Electron microscopy of stratospheric particles

A recent NASA program to collect stratospheric dust particles using high-flying WB57 aircraft has made available many more potential candidates for the study of extraterrestrial materials. This preliminary report provides an interpretation of the types of particles returned from one flag (W7017) collected in August, 1981 using a subset of 81 allocated particles. This particular collection period is after the Mt. St. Helen's eruptions. Therefore, the flag may contain significant quantities of volcanic debris in addition to the expected terrestrial contaminants [1]. All particles were mounted on nucleopore filters and have been examined using a modified JEOL100CX analytical electron microscope. For most of the particles, X-ray energy dispersive spectra and images were obtained at 40kV on samples which have not received any conductive coating. However, in order to improve resolution (to ~30A) some images are recorded at 100kV. In addition, 16 samples have been coated with a thin layer (<50A) of Au/Pd.

A scanning tunneling microscopy and potentiometry study of epitaxial thin films of La0.7Ca0.3MnO3

To investigate the role of grain boundaries and other growth related microstructure in manganite films, a scanning tunneling microscope is used to simultaneously probe surface topography and local potential distribution under current flow at nanometer level in films of epitaxial thin films of La0.7Ca0.3MnO3 deposited on single crystal SrTiO3 and NdGaO3 substrate by laser ablation. We have studied two types of films strained and strain relaxed. Thin (50nm) films (strained due to lattice mismatch between substrate and the film) show step growth (unit cell steps) and have very smooth surfaces. Relatively thicker films (strain relaxed, thickness 200nm) do not have these step growths and show rather smooth well connected grains. Charge transport in these films is not uniform on the nanometer level and is accompanied by potential jumps at the internal surfaces. In particular scattering from grain boundaries results in large variations in the local potential resulting in fields as high as 104-105V/cm located near the grain boundaries. We discuss the role of local strain and strain inhomogeneties in determining the current transport in these films and their resistance and magnetoresistivity. In this paper we attempt to correlate between bulk electronic properties with microscopic electronic conduction using scanning tunneling microscopy and scanning tunneling potentiometry.

Electron back scattered diffraction (EBSD) characterization of warm rolled and accumulative roll bonding (ARB) processed ferrite

An interstitial free (IF) steel was severely deformed using accumulative roll bonding (ARB) process and warm rolling. The maximum equivalent strains for ARB and warm rolling were 4.8 and 4.0, respectively. The microstructure and micro-texture were studied using optical microscopy and scanning electron microscopy equipped with electron back scattered diffraction (EBSD). The grain size and misorientation obtained by both methods are in the same range. The microstructure in the ARB samples after 6 cycles is homogeneous, although a grain size gradient is observed at the layers close to the surface. The through thickness texture gradient in the ARB samples is different from the warm rolled samples. While a shear texture (⟨110⟩//rolling plane normal direction (ND)) at the surface and rolling texture at the center region is developed in the ARB  samples, the overall texture is weak. The warm rolled samples display a sharp rolling texture through the thickness with increasing the sharpness toward the center. These differences are attributed to the fact that the central region of ARB strip is comprised of material that was once at the surface. The ARB process  can suppress the formation of shear bands which are conventional at warm rolled IF steels. EBSD study on the sample with 6th cycle of ARB following the annealing at 750 ◦C verified a texture gradient through the thickness of the sheet. The shear orientations at the surface and at the quarter thickness layers can be identified even after annealing. The overall weak texture and existence of shear orientations make ARB processed samples unfavorable for sheet metal forming in compare with warm rolled samples.

Microbiological or Chemical Models of Enamel Secondary Caries Compared by Polarized-Light Microscopy and Energy Dispersive X-ray Spectroscopy

Different secondary caries models may present different results. The purpose of this study was to compare different in vitro secondary caries models, evaluating the obtained results by polarized-light microscopy (PLM), scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDS). Standardized human enamel specimens (n = 12) restored with different materials (Z250 conventional composite resin-CRZ, Freedom polyacid-modified composite resin-CRF, Vitremer resin-modified glass-ionomer-GIV, and Fuji IX conventional glass-ionomer cement-GIF) were submitted to microbiological (MM) or chemical caries models (CM). The control group was not submitted to any caries model. For MM, specimens were immersed firstly in sucrose broth inoculated with Streptococcus mutans ATCC 35688, incubated at 37 degrees C/5% CO(2) for 14 days and then in remineralizing solution for 14 days. For CM, specimens were submitted to chemical pH-cycling. Specimens were ground, submitted to PLM and then were dehydrated, gold-sputtered and submitted to SEM and EDS. Results were statistically analyzed by Kruskall-Wallis and Student-Newman-Keuls tests (alpha = 0.05). No differences between in vitro caries models were found. Morphological differences in enamel demineralization were found between composite resin and polyacid-modified composite resin (CRZ and CRF) and between the resin-modified glass-ionomer and the glass-ionomer cement (GIF and GIV). GIF showed higher calcium concentration and less demineralization, differing from the other materials. In conclusion, the glass-ionomer cement showed less caries formation under both in vitro caries models evaluated. (C) 2009 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater 90B: 635-640, 2009

Ability of different restorative materials to prevent in situ secondary caries: analysis by polarized light-microscopy and energy-dispersive X-ray

Secondary caries is the main cause of direct restoration replacement. The purpose of this study was to analyze enamel adjacent to different restorative materials after in situ cariogenic challenge using polarized-light microscopy (PLM), scanning electron microscopy (SEM) and energy-dispersive X-ray analysis (EDS). Twelve volunteers, with a low level of dental plaque, a low level of mutans streptococci, and normal salivary flow, wore removable palatal acrylic appliances containing enamel specimens restored with Z250 composite, Freedom composite, Fuji IX glass-ionomer cement, or Vitremer resin-modified glass-ionomer for 14 days. Volunteers dripped one drop of 20% sucrose solution (n = 10) or distilled water (control group) onto each specimen 8 times per day. Specimens were removed from the appliances and submitted to PLM for examination of the lesion area (in mm(2)), followed by dehydration, gold-sputtering, and submission to SEM and EDS. The calcium (Ca) and phosphorus (P) contents were evaluated in weight per cent (%wt). Differences were found between Z250 and Vitremer, and between Z250 and FujiIX, when analyzed using PLM. Energy-dispersive X-ray analysis results showed differences between the studied materials regarding Ca %wt. In conclusion, enamel adjacent to glass-ionomer cement presented a higher Ca %wt, but this material did not completely prevent enamel secondary caries under in situ cariogenic challenge.

Correlative light-electron fractography of interlaminar fracture in a carbon-epoxy composite

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

The discriminative bilateral filter: An enhanced denoising filter for electron microscopy data

Advances in three-dimensional (313) electron microscopy (EM) and image processing are providing considerable improvements in the resolution of subcellular volumes, macromolecular assemblies and individual proteins. However, the recovery of high-frequency information from biological samples is hindered by specimen sensitivity to beam damage. Low dose electron cryo-microscopy conditions afford reduced beam damage but typically yield images with reduced contrast and low signal-to-noise ratios (SNRs). Here, we describe the properties of a new discriminative bilateral (DBL) filter that is based upon the bilateral filter implementation of Jiang et al. (Jiang, W., Baker, M.L., Wu, Q., Bajaj, C., Chin, W., 2003. Applications of a bilateral denoising filter in biological electron microscopy. J. Struc. Biol. 128, 82-97.). In contrast to the latter, the DBL filter can distinguish between object edges and high-frequency noise pixels through the use of an additional photometric exclusion function. As a result, high frequency noise pixels are smoothed, yet object edge detail is preserved. In the present study, we show that the DBL filter effectively reduces noise in low SNR single particle data as well as cellular tomograms of stained plastic sections. The properties of the DBL filter are discussed in terms of its usefulness for single particle analysis and for pre-processing cellular tomograms ahead of image segmentation. (c) 2006 Elsevier Inc. All rights reserved.

Structure–property relationships of silk-modified mesoporous bioglass scaffolds

Porous mesopore-bioglass (MBG) scaffolds have been proposed as a new class of bone regeneration materials due to their apatite-formation and drug-delivery properties; however, the material’s inherent brittleness and high degradation and surface instability are major disadvantages, which compromise its mechanical strength and cytocompatibility as a biological scaffold. Silk, on the other hand, is a native biomaterial and is well characterized with respect to biocompatibility and tensile strength. In this study we set out to investigate what effects blending silk with MBG had on the physiochemical, drug-delivery and biological properties of MBG scaffolds with a view to bone tissue engineering applications. Transmission electron microscopy (TEM), scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR) were the methods used to analyze the inner microstructure, pore size and morphology, and composition of MBG scaffolds, before and after addition of silk. The effect of silk modification on the mechanical property of MBG scaffolds was determined by testing the compressive strength of the scaffolds and also compressive strength after degradation over time. The drug-delivery potential was evaluated by the release of dexamethasone (DEX) from the scaffolds. Finally, the cytocompatibility of silk-modified scaffolds was investigated by the attachment, morphology, proliferation, differentiation and bone-relative gene expression of bone marrow stromal cells (BMSCs). The results showed that silk modification improved the uniformity and continuity of pore network of MBG scaffolds, and maintained high porosity (94%) and large-pore size (200–400 mm). There was a significant improvement in mechanical strength, mechanical stability, and control of burst release of DEX in silkmodified MBG scaffolds. Silk modification also appeared to provide a better environment for BMSC attachment, spreading, proliferation, and osteogenic differentiation on MBG scaffolds.

Bioactive inorganic materials/alginate composite microspheres with controllable drug-delivery ability

Alginate microspheres are considered a promising material as a drug carrier in bone repair due to excellent biocompatibility, but their main disadvantage is low drug entrapment efficiency and non-controllable release. The aim of this study was to investigate the effect of incorporating mesoporous bioglass (MBG), non-mesoporous bioglass (BG) or hydroxyapatite (HAp) into alginate microspheres on their drug-loading and release properties. X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and atomic emission spectroscopy (AES) were used to analyse the composition, structure and dissolution of bioactive inorganic materials and their microspheres. Dexamethasone (DEX)-loading and release ability of four microspheres were tested in phosphate buffered saline with varying pHs. Results showed that the drug-loading capacity was enhanced with the incorporation of bioactive inorganic materials into alginate microspheres. The MBG/Alginate microspheres had the highest drug loading ability. DEX release from alginate microspheres correlated to the dissolution of MBG, BG and HAp in PBS, and that the pH was an efficient factor in controlling the DEX release; a high pH resulted in greater DEX release, whereas a low pH delayed DEX release. In addition, MBG/alginate, BG/alginate and HAp/alginate microspheres had varying apatite-formation and dissolution abilities, which indicate that the composites would behave differently with respect to bioactivity. The study suggests that microspheres made of a composite of bioactive inorganic materials and alginate have a bioactivity and degradation profile which greatly improves their drug delivery capacity, thus enhancing their potential applications as bioactive filler materials for bone tissue regeneration.

Ordering of Ge islands on Si(001) substrates patterned by nanoindentation

Spatial organization of Ge islands, grown by physical vapor deposition, on prepatterned Si(001) substrates has been investigated. The substrates were patterned prior to Ge deposition by nanoindentation. Characterization of Ge dots is performed by atomic force microscopy and scanning electron microscopy. The nanoindents act as trapping sites, allowing ripening of Ge islands at those locations during subsequent deposition and diffusion of Ge on the surface. The results show that island ordering is intrinsically linked to the nucleation and growth at indented sites and it strongly depends on pattern parameters.

Microstructural studies of quenched partially-melted Y-123 materials and Y-123 with Y-211, PtO2 and CeO2 additions

The microstructure of YBa2Cu3O7-delta (Y-123) materials partially-melted in air and quenched from the temperature range 900-1100 degrees C, has been characterized using a combination of X-ray diffractometry, optical microscopy, scanning electron microscopy, electron microprobe analyses, transmission electron microscopy and energy and wave dispersive X-ray spectrometries. The microstructural studies reveal significant changes in the character of the quenched partial-melt as a function of temperature and time before quenching. BaCu2O2 and BaCuO2 are found to co-exist in stoichiometric samples quenched from the temperature range 920-960 degrees C. Under suitable cooling conditions, large pockets of melt cristallize as BaCuO2 with an exsolution of BaCu2O2 in the form of thin plates (approximate to 50-100 nm thick) along facets. Y2BaCuO5 (Y-211) additions are associated with the formation of BaCu2O2 at 1100 degrees C. Preliminary results on the effects of PtO2 and CeO2 additions to Y-123 (and Y-123 with Y-211 additions) show that these enhace the formation of BaCu2O2 at the melting temperature of 1100 degrees C. (C) 1998 Elsevier Science S.A. All rights reserved.

Microstructural characterization of quenched melt-textured YBa2Cu3O7-δ materials

The microstructure of YBa2Cu3O7-δ (YBCO) materials, melt-textured in air and quenched from the temperature range 900-990°C, has been characterized using a combination of x-ray diffractometry, optical microscopy, scanning electron microscopy, transmission electron microscopy, and energy dispersive x-ray spectrometry. BaCu2O2 and BaCuO2 were found to coexist in samples quenched from the temperature range 920-960°C. The formation of BaCu2O2 preceded the formation of YBCO. Once the YBCO had formed, BaCu2O2 was present at the solidification front filling the space between nearly parallel platelets of YBCO. Large Y2BaCuO5 particles at the solidification front appeared divided into smaller ones as a result of their dissolution in the liquid that quenched as BaCu2O2.

Electrical property and characterization of nano-SnO2/wollastonite composite materials

Nano-tin oxide was deposited on the surface of wollastonite using the mixed solution including stannic chloride pentahydrate precursor and wollastonite by a hydrolysis precipitation process. The antistatic properties of the wollastonite materials under different calcined conditions and composite materials (nano-SnO2/wollastonite, SW) were measured by rubber sheeter and four-point probe (FPP) sheet resistance measurement. Effects of hydrolysis temperature and time, calcination temperature and time, pH value and nano-SnO2 coating amount on the resistivity of SW powders were studied, and the optimum experimental conditions were obtained. The microstructure and surface properties of wollastonite, precipitate and SW were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy-dispersive X-ray spectrometry (EDS), specific surface area analyzer (BET), thermogravimetry (TG), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), and Fourier translation infrared spectroscopy (FTIR) respectively. The results showed that the nano-SnO2/wollastonite composite materials under optimum preparation conditions showed better antistatic properties, the resistivity of which was reduced from 1.068 × 104 Ω cm to 2.533 × 103 Ω cm. From TG and XRD analysis, the possible mechanism for coating of SnO2 nanoparticles on the surface of wollastonite was proposed. The infrared spectrum indicated that there were a large number of the hydroxyl groups on the surface of wollastonite. This is beneficial to the heterogeneous nucleation reaction. Through morphology, EDS and XPS analysis, the surface of wollastonite fiber was coated with a layer of 10–15 nm thickness of tin oxide grains the distribution of which was uniform.

In situ Raman studies of the selective oxidation of methanol to formaldehyde and ethene to ethylene oxide on a polycrystalline silver catalyst

The combined techniques of in situ Raman microscopy and scanning electron microscopy (SEM) have been used to study the selective oxidation of methanol to formaldehyde and the ethene epoxidation reaction over polycrystalline silver catalysts. The nature of the oxygen species formed on silver was found to depend critically upon the exact morphology of the catalyst studied. Bands at 640, 780 and 960 cm-1 were identified only on silver catalysts containing a significant proportion of defects. These peaks were assigned to subsurface oxygen species situated in the vicinity of surface dislocations, AgIII=O sites formed on silver atoms modified by the presence of subsurface oxygen and O2 - species stabilized on subsurface oxygen-modified silver sites, respectively. The selective oxidation of methanol to formaldehyde was determined to occur at defect sites, where reaction of methanol with subsurface oxygen initially produced subsurface OH species (451 cm-1) and adsorbed methoxy species. Two distinct forms of adsorbed ethene were identified on oxidised silver sites. One of these was created on silver sites modified by the interaction of subsurface oxygen species, and the other on silver crystal planes containing a surface coverage of atomic oxygen species. The selective oxidation of ethene to ethylene oxide was achieved by the reaction between ethene adsorbed on modified silver sites and electrophilic AgIII=O species, whereas the combustion reaction was perceived to take place by the reaction of adsorbed ethene with nucleophilic surface atomic oxygen species. Defects were determined to play a critical role in the epoxidation reaction, as these sites allowed the rapid diffusion of oxygen into subsurface positions, and consequently facilitated the formation of the catalytically active AgIII=O sites.