be fitted using a minimum of 2 gaussian peaks, demonstrating the multiplicity of O environments. The detection of other elements in the XPS analysis further demonstrated that, in nominally pure Ti plates, the surface chemical composition deviates considerably from that of the bulk. The data obtained from the plates were confirmed by examination of a Ti abutment. The handling of Ti plates with stainless steel tweezers was investigated. No obvious change in surface chemistry was detected. All the above results bring into serious questions the validity of rigorous protocols demanded, in some techniques, in the handling and use of Ti implants.
Dental Implants↗
Ion implantation: surface treatment for improving the bone integration of titanium and Ti6Al4V dental implants.
Dental implants subjected to surface treatment have shown better bone integration than implants which have only been turned (machined). Three main types of treatment are presently available: the addition of material or coating, the removal of material, and surface modification. Ion implantation corresponds to the third approach. A histomorphometric study is made following the rabbit tibial bone placement of 88 commercial dental implants of pure titanium and Ti6AI4V subjected to surface treatment in the form of different ion implants (C+, CO+, N+, Ne+). Light microscopic, scanning electron microscopic (SEM), electron microsonde (EDS) and X-ray photoelectron spectroscopy (XPS) studies were made. The results indicate improved bone integration (expressed as percentage bone-implant contact) in those specimens subjected to ion implantation versus the non-treated controls, the difference being statistically significant for the groups treated with C+ and CO+. In these groups, XPS showed a Ti-O-C junction (bone-implant interface) involving covalent type bonds, these being stronger and more stable than the ion-type bonds usually established between the titanium oxide and bone.
Alloys↗
Formation of dental silicate cement.
Explore the source record for details and available documents.
Chemical Phenomena↗
Stomatal movements and ion fluxes within epidermis of Commelina communis L.
Explore the source record for details and available documents.
Calcium↗
The identification of asbestos dust with an electron microscope microprobe analyser.
Explore the source record for details and available documents.
Asbestos↗
Cryopreparation of mammalian tissue for X-ray microanalysis in STEM.
A cryopreparation technique for studies of ultrastructure and distribution of diffusible elements in biological tissue is described. Electron microscopical contrast and characteristic X-ray spectra are found to be poor in completely frozen-hydrated ultrathin cryosections of fresh chemically untreated tissue. Both STEM contrast and detection of characteristic X-rays are enhanced by careful freeze-drying in the microscope. Although the ultrastructure is affected by ice crystals, intracellular compartments can be identified by STEM without staining and studied by X-ray microanalysis.
Animals↗
The application of scanning transmission electron microscopy (STEM) to the study of thin anodic films on nickel and nickel-molybdenum alloys.
Anodized thin-film samples of nickel, molybdenum and a nickel-13 w/o molybdenum alloy have been analysed by scanning transmission electron microscopy, using selected area diffraction, microdiffraction and X-ray micro-analysis. Thin-film samples were obtained by ion thinning with argon and by electropolishing in acetic acid-perchloric acid. Electropolishing is the preferred technique for these studies, producing a surface with roughness on a scale of 1 nm. The anodized films on nickel and nickel 13 w/o molybdenum alloy exhibit a rugosity with a 'particle' size of 3 nm. The crystal structure of the films is similar to f.c.c. nickel oxide. Molybdenum enrichment was detected in the anodized alloy surfaces but there is no electron diffraction evidence for a crystalline molybdenum oxide. The electron diffraction pattern from anodized pure molybdenum suggests that the surface film is amorphous.
Alloys↗
Soft X-ray microscopy of ultrathin resin sections.
Explore the source record for details and available documents.
Electron Probe Microanalysis↗