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Sample records for sem tem xrd

  1. Analyzing the scale of the bainitic ferrite plates by XRD, SEM and TEM

    International Nuclear Information System (INIS)

    Garcia-Mateo, Carlos; Jimenez, Jose A.; Lopez-Ezquerra, Belen; Rementeria, Rosalia; Morales-Rivas, Lucia; Kuntz, Matthias; Caballero, Francisca G.

    2016-01-01

    Since the major strengthening mechanisms in nanocrystalline bainitic steels arise from the exceptionally small size of the bainitc ferrite plate, accurate determination of this parameter is fundamental for quantitative relating the microstructure to the mechanical properties. In this work, the thickness of the bainitic ferrite subunits obtained by different bainitic heat treatments was determined in two steels, with carbon contents of 0.3 and 0.7 wt.%, from SEM and TEM micrographs. As these measurements were made on 2D images taken from random sections, the method includes some stereological correction factors to obtain accurate information. Finally, the determined thicknesses of bainitic ferrite plates were compared with the crystallite size calculated from the analysis of X-ray diffraction peak broadening. Although in some case the values obtained for crystallite size and plate thickness can be similar, this study confirms that indeed they are two different parameters. - Highlights: •Bainitic microstructure in a nanostructured and sub-micron steel •Bainitic ferrite plate thickness measured by SEM and TEM •Crystallite size determined by X-ray analysis

  2. Analyzing the scale of the bainitic ferrite plates by XRD, SEM and TEM

    Energy Technology Data Exchange (ETDEWEB)

    Garcia-Mateo, Carlos, E-mail: cgm@cenim.csic.es [Department of Physical Metallurgy, Spanish National Center for Metallurgical Research (CENIM-CSIC), Avda. Gregorio del Amo 8, E-28040 Madrid (Spain); Jimenez, Jose A.; Lopez-Ezquerra, Belen; Rementeria, Rosalia; Morales-Rivas, Lucia [Department of Physical Metallurgy, Spanish National Center for Metallurgical Research (CENIM-CSIC), Avda. Gregorio del Amo 8, E-28040 Madrid (Spain); Kuntz, Matthias [Robert-Bosch GmbH, Materials and Process Engineering Metals, Renningen, 70465 Stuttgart (Germany); Caballero, Francisca G. [Department of Physical Metallurgy, Spanish National Center for Metallurgical Research (CENIM-CSIC), Avda. Gregorio del Amo 8, E-28040 Madrid (Spain)

    2016-12-15

    Since the major strengthening mechanisms in nanocrystalline bainitic steels arise from the exceptionally small size of the bainitc ferrite plate, accurate determination of this parameter is fundamental for quantitative relating the microstructure to the mechanical properties. In this work, the thickness of the bainitic ferrite subunits obtained by different bainitic heat treatments was determined in two steels, with carbon contents of 0.3 and 0.7 wt.%, from SEM and TEM micrographs. As these measurements were made on 2D images taken from random sections, the method includes some stereological correction factors to obtain accurate information. Finally, the determined thicknesses of bainitic ferrite plates were compared with the crystallite size calculated from the analysis of X-ray diffraction peak broadening. Although in some case the values obtained for crystallite size and plate thickness can be similar, this study confirms that indeed they are two different parameters. - Highlights: •Bainitic microstructure in a nanostructured and sub-micron steel •Bainitic ferrite plate thickness measured by SEM and TEM •Crystallite size determined by X-ray analysis.

  3. Synthesis of Co/MCM-41catalysts and characterization by XRD, EDX, DTA/TG, SEM and TEM

    International Nuclear Information System (INIS)

    Sousa, B.V.; Rodrigues, M.G.F.

    2009-01-01

    Full text: In this work, molecular sieve MCM-41 was prepared as well as the Co/MCM-41 catalyst, via humid impregnation with concentration of 5 wt.% and 10 wt.% Co/MCM- 41. The attainment of the mesoporous molecular sieve, Si-MCM-41, was confirmed by the x-ray diffractogram. It was verified that after the calcination all the bromine (Br) was removed indicating that the calcination process removed all surfactant in the mesoporous structure. XRD and EDX analyses indicated that cobalt was found in the form of Co3O2 in the Co/MCM-41 catalysts. The diffraction standards showed that the impregnation and calcination processes caused changes in the structure only for catalyst with 10 wt.% Co/MCM-41. The DTA/TG curves showed that cobalt nitrate was totally decomposed on the MCM-41. From the images of SEM, it was possible to observe that the Co/MCM-41 catalysts were composed by clusters of small crystals. The images obtained from TEM showed clearly the presence of metal cobalt particles in a well dispersed form for catalyst with 5 wt.% Co/MCM41, except for the catalyst with 10 wt.% Co/MCM41. (author)

  4. Determination of Size Distributions in Nanocrystalline Powders by TEM, XRD and SAXS

    DEFF Research Database (Denmark)

    Jensen, Henrik; Pedersen, Jørgen Houe; Jørgensen, Jens Erik

    2006-01-01

    Crystallite size distributions and particle size distributions were determined by TEM, XRD, and SAXS for three commercially available TiO2 samples and one homemade. The theoretical Guinier Model was fitted to the experimental data and compared to analytical expressions. Modeling of the XRD spectra...... the size distribution obtained from the XRD experiments; however, a good agreement was obtained between the two techniques. Electron microscopy, SEM and TEM, confirmed the primary particle sizes, the size distributions, and the shapes obtained by XRD and SAXS. The SSEC78 powder and the commercially...

  5. XRD and SEM study of alumina silicate porcelain insulator

    Science.gov (United States)

    Duddi, Dharmender; Singh, G. P.; Kalra, Swati; Shekhawat, M. S.; Tak, S. K.

    2018-05-01

    Higher strength electrical porcelain is a requirement of industry. This will be achieved by a specific composition of raw materials, which is consisted of clays and feldspars. Water absorption, particle size and insulating properties are of special interest now a day. China clay, Ball clay and Quartz are widely used by ceramic industries in Bikaner district of Rajasthan. Sample for present study were prepared by mixing of above clay, feldspar with MnO2, then shrinkage is observed. Bar shaped samples were prepared and heated up to a temperature of about 1185° C to observe shrinkage. For phase study of XRD and SEM are observed.

  6. The principle of electron microscopy; SEM and TEM

    International Nuclear Information System (INIS)

    Fauzi, S.H.

    1992-01-01

    The article reviews the principle of electron microscopy which is used in scanning electron microscope (SEM) and transmission electron microscope (TEM). These instruments are important for the examination and analysis of the microstructural properties of solid objects. Relevance physical concept lies behind the devices are given. The main components of each device are also discussed

  7. Characterization of some biological specimens using TEM and SEM

    Science.gov (United States)

    Ghosh, Nabarun; Smith, Don W.

    2009-05-01

    The advent of novel techniques using the Transmission and Scanning Electron Microscopes improved observation on various biological specimens to characterize them. We studied some biological specimens using Transmission and Scanning Electron Microscopes. We followed negative staining technique with Phosphotungstic acid using bacterial culture of Bacillus subtilis. Negative staining is very convenient technique to view the structural morphology of different samples including bacteria, phage viruses and filaments in a cell. We could observe the bacterial cell wall and flagellum very well when trapped the negative stained biofilm from bacterial culture on a TEM grid. We cut ultra thin sections from the fixed root tips of Pisum sativum (Garden pea). Root tips were pre fixed with osmium tetroxide and post fixed with uranium acetate and placed in the BEEM capsule for block making. The ultrathin sections on the grid under TEM showed the granular chromatin in the nucleus. The protein bodies and large vacuoles with the storage materials were conspicuous. We followed fixation, critical point drying and sputter coating with gold to view the tissues with SEM after placing on stubs. SEM view of the leaf surface of a dangerous weed Tragia hispida showed the surface trichomes. These trichomes when break on touching releases poisonous content causing skin irritation. The cultured tissue from in vitro culture of Albizia lebbeck, a tree revealed the regenerative structures including leaf buds and stomata on the tissue surface. SEM and TEM allow investigating the minute details characteristic morphological features that can be used for classroom teaching.

  8. Infrared spectra, Raman laser, XRD, DSC/TGA and SEM ...

    Indian Academy of Sciences (India)

    Administrator

    cussed and the X-ray diffraction, scanning electron microscopy (SEM) and atomic force microscope (AFM) ... acetamide as a simple organic compound at high tempera- ture has less ..... properties of selenium surface, AFM-microscopy tapping.

  9. XRD and TEM analysis of microstructure in the welding zone of 9Cr ...

    Indian Academy of Sciences (India)

    Unknown

    XRD and TEM analysis of microstructure in the welding zone of. 9Cr–1Mo–V–Nb ... steel, which has highest Cr content in the heat-resisting. Cr–Mo ... This research provides essential ... film samples were observed under TEM and select elec-.

  10. Determination of grain size by XRD profile analysis and TEM counting in nano-structured Cu

    International Nuclear Information System (INIS)

    Zhong Yong; Ping Dehai; Song Xiaoyan; Yin Fuxing

    2009-01-01

    In this work, a serial of pure copper sample with different grain sizes from nano- to micro-scale were prepared by sparkle plasma sintering (SPS) and following anneal treatment at 873 K and 1073 K, respectively. The grain size distributions of these samples were determined by both X-ray diffraction (XRD) profile analysis and transmission electronic microscope (TEM) micrograph counting. Although these two methods give similar distributions of grain size in the case of as-SPS sample with nano-scale grain size (around 10 nm), there are apparent discrepancies between the grain size distributions of the annealed samples obtained from XRD and TEM, especially for the sample annealed at 1073 K after SPS with micro-scale grain size (around 2 μm), which TEM counting provides much higher values of grain sizes than XRD analysis does. It indicates that for large grain-sized material, XRD analysis lost its validity for determination of grain size. It might be due to some small sized substructures possibly existed in even annealed (large grain-sized) samples, whereas there is no substructures in as-SPS (nanocrystalline) sample. Moreover, it has been found that the effective outer cut-off radius R e derived from XRD analysis coincides with the grain sizes given by TEM counting. The potential relationship between grain size and R e was discussed in the present work. These results might provide some new hints for deeper understanding of the physical meaning of XRD analysis and the parameters derived.

  11. Characterization of crystallite morphology for doped strontium fluoride nanophosphors by TEM and XRD

    Energy Technology Data Exchange (ETDEWEB)

    O' Connell, J.H. [Centre for HRTEM, Nelson Mandela Metropolitan University, PO Box 77000, Port Elizabeth ZA6031 (South Africa); Lee, M.E., E-mail: Michael.lee@nmmu.ac.za [Centre for HRTEM, Nelson Mandela Metropolitan University, PO Box 77000, Port Elizabeth ZA6031 (South Africa); Yagoub, M.Y.A.; Swart, H.C.; Coetsee, E. [Department of Physics, University of the Free State, PO Box 339, Bloemfontein ZA9300 (South Africa)

    2016-01-01

    Crystallite morphology for Eu-doped and undoped SrF{sub 2} nanophosphors have been determined by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The values for average crystallite size obtained by the application of the Scherrer equation and the full width at half maximum (FWHM) values for XRD peaks are compared to the results obtained using the hollow cone dark field (HCDF) TEM imaging technique. In the case of the TEM analysis, a bimodal crystallite size distribution was revealed with one of the distributions having a measured range of crystallite sizes which was in good agreement with the XRD data. HCDF in combination with FIB specimen preparation was found to be a promising technique for the determination of crystallite size distributions in nanophosphors which might facilitate a better understanding of their scintillation properties.

  12. Characterization of crystallite morphology for doped strontium fluoride nanophosphors by TEM and XRD

    International Nuclear Information System (INIS)

    O'Connell, J.H.; Lee, M.E.; Yagoub, M.Y.A.; Swart, H.C.; Coetsee, E.

    2016-01-01

    Crystallite morphology for Eu-doped and undoped SrF_2 nanophosphors have been determined by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The values for average crystallite size obtained by the application of the Scherrer equation and the full width at half maximum (FWHM) values for XRD peaks are compared to the results obtained using the hollow cone dark field (HCDF) TEM imaging technique. In the case of the TEM analysis, a bimodal crystallite size distribution was revealed with one of the distributions having a measured range of crystallite sizes which was in good agreement with the XRD data. HCDF in combination with FIB specimen preparation was found to be a promising technique for the determination of crystallite size distributions in nanophosphors which might facilitate a better understanding of their scintillation properties.

  13. stainless steel by SEM-XRD and image analysis

    Directory of Open Access Journals (Sweden)

    Robinson Constanzo-R.

    2014-01-01

    Full Text Available El objetivo de este trabajo fue realizar un análisis cualitativ o de la distribución de un electrodepósito de cobre en el inter ior de electrodos porosos (EP de acero inoxidable y carbono grafito. Para ello, se reali zaron pruebas de electrodepositación de cobre a nivel de labora torio, con un posterior análisis de cortes de muestras de acero y grafito vía Microscopía Estereoscópica, Microscopía SEM-DRX y Análisis de Imagen, los cuales mostraron que el cobre no se deposita en forma uniforme al interior del electrodo. En el electrodo de acero, la penetra ción del depósito en el espesor fue alrededor de 50%, mientras que para el grafito a lrededor de 90%. En forma general, se observó un aumento de la cantidad de depósito hacia el extremo frente al ánodo y con sitios de difer ente crecimiento en depósito de cobre. Esto demuestra una distr ibución de corriente y potencial, función de parámetros físicos de electrodo y de la s características fisicoquímicas e hidrodinámicos del electroli to.

  14. Morphologic characterization for XRD and TEM of polyamide 6 and 66 nanocomposites with bentonite regional clay

    International Nuclear Information System (INIS)

    Leite, Amanda M.D.; Medeiros, Vanessa da N.; Maia, Larissa F.; Araujo, Edcleide M.; Lira, Helio L.

    2009-01-01

    Polyamide 6 and 66 nanocomposites with clay consisting of silicates layer from Paraiba were produced. The clay was modified being used the quaternary salt of ammonium Cetremide, this so there is a better interaction of the clay with polymeric matrix. The clay without treatment (MMT) and treated clay was evaluated by XRD that showed the insertion of the salt molecules into silicates layer. The nanocomposites were obtained from polyamide 6 and 66 were verified that these presented morphological structure composed of exfoliated/partially exfoliated, analyzed by XRD and TEM. (author)

  15. Graphene oxide and reduced graphene oxide studied by the XRD, TEM and electron spectroscopy methods

    International Nuclear Information System (INIS)

    Stobinski, L.; Lesiak, B.; Malolepszy, A.; Mazurkiewicz, M.; Mierzwa, B.; Zemek, J.; Jiricek, P.; Bieloshapka, I.

    2014-01-01

    Highlights: • Graphene oxide (FL-GOc) and reduced graphene oxide (FL-RGOc): XRD, TEM, XPS, REELS. • FL-GOc: stacking nanostructure—22 × 6 nm (DxH), 0.9 nm layers separation (XRD). • FL-RGOc: stacking nanostructure—8 × 1 nm (DxH), 0.4 nm layers separation (XRD). • Reduction: oxygen group degradation, decreasing distance between graphene layers. • Number of graphene layers in stacking nanostructure: 6–7 (FL-GOc), 2–3 (FL-RGOc). - Abstract: The commercial and synthesised few-layer graphene oxide, prepared using oxidation reactions, and few-layer reduced graphene oxide samples were structurally and chemically investigated by the X-ray diffraction (XRD), transmission electron microscopy (TEM) and electron spectroscopy methods, i.e. X-ray photoelectron spectroscopy (XPS) and reflection electron energy loss spectroscopy (REELS). The commercial graphene oxide (FL-GOc) shows a stacking nanostructure of about 22 × 6 nm average diameter by height with the distance of 0.9 nm between 6-7 graphene layers, whereas the respective reduced graphene oxide (FL-RGOc)—about 8 × 1 nm average diameter by height stacking nanostructure with the distance of 0.4 nm between 2-3 graphene layers (XRD). The REELS results are consistent with those by the XRD indicating 8 (FL-GOc) and 4 layers (FL-RGOc). In graphene oxide and reduced graphene oxide prepared from the graphite the REELS indicates 8–11 and 7–10 layers. All graphene oxide samples show the C/O ratio of 2.1–2.3, 26.5–32.1 at% of C sp 3 bonds and high content of functional oxygen groups (hydroxyl—C-OH, epoxy—C-O-C, carbonyl—C=O, carboxyl—C-OOH, water) (XPS). Reduction increases the C/O ratio to 2.8–10.3, decreases C sp 3 content to 11.4–20.3 at% and also the content of C-O-C and C=O groups, accompanied by increasing content of C-OH and C-OOH groups. Formation of additional amount of water due to functional oxygen group reduction leads to layer delamination. Removing of functional oxygen groups

  16. XRD, TEM, and thermal analysis of Arizona Ca-montmorillonites modified with didodecyldimethylammonium bromide.

    Science.gov (United States)

    Sun, Zhiming; Park, Yuri; Zheng, Shuilin; Ayoko, Godwin A; Frost, Ray L

    2013-10-15

    An Arizona SAz-2 calcium montmorillonite was modified by a typical dialkyl cationic surfactant (didodecyldimethylammonium bromide, abbreviated to DDDMA) through direct ion exchange. The obtained organoclays were characterized by X-ray diffraction (XRD), high-resolution transmission electron microscopy (HR-TEM), high-resolution thermogravimetric analysis (HR-TG), and infrared emission spectroscopy (IES). The intercalation of surfactants greatly increased the basal spacing of the interlayers and the conformation arrangement of the loaded surfactant were assessed based on the XRD and TEM measurements. This work shows that the dialkyl surfactant can be directly intercalated into the montmorillonite without first undergoing Na(+) exchange. Moreover, the thermal stability of organoclays and the different arrangements of the surfactant molecules intercalated in the SAz-2 Ca-montmorillonite were determined by a combination of TG and IES techniques. The detailed conformational ordering of different intercalated surfactants under different conditions was also studied. The surfactant molecule DDDMA has proved to be thermally stable even at 400°C which indicates that the prepared organoclay is stable to significantly high temperatures. This study offers new insights into the structure and thermal stabilities of SAz-2 Ca-montmorillonite modified with DDDMA. The experimental results also confirm the potential applications of organic SAz-2 Ca-montmorillonites as adsorbents and polymer-clay nanocomposites. Copyright © 2013 Elsevier Inc. All rights reserved.

  17. Synthesis, XRD, TEM, EPR, and Optical Absorption Spectral Studies of CuZnO2 Nanocompound

    Directory of Open Access Journals (Sweden)

    T. Ravindra Reddy

    2014-01-01

    Full Text Available Synthesis of nano CuZnO2 compound is carried out by thermal decomposition method. The crystalline phase of the material is characterized by XRD. The calculated unit cell constants are a=3.1 Å and c=3.4786 Å and are of tetragonal structure. The unit cell constants are different from wurtzite (hexagonal which indicate that a nanocompound is formed. Further TEM images reveal that the metal ion is in tetragonal structure with oxygen ligands. The prepared CuZnO2 is then characterized for crystallite size analysis by employing transmission electron microscopy (TEM. The size is found to be 100 nm. Uniform bright rings are noticed in the TEM picture suggesting that the nanocrystals have preferential instead of random orientations. The selected-area electron diffraction (SAED pattern clearly indicates the formation of CuO-ZnO nanocompound. The nature of bonding is studied by electron paramagnetic resonance (EPR. The covalency character is about 0.74 and thus the compound is electrically less conductive. Optical absorption spectral studies suggest that Cu(II is placed in tetragonal elongation crystal field. The spin-orbit coupling constant, λ, is calculated using the EPR and optical absorption spectral results suggest some covalent bond between metal and ligand. Near infrared (NIR spectra are due to hydroxyl and water fundamentals.

  18. Microstructural Characterization of Water-Rich Boehmite (AlO(OH)): TEM Correlation of Apparently Divergent XRD and TGA Results

    International Nuclear Information System (INIS)

    Allard, L.F.; Anovitz, L.M.; Benezeth, P.; Coffey, D.W.; Palmer, D.A.; Porter, W.D.; Wesolowski, D.J.

    1999-01-01

    An understanding of the solid-phase thermodynamics and aqueous speciation of aluminum is critical to our ability to understand and predict processes in a wide variety of geologic and industrial settings. Boehmite (AIO(OH)) is an important phase in the system Al 2 O 3 -H 2 O that has been the subject of a number of structural and thermodynamic studies since its initial synthesis [l] and discovery in nature [2]. Unfortunately, it has long been recognized that thermogravimetric analysis (TGA) of both synthetic and natural boehmite samples (that appear well crystallized by powder XRD methods) yields significant excess water - typically losing 16-16.5 wt. % on heating as compared with a nominal expected weight loss of 15.0 wt. % [3,4]. The boehmite used in our experiments was synthesized hydrothermally from acid-washed gibbsite (Al(OH) 3 ) at 200C. Powder XRD and SEM examination showed no evidence of the presence a contaminant phase. The TGA patterns do not suggest that this is due to adsorbed water, so a structural source is likely. We therefore undertook to examine this material by TEM to clarify this phenomenon

  19. Characterising palladium-silver and palladium-nickel alloy membranes using SEM, XRD and PIXE

    International Nuclear Information System (INIS)

    Keuler, J.N.; Lorenzen, L.; Sanderson, R.D.; Prozesky, V.; Przybylowicz, W.J.

    1999-01-01

    Palladium alloy membranes were prepared by successive electroless plating steps on an alumina-zirconia support membrane. Palladium, silver and nickel were deposited in layers and then the metal films were heat treated for 5 h in a hydrogen atmosphere at 650 deg. C. The topography of the metal coatings and cross-sections of the films (before and after heating) were characterised using scanning electron microscopy (SEM). XRD was used to determine the crystal phase of the alloy coatings. Both SEM and XRD provide only surface information and therefore micro-PIXE was used to extract depth information of the alloy coating. Concentration profiles across the thickness of the films were constructed to determine penetration of the coating into the support membrane pores during electroless plating and to investigate diffusion of coated layers during the heating step

  20. XRD and SEM analysis of hydroxyapatite during immersion in stimulated physiological solutions

    International Nuclear Information System (INIS)

    Yusof Abdullah; Idris Besar; Rosmamuhamadani Ramli; Abd Razak Daud

    2000-01-01

    XRD and SEM techniques were used to analyse the apatite layer developed on the synthetic hydroxyapatite surface following immersion in the simulated body fluid (SBF) that mimics the conditions of material experiences after implantation in the human body. Initially, the new layers formed after 7 day's incubation and increased with immersion time as crystallization of apatite phase. The XRD confirmed that the deposited layer was hydroxyapatite and crystallographically. With time, the crystal growth become more random and the intensity of the peaks decreased. During immersion, hydroxyapatite was precipitated from the SBF and coherently scattered with very small crystal. The SEM observation shows that the new precipitates were increased as well as incubation period increased. Therefore, hydroxyapatite ceramics are suggested to have very good biocompatibility. (Author)

  1. MORPHOLOGICAL ASPECTS OF HUMAN LENS CAPSULES - A COMPARATIVE LM, SEM AND TEM EXAMINATION

    NARCIS (Netherlands)

    JONGEBLOED, WL; KALICHARAN, D; LOS, LI; VANDERVEEN, G; WORST, JGF

    1991-01-01

    Lens capsules of patients of advanced age, obtained after extracapsular cataract surgery, were carefully prepared for a combined LM, TEM and SEM investigation, after preliminary washing and mounting onto a holder in a buffer solution. After pre-fixation with GA, samples were postfixed for LM/TEM and

  2. HUMAN CAPSULE EPITHELIAL-CELL DEGENERATION A LM, SEM AND TEM INVESTIGATION

    NARCIS (Netherlands)

    JONGEBLOED, WL; KALICHARAN, D; WORST, JGF

    1993-01-01

    The degeneration of the capsule epithelium of cataractous lenses has been studied with LM, SEM on TEM with emphases on TEM. The observed degeneration of the epithelial cells can be described as follows: The cell nucleus becomes picnotic and desintegrates as result of change of the chromatin.

  3. XRD, SEM and infrared study into the intercalation of sodium hexadecyl sulfate (SHS) into hydrocalumite.

    Science.gov (United States)

    Zhang, Ping; Wang, Tianqi; Zhang, Longlong; Wu, Daishe; Frost, Ray L

    2015-12-05

    Hydrocalumite (CaAl-LDH-Cl) interacted with a natural anionic surfactant, sodium hexadecyl sulfate (SHS), was performed using an intercalation method. To understand the intercalation behavior and characterize the resulting products, powder X-ray diffraction (XRD), scan electron microscopy (SEM) and mid-infrared (MIR) spectroscopy combined with near-infrared (NIR) spectroscopy technique were used. The XRD analysis indicated that SHS was intercalated into CaAl-LDH-Cl successfully, resulting in an expansion of the interlayer (from 0.78 nm to 2.74 nm). The bands of C-H stretching vibrations of SHS were observed in the near-infrared spectra, which indicated that the resulting products were indeed CaAl-LDH-SHS. In addition, the bands of water stretching vibrations and OH groups shifted to higher wavenumbers when SHS was intercalated into CaAl-LDH-Cl interlayer space. Copyright © 2015 Elsevier B.V. All rights reserved.

  4. XRD, TEM, IR, Raman and NMR Spectroscopy of In Situ Crystallization of Lithium Disilicate Glass

    Science.gov (United States)

    Fuss, T.; Mogus-Milankovic, A.; Ray, C. S.; Lesher, C. E.; Youngman, R.; Day, D. E.

    2006-01-01

    The structure of a Li2O-2SiO2 (LS2) glass was investigated as a function of pressure and temperature up to 6 GPa and 750 C respectively, using XRD, TEM, IR, Raman and NMR spectroscopy. Glass densified at 6 GPa has an average Si-O-Si bond angle approx.7deg lower than that found in glass processed at 4.5 GPa. At 4.5 GPa, lithium disilicate crystallizes from the glass, while at 6 GPa a new high pressure form of lithium metasilicate crystallizes. The new phase, while having lithium metasilicate crystal symmetry, contains at least 4 different Si sites. NMR results for 6 GPa sample indicate the presence of Q4 species with (Q(sup 4))Si-O-Si(Q(sup 4)) bond angles of approx.157deg. This is the first reported occurrence of Q(sup 4) species with such large bond angles in alumina free alkali silicate glass. No five- or six- coordinated Si are found.

  5. Structure and surface morphology studies of cerium oxide system using XRD and SEM analysis

    International Nuclear Information System (INIS)

    Ahmad Jais Alimin; Farid Nasir Ani; Wan Azelee Wan Abu Bakar

    2000-01-01

    Conventional Precious Group Materials (PGM) catalyst systems have been using CeO 2 as an Oxygen Storage Capacity component in the catalyst washcoat. Due to the limitations of the PGM catalyst, researches are now focusing on improving or replacing this conventional system. In a previous work, the potential of a copper-ceria (Cu-Ce) oxide as a catalyst system has been identified. In this paper, the morphology and characterisation of Cu-Ce oxides analysed using XRD and SEM will be described. The Cu-Ce samples were prepared at a fixed ratio under temperatures of 400 o C and 800 o C. XRD diffractograms showed CeO 2 is in a cubic phase at 400 o C and 800 o C. At 800 o C, the CuO particle is visible, presumably has incorporated with the lattice structure of ceria, indicating an absent of solid state condition between copper and ceria. Analysis by SEM revealed significant increase in particle sizes with increasing calcination temperatures. (Author)

  6. Morphological, chemical and structural characterisation of deciduous enamel: SEM, EDS, XRD, FTIR and XPS analysis.

    Science.gov (United States)

    Zamudio-Ortega, C M; Contreras-Bulnes, R; Scougall-Vilchis, R J; Morales-Luckie, R A; Olea-Mejía, O F; Rodríguez-Vilchis, L E

    2014-09-01

    The purpose of this study was to characterise the enamel surface of sound deciduous teeth in terms of morphology, chemical composition, structure and crystalline phases. The enamel of 30 human deciduous teeth was examined by: Scanning Electron Microscopy (SEM), Energy Dispersive X-Ray Spectroscopy (EDS), X-ray Powder Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), and X-ray Photoelectron Spectroscopy (XPS). Chemical differences between incisors and canines were statistically evaluated using the Mann-Whitney U test (p ≤ 0.05). Three enamel patterns were observed by SEM: 'mostly smooth with some groves', 'abundant microporosities' and 'exposed prisms'. The average Ca/P molar ratios were 1.37 and 1.03 by EDS and XPS, respectively. The crystallite size determined by XRD was 210.82 ± 16.78 Å. The mean ratio between Ca bonded to phosphate and Ca bonded to hydroxyl was approximately 10:1. The enamel of sound deciduous teeth showed two main patterns: 'mostly smooth with some groves' and 'abundant microporosities'. 'Exposed prisms' was a secondary pattern. There were slight variations among the Ca/P molar ratios found by EDS and XPS, suggesting differences in the mineral content from the enamel surface to the interior. The crystalline phases found in enamel were hydroxyapatite and carbonate apatite, with major type B than type A carbonate incorporation.

  7. Swelling induced by alpha decay in monazite and zirconolite ceramics: A XRD and TEM comparative study

    Science.gov (United States)

    Deschanels, X.; Seydoux-Guillaume, A. M.; Magnin, V.; Mesbah, A.; Tribet, M.; Moloney, M. P.; Serruys, Y.; Peuget, S.

    2014-05-01

    Zirconolite and monazite matrices are potential ceramics for the containment of actinides (Np, Cm, Am, Pu) which are produced over the reprocessing of spent nuclear fuel. Actinides decay mainly through the emission of alpha particles, which in turn causes most ceramics to undergo structural and textural changes (amorphization and/or swelling). In order to study the effects of alpha decays on the above mentioned ceramics two parallel approaches were set up. The first involved the use of an external irradiation source, Au, which allowed the deposited recoil energy to be simulated. The second was based on short-lived actinide doping with 238Pu, (i.e. an internal source), via the incorporation of plutonium oxide into both the monazite and zirconolite structures during synthesis. In both types of irradiation experiments, the zirconolite samples became amorphous at room temperature with damage close to 0.3 dpa; corresponding to a critical dose of 4 × 1018 α g-1 (i.e. ∼1.3 × 1021 keV cm-3). Both zirconolite samples also showed the same degree of macroscopic swelling at saturation (∼6%), with ballistic processes being the predominant damaging effect. In the case of the monazite however, the macroscopic swelling and amorphization were dependent on the nature of the irradiation. Externally, (Au), irradiated samples became amorphous while also demonstrating a saturation swelling of up to 8%. In contrast to this, the swelling of the 238Pu doped samples was much smaller at ∼1%. Also, unlike the externally (Au) irradiated monazite these 238Pu doped samples remained crystalline up to 7.5 × 1018 α g-1 (0.8 dpa). XRD, TEM and swelling measurements were used to fully characterize and interpret this behavior. The low swelling and the conservation of the crystalline state of 238Pu doped monazite samples indicates that alpha annealing took place within this material.

  8. Speciation of uranium in minerals by Sem, Tem, μ-PIXE, XPS and XAFS

    International Nuclear Information System (INIS)

    Toshihiko Ohnuki; Hiroshi Isobe; Tomihiro Kamiya; Takuro Sakai; Takashi Murakami

    2001-01-01

    Many kinds of electromagnetic waves and particle beams are used as analytical probes for the investigation of uranium-mineralogy and speciation. The representatives of the probes are SEM, TEM, μ-PIRE, XPS and XAFS. Each of these analytical probes has its own advantages and disadvantages. We have performed studies to compare the advantages and disadvantages on the basis of the analysis of the distribution and speciation of U containing rock samples collected at the Koongarra uranium deposit, Australia. The spatial resolutions of the probes are in the order of TEM>SEM, μ-PIXE>XFAS, XPS. The lower detection limits of the probes are in the order of μ-PIXE< TEM, SEM< XFAS, XPS. Oxidation state of U was determined by XFAS and XPS. These results indicate that combination of the above probes can give us sufficient data on U speciation not only in natural rock samples but in solid samples obtained in the laboratory. (authors)

  9. XRD and SEM study on the phase separation and crystallization behavior for an amorphous Cu+ conductor

    International Nuclear Information System (INIS)

    Yang Yuan; Hou Jianguo; Yu Wenhai

    1990-01-01

    The X-ray diffraction (XRD) and scanning electron microscopy (SEM) study was carried out for an amorphous Cu + conductor 0.4 CuI-0.3 Cu 2 O-0.3 P 2 O 5 with the simultaneous conductivity measurement in the isothermal heat treament process. The results indicated that the initial amorphous material was phase-separated. In the course of time the separated amorphous phase disappeared, the crystalline γ-CuI and Cu 2 P 2 O 7 formed in sequence and grew up gradually. The correlation of the phase separation and crystallization behavior with the conductivity anomaly confirmed again the interface effect between different phases in amorphous fast ionic conductors and its universality

  10. MICROORGANISMS FOUND IN SECONDARY CATARACT MATERIAL OF ECCE PATIENTS, A STUDY WITH SEM AND TEM

    NARCIS (Netherlands)

    KALICHARAN, D; JONGEBLOED, WL; LOS, LI; WORST, JGF

    1993-01-01

    Globular secondary cataract material, removed from 24 patients with ECCE after ophthalmic cleaning of the anterior capsule, were investigated with SEM and TEM. Besides spherical, somewhat oval shaped bodies of various shape and size comparable with those found in cataractous lenses, (an)aerobic

  11. Automated SEM and TEM sample preparation applied to copper/low k materials

    Science.gov (United States)

    Reyes, R.; Shaapur, F.; Griffiths, D.; Diebold, A. C.; Foran, B.; Raz, E.

    2001-01-01

    We describe the use of automated microcleaving for preparation of both SEM and TEM samples as done by SELA's new MC500 and TEMstation tools. The MC500 is an automated microcleaving tool that is capable of producing cleaves with 0.25 μm accuracy resulting in SEM-ready samples. The TEMstation is capable of taking a sample output from the MC500 (or from SELA's earlier MC200 tool) and producing a FIB ready slice of 25±5 μm, mounted on a TEM-washer and ready for FIB thinning to electron transparency for TEM analysis. The materials selected for the tool set evaluation mainly included the Cu/TaN/HOSP low-k system. The paper is divided into three sections, experimental approach, SEM preparation and analysis of HOSP low-k, and TEM preparation and analysis of Cu/TaN/HOSP low-k samples. For the samples discussed, data is presented to show the quality of preparation provided by these new automated tools.

  12. Application of SEM/EBSD and FEG-TEM/CBED to determine eutectic solidification mechanisms

    International Nuclear Information System (INIS)

    Nogita, K.; Dahle, A.K.; Drennan, J.

    2002-01-01

    Full text: This study shows the application of electron backscatter diffraction (EBSD) in SEM and convergent beam electron diffraction (CBED) in FEG-TEM to determine eutectic nucleation and growth in hypoeutectic Al-Si foundry alloys. Because the eutectic reaction is often the final stage of solidification it can be expected to have a significant impact on the formation of casting defects, particularly porosity. Previous EBSD work by Nogita and Dahle (2001), Dahle et al (2001), has shown that the eutectic nucleates on the primary phase in the unmodified alloy, and eutectic grains are nucleated in the intergranular liquid, instead of filling the dendrite envelopes, when Sr or Sb is added. However, the orientation relationship between silicon and aluminium in the eutectic has so far not been determined because of difficulties with sample preparation for EBSD and also detection limitations of Kikuchi refraction of silicon and aluminium, particularly in modified alloys with a refined eutectic. The combination of the EBSD technique in SEM and CBED in TEM analyses can provide crystallographic orientation relationships between primary aluminium dendrites, eutectic aluminium and silicon, which are important to explicitly define the solidification mode of the eutectic in hypoeutectic Al-Si alloys. These relationships are influenced, and altered, by the addition of certain elements. This paper also describes the sample preparation techniques for SEM and TEM for samples with different eutectic structures. The advantages the techniques are discussed. Copyright (2002) Australian Society for Electron Microscopy Inc

  13. Nickel oxide reduction studied by environmental TEM and in situ XRD

    DEFF Research Database (Denmark)

    Jeangros, Q.; Hansen, Thomas Willum; Wagner, Jakob Birkedal

    2012-01-01

    Paar furnace and a mass spectrometer to complement and extrapolate the ETEM data to higher pressures and gas flows. Diffraction peak intensities, crystallite sizes (obtained using the Scherrer formula) and H2/H2O mass spectrometer signals are monitored. The recorded images and diffraction patterns show...... that the presence and stagnation of H2O vapour created upon reduction blocks H2 access to the reactive sites, decreasing the reaction rate at a high conversion fraction. The gas flow is low and may not evacuate the product gas efficiently around the Ni(O) particles. Complementary XRD experiments point towards...... the same conclusion and underline the impact of the pressure and gas flow on the kinetics. It is possible to determine an approximate activation energy for NiO reduction inside the ETEM using the Kissinger method [8], which is based on measurements of the shift in the temperature at which the reaction rate...

  14. Polycrystalline oxides formation during transient oxidation of (001) Cu-Ni binary alloys studied by in situ TEM and XRD

    International Nuclear Information System (INIS)

    Yang, J.C.; Li, Z.Q.; Sun, L.; Zhou, G.W.; Eastman, J.A.; Fong, D.D.; Fuoss, P.H.; Baldo, P.M.; Rehn, L.E.; Thompson, L.J.

    2009-01-01

    The nucleation and growth of Cu 2 O and NiO islands due to oxidation of Cu x Ni 1-x (001) films were monitored, at various temperatures, by in situ ultra-high vacuum (UHV) transmission electron microscopy (TEM) and in situ synchrotron X-ray diffraction (XRD). In remarkable contrast to our previous observations of Cu and Cu-Au oxidation, irregular-shaped polycrystalline oxide islands formed with respect to the Cu-Ni alloy film, and an unusual second oxide nucleation stage was noted. In situ XRD experiments revealed that NiO formed first epitaxially, then other orientations appeared, and finally polycrystalline Cu 2 O developed as the oxidation pressure was increased. The segregation of Ni and Cu towards or away, respectively, from the alloy surface during oxidation could disrupt the surface and cause polycrystalline oxide formation.

  15. Characterization of ash pond ashes from 3rd thermal power plant by SEM/EDX and XRD methods

    OpenAIRE

    A Minjigmaa; Ts Zolzaya; E Bayanjargal; B Davaabal; J Temuujin

    2014-01-01

      Coal combustion by products from ash pond of 3rdthermal power plant of Ulaanbaatar city have been collected in 2010 and 2013 years. The ash samples have been characterized by XRD, XRF and SEM-EDX methods in order to evaluate their chemical and mineralogical composition changes with disposed times. The mineralogical composition of ash varies with time though the chemical composition of the ashes were close each other. Possibly, inefficient operating condition of the TPS shows influence on th...

  16. Moessbauer, TEM/SAED and XRD investigation on waste dumps of the Valea lui Stan gold mines

    Energy Technology Data Exchange (ETDEWEB)

    Constantinescu, Serban Grigore, E-mail: sconst@infim.ro [National Institute of Materials Physics, Bucharest-Magurele (Romania); Udubasa, Sorin S.; Udubasa, Gheorghe [University of Bucharest, Fac. of Geology and Geophysics (Romania); Kuncser, Victor; Popescu-Pogrion, Nicoleta; Mercioniu, Ionel; Feder, Marcel [National Institute of Materials Physics, Bucharest-Magurele (Romania)

    2012-03-15

    The complementary investigation techniques, Moessbauer spectroscopy, transmission electron microscopy with selected area electron diffraction (TEM/SAED), X-ray diffraction (XRD) have been used to investigate the fate of the Valea lui Stan, Romania, gold-ore nanoscale-minerals during the long time of residence in the waste dumps. The preliminary investigations showed such waste dumps to contain significant amount of metals which cannot be identified by conventional methods. An intense research activity started up in order to evaluate the possibilities to recycle Valea lui Stan waste dumps and to recover metals by chemical or phytoextraction procedures. The waste dumps naturally show different mineral constituents with clay minerals as major phases, observed by XRD-technique. Although the waste dumps materials have whitish-yellowish colours, MOeSSBAUER technique evidences the presence of the finely dispersed iron bearing minerals. The authors are focusing to inspect and analyze Fe-compounds in the samples collected from Valea lui Stan's waste dumps in order to identify the magnetic phases by Moessbauer technique.

  17. Characterization of mineral particles in winter fog of Beijing analyzed by TEM and SEM.

    Science.gov (United States)

    Li, Weijun; Shao, Longyi

    2010-02-01

    Aerosol samples were collected during winter fog and nonfog episodes in Beijing. Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) were applied to study morphologies, sizes, and compositions of aerosol particles. TEM observation indicates that most mineral particles collected in fog episode are scavenged in fog droplets. Number-size distributions of mineral particles collected in fog and nonfog episodes show two main peaks at the ranges of 0.1-0.3 and 1-2.5 microm, respectively. Based on their major compositions, mineral particles mainly include Si-rich, Ca-rich, and S-rich. Average S/Ca ratio of mineral particles collected in fog episode is 6.11, being eight times higher than that in nonfog episodes. Development mechanism of individual mineral particles in fog droplets is proposed. It is suggested that mineral particles with abundant alkaline components (e.g., "Ca-rich" particles) occurred in air should alleviate acidic degree of fog and contribute to complexity of fog droplets in Beijing.

  18. ERDA, RBS, TEM and SEM characterization of microstructural evolution in helium-implanted Hastelloy N alloy

    Energy Technology Data Exchange (ETDEWEB)

    Gao, Jie [Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800 (China); School of Physical Sciences, University of Chinese Academy of Sciences, Beijing 100049 (China); Bao, Liangman [Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800 (China); Huang, Hefei, E-mail: huanghefei@sinap.ac.cn [Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800 (China); Li, Yan, E-mail: liyan@sinap.ac.cn [Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800 (China); Lei, Qiantao [Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800 (China); Institute of Modern Physics, Fudan University, Shanghai 200433 (China); Deng, Qi [Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800 (China); Liu, Zhe; Yang, Guo [Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800 (China); School of Physical Sciences, University of Chinese Academy of Sciences, Beijing 100049 (China); Shi, Liqun [Institute of Modern Physics, Fudan University, Shanghai 200433 (China)

    2017-05-15

    Hastelloy N alloy was implanted with 30 keV, 5 × 10{sup 16} ions/cm{sup 2} helium ions at room temperature, and subsequent annealed at 600 °C for 1 h and further annealed at 850 °C for 5 h in vacuum. Using elastic recoil detection analysis (ERDA) and transmission electron microscopy (TEM), the depth profiles of helium concentration and helium bubbles in helium-implanted Hastelloy N alloy were investigated, respectively. The diffusion of helium and molybdenum elements to surface occurred during the vacuum annealing at 850 °C (5 h). It was also observed that bubbles in molybdenum-enriched region were much larger in size than those in deeper region. In addition, it is worth noting that plenty of nano-holes can be observed on the surface of helium-implanted sample after high temperature annealing by scanning electron microscope (SEM). This observation provides the evidence for the occurrence of helium release, which can be also inferred from the results of ERDA and TEM analysis.

  19. Site specific SEM/FIB/TEM for analysis of lubricated sliding wear of aluminium alloy composites

    International Nuclear Information System (INIS)

    Walker, J C; Jones, H; Rainforth, W M

    2006-01-01

    Although extensive research has been undertaken into the dry sliding wear of aluminium alloys, only limited work has been reported on lubricated wear. In this paper, the lubricated sliding wear of some powder derived aluminium alloy composites is reported. Stereo pairs of the worn surface were obtained in the SEM and digitally reconstructed to give an accurate projection of the surface topography. Analysis of the average surface roughness (R a ) along chosen sections provided quantitative information about the wear mechanism. Following this, dual beam focused ion beam (FIB) was undertaken to further explore the features revealed by the SEM surface reconstructions, with TEM sections removed from selected regions. Surface deformation was confined to a narrow layer, typically 1μm thick. Subgrain size within the subsurface layer was comparable to that found in dry sliding wear tests. Reinforcement fracture occurred in the surface particles only. The resultant fragments were often incorporated back into the surface following detachment, such that the total volume fraction reinforcement at the surface was greater than in the bulk. Thus, the dynamic surface topography was a result of three factors: surface deformation, local detachment of reinforcement and re-incorporation of the fragments back into the surface

  20. Radiometric, SEM and XRD investigation of the Chituc black sands, southern Danube Delta, Romania

    International Nuclear Information System (INIS)

    Margineanu, R.M.; Blebea-Apostu, Ana-Maria; Celarel, Aurelia; Gomoiu, Claudia-Mariana; Costea, C.; Dumitras, Delia; Ion, Adriana; Duliu, O.G.

    2014-01-01

    The black sand of the Chituc marine sand bank, northern of the city of Navodari (Romania), presents anomalous high radioactivity. Field measurements recorded in some places dose rate up to 200 nSv/h, significantly overpassing the average value of 44 ± 20 nSv/h along the entire Southern sector of Romanian Black Sea shore. Gamma ray spectrometry performed on both Slanic-Prahova Underground Low Background Laboratory and Geological Institute of Romania Radiometric Facilities showed with clarity the dominance of 228 Ac radioisotope in the 50 microns fraction together with the 226 Ra and traces of 40 K. No significant amount of anthropogenic 137 Cs was identified. Based on radiometric as well as on SEM–EDAX and XRD determinations we come to the conclusion that the evidenced radioactivity could be attributed to both uranium and thorium series in the zircon and monazite fractions and to a lesser extent to potassium in the feldspars. - Highlights: • High background radioactivity (up to 200 nSv/h) evidenced. • Radiometric measurements showed a maximum radioactivity of U and Th confined to 50–100 μm fraction. • XRD and SEM–EDAX data revealed the presence of k-feldspars, ilmenite, zircone, monazite and garnets

  1. Multi-scale characterization by FIB-SEM/TEM/3DAP.

    Science.gov (United States)

    Ohkubo, T; Sepehri-Amin, H; Sasaki, T T; Hono, K

    2014-11-01

    In order to improve properties of functional materials, it is important to understand the relation between the structure and the properties since the structure has large effect to the properties. This can be done by using multi-scale microstructure analysis from macro-scale to nano and atomic scale. Scanning electron microscope (SEM) equipped with focused ion beam (FIB), transmission electron microscope (TEM) and 3D atom probe (3DAP) are complementary analysis tools making it possible to know the structure and the chemistry from micron to atomic resolution. SEM gives us overall microstructural and chemical information by various kinds of detectors such as secondary electron, backscattered electron, EDS and EBSD detectors. Also, it is possible to analyze 3D structure and chemistry via FIB serial sectioning. In addition, using TEM we can focus on desired region to get more complementary information from HRTEM/STEM/Lorentz images, SAED/NBD patterns and EDS/EELS to see the detail micro or nano-structure and chemistry. Especially, combination of probe Cs corrector and split EDS detectors with large detector size enable us to analyze the atomic scale elemental distribution. Furthermore, if the specimen has a complicated 3D nanostructure, or we need to analyze light elements such as hydrogen, lithium or boron, 3DAP can be used as the only technique which can visualize and analyze distribution of all constituent atoms of our materials within a few hundreds nm area. Hence, site-specific sample preparation using FIB/SEM is necessary to get desired information from region of interest. Therefore, this complementary analysis combination works very well to understand the detail of materials.In this presentation, we will show the analysis results obtained from some of functional materials by Carl Zeiss CrossBeam 1540EsB FIB/SEM, FEI Tecnai G(2) F30, Titan G2 80-200 TEMs and locally build laser assisted 3DAP. As the one of the example, result of multi-scale characterization for

  2. In situ TEM/SEM electronic/mechanical characterization of nano material with MEMS chip

    International Nuclear Information System (INIS)

    Wang Yuelin; Li Tie; Zhang Xiao; Zeng Hongjiang; Jin Qinhua

    2014-01-01

    Our investigation of in situ observations on electronic and mechanical properties of nano materials using a scanning electron microscope (SEM) and a transmission electron microscope (TEM) with the help of traditional micro-electro-mechanical system (MEMS) technology has been reviewed. Thanks to the stability, continuity and controllability of the loading force from the electrostatic actuator and the sensitivity of the sensor beam, a MEMS tensile testing chip for accurate tensile testing in the nano scale is obtained. Based on the MEMS chips, the scale effect of Young's modulus in silicon has been studied and confirmed directly in a tensile experiment using a transmission electron microscope. Employing the nanomanipulation technology and FIB technology, Cu and SiC nanowires have been integrated into the tensile testing device and their mechanical, electronic properties under different stress have been achieved, simultaneously. All these will aid in better understanding the nano effects and contribute to the designation and application in nano devices. (invited papers)

  3. SEM and TEM characterization of microstructure of stainless steel composites reinforced with TiB2

    International Nuclear Information System (INIS)

    Sulima, Iwona; Boczkal, Sonia; Jaworska, Lucyna

    2016-01-01

    Steel-8TiB 2 composites were produced by two new sintering techniques, i.e. Spark Plasma Sintering (SPS) and High Pressure-High Temperature (HP-HT) sintering. This study discusses the impact of these sintering methods on the microstructure of steel composites reinforced with TiB 2 particles. Scanning electron microscopy (SEM), wavelength dispersive spectroscopy (WDS), X-ray diffraction, electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM) were used to analyze the microstructure evolution in steel matrix composites. The results of microscopic examinations revealed a close relationship between the composite microstructure and the methods and conditions of sintering. Substantial differences were observed in the grain size of materials sintered by HP-HT and SPS. It has been demonstrated that the composites sintered by HP-HT tend to form a chromium-iron-nickel phase in the steel matrix. In contrast, the microstructure of the composites sintered by SPS is characterized by the presence of complex borides and chromium-iron phase. - Highlights: •The steel-8TiB 2 composites were fabricated by Spark Plasma Sintering (SPS) and High Pressure-High Temperature (HP-HT). •Sintering techniques has an important effect on changes in the microstructure of steel-8TiB 2 composites. •New phases of different size and morphology were identified.

  4. SEM and TEM Characterization of As-Fabricated U-7Mo Disperson Fuel Plates

    International Nuclear Information System (INIS)

    Keiser, D.D. Jr.; Yao, B.; Perez, E.; Sohn, Y.H.

    2009-01-01

    The starting microstructure of a dispersion fuel plate can have a dramatic impact on the overall performance of the plate during irradiation. To improve the understanding of the as-fabricated microstructures of dispersion fuel plates, SEM and TEM analysis have been performed on RERTR-9A archive fuel plates, which went through an additional hot isostatic procsssing (HIP) step during fabrication. The fuel plates had depleted U-7Mo fuel particles dispersed in either Al-2Si or 4043 Al alloy matrix. For the characterized samples, it was observed that a large fraction of the ?-phase U-7Mo alloy particles had decomposed during fabrication, and in areas near the fuel/matrix interface where the transformation products were present significant fuel/matrix interaction had occurred. Relatively thin Si-rich interaction layers were also observed around the U-7Mo particles. In the thick interaction layers, (U)(Al,Si)3 and U6Mo4Al43 were identified, and in the thin interaction layers U(Al,Si)3, U3Si3Al2, U3Si5, and USi1.88-type phases were observed. The U3Si3Al2 phase contained some Mo. Based on the results of this work, exposure of dispersion fuel plates to relatively high temperatures during fabrication impacts the overall microstructure, particularly the nature of the interaction layers around the fuel particles. The time and temperature of fabrication should be carefully controlled in order to produce the most uniform Si-rich layers around the U-7Mo particles.

  5. Variations in fixation techniques for field emission SEM and TEM of zebrafish (Branchydanio rerio) embryo inner and outer membranes

    NARCIS (Netherlands)

    Kalicharan, D; Jongebloed, WL; Rawson, DM; Zhang, TT

    1998-01-01

    The morphology of embryos of the fresh water teleost, Brachydania rerio (zebrafish), was examined in a parallel FE-SEM/TEM study, after various pre- and post-fixation regimes. Special attention was paid to the chorion, the contents of the peri-vitelline space, the plasma membrane, the syncytial

  6. Characterization of ash pond ashes from 3rd thermal power plant by SEM/EDX and XRD methods

    Directory of Open Access Journals (Sweden)

    A Minjigmaa

    2014-10-01

    Full Text Available   Coal combustion by products from ash pond of 3rdthermal power plant of Ulaanbaatar city have been collected in 2010 and 2013 years. The ash samples have been characterized by XRD, XRF and SEM-EDX methods in order to evaluate their chemical and mineralogical composition changes with disposed times. The mineralogical composition of ash varies with time though the chemical composition of the ashes were close each other. Possibly, inefficient operating condition of the TPS shows influence on the mineralogical composition.DOI: http://dx.doi.org/10.5564/mjc.v14i0.201Mongolian Journal of Chemistry 14 (40, 2013, p61-65

  7. Bone matrix calcification during embryonic and postembryonic rat calvarial development assessed by SEM-EDX spectroscopy, XRD, and FTIR spectroscopy.

    Science.gov (United States)

    Henmi, Akiko; Okata, Hiroshi; Anada, Takahisa; Yoshinari, Mariko; Mikami, Yasuto; Suzuki, Osamu; Sasano, Yasuyuki

    2016-01-01

    Bone mineral is constituted of biological hydroxyapatite crystals. In developing bone, the mineral crystal matures and the Ca/P ratio increases. However, how an increase in the Ca/P ratio is involved in maturation of the crystal is not known. The relationships among organic components and mineral changes are also unclear. The study was designed to investigate the process of calcification during rat calvarial bone development. Calcification was evaluated by analyzing the atomic distribution and concentration of Ca, P, and C with scanning electron microscopy (SEM)-energy-dispersive X-ray (EDX) spectroscopy and changes in the crystal structure with X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy. Histological analysis showed that rat calvarial bone formation started around embryonic day 16. The areas of Ca and P expanded, matching the region of the developing bone matrix, whereas the area of C became localized around bone. X-ray diffraction and FTIR analysis showed that the amorphous-like structure of the minerals at embryonic day 16 gradually transformed into poorly crystalline hydroxyapatite, whereas the proportion of mineral to protein increased until postnatal week 6. FTIR analysis also showed that crystallization of hydroxyapatite started around embryonic day 20, by which time SEM-EDX spectroscopy showed that the Ca/P ratio had increased and the C/Ca and C/P ratios had decreased significantly. The study suggests that the Ca/P molar ratio increases and the proportion of organic components such as proteins of the bone matrix decreases during the early stage of calcification, whereas crystal maturation continues throughout embryonic and postembryonic bone development.

  8. Effect of interparticle interactions on size determination of zirconia and silica based systems – A comparison of SAXS, DLS, BET, XRD and TEM

    Science.gov (United States)

    Pabisch, Silvia; Feichtenschlager, Bernhard; Kickelbick, Guido; Peterlik, Herwig

    2012-01-01

    The aim of this work is a systematic comparison of size characterisation methods for two completely different model systems of oxide nanoparticles, i.e. amorphous spherical silica and anisotropic facet-shaped crystalline zirconia. Size and/or size distribution were determined in a wide range from 5 to 70 nm using small-angle X-ray scattering (SAXS), dynamic light scattering (DLS), nitrogen sorption (BET), X-ray diffraction (XRD) and transmission electron microscopy (TEM). A nearly perfect coincidence was observed only for SAXS and TEM for both types of particles. For zirconia nanoparticles considerable differences between different measurement methods were observed. PMID:22347721

  9. Investigation of structural resorption behavior of biphasic bioceramics with help of gravimetry, μCT, SEM, and XRD.

    Science.gov (United States)

    de Wild, Michael; Amacher, Fabienne; Bradbury, Christopher R; Molenberg, Aart

    2016-04-01

    Resorbable bone substitute materials are widely used for bone augmentation after tumor resection, parallel to implant placement, or in critical size bone defects. In this study, the structural dissolution of a biphasic calcium phosphate bone substitute material with a hydroxyapatite (HA)/tricalcium phosphate (β-TCP) ratio of 60/40 was investigated by repeatedly placing porous blocks in EDTA solution at 37 °C. At several time points, the blocks were investigated by SEM, µCT, and gravimetry. It was found that always complete 2-3 µm sized grains were removed from the structure and that the β-TCP is dissolved more rapidly. This selective dissolution of the β-TCP grains was confirmed by XRD measurements. The blocks were eroded from the outside toward the center. The structure remained mechanically stable because the central part showed a delayed degradation and because the slower dissolving HA grains preserved the integrity of the structure. © 2015 Wiley Periodicals, Inc.

  10. (AN)AEROBIC BACTERIA FOUND IN SECONDARY-CATARACT MATERIAL - A SEM/TEM STUDY

    NARCIS (Netherlands)

    KALICHARAN, D; JONGEBLOED, WL; LOS, LI; WORST, JGF

    1992-01-01

    Twentyfour patients, who had marked reduction of vision due to secondary-cataract developed after an ECCE, were treated by surgical cleaning of the posterior lens capsule. During this procedure globular secondary-cataract material was removed and collected for morphological examination by SEM and

  11. Characterization of ceramics from the archaeological site of San Miguel Ixtapan, Mexico State, Mexico, using NAA, SEM, XRD and PIXE techniques

    International Nuclear Information System (INIS)

    Tenorio, D.; Monroy-Guzman, F.; Longoria, L.C.; Almazan-Torres, M.G.; Universidad Autonoma del Estado de Mexico, Toluca; Rodriguez-Garcia, N.L.

    2005-01-01

    Ceramic samples found in San Miguel Ixtapan, Mexico State, Mexico, were analyzed by means of NAA, PIXE, SEM and XRD. Statistical treatments such as bivariate cluster and principal-components analysis were applied to the data set. The origins of these ceramic samples were classified as local, regional and foreign. (author)

  12. A novel approach to TEM preparation with a (7-axis stage) triple-beam FIB-SEM system

    Science.gov (United States)

    Clarke, Jamil J.

    2015-10-01

    Preparation of lamellae from bulk to grid for Cs-corrected Transmission Electron Microscope (TEM) observation has mostly become routine work on the latest FIB-SEM systems, with standardized techniques that often are left to automation for the initial steps. The finalization of lamellae however, has mostly become, non-routine, non-repeatable and often driven by user experience level in most cases to produce high quality damage-less cross section. Materials processing of the latest technologies, with ever-shrinking Nano-sized structures pose challenges to modern FIB-SEM systems. This can often lead to specialized techniques and hyper-specific functions for producing ultra-thin high quality lamellae that often are lab specific, preventing practical use of such techniques across multiple materials and applications. Several factors that should be incorporated in processing fine structured materials successfully include how the use of electron and ion scan conditions can affect a thin section during ion milling, the type of ion species applied for material processing during the finalization of lamellae with gallium ions or of a smaller ion species type such as Ar/Xe, sample orientation of the lamella during the thinning process which is linked to ion beam incident angle as a direct relationship in the creation of waterfall effects or curtain effects, and how software can be employed to aid in the reduction of these artifacts with reproducible results regardless of FIB-SEM experience for site-specific lift outs. A traditional TEM preparation was performed of a fine structure specimen in pursuit of a process technique to produce a high quality TEM lamella which would address all of the factors mentioned. These new capabilities have been refined and improved upon during the FIB-SEM design and development stages with an end result of a new approach that yields an improvement in quality by the reduction of common ion milling artifacts such as curtain effects, amorphous

  13. Mössbauer, XRD and TEM Study on the Intercalation and the Release of Drugs in/from Layered Double Hydroxides

    Directory of Open Access Journals (Sweden)

    E. Kuzmann

    2015-12-01

    Full Text Available Layered double hydroxides (LDHs are one of the very important nano-carriers for drug delivery, due to their many advantageous features, such as the ease and low-cost of preparation, low cytotoxicity, good biocompatibility, protection for the intercalated drugs, and the capacity to facilitate the uptake of the loaded drug in the cells. In our previous studies, Mössbauer spectroscopy was applied to monitor structural changes occurring during the incorporation of Fe(III in MgFe- and CaFe-LDHs, and the intercalation of various organic compounds in anionic form. Recently, we have successfully elaborated a protocol for the intercalation and release of indol-2-carboxylate and L-cysteinate in CaFe-LDH. The corresponding structural changes in the LDH samples were studied by XRD, HR-TEM and 57Fe Mössbauer spectroscopy. The Mössbauer spectra reflected small but significant changes upon both the intercalation and the release of drugs. The changes in the basal distances could be followed by XRD measurements, and HR-TEM images made these changes visible.

  14. XRF, XRD and SEM facilities in the School of Materials and Mineral Resources Engineering, Universiti Sains Malaysia

    International Nuclear Information System (INIS)

    Azmi Rahmat

    1996-01-01

    The School has acquired excellent facilities for elemental analysis by XRF and EDX and phase analysis by XRD. The type of research work carried out in the School is described. The school also assists the local industries in trying to solve their problems fully utilizing these facilities along with other testing units

  15. TEM and SEM observation of uranium induced renal necrosis and the result of chelates treatment on rats

    International Nuclear Information System (INIS)

    Sun Shiquan; Li Baoxing; Lai Chixiang; You Zhanyun

    1987-01-01

    The TEM (transmission electron microscope) and SEM (scanning electron microscope) observation of uranium induced renal necrosis and the result of chelates treatment on rats are reported. Ultrastructural changes in kidney related with the impairment of intracellular fluid transportation can be found after acute uranium intoxication in rats, such as: condensation and swelling of mitochondria, matrix edema, dilatation of intercellular space, disappearance of basal folds, thickening of basal web, intensification of basal lamina of the proximal convoluted tubule epithelium cells, and foot processes swelling, diminishing of endothelium fenestrae of the renal glomerulus. Heavy metal chelates DTPA and H-73-10 treatment may result in intracellular fluid accumulation and condensed grannule formation in lysosome. Treatment with these chelates in the critical stage of uranium intoxication may accelerate the necrosis instead of diminishing. This may be related to the augment of the load of lysosome and intracellular system of fluid transportation

  16. SEM, TEM, and IHC Analysis of the Sinus Node and Its Implications for the Cardiac Conduction System

    Directory of Open Access Journals (Sweden)

    D. Mandrioli

    2013-01-01

    Full Text Available More than 100 years after the discovery of the sinus node (SN by Keith and Flack, the function and structure of the SN have not been completely established yet. The anatomic architecture of the SN has often been described as devoid of an organized structure; the origin of the sinus impulse is still a matter of debate, and a definite description of the long postulated internodal specialized tract conducting the impulse from the SN to the atrioventricular node (AVN is still missing. In our previously published study, we proposed a morphologically ordered structure for the SN. As a confirmation of what was presented then, we have added the results of additional observations regarding the structural particularities of the SN. We investigated the morphology of the sinus node in the human hearts of healthy individuals using histochemical, immunohistochemical, optical, and electron microscopy (SEM, TEM. Our results confirmed that the SN presents a previously unseen highly organized architecture.

  17. Some critical aspects of FT-IR, TGA, powder XRD, EDAX and SEM studies of calcium oxalate urinary calculi.

    Science.gov (United States)

    Joshi, Vimal S; Vasant, Sonal R; Bhatt, J G; Joshi, Mihir J

    2014-06-01

    Urinary calculi constitute one of the oldest afflictions of humans as well as animals, which are occurring globally. The calculi vary in shape, size and composition, which influence their clinical course. They are usually of the mixed-type with varying percentages of the ingredients. In medical management of urinary calculi, either the nature of calculi is to be known or the exact composition of calculi is required. In the present study, two selected calculi were recovered after surgery from two different patients for detailed examination and investigated by using Fourier-Transform infrared spectroscopy (FT-IR), thermo-gravimetric analysis (TGA), powder X-ray diffraction (XRD), scanning electron microscopy and energy dispersive analysis of X-rays (EDAX) techniques. The study demonstrated that the nature of urinary calculi and presence of major phase in mixed calculi could be identified by FT-IR, TGA and powder XRD, however, the exact content of various elements could be found by EDAX only.

  18. Investigation of composition and structure of spongy and hard bone tissue using FTIR spectroscopy, XRD and SEM

    Science.gov (United States)

    Al-Akhras, M.-Ali H.; Hasan Qaseer, M. K.; Albiss, B. A.; Alebrhim, M. Anwar; Gezawa, Umar S.

    2018-02-01

    Valuable structural and chemical features can be obtained for spongy and hard bone by infrared spectroscopy and X-ray diffraction. A better understanding of chemical and structural differences between spongy and hard bone is a very important contributor to bone quality. Our data according to IR data showed that the collagen cross-links occurred to be higher in spongy bone, and crystallinity was lower in spongy bone. Deconvolution of the infrared band near 870 cm-1 reveals evidence for A2-type carbonate substitution on hydroxyapatite of spongy bone in addition to the A and B type carbonate substitution that are also found in hard bone. IR and XRD data confirmed the results of each other since full width at half maximum of 002-apatite pattern of XRD showed that the crystallinity was lower in spongy bone. The microstructure was examined by using scanning electron microscope and the result showed that the lattice of thin threads in spongy bone and is less dense than hard bone.

  19. In situ oxidation of zirconium binary alloys by environmental SEM and analysis by AFM, FIB, and TEM

    International Nuclear Information System (INIS)

    Proff, C.; Abolhassani, S.; Dadras, M.M.; Lemaignan, C.

    2010-01-01

    Binary Zr-alloys containing 1%Fe and 1% Ni (large precipitates) and 1% Cr and 0.6% Nb (small precipitates), as well as a pure Zr sample were exposed in situ at 130 Pa water vapour pressure at 415 o C in an environmental SEM. The surface topography and composition of each sample was characterised before in situ experiments, during and after oxidation. After oxidation the surface was characterised by SEM and EDS, AFM and TEM combined with EDS. Focused ion beam was used to prepare cross sections of the metal-oxide interface and for the preparation of TEM thin foils. The oxidation behaviour of precipitates for these alloying elements can be characterised into two large families, those which show a rapid oxidation and those which induce a delayed oxidation in comparison with the Zr-matrix. At 415 o C after 1 h of oxidation for Zr1%Fe and Zr1%Ni, the formation of protrusions could be detected at the surface, being related to underlying SPP in the oxide. On Zr1%Cr and Zr0.6%Nb unoxidised SPPs were observed in the oxide, close to the metal-oxide interface. These SPPs were, however, oxidised close to the outer surface of the oxide. The surface roughness was increased for all materials after in situ oxidation, however, only for Zr1%Fe and Zr1%Ni protrusions appeared on the surface during oxidation. It was subsequently demonstrated that these latter correspond to the position of SPPs. For Zr1%Fe the surface roughness increased more than in the other materials and on these protrusions small iron oxide crystals have been observed at the surface. These observations confirm that Fe has a different behaviour compared to the other SPP forming elements, and it diffuses out to the free surface of the material. These alloying elements being the constituents of the commercial alloys (Fe and Cr for Zircaloy-4; Fe, Cr and Ni for Zircaloy-2 and Nb for all Nb-containing alloys), this study allows to separate their individual influence and can allow a subsequent comparison to the behaviour

  20. Removal of industrial dyes and heavy metals by Beauveria bassiana: FTIR, SEM, TEM and AFM investigations with Pb(II).

    Science.gov (United States)

    Gola, Deepak; Malik, Anushree; Namburath, Maneesh; Ahammad, Shaikh Ziauddin

    2017-10-01

    Presence of industrial dyes and heavy metal as a contaminant in environment poses a great risk to human health. In order to develop a potential technology for remediation of dyes (Reactive remazol red, Yellow 3RS, Indanthrene blue and Vat novatic grey) and heavy metal [Cu(II), Ni(II), Cd(II), Zn(II), Cr(VI) and Pb(II)] contamination, present study was performed with entomopathogenic fungi, Beauveria bassiana (MTCC no. 4580). High dye removal (88-97%) was observed during the growth of B. bassiana while removal percentage for heavy metals ranged from 58 to 75%. Further, detailed investigations were performed with Pb(II) in terms of growth kinetics, effect of process parameters and mechanism of removal. Growth rate decreased from 0.118 h -1 (control) to 0.031 h -1 , showing 28% reduction in biomass at 30 mg L -1 Pb(II) with 58.4% metal removal. Maximum Pb(II) removal was observed at 30 °C, neutral pH and 30 mg L -1 initial metal concentration. FTIR analysis indicated the changes induced by Pb(II) in functional groups on biomass surface. Further, microscopic analysis (SEM and atomic force microscopy (AFM)) was performed to understand the changes in cell surface morphology of the fungal cell. SEM micrograph showed a clear deformation of fungal hyphae, whereas AFM studies proved the increase in surface roughness (RSM) in comparison to control cell. Homogenous bioaccumulation of Pb(II) inside the fungal cell was clearly depicted by TEM-high-angle annular dark field coupled with EDX. Present study provides an insight into the mechanism of Pb(II) bioremediation and strengthens the significance of using entomopathogenic fungus such as B. bassiana for metal and dye removal.

  1. Study of copper deposit on a porous electrode of carbon and stainless steel by sem-xrd and image analysis

    OpenAIRE

    Constanzo-R., Robinson; Pagliero-N., Antonio; Vergara-G., Froilán

    2014-01-01

    El objetivo de este trabajo fue realizar un análisis cualitativ o de la distribución de un electrodepósito de cobre en el inter ior de electrodos porosos (EP) de acero inoxidable y carbono grafito. Para ello, se reali zaron pruebas de electrodepositación de cobre a nivel de labora torio, con un posterior análisis de cortes de muestras de acero y grafito vía Microscopía Estereoscópica, Microscopía SEM-DRX y Análisis de Imagen, los cuales mostraron que el cobre no se deposita en forma uniforme ...

  2. Characterisation of rust surfaces formed on mild steel exposed to marine atmospheres using XRD and SEM/Micro-Raman techniques

    International Nuclear Information System (INIS)

    Fuente, D. de la; Alcántara, J.; Chico, B.; Díaz, I.; Jiménez, J.A.; Morcillo, M.

    2016-01-01

    Highlights: • SEM/Micro-Raman is very useful for characterizing rust phases morphologies. • SEM/Micro-Raman enables unequivocal rust phases identification. • γ-FeOOH basically presents two types of morphologies: globular and laminar. • Fe 3 O 4 presents two morphologies: flat patches and black doughnut-type formations. • β-FeOOH presents highly porous morphologies comprised by fine prismatic crystals. - Abstract: The exposure of mild steel to marine atmospheres gives rise to the formation of various corrosion products, mainly lepidocrocite, goethite, magnetite and akaganeite. In this study, Grazing Incidence X-Ray Diffraction, Micro-X-Ray Diffraction and Scanning Electron Microscopy/Micro-Raman are used to characterise rust layer surfaces and to identify the principal component rust phases and their morphology. The main conclusion reached is that lepidocrocite is preferentially located on the outermost surface while magnetite and akaganeite form mostly close to base steel. The Scanning Electron Microscopy/Micro-Raman technique has been very useful for characterising (identifying) the wide variety of morphologies presented by the rust phases.

  3. SEM and TEM characterization of the microstructure of post-compressed TiB2/2024Al composite.

    Science.gov (United States)

    Guo, Q; Jiang, L T; Chen, G Q; Feng, D; Sun, D L; Wu, G H

    2012-02-01

    In the present work, 55 vol.% TiB(2)/2024Al composites were obtained by pressure infiltration method. Compressive properties of 55 vol.% TiB(2)/2024Al composite under the strain rates of 10(-3) and 1S(-1) at different temperature were measured and microstructure of post-compressed TiB(2)/2024Al composite was characterized by scanning electron microscope (SEM) and transmission electron microscope (TEM). No trace of Al(3)Ti compound flake was found. TiB(2)-Al interface was smooth without significant reaction products, and orientation relationships ( [Formula: see text] and [Formula: see text] ) were revealed by HRTEM. Compressive strength of TiB(2)/2024Al composites decreased with temperature regardless of strain rates. The strain-rate-sensitivity of TiB(2)/2024Al composites increased with the increasing temperature. Fracture surface of specimens compressed at 25 and 250°C under 10(-3)S(-1) were characterized by furrow. Under 10(-3)S(-1), high density dislocations were formed in Al matrix when compressed at 25°C and dynamic recrystallization occurred at 250°C. Segregation of Mg and Cu on the subgrain boundary was also revealed at 550°C. Dislocations, whose density increased with temperature, were formed in TiB(2) particles under 1S(-1). Deformation of composites is affected by matrix, reinforcement and strain rate. Copyright © 2011 Elsevier Ltd. All rights reserved.

  4. First ultrastructural data on the human tapeworm Taenia asiatica eggs by scanning and transmission electron microscopy (SEM, TEM).

    Science.gov (United States)

    Galán-Puchades, M Teresa; Yang, Yichao; Marcilla, Antonio; Choe, Seongjun; Park, Hansol; Osuna, Antonio; Eom, Keeseon S

    2016-09-01

    Humans are definitive hosts of three species of the Taenia genus, namely Taenia solium, Taenia saginata and Taenia asiatica. The relative novelty of the latter explains the lack of knowledge concerning certain relevant aspects related to this parasite, such as its definite geographical distribution and whether its eggs can infect humans or not. So far, only the eggs of T. solium are known to be infective for humans, producing cysticercosis. Although eggs contain the infective stage, the oncosphere, there is a lack of research on the ultrastructure of eggs of human taeniids. We show, for the first time, the ultrastructure of eggs of T. asiatica by means of SEM and TEM analyses. We detected all the envelopes, namely the egg shell, vitelline layer, outer embryophoric membrane, embryophore, granular layer, basal membrane, oncospheral membrane and oncospheral tegument. Hooks surrounded by myofibrils and glycogen-like particles, the two types of secretory granules of the penetration glands, as well as several nuclei and mitochondria were also revealed in the oncospheres. In addition to the already known structures in eggs from other Taenia species, the presence of two types of small vesicles is described herein, possibly corresponding to exosomes and ectosomes because of their shape and size, which could participate in the host/parasite intercellular communication.

  5. Evaluation of the effects of biodegradable nanoparticles on a vaccine delivery system using AFM, SEM, and TEM.

    Science.gov (United States)

    Kim, Bum-Gil; Kang, Ik-Joong

    2008-09-01

    Hepatitis B is a deadly disease, and is carried by 30% of the world's population. Antibodies are produced through a series of three manual vaccinations during infancy and childhood. However, the current needle vaccination not only induces pain in patients, but also can be inconvenient to administer. This is particularly true for the case of newborn babies. Intranasal vaccination is emerging as an alternative parenteral drug delivery method that facilitates drug delivery without causing pain. Chitosan, which is obtained through the deacetylation of chitin from crustacea, is a cationic polymer that is biodegradable, avirulent, and highly absorptive. In this study, ionic gelation between chitosan and TPP was conducted to synthesize chitosan nanoparticles with sizes of 200-400 nm and a surface potential of 55-60 mV, and which can be used as Hepatitis B vaccine carriers. Then, Hepatitis B antigen protein was impregnated to manufacture chitosan-recombinant gene vaccine protein (RGVP) nanoparticles. AFM, SEM, TEM, and STEM were used to analyze the manufactured nanoparticles, whose function as drug carriers and whose usefulness for intranasal vaccination were confirmed through in vivo tests with SD rats.

  6. FE-SEM, FIB and TEM Study of Surface Deposits of Apollo 15 Green Glass Volcanic Spherules

    Science.gov (United States)

    Ross, Daniel K.; Thomas-Keprta, K. L.; Rahman, Z.; Wentworth, S. J.; McKay, D. S.

    2011-01-01

    Surface deposits on lunar pyroclastic green (Apollo 15) and orange (Apollo 17) glass spherules have been attributed to condensation from the gas clouds that accompanied fire-fountain eruptions. The fire fountains cast molten lava high above the lunar surface and the silicate melt droplets quenched before landing producing the glass beads. Early investigations showed that these deposits are rich in sulfur and zinc. The deposits are extremely fine-grained and thin, so that it was never possible to determine their chemical compositions cleanly by SEM/EDX or electron probe x-ray analysis because most of the excited volume was in the under-lying silicate glass. We are investigating the surface deposits by TEM, using focused ion beam (FIB) microscopy to extract and thin the surface deposits. Here we report on chemical mapping of a FIB section of surface deposits of an Apollo green glass bead 15401using the ultra-high resolution JEOL 2500 STEM located at NASA Johnson Space Center.

  7. Vacancy ordered γ-Fe{sub 2}O{sub 3} nanoparticles functionalized with nanohydroxyapatite: XRD, FTIR, TEM, XPS and Mössbauer studies

    Energy Technology Data Exchange (ETDEWEB)

    Ramos Guivar, Juan A., E-mail: juan.ramos5@unmsm.edu.pe [Faculty of Physical Sciences, National University of San Marcos, P. O. Box 14- 0149, Lima 14 (Peru); Sanches, Edgar A., E-mail: sanches.ufam@gmail.com [Federal University of Amazonas, Department of Physics, Manaus/AM (Brazil); Bruns, Florian, E-mail: f.bruns@tu-braunschweig.de [Institut für Physik der Kondensierten Materie, Technische Universität Braunschweig, 38110 Braunschweig (Germany); Sadrollahi, Elaheh, E-mail: elahe.sadrollahi@gmail.com [Institut für Physik der Kondensierten Materie, Technische Universität Braunschweig, 38110 Braunschweig (Germany); Morales, M.A., E-mail: marco.moralestorres@gmail.com [Department of Theoretical and Experimental Physics, UFRN, Natal, RN 59078- 970 (Brazil); López, Elvis O., E-mail: lopmezel@gmail.com [Brazilian Center for Research in Physics (CBPF), Rio de Janeiro, RJ 22290-180 (Brazil); Litterst, F. Jochen, E-mail: litterst@cbpf.br [Institut für Physik der Kondensierten Materie, Technische Universität Braunschweig, 38110 Braunschweig (Germany); Brazilian Center for Research in Physics (CBPF), Rio de Janeiro, RJ 22290-180 (Brazil)

    2016-12-15

    Graphical abstract: Possible bonding configuration in the γ-Fe{sub 2}O{sub 3} nanoparticles functionalized with nanoHAp. - Highlights: • Coprecipitation in alkaline medium for the synthesis of vacancy ordered γ-Fe{sub 2}O{sub 3}@HAp nanocomposite. • Samples were characterized by XRD, FTIR, XPS, TEM, VSM and Mössbauer spectroscopy. • The functionalization is explained with the binding of two oxygens of chemisorbed H{sub 2}O molecules at the common interface of HAp/C{sub 6}H{sub 8}O{sub 7}/γ-Fe{sub 2}O{sub 3}. - Abstract: Vacancy ordered maghemite (γ-Fe{sub 2}O{sub 3}) nanoparticles functionalized with nanohydroxyapatite (HAp – Ca{sub 10}(PO{sub 4}) {sub 6}(OH){sub 2}) have been successfully synthesized using an inexpensive co-precipitation chemical route. Evidence for the presence of vacancy order in maghemite was shown by the superstructure lines observed in X-ray diffraction. The adsorption of carboxyl groups of citric acid (C{sub 6}H{sub 8}O{sub 7}) onto γ-Fe{sub 2}O{sub 3} nanoparticles was investigated by FTIR, XPS and Mössbauer spectroscopy. From XPS surface analysis, two binding energies related to oxygen were attributed to bindings between C{sub 6}H{sub 8}O{sub 7}/γ- Fe{sub 2}O{sub 3} and C{sub 6}H{sub 8}O{sub 7}/HAp from an interfacial reaction promoted by strongly adsorbed H{sub 2}O molecules at the surface of these nanomaterials. Le Bail refinement of the XRD patterns showed the formation of well-crystallized pure tetragonal maghemite before and after functionalization with nanoHAp. The temperature dependence of hyperfine parameters of pure and functionalized γ-Fe{sub 2}O{sub 3} nanoparticles was investigated via Mössbauer spectroscopy. TEM revealed the formation of quasi-spherical γ- Fe{sub 2}O{sub 3} nanoparticles with an average diameter of ca. 12 nm and 16 nm before and after functionalization with nanoHAp in agreement with Le Bail refinement. Magnetometry measurements showed a saturation magnetization of 12 emu/g and a blocking

  8. TEM/SEM investigation of microstructural changes within the white etching area under rolling contact fatigue and 3-D crack reconstruction by focused ion beam

    International Nuclear Information System (INIS)

    Grabulov, A.; Ziese, U.; Zandbergen, H.W.

    2007-01-01

    The white etching area (WEA) surrounding the cracks formed under high-cycle rolling contact fatigue was investigated by transmission electron microscopy (TEM) and Dual Beam (scanning electron microscopy (SEM)/focused ion beam). SEM revealed the initiation of cracks formed around artificially introduced Al 2 O 3 inclusions in the model steel (composition similar to SAE 52100). TEM investigations showed a microstructural difference between the WEA (formation of nanocrystalline ferrite) and the steel matrix (tempered martensitic structure). A three-dimensional image of the crack reconstructed from ∼400 Dual Beam cross-section images is reported

  9. Characterization of wet precipitation by X-ray diffraction (XRD) and scanning electron microscopy (SEM) in the metropolitan area of Porto Alegre, Brazil

    Energy Technology Data Exchange (ETDEWEB)

    Montanari Migliavacca, Daniela [Instituto de Biociencias, Programa de Pos-Graduacao em Ecologia, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91509-900 Porto Alegre, RS (Brazil); Fundacao Estadual de Protecao Ambiental Henrique Luis Roessler, RS. Rua Carlos Chagas 55/802, 90030-020 Porto Alegre, RS (Brazil); Calesso Teixeira, Elba, E-mail: gerpro.pesquisa@fepam.rs.gov.br [Fundacao Estadual de Protecao Ambiental Henrique Luis Roessler, RS. Rua Carlos Chagas 55/802, 90030-020 Porto Alegre, RS (Brazil); Gervasoni, Fernanda; Vieira Conceicao, Rommulo [Instituto de Geociencias, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91509-900 Porto Alegre, RS (Brazil); Raya Rodriguez, Maria Teresa [Instituto de Biociencias, Programa de Pos-Graduacao em Ecologia, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91509-900 Porto Alegre, RS (Brazil)

    2009-11-15

    The purpose of this study is to assess the composition of wet precipitation in three sites of the metropolitan area of Porto Alegre. Besides the variables usually considered, such as pH, conductivity, major ions (Cl{sup -}, NO{sub 3}{sup -}, F{sup -}, SO{sub 4}{sup 2-}, Na{sup +}, K{sup +}, Mg{sup 2+}, NH{sub 4}{sup +} and Ca{sup 2+}) and metallic elements (Cd, Co, Cr, Cu, Fe, Mn and Ni), the suspended matter was examined by X-ray diffraction (XRD) and scanning electron microscopy (SEM), with energy dispersive system (EDS), for better identification of possible anthropogenic material in this wet precipitation. Results showed an alkaline pH in the samples analyzed and higher concentrations for Na{sup +}, Cl{sup -} and SO{sub 4}{sup 2-}. The acidification and neutralization potential between anions (SO{sub 4}{sup 2-} + NO{sub 3}{sup -}) and cations (Ca{sup 2+} + Mg{sup 2+} + K{sup +} + NH{sub 4}{sup +}) showed a good correlation (0.922). The metallic elements with highest values were Zn, Fe and Mn. Results of XRD identified the presence of some minerals such as quartz, feldspar, mica, clay, carbonates and sulfates. In samples analyzed with SEM, we detected pyroxene, biotite, amphibole and oxides. Cluster analysis (CA) was applied to the data matrix to identify potential pollution sources of metals (natural or anthropogenic) and the association with minerals found in the analysis of SEM.

  10. Correlation of superconducting properties and microstructure in MgB{sub 2} using SEM, EPMA and TEM

    Energy Technology Data Exchange (ETDEWEB)

    Birajdar, Balaji I.

    2008-04-14

    This thesis can be subdivided as follows: (I) Development of the quantitative electron microscopy and spectroscopy methods essential for the microstructural analysis of MgB{sub 2} and thereby assess the performance of two energy-filtered TEMs. (II) Application of these methods to few selected samples: (a) Pure and Al-alloyed MgB{sub 2} bulk samples prepared by solid-state reaction or by mechanical alloying, (b) In-situ and ex-situ MgB{sub 2} wires and tapes with and without SiC additives prepared by different variants of the powder-in-tube technology. Quantitative B analysis by EDX spectroscopy was applied in the SEM and TEM, which is a major achievement. (III) Establishing a model which quantitatively explains the correlation between microstructure and critical current density as a function of magnetic field. The actual Al mole fraction in the MgB{sub 2} matrix was found to be less than the nominal Al mole fraction and the difference increased with increasing Al mole fraction. Al is incorporated into MgB{sub 2} grains of {approx}1{mu}m size by substitution of Mg atoms causing T{sub c} and c lattice parameter to decrease at a rate of 1.56 K and 1.15 pm per at.% of Al alloying. Precipitation of Al was not detected up to highest Al mole fractions but Al was inhomogeneously distributed in the sample, which explained the broadening of the superconducting transition width ({delta}T{sub c}) with increasing Al mole fraction. For wires and tapes, significant differences were observed in the microstructure of in-situ and ex-situ samples. This holds particularly if SiC was added and yielded Mg{sub 2}Si for in-situ samples annealed at 600 -650 C and Mg-Si-O phases for ex-situ samples annealed between 900 -1050 C. Four microstructural parameters were identified as relevant for the I{sub c} of wires and tapes and these were: 1) MgB{sub 2} grain size which lies in the range of 20-1000 nm, 2) colony size (colony is a dense arrangement of MgB{sub 2} grains) which lies in the range

  11. Phosphorus Sorption Characteristics in Aluminum-based Water Treatment Residuals Reacted with Dairy Wastewater: 1. Isotherms, XRD, and SEM-EDS Analysis.

    Science.gov (United States)

    Zohar, Iris; Massey, Michael S; Ippolito, James A; Litaor, M Iggy

    2018-05-01

    We examined P sorption characteristics in Al-based water treatment residuals (Al-WTR) generated from slightly alkaline surface water and in an organic residual composite (WW-Al/O-WTR), produced by using the Al-WTR to treat organic-rich and high P concentration dairy wastewater. Solids from both residuals were examined using scanning electron microscopy-energy dispersive spectroscopy (SEM-EDS) and X-ray diffraction (XRD), and exposed to P additions of 0 to 4000 mg L in a sorption experiment. The Al-WTR removed ∼97% of the added P, whereas WW-Al/O-WTR removed only 78% of the added P in the addition range of 0 to 100 mg P L. With P additions of ≥100 mg L, the removal rate declined to XRD indicated that the major mineral was calcite, with some silica and poorly crystalline Al hydroxides. Analysis by SEM-EDS, which used three-element overlay maps of the residual surfaces, indicated that P was sparsely sorbed on both calcic and Al (hydr)oxide surfaces, along with a few clusters, even at low P concentrations of the treated waters. Ternary clusters of P, Al, and Ca were more abundant on the WW-Al/O-WTR. Carbon distribution suggested that organic substances covered Al surfaces. Sorption of P onto WW-Al/O-WTR may be reversible due to relatively weak Ca-P and Al-P bonds induced by the slight alkaline nature and in the presence of organic moieties, enhancing the WW-Al/O-WTR potential to act as a P source, rather than a P sink, in agricultural applications. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

  12. A detailed TEM and SEM study of Ni-base alloys oxide scales formed in primary conditions of pressurized water reactor

    International Nuclear Information System (INIS)

    Sennour, Mohamed; Marchetti, Loic; Martin, Frantz; Perrin, Stephane; Molins, Regine; Pijolat, Michele

    2010-01-01

    The oxide film formed on nickel-based alloys in pressurized water reactors (PWR) primary coolant conditions (325 o C, aqueous media) is very thin, in the range of 1-100 nm thick, depending on the surface state and on the corrosion test duration. The nature and the structure of this scale have been investigated by Transmission Electron Microscopy (TEM) and Scanning Electron Microscopy (SEM). TEM observations revealed an oxide layer divided in two parts. The internal layer was mainly composed of a continuous spinel layer, identified as a mixed iron and nickel chromite (Ni (1-x) Fe x Cr 2 O 4 ). Moreover, nodules of Cr 2 O 3 , with a size about 5 nm, were present at the interface between this spinel and the alloy. No chromium depletion was observed in the alloy, at the alloy/oxide interface. The external layer is composed of large crystallites corresponding to a spinel structure rich in iron (Ni (1-z) Fe (2+z) O 4 ) resulting from precipitation phenomena. SEM and TEM observations showed a link between the nucleation and/or the growth of crystallites of nickel ferrite and the crystallographic orientation of the substrate. A link between the presence of surface defects and the nucleation of the crystallites was also underlined by SEM observations. Partially hydrated nickel hydroxide, was also observed by TEM in the external scale. Based on these results, some considerations about the mechanism of formation of this oxide layer are discussed.

  13. Investigation of the agglomeration and amorphous transformation effects of neutron irradiation on the nanocrystalline silicon carbide (3C-SiC) using TEM and SEM methods

    Energy Technology Data Exchange (ETDEWEB)

    Huseynov, Elchin M., E-mail: elchin.h@yahoo.com [Department of Nanotechnology and Radiation Material Science, National Nuclear Research Center, Inshaatchilar pr. 4, AZ 1073 Baku (Azerbaijan); Institute of Radiation Problems of Azerbaijan National Academy of Sciences, B.Vahabzade 9, AZ 1143 Baku (Azerbaijan)

    2017-04-01

    Nanocrystalline 3C-SiC particles irradiated by neutron flux during 20 h in TRIGA Mark II light water pool type research reactor. Silicon carbide nanoparticles were analyzed by Scanning Electron Microscope (SEM) and Transmission Electron Microscopy (TEM) devices before and after neutron irradiation. The agglomeration of nanoparticles was studied comparatively before and after neutron irradiation. After neutron irradiation the amorphous layer surrounding the nanoparticles was analyzed in TEM device. Neutron irradiation defects in the 3C-SiC nanoparticles and other effects investigated by TEM device. The effect of irradiation on the crystal structure of the nanomaterial was studied by selected area electron diffraction (SAED) and electron diffraction patterns (EDP) analysis.

  14. XRD and SEM/EDS characterization of coconut fibers in raw and treated forms used in the treatment of strontium in aqueous solution

    Energy Technology Data Exchange (ETDEWEB)

    Fonseca, Heverton C.O.; Garcia, Rafael H.L.; Ferreira, Robson J.; Silva, Flavia R.O.; Potiens Junior, Ademar J.; Sakata, Solange K., E-mail: sksakata@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2015-07-01

    {sup 90}Sr, a radioactive isotope of strontium, is one of the fission products and quite often present in the radioactive waste produced by nuclear power plants. Recently, the removal efficiency of strontium by treated coconut fibers was evaluated and reached up to 95% in an aqueous solution. This work presents the characterization of raw and treated coconut fibers with different concentrations of hydrogen peroxide in basic medium using X-ray diffraction (XRD) and scanning electron microscopy/energy dispersive spectroscopy (SEM / EDS). The analysis of X-ray diffraction shows a crystallinity of 37.6% for raw coconut fiber and crystallinity of 45.4% and 50.6% for coconut fibers 1 and 2, respectively. These results showed that the different degrees of degradation of organic matter can affect the crystallinity of the treated. This study of morphology and crystallinity of theses biosorbent materials with strontium will help in comprehension of the effects of alkaline hydrogen peroxide treatment and it will demonstrate the potential of strontium uptake by coconut fibers. (author)

  15. XRD and SEM/EDS characterization of coconut fibers in raw and treated forms used in the treatment of strontium in aqueous solution

    International Nuclear Information System (INIS)

    Fonseca, Heverton C.O.; Garcia, Rafael H.L.; Ferreira, Robson J.; Silva, Flavia R.O.; Potiens Junior, Ademar J.; Sakata, Solange K.

    2015-01-01

    90 Sr, a radioactive isotope of strontium, is one of the fission products and quite often present in the radioactive waste produced by nuclear power plants. Recently, the removal efficiency of strontium by treated coconut fibers was evaluated and reached up to 95% in an aqueous solution. This work presents the characterization of raw and treated coconut fibers with different concentrations of hydrogen peroxide in basic medium using X-ray diffraction (XRD) and scanning electron microscopy/energy dispersive spectroscopy (SEM / EDS). The analysis of X-ray diffraction shows a crystallinity of 37.6% for raw coconut fiber and crystallinity of 45.4% and 50.6% for coconut fibers 1 and 2, respectively. These results showed that the different degrees of degradation of organic matter can affect the crystallinity of the treated. This study of morphology and crystallinity of theses biosorbent materials with strontium will help in comprehension of the effects of alkaline hydrogen peroxide treatment and it will demonstrate the potential of strontium uptake by coconut fibers. (author)

  16. Extensive FE-SEM/EDS, HR-TEM/EDS and ToF-SIMS studies of micron- to nano-particles in anthracite fly ash

    Energy Technology Data Exchange (ETDEWEB)

    Ribeiro, Joana [Centro de Geologia, Universidade do Porto, Rua do Campo Alegre, 687, 4169-007 Porto (Portugal); DaBoit, Kátia [Institute of Environmental Research and Human Development, IPADHC, Capivari de Baixo, Santa Catarina (Brazil); Flores, Deolinda [Centro de Geologia, Universidade do Porto, Rua do Campo Alegre, 687, 4169-007 Porto (Portugal); Departamento de Geociências, Ambiente e Ordenamento do Território, Faculdade de Ciências, Universidade do Porto, Rua do Campo Alegre, 687, 4169-007 Porto (Portugal); Kronbauer, Marcio A. [Laboratory of Environmental Researches and Nanotechnology Development, Centro Universitário La Salle, Victor Barreto, 2288 Centro 92010-000, Canoas, RS (Brazil); Silva, Luis F.O., E-mail: felipeqma@hotmail.com [Laboratory of Environmental Researches and Nanotechnology Development, Centro Universitário La Salle, Victor Barreto, 2288 Centro 92010-000, Canoas, RS (Brazil); Environmental Science and Nanotechnology Department, Catarinense Institute of Environmental Research and Human Development, IPADHC, Capivari de Baixo, Santa Catarina (Brazil)

    2013-05-01

    The generation of anthropogenic carbonaceous matter and mixed crystalline/amorphous mineral ultrafine/nano-particles in the 1 to 100 nm size range by worldwide coal power plants represents serious environmental problems due to their potential hazards. Coal fly ash (CFA) that resulted from anthracite combustion in a Portuguese thermal power plant was studied in this work. The physico-chemical characterization of ultrafine/nano-particles present in the CFA samples and their interaction with environment are the aim of this study. The methodologies applied for this work were field emission scanning electron microscopy (FE-SEM) with energy dispersive X-ray spectroscopy (EDS), high-resolution transmission electron microscopy with energy dispersive X-ray spectroscopy (HR-TEM/EDS) and time of flight secondary ion mass spectrometry (ToF-SIMS). Some hazardous volatile elements, C, N, S and Hg contents were also determined in the studied samples. Generally, the CFA samples comprise carbonaceous, glassy and metallic solid spheres with some containing mixed amorphous/crystalline phases. The EDS analysis coupled with the FE-SEM and HR-TEM observations of the fly ash particles with 100 to 0.1 nm demonstrates that these materials contain a small but significant proportion of encapsulated HVEs. In addition, the presence of abundant multi-walled carbon nanotubes (MWCNTs) and amorphous carbon particles, both containing hazardous volatile elements (HVEs), was also evidenced by the FE-SEM/EDS and HR-TEM/EDS analysis. A wide range of organic and inorganic compounds was determined by chemical maps obtained in ToF-SIMS analysis. - Highlights: ► We examine changes in the level of ultrafine and nanoparticles of coal mining. ► Increasing geochemical information will increase human health information in this area. ► Electron bean and Tof-SIMS increase area information.

  17. Chemical and structural analysis of the bone-implant interface by TOF-SIMS, SEM, FIB and TEM: Experimental study in animal

    International Nuclear Information System (INIS)

    Palmquist, Anders; Emanuelsson, Lena; Sjövall, Peter

    2012-01-01

    Although bone-anchored implants are widely used in reconstructive medicine, the mechanism of osseointegration is still not fully understood. Novel analytical tools are needed to further understand this process, where both the chemical and structural aspects of the bone-implant interface are important. The aim of this study was to evaluate the advantages of combining time-of-flight secondary ion mass spectroscopy (TOF-SIMS) with optical (LM), scanning (SEM) and transmission electron microscopy (TEM) techniques for studying the bone-implant interface of bone-anchored implants. Laser-modified titanium implants with surrounded bone retrieved after 8 weeks healing in rabbit were dehydrated and resin embedded. Three types of sample preparation were studied to evaluate the information gained by combining TOF-SIMS, SEM, FIB and TEM. The results show that imaging TOF-SIMS can provide detailed chemical information, which in combination with structural information from microscopy methods provide a more complete characterization of anatomical structures at the bone-implant interface. By investigating various sample preparation techniques, it is shown that grinded cross section samples can be used for chemical imaging using TOF-SIMS, if careful consideration of potential preparation artifacts is taken into account. TOF-SIMS analysis of FIB-prepared bone/implant cross section samples show distinct areas corresponding to bone tissue and implant with a sharp interface, although without chemical information about the organic components.

  18. SEM-EDS and XRD study of a NiCrAlU alloy at temperatures from 800 celsius degree to 1300 celsius degree

    International Nuclear Information System (INIS)

    Al-Badairy, H.; Fox, P.

    2004-01-01

    Full text.The oxidation behaviour of a 74.5wt%Ni, 20wt%Cr, 5wt%Al and 0.5wt%U alloy was examined using Scanning Electron Microscopy with X-ray Energy Dispersive Spectroscopy (SEM-EDS) and X-ray Diffractometry (XRD). The oxidation temperature ranged from 800 to 1300 celsius degree in laboratory air with oxidation times up to 120h. Analysis showed that during short term oxidation (40h) at the lower temperatures there was evidence of the formation of Cr, Ni and Al oxides. With increasing oxidation time, the Cr-rich oxide became predominant with the presence of islands of Ni-rich oxide, but no uranium was detected at the outermost layer of the scale. The scale was of flat topography with spallation occurring after 40h oxidation at 900 celsius degree and increasing with increasing temperature and time. Cross-sectional investigations indicated the presence of an internal oxidation zone comprising an Al-rich oxide beneath the outer Cr-rich scale with significant amounts of uranium. The depth of this zone varied from 1 micron to 60 microns and increased with increasing the oxidation temperature and time. At higher temperatures (above 1000 celsius degree), the internal oxidation zone ceased to grow due to the formation of a complete layer of alumina which protected the metal substrate from further degradation. The constituents of the scales formed reflect the selective oxidation of Cr and Al as a result of the higher reactivity of aluminium and chromium compared to nickel and the greater stability of Al 2 O 3 and Cr 2 O 3 compared to NiO. This study showed that Al-rich oxide was not the predominant protective oxide and the presence of uranium was restricted to the grain boundaries of the metal substrate and to within the internal oxidation zone. It appeared that the Cr-rich scale formed on this alloy does not to convolute. This may be due to the influence of uranium since Cr-rich scales forming on NiCrAl containing no uranium are often convoluted

  19. Investigation on by-products of bioenergy systems (anaerobic digestion and gasification) as potential crop nutrient using FTIR, XRD, SEM analysis and phyto-toxicity test.

    Science.gov (United States)

    Kataki, Sampriti; Hazarika, Samarendra; Baruah, D C

    2017-07-01

    Success and acceptability of the bio energy conversion technology to a large extent depend upon management of the inevitable by-products generated during the conversion process. By-products can be considered favourable as organic fertilizer as they retain nutrients with varying composition depending upon input biomass. However, characteristics of these heterogeneous resources with respect to feedstock and processing conditions have to be assessed to state on their agricultural and environmental benefits. Therefore, 3 types of anaerobic digestion by-products (digestate) from surplus biomass viz. cow dung, Ipomoea carnea:cow dung (60:40 dry weight basis) and rice straw:green gram stover:cow dung (30:30:40 dry weight basis) and one gasification by-product (biochar) from rice husk are considered to understand the fertilizer prospects. Considering 3 potential application options, digestate from each feedstock option was further processed as separated solid, separated liquid and ash from solid digestates. Thus, a total of 10 by-products were investigated for understanding their prospects as fertilizer using Fourier Transform Infrared Spectroscopy (FTIR), X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Energy Dispersive X ray Spectroscopy (EDX) and phyto-toxicity test to have a broad insight in terms of their organic, mineral, elemental composition, morphological feature and potential phyto-toxicity. In general, irrespective of origin of feedstock, solid digestate, ash digestate and char showed similarity in terms of composition of functional groups with some degree of variation in relative content as reflected by FTIR analysis. Dominance of organic functional groups in separated solid digestates compared to liquid fraction indicated the former as favourable organic amendments. Quartz was the prevalent mineral phase in all separated solid, ash digestate and rice husk char. Digestates in ash phase represent more concentrated plant nutrient source with

  20. Identification of the silver state in the framework of Ag-containing zeolite by XRD, FTIR, photoluminescence, 109Ag NMR, EPR, DR UV-vis, TEM and XPS investigations.

    Science.gov (United States)

    Popovych, Nataliia; Kyriienko, Pavlo; Soloviev, Sergiy; Baran, Rafal; Millot, Yannick; Dzwigaj, Stanislaw

    2016-10-26

    Silver has been identified in the framework of Ag x SiBEA zeolites (where x = 3-6 Ag wt%) by the combined use of XRD, 109 Ag MAS NMR, FTIR, diffuse reflectance UV-visible, EPR and XPS spectroscopy. The incorporation of Ag ions into the framework of SiBEA zeolite has been evidenced by XRD. The consumption of OH groups as a result of their reaction with the silver precursor has been monitored by FTIR and photoluminescence spectroscopy. The changes in the silver state as a function of Ag content and thermal and hydrogen treatment at 573 K have been identified by 109 Ag MAS NMR, EPR, DR UV-visible, TEM and XPS investigations. The acidity of AgSiBEA has been investigated by FTIR spectroscopy of adsorbed CO and pyridine used as probe molecules.

  1. Strain and grain size of TiO2 nanoparticles from TEM, Raman spectroscopy and XRD: The revisiting of the Williamson-Hall plot method

    Science.gov (United States)

    Kibasomba, Pierre M.; Dhlamini, Simon; Maaza, Malik; Liu, Chuan-Pu; Rashad, Mohamed M.; Rayan, Diaa A.; Mwakikunga, Bonex W.

    2018-06-01

    The Williamson-Hall (W-H) equation, which has been used to obtain relative crystallite sizes and strains between samples since 1962, is revisited. A modified W-H equation is derived which takes into account the Scherrer equation, first published in 1918, (which traditionally gives more absolute crystallite size prediction) and strain prediction from Raman spectra. It is found that W-H crystallite sizes are on average 2.11 ± 0.01 times smaller than the sizes from Scherrer equation. Furthermore the strain from the W-H plots when compared to strain obtained from Raman spectral red-shifts yield factors whose values depend on the phases in the materials - whether anatase, rutile or brookite. Two main phases are identified in the annealing temperatures (350 °C-700 °C) chosen herein - anatase and brookite. A transition temperature of 550 °C has been found for nano-TiO2 to irreversibly transform from brookite to anatase by plotting the Raman peak shifts against the annealing temperatures. The W-H underestimation on the strain in the brookite phase gives W-H/Raman factor of 3.10 ± 0.05 whereas for the anatase phase, one gets 2.46 ± 0.03. The new βtot2cos2θ-sinθ plot and when fitted with a polynomial yield less strain but much better matching with experimental TEM crystallite sizes and the agglomerates than both the traditional Williamson-Hall and the Scherrer methods. There is greater improvement in the model when linearized - that is the βtotcos2θ-sinθ plot rather than the βtot2cos2θ-sinθ plot.

  2. XRD, DRS, and SEM stundies of the effects of metal dopants (Pt and Au) on the structural and optical properties of TiO2

    CSIR Research Space (South Africa)

    Moloantoa, JR

    2011-07-01

    Full Text Available Au and Pt doped TiO2 nanocrystlas were prepared using the sol gel method. Diffuse Reflectance Spectroscopy (DRS) was used to study the characteristics of these precious metals and X-ray diffraction (XRD) with calculated lattice parameters was used...

  3. Monolayer to MTS: using SEM, HIM, TEM and SERS to compare morphology, nanosensor uptake and redox potential in MCF7 cells

    Science.gov (United States)

    Jamieson, L. E.; Bell, A. P.; Harrison, D. J.; Campbell, C. J.

    2015-06-01

    Cellular redox potential is important for the control and regulation of a vast number of processes occurring in cells. When the fine redox potential balance within cells is disturbed it can have serious consequences such as the initiation or progression of disease. It is thought that a redox gradient develops in cancer tumours where the peripheral regions are well oxygenated and internal regions, further from vascular blood supply, become starved of oxygen and hypoxic. This makes treatment of these areas more challenging as, for example, radiotherapy relies on the presence of oxygen. Currently techniques for quantitative analysis of redox gradients are limited. Surface enhanced Raman scattering (SERS) nanosensors (NS) have been used to detect redox potential in a quantitative manner in monolayer cultured cells with many advantages over other techniques. This technique has considerable potential for use in multicellular tumour spheroids (MTS) - a three dimensional (3D) cell model which better mimics the tumour environment and gradients that develop. MTS are a more realistic model of the in vivo cellular morphology and environment and are becoming an increasingly popular in vitro model, replacing traditional monolayer culture. Imaging techniques such as transmission electron microscopy (TEM), scanning electron microscopy (SEM) and helium ion microscopy (HIM) were used to investigate differences in morphology and NS uptake in monolayer culture compared to MTS. After confirming NS uptake, the first SERS measurements revealing quantitative information on redox potential in MTS were performed.

  4. Characterization of low alloy ferritic steel–Ni base alloy dissimilar metal weld interface by SPM techniques, SEM/EDS, TEM/EDS and SVET

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Siyan; Ding, Jie; Ming, Hongliang; Zhang, Zhiming; Wang, Jianqiu, E-mail: wangjianqiu@imr.ac.cn

    2015-02-15

    The interface region of welded A508–Alloy 52 M is characterized by scanning probe microscope (SPM) techniques, scanning electron microscopy (SEM)/energy dispersive spectroscopy (EDS), transmission electron microscopy (TEM)/Energy Dispersive Spectroscopy (EDS) and scanning vibrate electrode technique (SVET). The regions along the welded A508–Alloy 52 M interface can be categorized into two types according to their different microstructures. In the type-I interface region, A508 and Alloy 52 M are separated by the fusion boundary, while in the type-II interface region, A508 and Alloy 52 M are separated by a martensite zone. A508, martensite zone and grain boundaries in Alloy 52 M are ferromagnetic while the Alloy 52 M matrix is paramagnetic. The Volta potentials measured by scanning Kelvin probe force microscopy (SKPFM) of A508, martensite zone and Alloy 52 M follow the order: V{sub 52} {sub M} > V{sub A508} > V{sub martensite}. The corrosion behavior of A508–Alloy 52 M interface region is galvanic corrosion, in which Alloy 52 M is cathode while A508 is anode. The martensite dissolves faster than Alloy 52 M, but slower than A508 in the test solution. - Highlights: • The A508–Alloy 52 M interface regions can be categorized into two types. • The chromium depleted region is observed along the Alloy 52 M grain boundary. • The Alloy 52 M grain boundaries which are close to the interface are ferromagnetic. • Martensite zone has lower Volta potential but higher corrosion resistance than A508.

  5. Characterisation of Pb(Mn{sub 1/3}Nb{sub 2/3})O{sub 3} ceramics by SEM, XRD, XPS and dielectric permittivity tests

    Energy Technology Data Exchange (ETDEWEB)

    Molak, A. [Institute of Physics, University of Silesia, Ul. Uniwersytecka 4, PL-40-007 Katowice (Poland)]. E-mail: molak@us.edu.pl; Talik, E. [Institute of Physics, University of Silesia, Ul. Uniwersytecka 4, PL-40-007 Katowice (Poland); Kruczek, M. [Institute of Physics, University of Silesia, Ul. Uniwersytecka 4, PL-40-007 Katowice (Poland); Paluch, M. [Institute of Physics, University of Silesia, Ul. Uniwersytecka 4, PL-40-007 Katowice (Poland); Ratuszna, A. [Institute of Physics, University of Silesia, Ul. Uniwersytecka 4, PL-40-007 Katowice (Poland); Ujma, Z. [Institute of Physics, University of Silesia, Ul. Uniwersytecka 4, PL-40-007 Katowice (Poland)

    2006-03-15

    The Pb(Mn{sub 1/3}Nb{sub 2/3})O{sub 3} ceramics has been obtained from oxides by sintering in air, using a two-stage process with precursor columbite-like (Mn{sub 0.5}Nb)O{sub 3} phase. The PbO oxide was added in the second stage. Analysis of the X-ray diffraction pattern shows that the ceramics consist of 91% of major perovskite phase. A monoclinic distortion of the perovskite structure was found. The cell parameters are a = 12.193(3) A, b = 11.966(6) A, c 12.144(2) A, {beta} = 90{sup o}10.7'. The microanalysis made with SEM exhibited fluctuation in chemical composition of the perovskite phase. Precipitation of MnO{sub 2}, PbO and the Pb-Mn-Nb-O phase different from perovskite was found. The X-ray photoelectron spectroscopy was used to study the electronic structure of the Pb(Mn{sub 1/3}Nb{sub 2/3})O{sub 3} ceramics. The core levels of lead, manganese, niobium and oxygen were measured. The shape of valence band ridge is influenced by Mn 3d states. The real average chemical composition obtained from the XPS measurement is Pb{sub 0.99}(Mn{sub 0.42}Nb{sub 0.67})O{sub 2.92}. Broadband dielectric measurement was carried out in 10{sup -2} to 10{sup 6} Hz and within 80-700 K ranges. The dominant relaxation process exhibits characteristic times typical for ionic processes {tau} {sub 0,H} = 1 x 10{sup -11} s for the higher temperature range and, {tau} {sub 0,L} = 1 x 10{sup -9} s for lower temperatures. The activation energy of relaxation process, E {sub M,H} = 0.43 eV and E {sub M,L} = 0.34 eV corresponds to activation energy of electric conductivity. The dielectric relaxation is ascribed to dipoles created by oxygen vacancies and/or Mn-V {sub O} complexes.

  6. Conservation of Moroccan manuscript papers aged 150, 200 and 800 years. Analysis by infrared spectroscopy (ATR-FTIR), X-ray diffraction (XRD), and scanning electron microscopy energy dispersive spectrometry (SEM-EDS).

    Science.gov (United States)

    Hajji, Latifa; Boukir, Abdellatif; Assouik, Jamal; Lakhiari, Hamid; Kerbal, Abdelali; Doumenq, Pierre; Mille, Gilbert; De Carvalho, Maria Luisa

    2015-02-05

    The preservation of manuscripts and archive materials is a serious problem for librarians and restorers. Paper manuscript is subjected to numerous degradation factors affecting their conservation state. This research represents an attempt to evaluate the conservation restoration process applied in Moroccan libraries, especially the alkaline treatment for strengthening weakened paper. In this study, we focused on six samples of degraded and restored paper taken from three different Moroccan manuscripts aged 150, 200 and 800 years. In addition, the Japanese paper used in restoration has been characterized. A modern paper was also analyzed as reference. A three-step analytical methodology based on infrared spectroscopy (ATR-FTIR), X-ray diffraction (XRD) and scanning electron microscopy coupled to energy dispersive spectrometry (SEM-EDS) analysis was developed before and after restoration in order to determine the effect of the consolidation treatment on the paper structure. The results obtained by XRD and ATR-FTIR disclosed the presence of barium sulfate (BaSO4) in all restored paper manuscripts. The presence of calcium carbonate (CaCO3) in all considered samples was confirmed by FTIR spectroscopy. The application of de-acidification treatment causes significant changes connected with the increase of intensity mostly in the region 1426 cm(-1), assigned to the asymmetric and symmetric CO stretching mode of calcite, indicating the effectiveness of de-acidification procedure proved by the rise of the alkaline reserve content allowing the long term preservation of paper. Observations performed by SEM magnify the typical paper morphology and the structure of fibbers, highlighting the effect of the restoration process, manifested by the reduction of impurities. Copyright © 2014 Elsevier B.V. All rights reserved.

  7. Studies the alterations of biochemical and mineral contents in bone tissue of mus musculus due to aluminum toxicity and the protective action of desferrioxamine and deferiprone by FTIR, ICP-OES, SEM and XRD techniques.

    Science.gov (United States)

    Sivakumar, S; Khatiwada, Chandra Prasad; Sivasubramanian, J

    2014-05-21

    The present study has attempt to analyze the changes in the biochemical and mineral contents of aluminum intoxicated bone and determine the protective action of desferrioxamine (DFO) and deferiprone (DFP) by using Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), inductively coupled plasma optical emission spectroscopy (ICP-OES), and scanning electron microscopy (SEM) techniques for four groups of animals such as control (Group I), aluminum intoxicated (Group II), Al+DFP (Group III) and Al+DFO+DFP (Group IV) treated groups respectively. The FTIR spectra of the aluminum intoxicated bone showed significant alteration in the biochemical constituents. The bands ratio at I1400/I877 significantly decreased from control to aluminum, but enhanced it by Al+DFP to Al+DFO+DFP treated bone tissue for treatments of 16 weeks. This result suggests that DFO and DFP are the carbonate inhibitor, recovered from chronic growth of bone diseases and pathologies. The alteration of proteins profile indicated by Amide I and Amide II, where peak area values decreased from control to aluminum respectively, but enhanced by treated with DFP (p.o.) and DFO+DFP (i.p.) respectively. The XRD analysis showed a decrease in crystallinity due to aluminum toxicity. Further, the Ca, Mg, and P contents of the aluminum exposed bone were less than those of the control group, and enhanced by treatments with DFO and DFP. The concentrations of trace elements were found by ICP-OES. Therefore, present study suggests that due to aluminum toxicity severe loss of bone minerals, decrease in the biochemical constituents and changes in the surface morphology. Copyright © 2014 Elsevier B.V. All rights reserved.

  8. M23C6 carbides and Cr2N nitrides in aged duplex stainless steel: A SEM, TEM and FIB tomography investigation.

    Science.gov (United States)

    Maetz, J-Y; Douillard, T; Cazottes, S; Verdu, C; Kléber, X

    2016-05-01

    The precipitation evolution during ageing of a 2101 lean duplex stainless steel was investigated, revealing that the precipitate type and morphology depends on the nature of the grain boundary. Triangular M23C6 carbides precipitate only at γ/δ interfaces and rod-like Cr2N nitrides precipitate at both γ/δ and δ/δ interfaces. After 15min of ageing, the M23C6 size no longer evolves, whereas that of the Cr2N continues to evolve. For Cr2N, the morphology is maintained at γ/δ interfaces, whereas percolation occurs to form a continuous layer at δ/δ interfaces. By combining 2D and 3D characterisation at the nanoscale using transmission electron microscopy (TEM) and focused ion beam (FIB) tomography, a complete description of the precipitation evolution was obtained, including the composition, crystallographic structure, orientation relationship with the matrix phases, location, morphology, size and volume fraction. Copyright © 2016 Elsevier Ltd. All rights reserved.

  9. SEM and TEM Observation of the Surfaces of the Fine-Grained Particles Retrieved from the Muses-C Regio on the Asteroid 25413 Itokawa

    Science.gov (United States)

    Noguchi, T.; Nakamura, T.; Zolensky, Michael E.; Tanaka, M.; Hashimoto, T.; Konno, M.; Nakato, A.; Ogami, T.; Fujimura, A.; Abe, M.; hide

    2011-01-01

    Surface materials on airless solar system bodies exposed to interplanetary space are gradually changed their visible to near-infrared reflectance spectra by the process called "space weathering", which makes the spectra darker and redder. Hapke et al. proposed a model of space weathering: vapor deposition of nanophase reduced iron (npFe(sup 0)) on the surfaces of the grains within the very surface of lunar regolith. This model has been proved by detailed observation of the surfaces of the lunar soil grains by transmission electron microscope (TEM). They demonstrated that npFe(sup 0) was formed by a combination of vapor deposition and irradiation effects. In other words, both micrometeorite impacts and irradiation by solar wind and galactic cosmic ray play roles on the space weathering on the Moon. Because there is a continuum of reflectance spectra from those of Q-type asteroids (almost the same as those of ordinary chondrites) to those of S-type asteroids, it is strongly suggested that reflectance spectra of asteroids composed of ordinary chondrite-like materials were modified over time to those of S-type asteroids due to space weathering. It is predicted that a small amount of npFe(sup 0) on the surface of grains in the asteroidal regolith composed of ordinary chondrite-like materials is the main agent of asteroidal space weathering.

  10. Kinetic and morphological differentiation of ettringites in plain and blended Portland cements with metakaolin and the ASTM C 452-68 test. Part II: Morphological differentiation by SEM and XRD analysis

    Directory of Open Access Journals (Sweden)

    Talero, R.

    2009-03-01

    Full Text Available The same cementitious materials (OPCs, SRPCs and matekaolin, MK, the same blended cements and the same ASTM C 452-68 test than in Part I, were used. Other complementary determinations were: chemical analysis of cementing materials, SEM and XRD analysis of ettringites and specific properties of some cement tested and of their pastes.The experimental results have also demonstrated that when 7.0% SO3, equivalent to 15.05% of gypsum, was added to the M pozzolan-containing Portland cement and tested with the ASTM C 452-68 method, it was not found to behave aggressively but rather as “setting regulator ”, because the increase in mechanical strengths over time and setting times in these mixes were, therefore, similar to the pattern observed in any PC. However, when the gypsum content was raised to triple than that amount (21.0% SO3, it behaved aggressively. In both cases, logically, ettringite from both origins were involved in the resulting beneficial or adverse behavior.En esta Parte II se utilizaron los mismos materiales cementíceos (CPO, CPRS, y metakaolín, MK, los mismos cementos de mezcla y el mismo método de ensayo ASTM C 452-68 que en la Parte I. Otras determinaciones complementarias fueron: análisis químico de los materiales cementíceos, análisis por DRX y SEM de ettringitas y propiedades específicas de algunos cementos ensayados y de sus pastas.Los resultados experimentales obtenidos han demostrado también que, el 7.0% de SO3 presente en los 30 cementos de mezcla con MK, ensayados conforme el método ASTM C 452-68, no se comporta como agresivo sino como ”regulador de fraguado”, porque los tiempos de fraguado y el aumento de resistencias mecánicas fueron como los de cualquier CP. De aquí que algunos de esos cementos de mezcla puedan ser considerados “cementos hidráulicos expansivos”, el resto, no. Sin embargo, cuando la cantidad de yeso aportada fue el triple (21,0% SO3, se comportó como agresivo, motivo por el cual

  11. The effect of different growth media, carbon source and pgrs on dendrobium broga giant orchid's protocorm-like bodies (plbs) proliferation supported with sem and tem analysis

    International Nuclear Information System (INIS)

    Uddain, J.; Gnasekaran, P.; Zakaria, L.

    2015-01-01

    Dendrobium Broga Giant (Dendrobium Bobby Messina * Dendrobium Superbiens) is a new orchid hybrid in Malaysia. The aim of this study was to investigate the effect of different growth media, carbon sources and PGRs on Dendrobium Broga Giant orchid's protocorm-like bodies (PLBs) proliferation supported with SEM and TEM analysis. The PLBs were cultured on different strength of semi-solid and liquid MS medium and the proliferation rate was recorded based on the fresh weight basis. The maximum PLBs proliferation (12.31% 0.57) was obtained in MS semi-solid medium. PLBs were cultured on MS semi-solid media supplemented with different sucrose concentrations (0, 10, 20, 30 and 40 g L-1). The highest proliferation rate of PLBs (15.48% 1.20) was recorded from MS supplemented with 20 g L-1 sucrose. Different concentrations of BAP (0, 0.5, 1.0, 2.0 mg.L-1) and NAA (0, 0.5, 1.0, 2.0 mgL-1) were added to MS semi-solid medium. Combinations of 1.0 mg L-1 BAP and 0.5 mg.L-1 NAA produced higher PLBs proliferation. Micromorphological studies by SEM and TEM displayed trichome, leaf primordial, stomata, various sizes of mitochondria, vacuoles, different shapes of chloroplast were found in PLBs which ameliorated the slow proliferation nature of plantlets. (author)

  12. Is the TEM obsolescent?

    International Nuclear Information System (INIS)

    Williams, D.B.

    2002-01-01

    Full text: The TEM has undergone many revolutions since its invention 70 years ago, but is now a very mature instrument. The major functions of imaging, diffraction and analysis were invented decades ago. Much of the instrument development in the last 20 years has come in peripheral improvements such as ease of operation and computer control which, nevertheless, have made no substantial differences to basic operational methods. The TEM remains a predominantly manual instrument, still providing analog viewing and recording, well into the digital age. Indeed any operator of a Siemens Elmiskop 1 TEM from the 1950s would be more than skilled enough to operate a modern FEG TEM, with little more than a few minutes of training. It is arguable that no other cutting-edge scientific instrument is so basically unchanged in its method of operation over the last five decades, as the TEM. This state of affairs is a recipe for obsolescence. Students today are not interested in mastering the complexities of balancing potentiometers (which are still necessary for good centered dark-field operation) or manipulating sets of tilt controls to move from to , while fighting to maintain eucentricity and a recognizable image on the screen at 200 kX. Students are already masters of the mouse, keyboard or joystick and expect information to be generated, stored, processed and analyzed rapidly and efficiently under full computer control. We need to provide today's students with an instrument to challenge their skills, not those of their parents. There is nothing preventing the creation of a TEM that is under full computer control, except perhaps the notion that the TEM is an instrument worthy of mastery per se, rather than being simply a tool for the characterization of materials. In contrast, the SEM has never been seen as a 'real' electron microscope and consequently has found its way into many more research, education and commercial operations than the TEM. The SEM has also evolved

  13. XRD and FTIR crystallinity indices in sound human tooth enamel and synthetic hydroxyapatite

    International Nuclear Information System (INIS)

    Reyes-Gasga, José; Martínez-Piñeiro, Esmeralda L.; Rodríguez-Álvarez, Galois; Tiznado-Orozco, Gaby E.; García-García, Ramiro

    2013-01-01

    The crystallinity index (CI) is a measure of the percentage of crystalline material in a given sample and it is also correlated to the degree of order within the crystals. In the literature two ways are reported to measure the CI: X-ray diffraction and infrared spectroscopy. Although the CI determined by these techniques has been adopted in the field of archeology as a structural order measure in the bone with the idea that it can help e.g. in the sequencing of the bones in chronological and/or stratigraphic order, some debate remains about the reliability of the CI values. To investigate similarities and differences between the two techniques, the CI of sound human tooth enamel and synthetic hydroxyapatite (HAP) was measured in this work by X-ray diffraction (XRD) and Fourier Transform Infrared spectroscopy (FTIR), at room temperature and after heat treatment. Although the (CI) XRD index is related to the crystal structure of the samples and the (CI) FTIR index is related to the vibration modes of the molecular bonds, both indices showed similar qualitative behavior for heat-treated samples. At room temperature, the (CI) XRD value indicated that enamel is more crystalline than synthetic HAP, while (CI) FTIR indicated the opposite. Scanning (SEM) and transmission (TEM) images were also used to corroborate the measured CI values. - Highlights: • XRD and FTIR crystallinity indices for tooth enamel and synthetic HAP were obtained. • SEM and TEM images were more correlated with (CI) XRD than with (CI) FTIR . • Regardless of the temperature, (CI) XRD and (CI) FTIR showed similar behavior. • XRD and FTIR crystallinity indices resulted in a fast and qualitative measurement

  14. XRD and FTIR crystallinity indices in sound human tooth enamel and synthetic hydroxyapatite

    Energy Technology Data Exchange (ETDEWEB)

    Reyes-Gasga, José, E-mail: jreyes@fisica.unam.mx [Instituto de Física, UNAM, Circuito de la Investigación Científica s/n., Cd. Universitaria, Coyoacán 04510, México, D.F. (Mexico); Martínez-Piñeiro, Esmeralda L., E-mail: esmemapi@gmail.com [Instituto de Física, UNAM, Circuito de la Investigación Científica s/n., Cd. Universitaria, Coyoacán 04510, México, D.F. (Mexico); Rodríguez-Álvarez, Galois, E-mail: galoisborre@yahoo.com [Instituto de Física, UNAM, Circuito de la Investigación Científica s/n., Cd. Universitaria, Coyoacán 04510, México, D.F. (Mexico); Tiznado-Orozco, Gaby E., E-mail: gab0409@yahoo.com.mx [Unidad Académica de Odontología, Universidad Autónoma de Nayarit, Edificio E7, Ciudad de la Cultura “Amado Nervo”, C.P. 63190 Tepic, Nayarit (Mexico); García-García, Ramiro, E-mail: ramiro@fisica.unam.mx [Instituto de Física, UNAM, Circuito de la Investigación Científica s/n., Cd. Universitaria, Coyoacán 04510, México, D.F. (Mexico); and others

    2013-12-01

    The crystallinity index (CI) is a measure of the percentage of crystalline material in a given sample and it is also correlated to the degree of order within the crystals. In the literature two ways are reported to measure the CI: X-ray diffraction and infrared spectroscopy. Although the CI determined by these techniques has been adopted in the field of archeology as a structural order measure in the bone with the idea that it can help e.g. in the sequencing of the bones in chronological and/or stratigraphic order, some debate remains about the reliability of the CI values. To investigate similarities and differences between the two techniques, the CI of sound human tooth enamel and synthetic hydroxyapatite (HAP) was measured in this work by X-ray diffraction (XRD) and Fourier Transform Infrared spectroscopy (FTIR), at room temperature and after heat treatment. Although the (CI){sub XRD} index is related to the crystal structure of the samples and the (CI){sub FTIR} index is related to the vibration modes of the molecular bonds, both indices showed similar qualitative behavior for heat-treated samples. At room temperature, the (CI){sub XRD} value indicated that enamel is more crystalline than synthetic HAP, while (CI){sub FTIR} indicated the opposite. Scanning (SEM) and transmission (TEM) images were also used to corroborate the measured CI values. - Highlights: • XRD and FTIR crystallinity indices for tooth enamel and synthetic HAP were obtained. • SEM and TEM images were more correlated with (CI){sub XRD} than with (CI){sub FTIR}. • Regardless of the temperature, (CI){sub XRD} and (CI){sub FTIR} showed similar behavior. • XRD and FTIR crystallinity indices resulted in a fast and qualitative measurement.

  15. Combined XRD and XAS

    International Nuclear Information System (INIS)

    Ehrlich, S.N.; Hanson, J.C.; Lopez Camara, A.; Barrio, L.; Estrella, M.; Zhou, G.; Si, R.; Khalid, S.; Wang, Q.

    2011-01-01

    X-ray diffraction (XRD) and X-ray absorption fine structure (XAFS) are complementary techniques for investigating the structure of materials. XRD probes long range order and XAFS probes short range order. We have combined the two techniques at one synchrotron beamline, X18A at the NSLS, allowing samples to be studied in a single experiment. This beamline will allow for coordinated measurements of local and long range structural changes in chemical transformations and phase transitions using both techniques.

  16. A.C. impedance, XRD, DSC, SEM and charge/discharge studies on Al2O3, TiO2, SiO2 dispersoid LiPF6/PVC/PVdF-co-HFP composite polymer electrolytes by phase inversion

    Science.gov (United States)

    Vickraman, P.; Gopukumar, S.

    2017-07-01

    The PVC/PVdF-co-HFP composite polymer electrolyte membranes (CPEMs) by varying blend ratios 1:1, 1:2, and 2:1 with fixed content of Al2O3, TiO2 and SiO2 having soaked in 0.5 M LiPF6 in EC/DEC (1:1) v/v) have been prepared by phase inversion. CPEMs of higher ionic conductivity (not dependent on electrolyte uptake as observed in our study) ASA4 (3.61×10-4 Scm-1), TSA3 (1.53×10-4 Scm-1), and SSA3 (4.81×10-4 Scm-1) have been only chosen for XRD, DSC, SEM and electrochemical studies. In XRD, crystalline peaks (phases) of PVdF have been noted with/without change in intensity as well as FWHM which correspond to type of filler interaction with host matrix. In DSC, it is observed that shifts in baseline, melting endotherms, and area under the endotherms indicating the thermal hist ory of PVC (Tg = 82 ° C) and melting of VdF crystallites varied with nature of the filler dispersoid. In SEM, the coagulated fibrils of the polymer coiled with the sponge like structure has been mapped. The charge/discharge studies are carried out on these CPEMs at C/10 rate in the voltage range 2.8 V - 4.2 V, and it is noted that the TSA3 showed better cycling performance with good capacity retention i.e., 50 cycles with 66% capacity retention than ASA4 of 28 cycles with 65% and SSA3 of 5 cycles with 56%. In the present study Coulombic efficiency is concerned only for first cycle and it is noted that the TSA3 showed 71% than 66% and 62% respectively for SSA3 and ASA4.

  17. Infrared spectra, Raman laser, XRD, DSC/TGA and SEM ...

    Indian Academy of Sciences (India)

    Ga2O3, Se metal, SnO, Sb2O3, HgO and PbCO3 are formed upon the reaction of acetamide aqueous solutions with Ga(NO3)3, SeO2, SnCl2, SbCl3, HgCl2 and Pb(NO3)2, respectively, at 90°C. Different amorphous or crystalline phases can be obtained depending upon the experimental conditions (molar ratios, metal salts ...

  18. SEM Anthology

    Science.gov (United States)

    Rodgers, Michelle; Zimar, Heather

    2004-01-01

    The "SEM Anthology" is a compilation of articles by more than 30 enrollment management professionals from a variety of institutions across the country. This collection, which has appeared in SEM Monthly over the past year, chronicles Strategic Enrollment Management efforts at campuses nationwide. The book illustrates the successes and challenges…

  19. Deposition of ZnSO4 · 3Zn(OH2 · 4H2O films by SILAR method and their study by XRD, SEM and µ-Raman Depósito de películas de ZnSO4 • 3Zn(OH2 • 4H2O por el método SILAR y su estudio por DRX, SEM Y μ-RAMAN

    Directory of Open Access Journals (Sweden)

    F N Jiménez García

    2012-06-01

    Full Text Available ZnSO4 · 3Zn(OH2 · 4H2O(Zinc Sulfate Hidroxide Hidrate films were obtained on glass substrates by SILAR method. It was employed a precursorsolution of ZnSO4 and MnSO4 and water near boiling point complexed with 1 ml of NH4OH as a second solution. Films were treated on air at 300oC by 1 hour. Both films ZnSO4·3Zn(OH2·4H2O as ZnO are important protective against zinc corrosion because they are passive films that give a longer duration to material, it is therefore relevant to study their response to temperature changes. For those reasons films were analyzed before and after thermal treatment to study the structural and morphological changes by X ray diffraction (XRD, Scanning electron microscopy (SEM and Raman Microscopy techniques. It was found before thermal treatment by XRD thepresence of ZnSO4 · 3Zn(OH2 · 4H2O triclinic phase and after such treatment the ZnO hexagonal phase was evidenced. The morphology identified by SEM before thermal treatment was sheets formed by platelet like structure of micrometric size which changes after thermal treatment to a combination ofthose sheets with flowers like structure characteristic of ZnO hexagonal. By µ-Raman the hexagonal ZnO phase before thermal treatment as the triclinicZnSO4 · 3Zn(OH2 · 4H2O phase after thermal treatment were confirmed.One objective of this study was to obtain this protective corrosion material in a controlled manner by techiniques of low cost and high simplicity as Silarmethod. Which, even under temperture increases continue being protective corrosion although suffers phase changes because new phases have protectivecorrosive characteristics too.Se obtuvieron películas de ZnSO4 · 3Zn(OH2 · 4H2O (Zinc Sulfate Hidroxide Hidrate sobre sustratos de vidrio mediante procedimiento SILAR. Se empleó una solución precursora de ZnSO4 y MnSO4 y una segunda solución de agua a ebullición acomplejada con 1 ml de NH4OH. Se realizó tratamiento térmico en aire a 300oC por

  20. Overview - XRF and XRD

    International Nuclear Information System (INIS)

    Jenkins, R.

    1999-01-01

    Full text: While the roots of both X-ray Fluorescence Spectrometry (XRF) and X-ray Powder Diffractometry (XRD) go back 80 years or so, it is only in the last 30 years or so that both techniques have become widely used in the industrial and research environments. It is the experience of the author that all instrumental techniques go through four basic stages: 1. Innovation - someone has a bright idea 2. Application - people start to apply the bright idea 3. Frustration - the bright idea is found to have complications 4. Consolidation - the complications are understood and resolved. XRF went through these four stages by the mid 1980s. This means that, today, if one understands what one is doing, applies the correct (and generally well known) analytical strategy, there is a high probability that one will obtain the correct result. XRD, on the other hand, is still hovering between 3 and 4 on the list. Problems such as the effect of preferred orientation on intensities, difficulties in obtaining accurate data for larger d-spacings, etc., although better understood today, still pose significant challenges to those involved in both routine and research analysis. The development of low-cost computers has made a dramatic impact in both techniques and it is estimated that today, about 90% of all new spectrometer and diffractometer systems sold, are fully automated. There are about 30,000 X-ray spectrometers and about 25,000 diffractometers in use in the world today. Of these about one half are automated. The process of automation has brought its rewards as well as its consequences. In general, the automation of the two techniques has resulted in a poorer understanding of the instrumentation and methodology, on the part of the typical user. Many laboratories employ both techniques, since they are largely complimentary. This workshop will cover the basics of the two methods, highlighting the advantages and shortcomings of both. Copyright (1999) Australian X-ray Analytical

  1. Surface characterization of cottonseed meal products by SEM, SEM-EDS, XRD and XPS analysis

    Science.gov (United States)

    The utilization of cottonseed meal as a valuable industrial feedstock needs to be exploited. We have recently produced water-washed cottonseed meal, total cottonseed protein, sequentially extracted water- and alkali-soluble proteins, and two residues after the total and sequential protein extraction...

  2. XRD and FTIR crystallinity indices in sound human tooth enamel and synthetic hydroxyapatite.

    Science.gov (United States)

    Reyes-Gasga, José; Martínez-Piñeiro, Esmeralda L; Rodríguez-Álvarez, Galois; Tiznado-Orozco, Gaby E; García-García, Ramiro; Brès, Etienne F

    2013-12-01

    The crystallinity index (CI) is a measure of the percentage of crystalline material in a given sample and it is also correlated to the degree of order within the crystals. In the literature two ways are reported to measure the CI: X-ray diffraction and infrared spectroscopy. Although the CI determined by these techniques has been adopted in the field of archeology as a structural order measure in the bone with the idea that it can help e.g. in the sequencing of the bones in chronological and/or stratigraphic order, some debate remains about the reliability of the CI values. To investigate similarities and differences between the two techniques, the CI of sound human tooth enamel and synthetic hydroxyapatite (HAP) was measured in this work by X-ray diffraction (XRD) and Fourier Transform Infrared spectroscopy (FTIR), at room temperature and after heat treatment. Although the (CI)XRD index is related to the crystal structure of the samples and the (CI)FTIR index is related to the vibration modes of the molecular bonds, both indices showed similar qualitative behavior for heat-treated samples. At room temperature, the (CI)XRD value indicated that enamel is more crystalline than synthetic HAP, while (CI)FTIR indicated the opposite. Scanning (SEM) and transmission (TEM) images were also used to corroborate the measured CI values. © 2013.

  3. The luminal surface of thyroid cysts in SEM

    DEFF Research Database (Denmark)

    Zelander, T; Kirkeby, S

    1978-01-01

    Four of the five kinds of cells constituting the walls of thyroid cysts can be identified in the SEM. These are cuboidal cells, mucous cells, cells with large granules and ciliated cells. A correlation between SEM and TEM observations is attempted.......Four of the five kinds of cells constituting the walls of thyroid cysts can be identified in the SEM. These are cuboidal cells, mucous cells, cells with large granules and ciliated cells. A correlation between SEM and TEM observations is attempted....

  4. XRD alignment, calibration and performance

    International Nuclear Information System (INIS)

    Davy, L.

    2002-01-01

    Full text: The quality of any diffractometer system is very much dependent on the alignment, calibration and performance. The three subjects are very much related. Firstly, you must know how to carry out the full diffractometer alignment. XRD alignment is easy once you know how. The presentation will show you step by step to carry out the full alignment. Secondly, you need to know how to calibrate the diffractometer system. The presentation will show you how to calibrate the goniometer, detector etc. Thirdly, to prove the system is working within the manufacturer specification. The presentation will show you how to carry out the resolution, reproducibility and linearity test. Copyright (2002) Australian X-ray Analytical Association Inc

  5. Quantitative XRD analysis of {110} twin density in biotic aragonites.

    Science.gov (United States)

    Suzuki, Michio; Kim, Hyejin; Mukai, Hiroki; Nagasawa, Hiromichi; Kogure, Toshihiro

    2012-12-01

    {110} Twin densities in biotic aragonite have been estimated quantitatively from the peak widths of specific reflections in powder X-ray diffraction (XRD) patterns, as well as direct confirmation of the twins using transmission electron microscopy (TEM). Influence of the twin density on the peak widths in the XRD pattern was simulated using DIFFaX program, regarding (110) twin as interstratification of two types of aragonite unit layers with mirrored relationship. The simulation suggested that the twin density can be estimated from the difference of the peak widths between 111 and 021, or between 221 and 211 reflections. Biotic aragonite in the crossed-lamellar microstructure (three species) and nacreous microstructure (four species) of molluscan shells, fish otoliths (two species), and a coral were investigated. The XRD analyses indicated that aragonite crystals in the crossed-lamellar microstructure of the three species contain high density of the twins, which is consistent with the TEM examination. On the other hand, aragonite in the nacre of the four species showed almost no difference of the peak widths between the paired reflections, indicating low twin densities. The results for the fish otoliths were varied between the species. Such variation of the twin density in biotic aragonites may reflect different schemes of crystal growth in biomineralization. Copyright © 2012 Elsevier Inc. All rights reserved.

  6. Ao leitor sem medo

    Directory of Open Access Journals (Sweden)

    José Eisenberg

    2000-05-01

    Full Text Available O texto resenha Ao leitor sem medo, de Renato Janine Ribeiro (Belo Horizonte, UFMG, 1999.This text is a review of Ao leitor sem medo by Renato Janine Ribeiro (Belo Horizonte, UFMG, 1999

  7. Stereoscopic methods in TEM

    International Nuclear Information System (INIS)

    Thomas, L.E.

    1975-07-01

    Stereoscopic methods used in TEM are reviewed. The use of stereoscopy to characterize three-dimensional structures observed by TEM has become widespread since the introduction of instruments operating at 1 MV. In its emphasis on whole structures and thick specimens this approach differs significantly from conventional methods of microstructural analysis based on three-dimensional image reconstruction from a number of thin-section views. The great advantage of stereo derives from the ability to directly perceive and measure structures in three-dimensions by capitalizing on the unsurpassed human ability for stereoscopic matching of corresponding details on picture pairs showing the same features from different viewpoints. At this time, stereo methods are aimed mainly at structural understanding at the level of dislocations, precipitates, and irradiation-induced point-defect clusters in crystal and on the cellular irradiation-induced point-defect clusters in crystal and on the cellular level of biological specimens. 3-d reconstruction methods have concentrated on the molecular level where image resolution requirements dictate the use of very thin specimens. One recent application of three-dimensional coordinate measurements is a system developed for analyzing depth variations in the numbers, sizes and total volumes of voids produced near the surfaces of metal specimens during energetic ion bombardment. This system was used to correlate the void volumes at each depth along the ion range with the number of atomic displacements produced at that depth, thereby unfolding the entire swelling versus dose relationship from a single stereo view. A later version of this system incorporating computer-controlled stereo display capabilities is now being built

  8. In Situ TEM Electrical Measurements

    DEFF Research Database (Denmark)

    Canepa, Silvia; Alam, Sardar Bilal; Ngo, Duc-The

    2016-01-01

    understanding of complex physical and chemical interactions in the pursuit to optimize nanostructure function and device performance. Recent developments of sample holder technology for TEM have enabled a new field of research in the study of functional nanomaterials and devices via electrical stimulation...... influence the sample by external stimuli, e.g. through electrical connections, the TEM becomes a powerful laboratory for performing quantitative real time in situ experiments. Such TEM setups enable the characterization of nanostructures and nanodevices under working conditions, thereby providing a deeper...... and measurement of the specimen. Recognizing the benefits of electrical measurements for in situ TEM, many research groups have focused their effort in this field and some of these methods have transferred to ETEM. This chapter will describe recent advances in the in situ TEM investigation of nanostructured...

  9. Advanced SEM imaging

    International Nuclear Information System (INIS)

    Joy, D. C.; Newbury, D. E.

    1998-01-01

    The scanning electron microscope (SEM) represents the most promising tool for metrology, defect review, and for the analysis of ULSI structures, but both fundamental problems such as electron-solid interactions, and practical considerations such as electron-optical constraints, are now setting a limit to performance. This paper examines the directions in which an advanced SEM might be developed to overcome these constraints. The SEM also offers considerable promise as a tool for the high spatial resolution X-ray microanalysis, especially for those situations where a thin cross-section is not practical and first surface analysis is required. The ways in which this capability can be incorporated in an advanced SEM are examined

  10. Advanced SEM imaging

    International Nuclear Information System (INIS)

    Joy, D.C.; Newbury, D.E.; Newbury, D.E.

    1998-01-01

    The scanning electron microscope (SEM) represents the most promising tool for metrology, defect review, and for the analysis of ULSI structures, but both fundamental problems such as electron-solid interactions, and practical considerations such as electron-optical constraints, are now setting a limit to performance. This paper examines the directions in which an advanced SEM might be developed to overcome these constraints. The SEM also offers considerable promise as a tool for the high spatial resolution X-ray microanalysis, especially for those situations where a thin cross-section is not practical and first surface analysis is required. The ways in which this capability can be incorporated in an advanced SEM are examined. copyright 1998 American Institute of Physics

  11. Shocked quartz in the SEM: Distinction between amorphous and healed PDFs

    NARCIS (Netherlands)

    Hamers, M.F.; Pennock, G.M.; Drury, M.R.

    2012-01-01

    Combined SEM techniques show that different CL signatures of PDFs are related to fresh and healed microstructures of PDFs and host quartz. This is confirmed by TEM results. A combination of SEM techniques can give the same type of information as TEM

  12. Spin-polarized SEM

    International Nuclear Information System (INIS)

    Konoto, Makoto

    2007-01-01

    Development of highly effective evaluation technology of magnetic structures on a nanometric scale is a key to understanding spintronics and related phenomena. A high-resolution spin-polarized scanning electron microscope (spin SEM) developed recently is quite suitable for probing such nanostructures because of the capability of analyzing local magnetization vectors in three dimensions. Utilizing the spin SEM, a layered antiferromagnetic structure with the 1nm-alternation of bilayer-sheet magnetization has been successfully resolved. The real-space imaging with full analysis of the temperature-dependent magnetization vectors will be demonstrated. (author)

  13. SEM microcharacterization of semiconductors

    CERN Document Server

    Holt, D B

    1989-01-01

    Applications of SEM techniques of microcharacterization have proliferated to cover every type of material and virtually every branch of science and technology. This book emphasizes the fundamental physical principles. The first section deals with the foundation of microcharacterization in electron beam instruments and the second deals with the interpretation of the information obtained in the main operating modes of a scanning electron microscope.

  14. TEM turbulence optimisation in stellarators

    Science.gov (United States)

    Proll, J. H. E.; Mynick, H. E.; Xanthopoulos, P.; Lazerson, S. A.; Faber, B. J.

    2016-01-01

    With the advent of neoclassically optimised stellarators, optimising stellarators for turbulent transport is an important next step. The reduction of ion-temperature-gradient-driven turbulence has been achieved via shaping of the magnetic field, and the reduction of trapped-electron mode (TEM) turbulence is addressed in the present paper. Recent analytical and numerical findings suggest TEMs are stabilised when a large fraction of trapped particles experiences favourable bounce-averaged curvature. This is the case for example in Wendelstein 7-X (Beidler et al 1990 Fusion Technol. 17 148) and other Helias-type stellarators. Using this knowledge, a proxy function was designed to estimate the TEM dynamics, allowing optimal configurations for TEM stability to be determined with the STELLOPT (Spong et al 2001 Nucl. Fusion 41 711) code without extensive turbulence simulations. A first proof-of-principle optimised equilibrium stemming from the TEM-dominated stellarator experiment HSX (Anderson et al 1995 Fusion Technol. 27 273) is presented for which a reduction of the linear growth rates is achieved over a broad range of the operational parameter space. As an important consequence of this property, the turbulent heat flux levels are reduced compared with the initial configuration.

  15. A TEM Study on the Ti-Alloyed Grey Iron

    DEFF Research Database (Denmark)

    Moumeni, Elham; Tiedje, Niels Skat; Grumsen, Flemming Bjerg

    2014-01-01

    The microstructure of graphite flakes in titanium alloyed cast iron is studied using electron microscopy techniques. Dual beam SEM/FIB has been used for TEM sample preparation. A TEM study has been carried out on graphite flakes in grey cast iron using selected area electron diffraction. Based...... and that there is a high proportion of twins in the fine grained graphite. It appears that twinning and stacking faults are involved in the fine grained structure of the graphite. It is discussed how Ti addition affect crystal growth and may lead to formation of superfine graphite....

  16. Space Experiment Module (SEM)

    Science.gov (United States)

    Brodell, Charles L.

    1999-01-01

    The Space Experiment Module (SEM) Program is an education initiative sponsored by the National Aeronautics and Space Administration (NASA) Shuttle Small Payloads Project. The program provides nationwide educational access to space for Kindergarten through University level students. The SEM program focuses on the science of zero-gravity and microgravity. Within the program, NASA provides small containers or "modules" for students to fly experiments on the Space Shuttle. The experiments are created, designed, built, and implemented by students with teacher and/or mentor guidance. Student experiment modules are flown in a "carrier" which resides in the cargo bay of the Space Shuttle. The carrier supplies power to, and the means to control and collect data from each experiment.

  17. O Cinema sem Imagens

    Directory of Open Access Journals (Sweden)

    Paulo Andrade

    2001-12-01

    Full Text Available A obra cinematográfica de Marguerite Duras, praticamente desconhecida pelo grande público, estabeleça intricadas relações com sua obra literária, ao promover a indiscernibilidade entre os dois campo, sem, contudo, instituir qualquer tipo de subordinação de um ao outro. O processo de criação do filme Lê camion, de 1977, aponta para outras possibilidades de se pensar o cinema e a literatura.

  18. Evaluation of dislocation density in copper and brass α deformed by XRD peak width analysis

    International Nuclear Information System (INIS)

    Sousa, Talita Gama de

    2014-01-01

    The determination of dislocation density in metallic materials has been available for many years in scientific environment. This is due to the fact that the dislocations are the main responsible for plastic deformation, which, thereafter, markedly influences the mechanical properties. In this work, the dislocation density was analyzed through peak broadening of Xray diffraction (XRD) using Convolutional Multiple Whole Profile (CMWP) program. The measurements obtained by XRD were compared with those obtained from images observed by transmission electronic microscopy (TEM). The materials used in this study were pure copper and brass α as alloy 268 (6 % Cu and 34 % Zn), deformed by rolling and ECA (equal channel angular extrusion) processes. The results indicate that the XRD is a powerful tool for the characterization of the microstructure in relation to the dislocation density, as they were consistent to the TEM measurements, and also showed good relationship with measurements of hardness. Furthermore, through the dislocation density it was possible to verify the influence of stacking fault energy (SFE) in the evolution of the copper samples deformation process and its alloy, and that the presence of texture in rolled samples did not impair the measurements obtained by XRD technique. (author)

  19. Characterization of inorganic atmospheric particles in air quality program with SEM, TEM and XAS

    International Nuclear Information System (INIS)

    Ramirez L, R.; Esparza P, H.; Duarte M, A.

    2007-01-01

    Physical and chemical characterization of inorganic atmospheric particle samples collected on TSP and PM10 filters from January 2003 through December 2005 from three zones within the city of Hermosillo, Sonora; using Transmission Electron Microscopy, Scanning combined with EDS and Stanford University's Synchrotron X-Ray. The sample preparation for electron microscopy was deposited as an alcohol suspension using a sample holder. The different elements found amongst individual particles were Al, Ba, Bi, Br, Ca, Ce, Cl, Cr, Cu, Fe, K, La, Mn, Mg, Na, P, Pb, S, Si, Ti, U, V, W, Zn and Zr. These particles' morphology and chemical composition, illustrate an abundance of natural elements within the zone. However some of the elements present are directly related with human activities, and are of much interest from the public health and environmental perspectives. (Author)

  20. Microchip systems for imaging liquid and high temperature processes in TEM & SEM

    DEFF Research Database (Denmark)

    Jensen, Eric; Canepa, Silvia; Møller-Nilsen, Rolf Erling Robberstad

    2014-01-01

    Microchips systems have found their way into electron microscopes in order to make miniatureplatforms for controlled liquid and gaseous environments that also begin to include electricalcontacts and other types of interactions with the sample, such as application of forces andirradiation with light.......This presentation will explain the different types of microchip systems and give examples of someof the results we have achieved with our devices and examples of how such devices can be usedfor research related to energy storage and conversion.Heaters can be made in several ways, and monocrystalline silicon......]. Both systems will allowhigh resolution imaging of heterogeneous electrochemical processes such as those in batteries.Based on the suspended microfluidic channels, we are also developing microchips that enableultrafast freezing of processes in liquids....

  1. Antimicrobial Potential and Chemical Characterization of Serbian Liverwort (Porella arboris-vitae: SEM and TEM Observations

    Directory of Open Access Journals (Sweden)

    Amit Kumar Tyagi

    2013-01-01

    Full Text Available The chemical composition of Porella arboris-vitae extracts was determined by solid phase microextraction, gas chromatography-mass spectrometry (SPME GC-MS, and 66 constituents were identified. The dominant compounds in methanol extract of P. arboris-vitae were β-caryophyllene (14.7%, α-gurjunene (10.9%, α-selinene (10.8%, β-elemene (5.6%, γ-muurolene (4.6%, and allo-aromadendrene (4.3% and in ethanol extract, β-caryophyllene (11.8%, α-selinene (9.6%, α-gurjunene (9.4%, isopentyl alcohol (8.8%, 2-hexanol (3.7%, β-elemene (3.7%, allo-aromadendrene (3.7%, and γ-muurolene (3.3% were the major components. In ethyl acetate extract of P. arboris-vitae, undecane (11.3%, β-caryophyllene (8.4%, dodecane (6.4%, α-gurjunene (6%, 2-methyldecane (5.1%, hemimellitene (4.9%, and D-limonene (3.9% were major components. The antimicrobial activity of different P. arboris-vitae extracts was evaluated against selected food spoilage microorganisms using microbroth dilution method. The Minimal Inhibitory Concentration (MIC varied from 0.5 to 1.5 mg/mL and 1.25 to 2 mg/mL for yeast and bacterial strains, respectively. Significant morphological and ultrastructural alterations due to the effect of methanolic and ethanolic P. arboris-vitae extracts on S. Enteritidis have also been observed by scanning electron microscope and transmission electron microscope, respectively. The results provide the evidence of antimicrobial potential of P. arboris-vitae extracts and suggest its potential as natural antimicrobial agents for food preservation.

  2. SEM analysis for irradiated materials

    International Nuclear Information System (INIS)

    Liu Xiaosong; Yao Liang

    2008-06-01

    A radiation-proof Scanning Electron Microscope (SEM) system is introduced. It has been widely used in various areas. For analyzing radioactive samples, normal SEM system needs lots of alterations. Based on KYKY-2800B SEM, the sample room, belt line, operating table and aerator were updated. New radiation-proof SEM system has used to analytic surface contaminated samples and RPV materials samples. An elementary means of SEM analysis for radioactive samples was studied, and this examination supported some available references for further irradiated fuel researches. (authors)

  3. Chemical Species, Micromorphology, and XRD Fingerprint Analysis of Tibetan Medicine Zuotai Containing Mercury.

    Science.gov (United States)

    Li, Cen; Yang, Hongxia; Du, Yuzhi; Xiao, Yuancan; Zhandui; Sanglao; Wang, Zhang; Ladan, Duojie; Bi, Hongtao; Wei, Lixin

    2016-01-01

    Zuotai ( gTso thal ) is one of the famous drugs containing mercury in Tibetan medicine. However, little is known about the chemical substance basis of its pharmacodynamics and the intrinsic link of different samples sources so far. Given this, energy dispersive spectrometry of X-ray (EDX), scanning electron microscopy (SEM), atomic force microscopy (AFM), and powder X-ray diffraction (XRD) were used to assay the elements, micromorphology, and phase composition of nine Zuotai samples from different regions, respectively; the XRD fingerprint features of Zuotai were analyzed by multivariate statistical analysis. EDX result shows that Zuotai contains Hg, S, O, Fe, Al, Cu, and other elements. SEM and AFM observations suggest that Zuotai is a kind of ancient nanodrug. Its particles are mainly in the range of 100-800 nm, which commonly further aggregate into 1-30  μ m loosely amorphous particles. XRD test shows that β -HgS, S 8 , and α -HgS are its main phase compositions. XRD fingerprint analysis indicates that the similarity degrees of nine samples are very high, and the results of multivariate statistical analysis are broadly consistent with sample sources. The present research has revealed the physicochemical characteristics of Zuotai , and it would play a positive role in interpreting this mysterious Tibetan drug.

  4. Application of TEM to highly reactive metals

    International Nuclear Information System (INIS)

    Sherry, W.M.; Prinz, F.

    1982-01-01

    In the following a method for the preparation and observation of sodium TEM specimens and the first TEM micrograph ever to be published on the dislocation microstructure of sodium are reported. (orig./IHOE) [de

  5. Characterization of uranium silicide powder using XRD

    International Nuclear Information System (INIS)

    Garcia, Rafael H.L.; Saliba-Silva, Adonis M.; Carvalho, Elita F.U.; Lima, Nelson B.; Ichikawa, Rodrigo U.; Martinez, Luiz G.

    2013-01-01

    Uranium silicide (U 3 Si 2 ) is an intermetallic used as nuclear fuel in most modern MTR - Materials Test Reactor. Dispersed in aluminum, this fuel allows high uranium densities, up to 4.8 gU/cm 3 . At IPEN, the fabrication of fuel elements based on U 3 Si 2 for the IEA-R1 reactor is carried out in the Nuclear Fuel Center (CCN), by vacuum induction melting of uranium and silicon, followed by grinding. Before employed in a nuclear reactor, U 3 Si 2 must be submitted to a strict quality control, which includes granulometry, density, X-ray radiography for dispersion homogeneity, chemical and crystallographic characterization. Concerning phase composition for a qualified fuel, the fraction of U 3 Si 2 should be higher than 80wt.%. Aiming at the development of a routine methodology for quantification of phases via analysis of XRD data using the Rietved method, six samples from two production baths of CCN were submitted to X-ray diffraction. The data were analyzed using software GSAS and line profile analysis methods. The results suggest that fusion product have preferred orientation and grinding step is important for a better refinement. (author)

  6. Investigations into the Surface Strain/Stress State in a Single-Crystal Superalloy via XRD Characterization

    Directory of Open Access Journals (Sweden)

    Haodong Duan

    2018-05-01

    Full Text Available The present study was aimed at determining the surface strain/stress state in an Ni-based single-crystal (SC superalloy that was subjected to two different cooling rates from solid solution temperature through using the X-ray diffraction (XRD method. The normal stresses σ 11 s and σ 22 s were determined, then the Von Mises stresses ( σ V M s were derived from them. Field emission gun scanning electron microscope (FEG-SEM and transmission electron microscope (TEM micrographs were taken to illustrate the strain/stress state change. The precipitation of the secondary γ′ phases in the γ phase and the formation of the dislocation in the interphase upon a slower cooling rate caused the γ phase lattice distortion to increase, so a larger σ V M s of the γ phase was realized in comparison to the faster cooling sample. For both of the two cooling modes, we found that the σ V M s of the γ′ phase increased due to the growth of the γ′ phase during the aging process. Also, the aging process led to pronouncedly anisotropic lattice mismatches in the {331} and {004} planes. In addition, the surface strain/stress states of a cylinder sample and a tetragonal sample were also studied using a faster cooling rate, and σ 11 s and σ 22 s were analyzed to explain the influence of the shape factor on the stress anisotropy in the [001] and [ 1 1 ¯ 0 ] orientations. The strain in the [001] orientation of the γ phase is more sensitive to the shape change.

  7. Applications of the rotating orientation XRD method to oriented materials

    International Nuclear Information System (INIS)

    Guo Zhenqi; Li Fei; Jin Li; Bai Yu

    2009-01-01

    The rotating orientation x-ray diffraction (RO-XRD) method, based on conventional XRD instruments by a modification of the sample stage, was introduced to investigate the orientation-related issues of such materials. In this paper, we show its applications including the determination of single crystal orientation, assistance in crystal cutting and evaluation of crystal quality. The interpretation of scanning patterns by RO-XRD on polycrystals with large grains, bulk material with several grains and oriented thin film is also presented. These results will hopefully expand the applications of the RO-XRD method and also benefit the conventional XRD techniques. (fast track communication)

  8. Phase analysis of nano-phase materials using selected area electron diffraction in the TEM

    International Nuclear Information System (INIS)

    Labar, J. L.

    2002-01-01

    In analogy to X-ray power diffraction (XRD), we are developing a method to help phase identification when examining a large number of grains simultaneously by electron diffraction. Although XRD is well established, it can not be used for small quantities of materials (volumes below 1 mm 3 ). Examining a usual TEM sample with thickness of 100 nm and using a selected area of 1 mm in diameter, the selected area electron diffraction pattern (SAED) carries information about several thousands of grains from a material with an average grain size of about 10 nm. The accuracy of XRD can not be attained by electron diffraction (ED). However, simultaneous visual observation of the nanostructure is an additional benefit of TEM (beside the small amount of needed material). The first step of the development project was the development of a computer program ('ProcessDiffraction') that processes digital versions of SAED patterns and presents them in an XRD-like form (intensity vs. scattering vector). In the present version (V2.0.3) phase identification is carried out by comparing the measured distribution to 'Markers', i.e. data of known phases. XRD data cards are used if the detailed structure of a phase is not known. Kinematic electron diffraction intensities are calculated for phases with known atomic positions (Author)

  9. Characterization of materials used in the execution of historic oil paintings by XRD, SEM-EDS, TGA and LIBS analysis

    OpenAIRE

    Şerifaki, Kerem; Böke, Hasan; Yalçın, Şerife; İpekoğlu, Başak

    2009-01-01

    In this study, material characteristics of historic oil paintings in a 19th century church in Ayvali{dotless}k/Turkey were investigated to propose the treatments to be used in their conservation and protection. For this purpose, physical, chemical and mineralogical compositions and the microstructure of the paintings were determined by X-ray Diffraction, Scanning Electron Microscope, Thermo Gravimetric Analyzer, Differential Scanning Calorimeter, Infrared Spectroscopy and Laser Induced Breakd...

  10. Microstructural characterization of archaeological materials from the Chapatongo-Los Cerritos, Tula, Hidalgo site through Sem and XRD

    International Nuclear Information System (INIS)

    Rodriguez L, V.; Espinosa P, M.; Fournier, P.

    2004-01-01

    In one of the main epiclase s establishments of the region of Tula, they have been carried out extensive excavations recently in several sectors. Among the funeral offerings, as well as among the waste materials and recovered in architectural fillers of the place of Chapatongo-Los Cerritos. Diverse stony materials are included stone-beads fundamentally; and they were characterized through Scanning Electron Microscopy (MEB), Energy Dispersive X-ray Spectroscopy (EDS) and X-ray Diffraction (DRX). Morphologies with habits were identified as grooved with great ruggedness that present particles like inclusions of metallic oxides, surfaces with great porosity, lamellar structures, agglomerates, fibers of great extension. Likewise the constituent crystalline phases of the samples were identified: calcite, aragonite, calcium and potassium aluminosilicates, microcline and quartz. In the case of the crystalline phases like omphacite, nacrite and dickite are characteristic of the green stone-beads, these belong to the family of the jadeite phase, considered as precious materials in the pre hispanic world. (Author) 20 refs., 20 tabs., 23 figs

  11. Two novel approaches to study arthropod anatomy by using dualbeam FIB/SEM.

    Science.gov (United States)

    Di Giulio, Andrea; Muzzi, Maurizio

    2018-03-01

    Transmission Electron Microscopy (TEM) has always been the conventional method to study arthropod ultrastructure, while the use of Scanning Electron Microscopy (SEM) was mainly devoted to the examination of the external cuticular structures by secondary electrons. The new generation field emission SEMs are capable to generate images at sub-cellular level, comparable to TEM images employing backscattered electrons. The potential of this kind of acquisition becomes very powerful in the dual beam FIB/SEM where the SEM column is combined with a Focused Ion Beam (FIB) column. FIB uses ions as a nano-scalpel to slice samples fixed and embedded in resin, replacing traditional ultramicrotomy. We here present two novel methods, which optimize the use of FIB/SEM for studying arthropod anatomy. Copyright © 2017 Elsevier Ltd. All rights reserved.

  12. Composition and microstructure of MTA and Aureoseal Plus: XRF, EDS, XRD and FESEM evaluation.

    Science.gov (United States)

    Cianconi, L; Palopoli, P; Campanella, V; Mancini, M

    2016-12-01

    The aim of this study was to determine the chemical composition and the phases' microstructure of Aureoseal Plus (OGNA, Italy) and ProRoot MTA (Dentsply Tulsa Dental, USA) and to compare their characteristics. Study Design: Comparing Aureoseal Plus and ProRoot MTA microstructure by means of several analyses type. The chemical analysis of the two cements was assessed following the UNI EN ISO 196-2 norm. X-Ray fluorescence (XRF) was used to determine the element composition. The crystalline structure was analysed quantitatively using x-ray diffraction (XRD). Powders morphology was evaluated using a scanning electron microscope (SEM) with backscattering detectors, and a field emission scanning electron microscope (FESEM). Elemental analysis was performed by energy dispersive x-ray analysis (EDS). The semi-quantitative XRF analysis showed the presence of heavy metal oxides in both cements. The XRD spectra of the two cements reported the presence of dicalcium silicate, tricalcium silicate, tricalcium aluminate, tetracalcium aluminoferrite, bismuth oxide and gypsum. SEM analysis showed that ProRoot MTA powder is less coarse and more homogeneous than Aureoseal. Both powders are formed by particles of different shapes: round, prismatic and oblong. The EDS analysis showed that some ProRoot MTA particles, differently from Aureoseal, contain Ca, Si, Al and Fe. Oblong particles in ProRoot and Aureoseal are rich of bismuth. The strong interest in developing new Portland cement-based endodontic sealers will create materials with increased handling characteristics and physicochemical properties. A thorough investigation on two cement powders was carried out by using XRF, XRD, SEM and EDS analysis. To date there was a lack of studies on Aureoseal Plus. This cement is similar in composition to ProRoot MTA. Despite that it has distinctive elements that could improve its characteristics, resulting in a good alternative to MTA.

  13. Global gyrokinetic simulations of TEM microturbulence

    Science.gov (United States)

    Vernay, T.; Brunner, S.; Villard, L.; McMillan, B. F.; Jolliet, S.; Bottino, A.; Görler, T.; Jenko, F.

    2013-07-01

    Global gyrokinetic simulations of electrostatic temperature-gradient-driven trapped-electron-mode (TEM) turbulence using the δf particle-in-cell code ORB5 are presented. The electron response is either fully kinetic or hybrid, i.e. considering kinetic trapped and adiabatic passing electrons. A linear benchmark in the TEM regime against the Eulerian-based code GENE is presented. Two different methods for controlling the numerical noise, based, respectively, on a Krook operator and a so-called coarse-graining approach, are discussed and successfully compared. Both linear and non-linear studies are carried out for addressing the issue of finite-ρ*-effects and finite electron collisionality on TEM turbulence. Electron collisions are found to damp TEMs through the detrapping process, while finite-ρ*-effects turn out to be important in the non-linear regime but very small in the linear regime. Finally, the effects of zonal flows on TEM turbulence are briefly considered as well and shown to be unimportant in the temperature-gradient-driven TEM regime. Consistently, basically no difference is found between linear and non-linear critical electron temperature gradients in the TEM regime.

  14. TEMS: results of a specialist centre.

    Science.gov (United States)

    Flexer, S M; Durham-Hall, A C; Steward, M A; Robinson, J M

    2014-06-01

    Transanal endoscopic microsurgery (TEMS) is becoming more widespread due to the increasing body of evidence to support its role. Previous published data has reported recurrence rates in excess of 10% for benign polyps after TEMS. Bradford Royal Infirmary is a tertiary referral centre for TEMS and early rectal cancer in the UK. Data for all TEMS operations were entered into a prospective database over a 7-year period. Demographic data, complications and recurrence rates were recorded. Both benign adenomas and malignant lesions were included. A total of 164 patients (65% male), with a mean age of 68 years were included; 114 (70%) of the lesions resected were benign adenomas, and 50 (30%) were malignant lesions. Median polyp size was 4 (range 0.6-14.5) cm. Mean length of operation was 55 (range 10-120) min. There were no recurrences in any patients with a benign adenoma resected; two patients with malignant lesions developed recurrences. Three intra-operative complications were recorded, two rectal perforations (repaired primarily, one requiring defunctioning stoma), and a further patient suffered a blood loss of >300 ml requiring transfusion. Six patients developed strictures requiring dilation either endoscopically or under anaesthetic in the post-operative period. We have demonstrated that TEMS procedures performed in a specialist centre provide low rates of both recurrence and complication. Within a specialist centre, TEMS surgery should be offered to all patients for rectal lesions, both benign and malignant, that are amenable to TEMS.

  15. Secondary emission monitor (SEM) grids.

    CERN Multimedia

    Patrice Loïez

    2002-01-01

    A great variety of Secondary Emission Monitors (SEM) are used all over the PS Complex. At other accelerators they are also called wire-grids, harps, etc. They are used to measure beam density profiles (from which beam size and emittance can be derived) in single-pass locations (not on circulating beams). Top left: two individual wire-planes. Top right: a combination of a horizontal and a vertical wire plane. Bottom left: a ribbon grid in its frame, with connecting wires. Bottom right: a SEM-grid with its insertion/retraction mechanism.

  16. SEM: A Cultural Change Agent

    Science.gov (United States)

    Barnes, Bradley; Bourke, Brian

    2015-01-01

    The authors advance the concept that institutional culture is a purposeful framework by which to view SEM's utility, particularly as a cultural change agent. Through the connection of seemingly independent functions of performance and behavior, implications emerge that deepen the understanding of the influence of culture on performance outcomes…

  17. SAXS and TEM Investigation of Bentonite Structure

    International Nuclear Information System (INIS)

    Matusewicz, Michal; Liljestroem, Ville; Muurinen, Arto; Serimaa, Ritva

    2013-01-01

    A preliminary investigation of bentonite structure using Small-Angle X-ray Scattering (SAXS) and Transmission Electron Microscopy (TEM) is presented. Three types of clay were used: unchanged MX-80 bentonite and purified clays with sodium or calcium ions. Quantitative information in nano-scale - basal spacing, mean crystallite size - was obtained from SAXS, which was complemented by TEM to give qualitative information from micron to nanometre scale. SAXS seems to be a more reliable source of quantitative data than TEM. SAXS gives the averaged information about basal spacing. TEM in this study gives more qualitative information, but in a greater resolution range. The presented work is a starting point to combine more methods to obtain a better idea of bentonite structure. (authors)

  18. TEM of nanostructured metals and alloys

    International Nuclear Information System (INIS)

    Karnthaler, H.P.; Waitz, T.; Rentenberger, C.; Mingler, B.

    2004-01-01

    Nanostructuring has been used to improve the mechanical properties of bulk metals and alloys. Transmission electron microscopy (TEM) including atomic resolution is therefore appropriate to study these nanostructures; four examples are given as follows. (1) The early stages of precipitation at RT were investigated in an Al-Mg-Si alloy. By high resolution TEM it is shown that the precipitates lie on (0 0 1) planes having an ordered structure. (2) In Co alloys the fronts of martensitic phase transformations were analysed showing that the transformation strains are very small thus causing no surface relief. (3) Re-ordering and recrystallization were studied by in situ TEM of an Ni 3 Al alloy being nanocrystalline after severe plastic deformation. (4) In NiTi severe plastic deformation is leading to the formation of amorphous shear bands. From the TEM analysis it is concluded that the amorphization is caused by plastic shear instability starting in the shear bands

  19. Accelerator-tem interface facility and application

    International Nuclear Information System (INIS)

    Li Ming; He Jun; Yang Zheng; Zhou Lin; Liu Chuansheng; Guo Liping; Jiang Changzhong; Yang Shibo; Fu Dejun; Fan Xiangjun; Liu Jiarui; Lee, J.C.

    2010-01-01

    An accelerator-TEM interface facility has been established at Wuhan University. The system consists of an H800 TEM linked to a 200 kV ion implanter and a 2 x 1.7 MV tandetron accelerator. Measures were taken to isolate the TEM from mechanical vibration transmitted from the ion beam lines and good resolution was maintained with the TEM machine when operated under high zoom modes during the ion implantation. Nitrogen ions at 115 keV were successfully transported from the implanter into the TEM chamber through the interface system, and the ion currents measured at the entrance of the TEM column were between 20 and 180 nA. Structural evolution caused by ion irradiation in Si, GaAs, nanocrystal Ag were observed in situ. The TEM sample could be tilted by 52 degree and for low energy ion irradiation, real time observation was realized. The in situ observation showed that the critical implant dose for amorphization of Si is 2 x 10 14 cm -2 and it became fully amorphized at 3 x 10 15 cm -2 . Amorphization of GaAs started at 1 x 10 14 cm -2 , whereas for nanocrystal Ag, the starting dose was 6 x 10 14 cm -2 . The nuclear material C276 samples implanted with 115 keV Ar+ was also studied and dislocation loops with sizes of 3-12 nm were clearly observed after implantation to doses higher than 1 x 10 15 cm -2 . The density of the loops increased with the increase in the implant dose and evolution to polycrystalline and amorphous structures were observed at 5 x 10 15 cm -2 and 3 x 10 16 cm -2 , respectively. An in situ RBS/C chamber has been installed on the transport line of the accelerator-TEM interface system. This makes it possible to in situ measure composition and location of impurities in the lattice of the implanted samples. In addition, a 50 kV low-energy gaseous ion generator was installed close to the TEM chamber, which facilitates in situ TEM observation of helium bubbles formed in materials by helium implantation. (authors)

  20. The use of micro-XRD for the study of glaze color decorations

    Energy Technology Data Exchange (ETDEWEB)

    Pradell, T.; Molina, G. [Universitat Politecnica de Catalunya, Dpt. Fisica i Enginyeria Nuclear, Castelldefels (Spain); Molera, J.; Pla, J. [Universitat de Vic, GRTD, Escola Politecnica Superior, Vic (Spain); Labrador, A. [BM16-ESRF, LLS, BP 220, Grenoble Cedex (France); Lund University, MAX IV Laboratory, Lund (Sweden)

    2013-04-15

    The compounds responsible for the colors and decorations in glass and glazed ceramics include: coloring agents (transition-metal ions), pigments (micro- and nanoprecipitates of compounds that either do not dissolve or recrystallize in the glassy matrix) and opacifiers (microcrystalline compounds with high light scattering capability). Their composition, structure and range of stability are highly dependent not only on the composition but also on the procedures followed to obtain them. Chemical composition of the colorants and crystallites may be obtained by means of SEM-EDX and WDX. Synchrotron radiation micro-X-ray diffraction (SR-micro-XRD) has a small beam size adequate (10 to 50 microns footprint size) to obtain the structural information of crystalline compounds and high brilliance, optimal for determining the crystallites even when present in low amounts. In addition, in glass decorations the crystallites often appear forming thin layers (from 10 to 100 micrometers thick) and they show a depth-dependent composition and crystal structure. Their nature and distribution across the glass/glaze decorations gives direct information on the technology of production and stability and may be related to the color and appearance. A selection of glass and glaze coloring agents and decorations are studied by means of SR-micro-XRD and SEM-EDX including: manganese brown, antimony yellow, red copper lusters and cobalt blue. The selection includes Medieval (Islamic, and Hispano Moresque) and Renaissance tin-glazed ceramics from the 10th to the 17th century AD. (orig.)

  1. Accelerator-TEM interface facility and application

    International Nuclear Information System (INIS)

    Liu Chuansheng; Li Ming; He Jun; Yang Zheng; Zhou Lin; Wang Zesong; Guo Liping; Jiang Changzhong; Yang Shibo; Fu Dejun; Fan Xiangjun; Liu Jiarui; Lee J C

    2010-01-01

    An accelerator-TEM interface facility has been established at Wuhan University in 2008. The system consists of an H800 TEM linked to a 200 kV ion implanter and a 2 x 1.7 MV tandem accelerator. Nitrogen ions at 115 keV were successfully transported from the implanter into the TEM chamber through the interface system, and the ion currents measured at the entrance of the TEM column were between 20 and 180 nA. Structural evolution caused by ion irradiation in Si, GaAs, nanocrystal Ag was observed in situ. The in situ observation showed that the critical implantation dose for amorphization of Si is 10 14 cm -2 . The nuclear material C276 samples implanted with 115 keV Ar + was also studied, and dislocation loops sized at 3-12 nm were clearly observed after implantation to doses of over 1 x 10 15 cm -2 . The density of the loops increased with the dose. Evolution to polycrystalline and amorphous structures were observed at 5 x l0 15 cm -2 and 3 x 10 16 cm -2 , respectively. An in situ RBS/C chamber was installed on the transport line of the accelerator-TEM interface system. This enables in situ measurement of composition and location of the implanted species in lattice of the samples. In addition, a 50 kV low-energy gaseous ion generator was installed close to the TEM chamber, which facilitates in situ TEM observation of helium bubbles formed in helium-implanted materials. (authors)

  2. Cassette-based in-situ TEM sample inspection in the dual-beam FIB

    International Nuclear Information System (INIS)

    Kendrick, A B; Moore, T M; Zaykova-Feldman, L; Amador, G; Hammer, M

    2008-01-01

    A novel method is presented, combining site-specific TEM sample preparation and in-situ STEM analysis in a dual-beam microscope (FIB/SEM) fitted with a chamber mounted nano-manipulator. TEM samples are prepared using a modified in-situ, lift-out method, whereby the samples are thinned and oriented for immediate in-situ STEM analysis using the tilt, translation, and rotation capabilities of a FIB/SEM sample stage, a nano-manipulator, and a novel cassette. This cassette can provide a second tilt axis, orthogonal to the stage tilt axis, so that the STEM image contrast can be optimized to reveal the structural features of the sample (true STEM imaging in the FIB/SEM). The angles necessary for stage rotation and probe shaft rotation are calculated based on the position of the nano-manipulator relative to the stage and door and the stage tilt angle. A FIB/SEM instrument, equipped with a high resolution scanning electron column, can provide sufficiently high image resolution to enable many failure analysis and process control applications to be successfully carried out without requiring the use of a separate dedicated TEM/STEM instrument. The benefits of this novel approach are increased throughput and reduced cost per sample. Comparative analysis of different sample preparation methods is provided, and the STEM images obtained are shown.

  3. Framework for SEM contour analysis

    Science.gov (United States)

    Schneider, L.; Farys, V.; Serret, E.; Fenouillet-Beranger, C.

    2017-03-01

    SEM images provide valuable information about patterning capability. Geometrical properties such as Critical Dimension (CD) can be extracted from them and are used to calibrate OPC models, thus making OPC more robust and reliable. However, there is currently a shortage of appropriate metrology tools to inspect complex two-dimensional patterns in the same way as one would work with simple one-dimensional patterns. In this article we present a full framework for the analysis of SEM images. It has been proven to be fast, reliable and robust for every type of structure, and particularly for two-dimensional structures. To achieve this result, several innovative solutions have been developed and will be presented in the following pages. Firstly, we will present a new noise filter which is used to reduce noise on SEM images, followed by an efficient topography identifier, and finally we will describe the use of a topological skeleton as a measurement tool that can extend CD measurements on all kinds of patterns.

  4. SEM-based characterization techniques

    International Nuclear Information System (INIS)

    Russell, P.E.

    1986-01-01

    The scanning electron microscope is now a common instrument in materials characterization laboratories. The basic role of the SEM as a topographic imaging system has steadily been expanding to include a variety of SEM-based analytical techniques. These techniques cover the range of basic semiconductor materials characterization to live-time device characterization of operating LSI or VLSI devices. This paper introduces many of the more commonly used techniques, describes the modifications or additions to a conventional SEM required to utilize the techniques, and gives examples of the use of such techniques. First, the types of signals available from a sample being irradiated by an electron beam are reviewed. Then, where applicable, the type of spectroscopy or microscopy which has evolved to utilize the various signal types are described. This is followed by specific examples of the use of such techniques to solve problems related to semiconductor technology. Techniques emphasized include: x-ray fluorescence spectroscopy, electron beam induced current (EBIC), stroboscopic voltage analysis, cathodoluminescnece and electron beam IC metrology. Current and future trends of some of the these techniques, as related to the semiconductor industry are discussed

  5. [Identification of Dens Draconis and Os Draconis by XRD method].

    Science.gov (United States)

    Chen, Guang-Yun; Wu, Qi-Nan; Shen, Bei; Chen, Rong

    2012-04-01

    To establish an XRD method for evaluating the quality of Os Draconis and Dens Draconis and applying in judgement of the counterfeit. Dens Draconis, Os Draconis and the counterfeit of Os Draconis were analyzed by XRD. Their diffraction patterns were clustered analysis and evaluated their similarity degree. Established the analytical method of Dens Draconis and Os Draconis basing the features fingerprint information of the 10 common peaks by XRD pattern. Obtained the XRD pattern of the counterfeit of Os Draconis. The similarity degree of separate sources of Dens Draconis was high,while the similarity degree of separate sources of Os Draconis was significant different from each other. This method can be used for identification and evaluation of Os Draconis and Dens Draconis. It also can be used for identification the counterfeit of Os Draconis effectively.

  6. Quantitative in situ TEM tensile testing of an individual nickel nanowire

    International Nuclear Information System (INIS)

    Lu Yang; Peng Cheng; Ganesan, Yogeeswaran; Lou Jun; Huang Jianyu

    2011-01-01

    In this paper, we have demonstrated the usage of a novel micro-mechanical device (MMD) to perform quantitative in situ tensile tests on individual metallic nanowires inside a transmission electron microscope (TEM). Our preliminary experiment on a 360 nm diameter nickel nanowire showed that the sample fractured at an engineering stress of ∼ 1.2 GPa and an engineering strain of ∼ 4%, which is consistent with earlier experiments performed inside a scanning electron microscope (SEM). With in situ high resolution TEM imaging and diffraction capabilities, this novel experimental set-up could provide unique opportunities to reveal the underlying deformation and damage mechanisms for metals at the nanoscale.

  7. Moessbauer effect and TEM in mineralogy

    International Nuclear Information System (INIS)

    Ferrow, E.A.

    1994-01-01

    Moessbauer effect (ME) provides useful information on oxidation state, co-ordination number, co-ordination state, site occupancies, and magnetic properties of Fe-bearing phases. The information gained by ME together with the information provided by other conventional techniques is used to extract temperature, pressure, and kinetics of rock-forming processes. Nevertheless, ME requires that the phases studied are homogeneous over an extremely large volume and that Fe is a major component of the system. Transmission electron microscopy (TEM), on the other hand, provides similar information over a very small volume for a system of any component. However, present TEM spectrometers do not provide sufficient resolution to detect the mixed oxidation state. A complete characterisation of phases in rocks requires, therefore, that conventional techniques be combined with TEM. (orig.)

  8. International Conference on SEMS 2012

    CERN Document Server

    Liu, Chuang; Scientific explanation and methodology of science; SEMS 2012

    2014-01-01

    This volume contains the contributed papers of invitees to SEMS 2012 who have also given talks at the conference. The invitees are experts in philosophy of science and technology from Asia (besides China), Australia, Europe, Latin America, North America, as well as from within China. The papers in this volume represent the latest work of each researcher in his or her expertise; and as a result, they give a good representation of the cutting-edge researches in diverse areas in different parts of the world.

  9. Destructive interference of TEM and ITG turbulence

    International Nuclear Information System (INIS)

    Merz, F.; Jenko, F.

    2009-01-01

    Full text: Turbulence driven by ion temperature gradient (ITG) modes and trapped electron modes (TEMs) is generally considered the key mechanism for anomalous transport in fusion devices on ion scales. But while pure ITG and, to a lesser extent, also pure TEM turbulence have been studied in detail over the last years, not much is presently known about nonlinear interactions between ITG modes and TEMs, which are often present simultaneously in experimentally relevant situations. This important issue is addressed by means of linear and nonlinear gyrokinetic simulations with the GENE code. To examine the properties of the (linear) TEM and ITG instabilities in the (realistic) transitional regime, the GENE code is run as eigenvalue solver, which allows for a systematic study of dominant and subdominant modes. Corresponding nonlinear initial value computations show that the particle transport of the turbulent system can be completely suppressed if the two driving instabilities are active simultaneously. The direct comparison of the linear modes and the corresponding turbulent system reveals a coexistence of the two microinstabilities in a transitional regime even at the same wave number. The consequences of this dual turbulence drive for transport modeling is discussed. (author)

  10. In Situ TEM Creation of Nanowire Devices

    DEFF Research Database (Denmark)

    Alam, Sardar Bilal

    Integration of silicon nanowires (SiNWs) as active components in devices requires that desired mechanical, thermal and electrical interfaces can be established between the nanoscale geometry of the SiNW and the microscale architecture of the device. In situ transmission electron microscopy (TEM),...

  11. Test for English Majors (TEM) in China

    Science.gov (United States)

    Jin, Yan; Fan, Jinsong

    2011-01-01

    The purpose of the Test for English Majors (TEM) is to measure the English proficiency of Chinese university undergraduates majoring in English Language and Literature and to examine whether these students meet the required levels of English language abilities as specified in the National College English Teaching Syllabus for English Majors…

  12. Nonlinear entropy transfer in ETG-TEM turbulence via TEM driven zonal flows

    International Nuclear Information System (INIS)

    Asahi, Yuuichi; Tsutsui, Hiroaki; Tsuji-Iio, Shunji; Ishizawa, Akihiro; Sugama, Hideo; Watanabe, Tomohiko

    2015-01-01

    Nonlinear interplay of the electron temperature gradient (ETG) modes and the trapped electron modes (TEMs) was investigated by means of gyrokinetic simulation. Focusing on the situation where both TEMs and ETG modes are linearly unstable, the effects of TEM-driven zonal flows on ETG turbulence were examined by means of entropy transfer analysis. In a statistically steady turbulence where the TEM driven zonal flows are dominant, it turned out that the zonal flows meditate the entropy transfer of the ETG modes from the low to high radial wavenumber regions. The successive entropy transfer broadens the potential fluctuation spectrum in the radial wavenumber direction. In contrast, in the situation where ETG modes are unstable but TEMs are stable, the pure ETG turbulence does not produce strong zonal flows, leading to a rather narrow spectrum in the radial wavenumber space and a higher transport level. (author)

  13. 40 keV atomic resolution TEM

    International Nuclear Information System (INIS)

    Bell, David C.; Russo, Christopher J.; Kolmykov, Dmitry V.

    2012-01-01

    Here we present the first atomic resolution TEM imaging at 40 keV using an aberration-corrected, monochromated source TEM. Low-voltage High-Resolution Electron Microscopy (LVHREM) has several advantages, including increased cross-sections for inelastic and elastic scattering, increased contrast per electron and improved spectroscopy efficiency, decreased delocalization effects and reduced knock-on damage. Together, these often improve the contrast to damage ratio obtained on a large class of samples. Third-order aberration correction now allows us to operate the TEM at low energies while retaining atomic resolution, which was previously impossible. At low voltage the major limitation to resolution becomes the chromatic aberration limit. We show that using a source monochromator we are able to reduce the effect of chromatic aberration and achieve a usable high-resolution limit at 40 keV to less than 1 Å. We show various materials' examples of the application of the technique to image graphene and silicon, and compare atomic resolution images with electron multislice simulations. -- Highlights: ► We present the first atomic resolution images recorded at 40 keV using an aberration-corrected, monochromated TEM. ► We show information transfer measured to better than 1 Å. ► At 40 keV an aberration-corrected monochromated TEM is limited by fifth-order spherical aberration. ► We show that using a monochromator the effect of chromatic aberration is reduced to enable high resolution imaging. ► Low voltage high resolution electron microscopy will be beneficial for imaging the organic/inorganic materials interface.

  14. Non-coating fixation techniques or redundancy of conductive coating, low kV FE-SEM operation and combined SEM/TEM of biological tissues

    NARCIS (Netherlands)

    Jongebloed, WL; Stokroos, [No Value; Van der Want, JJL; Kalicharan, D

    Non-coating fixation methods, in particular the tannic acid/arginine/osmium tetroxide procedure, are employed for a number of reasons on the guinea-pig organ of Corti hair cell stereocilia glycocalyx and the imprints of the stereocilia at the bottom side of the tectorial membrane, and on the rat and

  15. The Effect of Nonnormality on CB-SEM and PLS-SEM Path Estimates

    OpenAIRE

    Z. Jannoo; B. W. Yap; N. Auchoybur; M. A. Lazim

    2014-01-01

    The two common approaches to Structural Equation Modeling (SEM) are the Covariance-Based SEM (CB-SEM) and Partial Least Squares SEM (PLS-SEM). There is much debate on the performance of CB-SEM and PLS-SEM for small sample size and when distributions are nonnormal. This study evaluates the performance of CB-SEM and PLS-SEM under normality and nonnormality conditions via a simulation. Monte Carlo Simulation in R programming language was employed to generate data based on the theoretical model w...

  16. Sexual Arousal and Sexually Explicit Media (SEM)

    DEFF Research Database (Denmark)

    Hald, Gert Martin; Stulhofer, Aleksandar; Lange, Theis

    2018-01-01

    -mainstream and mainstream SEM groups, and (iii) to explore the validity and predictive accuracy of the Non-Mainstream Pornography Arousal Scale (NPAS). METHODS: Online cross-sectional survey of 2,035 regular SEM users in Croatia. MAIN OUTCOMES MEASURES: Patterns of sexual arousal to 27 different SEM themes, sexual...

  17. XRD spectra of new YBaCuO superconductors

    Indian Academy of Sciences (India)

    superconductors of YBaCuO materials by solid state reac- tion. They used the ... The XRD spectra and critical temperatures are shown to be the same as that of ... samples were synthesized by solid state reaction using raw materials Y2O3 ...

  18. FTIR, XRD and DSC studies of nanochitosan, cellulose acetate and polyethylene glycol blend ultrafiltration membranes.

    Science.gov (United States)

    Vinodhini, P Angelin; K, Sangeetha; Thandapani, Gomathi; P N, Sudha; Jayachandran, Venkatesan; Sukumaran, Anil

    2017-11-01

    In the present work, a series of novel nanochitosan/cellulose acetate/polyethylene glycol (NCS/CA/PEG) blend flat sheet membranes were fabricated in different ratios (1:1:1, 1:1:2, 2:1:1, 2:1:2, 1:2:1, 2:2:1) in a polar solvent of N,N'-dimethylformamide (DMF) using the most popular phase inversion method. Nanochitosan was prepared by the ionotropic gelation method and its average particle size has been analyzed using Dynamic Light Scattering (DLS) method. The effect of blending of the three polymers was investigated using FTIR and XRD studies. FTIR results confirmed the formation of well-blended membranes and the XRD analysis revealed enhanced amorphous nature of the membrane ratio 2:1:2. DSC study was conducted to find out the thermal behavior of the blend membranes and the results clearly indicated good thermal stability and single glass transition temperature (T g ) of all the prepared membranes. Asymmetric nature and rough surface morphology was confirmed using SEM analysis. From the results it was evident that the blending of the polymers with higher concentration of nanochitosan can alter the nature of the resulting membranes to a greater extent and thus amorphous membranes were obtained with good miscibility and compatibility. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Influence of smectite suspension structure on sheet orientation in dry sediments: XRD and AFM applications.

    Science.gov (United States)

    Zbik, Marek S; Frost, Ray L

    2010-06-15

    The structure-building phenomena within clay aggregates are governed by forces acting between clay particles. Measurements of such forces are important to understand in order to manipulate the aggregate structure for applications such as dewatering of mineral processing tailings. A parallel particle orientation is required when conducting XRD investigation on the oriented samples and conduct force measurements acting between basal planes of clay mineral platelets using atomic force microscopy (AFM). To investigate how smectite clay platelets were oriented on silicon wafer substrate when dried from suspension range of methods like SEM, XRD and AFM were employed. From these investigations, we conclude that high clay concentrations and larger particle diameters (up to 5 microm) in suspension result in random orientation of platelets in the substrate. The best possible laminar orientation in the clay dry film, represented in the XRD 001/020 intensity ratio of 47 was obtained by drying thin layers from 0.02 wt.% clay suspensions of the natural pH. Conducted AFM investigations show that smectite studied in water based electrolytes show very long-range repulsive forces lower in strength than electrostatic forces from double-layer repulsion. It was suggested that these forces may have structural nature. Smectite surface layers rehydrate in water environment forms surface gel with spongy and cellular texture which cushion approaching AFM probe. This structural effect can be measured in distances larger than 1000 nm from substrate surface and when probe penetrate this gel layer, structural linkages are forming between substrate and clay covered probe. These linkages prevent subsequently smooth detachments of AFM probe on way back when retrieval. This effect of tearing new formed structure apart involves larger adhesion-like forces measured in retrieval. It is also suggested that these effect may be enhanced by the nano-clay particles interaction. 2010 Elsevier Inc. All

  20. Recent advances in FIB-TEM specimen preparation techniques

    International Nuclear Information System (INIS)

    Li Jian; Malis, T.; Dionne, S.

    2006-01-01

    Preparing high-quality transmission electron microscopy (TEM) specimens is of paramount importance in TEM studies. The development of the focused ion beam (FIB) microscope has greatly enhanced TEM specimen preparation capabilities. In recent years, various FIB-TEM foil preparation techniques have been developed. However, the currently available techniques fail to produce TEM specimens from fragile and ultra-fine specimens such as fine fibers. In this paper, the conventional FIB-TEM specimen preparation techniques are reviewed, and their advantages and shortcomings are compared. In addition, a new technique suitable to prepare TEM samples from ultra-fine specimens is demonstrated

  1. Characterization of Nb coating in HIE-ISOLDE QWR superconducting accelerating cavities by means of SEM-FIB and TEM

    CERN Document Server

    Bartova, Barbora; Taborelli, M; Aebersold, A B; Alexander, D T L; Cantoni, M; Calatroni, Sergio; CERN. Geneva. ATS Department

    2015-01-01

    The Quarter Wave Resonators (QWR) high-β cavities (0.3 m diameter and 0.9 m height) are made from OFE 3D-forged copper and are coated by DC-bias diode sputtering with a thin superconducting layer of niobium. The Nb film thickness, morphology, purity and quality are critical parameters for RF performances of the cavity. They have been investigated in a detailed material study.

  2. TEM-EELS: A personal perspective

    International Nuclear Information System (INIS)

    Egerton, R.F.

    2012-01-01

    The development of electron energy-loss spectroscopy in a transmission electron microscope (TEM-EELS) is illustrated through personal anecdote, highlighting some of the basic principles, instrumentation and personalities involved. The current state of the art is reviewed, together with some challenges for the future. -- Highlights: ► The history of EELS instrumentation is reviewed in a lighthearted manner. ► The current state of the art is summarized, together with some future possibilities. ► A couple of related mathematical puzzles are offered as a challenge to the reader.

  3. TEM investigations of laser ablated particles

    International Nuclear Information System (INIS)

    Fliegel, D.; Dundas, S.; Kosler, J.; Klementova, M.

    2009-01-01

    Full text: Laser ablation inductively coupled plasma mass spectrometry suffers from fractionation effects hindering a non matrix matched calibration strategy. Different reasons for elemental fractionation that are related to the laser ablation, the transport and the vaporization in the plasma are discussed. One major question to be addressed linked to the vaporization yield in the ICP is in which of mineralogical phase the different ablated particle sizes enter the plasma. This contribution will investigate particles generated by a 213 nm laser from different samples such as minerals and alloys with respect to their chemical and phase compositions using high resolution TEM. (author)

  4. Qualitative soil mineral analysis by EDXRF, XRD and AAS probes

    International Nuclear Information System (INIS)

    Singh, Virendra; Agrawal, H.M.

    2012-01-01

    Soil minerals study is vital in terms of investigating the major soil forming compounds and to find out the fate of minor and trace elements, essential for the soil–plant interaction purpose. X-ray diffraction (XRD) has been a popular technique to search out the phases for different types of samples. For the soil samples, however, employing XRD is not so straightforward due to many practical problems. In the current approach, principal component analysis (PCA) has been used to have an idea of the minerals present, in qualitative manner, in the soil under study. PCA was used on the elemental concentrations data of 17 elements, determined by the energy dispersive X-ray fluorescence (EDXRF) technique. XRD analysis of soil samples has been done also to identify the minerals of major elements. Some prior treatments, like removal of silica by polytetrafluoroethylene (PTFE) slurry and grinding with alcohol, were given to samples to overcome the peak overlapping problems and to attain fine particle size which is important to minimize micro-absorption corrections, to give reproducible peak intensities and to minimize preferred orientation. A 2θ step of 0.05°/min and a longer dwell time than normal were used to reduce interferences from background noise and to increase the counting statistics. Finally, the sequential extraction procedure for metal speciation study has been applied on soil samples. Atomic absorption spectroscopy (AAS) was used to find the concentrations of metal fractions bound to various forms. Applying all the three probes, the minerals in the soils can be studied and identified, successfully. - Highlights: ► Qualitative soil minerals analysis by EDXRF, AAS and XRD methods. ► There is a requirement of other means and methods due to inadequacy of XRD. ► Principal component analysis (PCA) provides an idea of minerals present in soil. ► Trace elements complexes can be determined by AAS probe. ► EDXRF, AAS and XRD, in combination, enable

  5. Automated transmission-mode scanning electron microscopy (tSEM for large volume analysis at nanoscale resolution.

    Directory of Open Access Journals (Sweden)

    Masaaki Kuwajima

    Full Text Available Transmission-mode scanning electron microscopy (tSEM on a field emission SEM platform was developed for efficient and cost-effective imaging of circuit-scale volumes from brain at nanoscale resolution. Image area was maximized while optimizing the resolution and dynamic range necessary for discriminating key subcellular structures, such as small axonal, dendritic and glial processes, synapses, smooth endoplasmic reticulum, vesicles, microtubules, polyribosomes, and endosomes which are critical for neuronal function. Individual image fields from the tSEM system were up to 4,295 µm(2 (65.54 µm per side at 2 nm pixel size, contrasting with image fields from a modern transmission electron microscope (TEM system, which were only 66.59 µm(2 (8.160 µm per side at the same pixel size. The tSEM produced outstanding images and had reduced distortion and drift relative to TEM. Automated stage and scan control in tSEM easily provided unattended serial section imaging and montaging. Lens and scan properties on both TEM and SEM platforms revealed no significant nonlinear distortions within a central field of ∼100 µm(2 and produced near-perfect image registration across serial sections using the computational elastic alignment tool in Fiji/TrakEM2 software, and reliable geometric measurements from RECONSTRUCT™ or Fiji/TrakEM2 software. Axial resolution limits the analysis of small structures contained within a section (∼45 nm. Since this new tSEM is non-destructive, objects within a section can be explored at finer axial resolution in TEM tomography with current methods. Future development of tSEM tomography promises thinner axial resolution producing nearly isotropic voxels and should provide within-section analyses of structures without changing platforms. Brain was the test system given our interest in synaptic connectivity and plasticity; however, the new tSEM system is readily applicable to other biological systems.

  6. XRD Investigation of Some Thermal Degraded Starch Based Materials

    Directory of Open Access Journals (Sweden)

    Mihai Todica

    2016-01-01

    Full Text Available The thermal degradation of some starch based materials was investigated using XRD method. The samples were obtained by thermal extrusion of mixtures of different proportions of starch, glycerol, and water. Such materials are suitable for the manufacturing of low pollutant packaging. Thermal degradation is one of the simplest ways to destroy such materials and this process is followed by structural modification of the local ordering of samples, water evaporation, crystallization, oxidation, or destruction of the chemical bonds. These modifications need to be studied in order to reduce to the minimum production of pollutant residues by burning process. XRD measurements show modification of the local ordering of the starch molecules depending on the temperature and initial composition of the samples. The molecular ordering perturbation is more pronounced in samples with low content of starch.

  7. XRD and HREM studies of nanocrystalline Cu and Pd

    International Nuclear Information System (INIS)

    Nieman, G.W.; Weertmen, J.R.; Siegel, R.W.

    1991-01-01

    Consolidated powders of nanocrystalline Cu and Pd have been studied by x-ray diffraction (XRD) and high resolution electron microscopy (HREM) as part of an investigation of the mechanical behavior of nanocrystalline pure metals. XRD line broadening measurements were made to estimate rain size, qualitative grain size distribution and average long range strains in a number of samples. Mean grain sized range from 4-60 nm and have qualitatively narrow grain size distributions. Long range lattice strains are of the order of 0.2-3% in consolidated samples. These strains apparently persist and even increase in Cu samples after annealing at 0.35 Tm (498K) for 2h, accompanied by an apparent increase in grain size of ≥2x. Grain size, grain size distribution width and internal strains vary somewhat among samples produced under apparently identical processing conditions. HREM studies show that twins, stacking faults and low-index facets are abundant in as-consolidated nanocrystalline Cu samples. In this paper methodology, results and analysis of XRD and HREM experiments are presented

  8. XRD is the main key to the mechanochemical processing

    International Nuclear Information System (INIS)

    Mozaffari, M.; Amighian, J.

    2000-01-01

    Mechanochemical processing is a process that makes use of chemical reactions mechanically activated by high-energy ball milling (HEBM). This technique has been the subject of great interest in recent years due to its promise for producing improved novel materials. Ultra fine powders in the range 10-100 nm can be obtained by mixing the right ratio of the components, appropriate for a desired phase. These raw materials together with several hardened-steel vial and milled for an optimum time using Spex or Planetary mills. In this process 2 factors, milling time and the ball to powder mass ratio, should carefully be optimized. These will be checked by successive XRD patterns. To see the ability of XRD in this technique, some single phase Ni-Al and Mn ferrites were prepared. The main key to the formation of different phases at any stage of processing was XRD patterns. Also by using Scherrer formula it was possible to measure the particle size of the milled powders. (Author)

  9. Environmental TEM in an Aberration Corrected Microscope

    DEFF Research Database (Denmark)

    Hansen, Thomas Willum; Wagner, Jakob Birkedal

    ‐resolution imaging. A gaseous atmosphere in the pole‐piece gap of the objective lens of the microscope alters both the incoming electron wave prior to interaction with the sample and the outgoing wave below the sample. Whereas conventional TEM samples are usually thin (below 10‐20 nm), the gas in the environmental...... the microscope column. The effects of gas on the electron wave in the objective lens are not well understood and needs further attention. Imaging samples with a simple geometry, such as gold particles on a flat graphene substrate and analyzing the variations in contrast, provides a means for understanding...... results from imaging in various elemental as well as di‐molecular gases and their effect on imaging and spectroscopy in the environmental transmission electron microscope....

  10. TEM investigations of microstructures of combustion aerosols

    International Nuclear Information System (INIS)

    Marquardt, A.; Hackfort, H.; Borchardt, J.; Schober, T.; Friedrich, J.

    1992-12-01

    In the incineration of organic material, apart from a series of gaseous pollutants, particulate pollutants or combustion aerosols also arise. The latter frequently consist of particles with a solid core of carbon to which a large number of inorganic and organic compounds are attached. These primarily include the polycyclic aromatic hydrocarbons (PAH) and their nitro-derivatives (NPAH), whose mutagenic or carcinogenic effect is known. The invisible particle sizes in the nanometer range, whose retention in the incineration off-gas is not state of the art, are of increasing significance for man and environment. On the one hand, they are deposited almost completely in the human lung. On the other hand, due to their fine dispersity they have along residence time in the atmosphere where they participate in chemical reactions and climatically significant processes. Important insights about the formation process of combustion aerosols are to be expected from the imaging of their microstructures in the transmission electron microscope (TEM). The present contribution describes the development and application of a representative sampling procedure for aerosols from a partial flow of flue gas from a fluidized-bed furnace. The method developed consists of electrically charging aerosol particles in situ and subsequently selectively precipitating them onto a microscope slide in an electric field. TEM studies of aerosol microstructures on the microscope slides revealed that in the combustion of petrol and heating oil under different combustion conditions in principle the same particle structures result, whereas in the incineration of used lubricating oil quite different particle structures were found. Results from the literature on aerosol microstructures in exhaust gases from petrol and diesel engines demonstrate agreement with the results of this study in the basic structure of the particles. (orig.) [de

  11. Developing 3D SEM in a broad biological context

    Science.gov (United States)

    Kremer, A; Lippens, S; Bartunkova, S; Asselbergh, B; Blanpain, C; Fendrych, M; Goossens, A; Holt, M; Janssens, S; Krols, M; Larsimont, J-C; Mc Guire, C; Nowack, MK; Saelens, X; Schertel, A; Schepens, B; Slezak, M; Timmerman, V; Theunis, C; Van Brempt, R; Visser, Y; GuÉRin, CJ

    2015-01-01

    When electron microscopy (EM) was introduced in the 1930s it gave scientists their first look into the nanoworld of cells. Over the last 80 years EM has vastly increased our understanding of the complex cellular structures that underlie the diverse functions that cells need to maintain life. One drawback that has been difficult to overcome was the inherent lack of volume information, mainly due to the limit on the thickness of sections that could be viewed in a transmission electron microscope (TEM). For many years scientists struggled to achieve three-dimensional (3D) EM using serial section reconstructions, TEM tomography, and scanning EM (SEM) techniques such as freeze-fracture. Although each technique yielded some special information, they required a significant amount of time and specialist expertise to obtain even a very small 3D EM dataset. Almost 20 years ago scientists began to exploit SEMs to image blocks of embedded tissues and perform serial sectioning of these tissues inside the SEM chamber. Using first focused ion beams (FIB) and subsequently robotic ultramicrotomes (serial block-face, SBF-SEM) microscopists were able to collect large volumes of 3D EM information at resolutions that could address many important biological questions, and do so in an efficient manner. We present here some examples of 3D EM taken from the many diverse specimens that have been imaged in our core facility. We propose that the next major step forward will be to efficiently correlate functional information obtained using light microscopy (LM) with 3D EM datasets to more completely investigate the important links between cell structures and their functions. Lay Description Life happens in three dimensions. For many years, first light, and then EM struggled to image the smallest parts of cells in 3D. With recent advances in technology and corresponding improvements in computing, scientists can now see the 3D world of the cell at the nanoscale. In this paper we present the

  12. Three dimensional rock microstructures: insights from FIB-SEM tomography

    Science.gov (United States)

    Drury, Martyn; Pennock, Gill; de Winter, Matthijs

    2016-04-01

    Most studies of rock microstructures investigate two-dimensional sections or thin slices of three dimensional grain structures. With advances of X-ray and electron tomography methods the 3-D microstructure can be(relatively) routinely investigated on scales from a few microns to cm. 3D studies are needed to investigate the connectivity of microstructures and to test the assumptions we use to calculate 3D properties from 2D sections. We have used FIB-SEM tomography to study the topology of melts in synthetic olivine rocks, 3D crystal growth microstructures, pore networks and subgrain structures. The technique uses a focused ion beam to make serial sections with a spacing of tens to hundreds of nanometers. Each section is then imaged or mapped using the electron beam. The 3D geometry of grains and subgrains can be investigated using orientation contrast or EBSD mapping. FIB-SEM tomography of rocks and minerals can be limited by charging of the uncoated surfaces exposed by the ion beam. The newest generation of FIB-SEMs have much improved low voltage imaging capability allowing high resolution charge free imaging. Low kV FIB-SEM tomography is now widely used to study the connectivity of pore networks. In-situ fluids can also be studied using cryo-FIB-SEM on frozen samples, although special freezing techniques are needed to avoid artifacts produced by ice crystallization. FIB-SEM tomography is complementary, in terms of spatial resolution and sampled volume, to TEM tomography and X-ray tomography, and the combination of these methods can cover a wide range of scales. Our studies on melt topology in synthetic olivine rocks with a high melt content show that many grain boundaries are wetted by nanometre scale melt layers that are too thin to resolve by X-ray tomography. A variety of melt layer geometries occur consistent with several mechanisms of melt layer formation. The nature of melt geometries along triple line junctions and quadruple points can be resolved

  13. TEM-145 and TEM-146 β-lactamases produced by Escherichia coli ...

    African Journals Online (AJOL)

    GREGO

    2007-03-05

    Mar 5, 2007 ... Key words: Escherichia coli, plasmid-mediated, TEM β-lactamase. ... Enterobacteriaceae, the most prevalent mechanism of resistance to ... the production of a relatively inhibitor-resistant OXA-type β-lactamase .... and 8.6 as transcripts of the E. coli chromosomal AmpC .... Mode of action and mechanisms of.

  14. EBSD and TEM Characterization of High Burn-up Mixed Oxide Fuel

    International Nuclear Information System (INIS)

    Teague, Melissa C; Gorman, Brian P.; Miller, Brandon D; King, Jeffrey

    2014-01-01

    Understanding and studying the irradiation behavior of high burn-up oxide fuel is critical to licensing of future fast breeder reactors. Advancements in experimental techniques and equipment are allowing for new insights into previously irradiated samples. In this work dual column focused ion beam (FIB)/scanning electron microscope (SEM) was utilized to prepared transmission electron microscope samples from mixed oxide fuel with a burn-up of 6.7% FIMA. Utilizing the FIB/SEM for preparation resulted in samples with a dose rate of <0.5 mRem/h compared to approximately 1.1 R/h for a traditionally prepared TEM sample. The TEM analysis showed that the sample taken from the cooler rim region of the fuel pellet had approximately 2.5x higher dislocation density than that of the sample taken from the mid-radius due to the lower irradiation temperature of the rim. The dual column FIB/SEM was additionally used to prepared and serially slice approximately 25 um cubes. High quality electron back scatter diffraction (EBSD) were collected from the face at each step, showing, for the first time, the ability to obtain EBSD data from high activity irradiated fuel

  15. TEM characterization of nanodiamond thin films.

    Energy Technology Data Exchange (ETDEWEB)

    Qin, L.-C.; Zhou, D.; Krauss, A. R.; Gruen, D. M.; Chemistry

    1998-05-01

    The microstructure of thin films grown by microwave plasma-enhanced chemical vapor deposition (MPCVD) from fullerene C{sub 60} precursors has been characterized by scanning electron microscopy (SEM), selected-area electron diffraction (SAED), bright-field electron microscopy, high-resolution electron microscopy (HREM), and parallel electron energy loss spectroscopy (PEELS). The films are composed of nanosize crystallites of diamond, and no graphitic or amorphous phases were observed. The diamond crystallite size measured from lattice images shows that most grains range between 3-5 nm, reflecting a gamma distribution. SAED gave no evidence of either sp2-bonded glassy carbon or sp3-bonded diamondlike amorphous carbon. The sp2-bonded configuration found in PEELS was attributed to grain boundary carbon atoms, which constitute 5-10% of the total. Occasionally observed larger diamond grains tend to be highly faulted.

  16. Silver Accumulation in the Green Microalga Coccomyxa actinabiotis: Toxicity, in Situ Speciation, and Localization Investigated Using Synchrotron XAS, XRD, and TEM.

    Science.gov (United States)

    Leonardo, Thomas; Farhi, Emmanuel; Pouget, Stéphanie; Motellier, Sylvie; Boisson, Anne-Marie; Banerjee, Dipanjan; Rébeillé, Fabrice; den Auwer, Christophe; Rivasseau, Corinne

    2016-01-05

    Microalgae are good candidates for toxic metal remediation biotechnologies. This study explores the cellular processes implemented by the green microalga Coccomyxa actinabiotis to take up and cope with silver over the concentration range of 10(-7) to 10(-2) M Ag(+). Understanding these processes enables us to assess the potential of this microalga for applications for bioremediation. Silver in situ speciation and localization were investigated using X-ray absorption spectroscopy, X-ray diffraction, and transmission electron microscopy. Silver toxicity was evaluated by monitoring microalgal growth and photochemical parameters. Different accumulation mechanisms were brought out depending on silver concentration. At low micromolar concentration, microalgae fixed all silver initially present in solution, trapping it inside the cells into the cytosol, mainly as unreduced Ag(I) bound with molecules containing sulfur. Silver was efficiently detoxified. When concentration increased, silver spread throughout the cell and particularly entered the chloroplast, where it damaged the photosystem. Most silver was reduced to Ag(0) and aggregated to form crystalline silver nanoparticles of face-centered cubic structure with a mean size of 10 nm. An additional minor interaction of silver with molecules containing sulfur indicated the concomitant existence of the mechanism observed at low concentration or nanoparticle capping. Nanoparticles were observed in chloroplasts, in mitochondria, on the plasma membrane, on cytosolic membrane structures, and in vacuoles. Above 10(-4) M Ag(+), damages were irreversible, and photosynthesis and growth were definitely inhibited. However, high silver amounts remained confined inside microalgae, showing their potential for the bioremediation of contaminated water.

  17. Advantages of TOF-SIMS analysis of hydroxyapatite and fluorapatite in comparison with XRD, HR-TEM and FT-IR.

    Science.gov (United States)

    Okazaki, Masayuki; Hirata, Isao; Matsumoto, Takuya; Takahashi, Junzo

    2005-12-01

    The chemical analysis of hydroxyapatite and fluorapatite was carried out using time-of-flight secondary ion mass spectrometry (TOF-SIMS). Hydroxyapatite and fluorapatite were synthesized at 80 +/- 1 degrees C and pH 7.4 +/- 0.2. Fluorapatite was better crystallized, with its (300) reflection shifted to a slightly higher angle. High-resolution transmission electron microscopy clearly revealed a typical, regular hexagonal cross section perpendicular to the c-axis for fluorapatite and a flattened hexagonal cross section for hydroxyapatite. FT-IR spectra of fluorapatite confirmed the absence of OH absorption peak--which was seen in hydroxyapatite at about 3570 cm(-1). TOF-SIMS mass spectra showed a peak at 40 amu due to calcium. In addition, a peak at 19 amu due to fluorine could be clearly seen, although the intensities of PO, PO2, and PO3 were very low. It was confirmed that TOF-SIMS clearly showed the differences between positive and negative mass spectra of hydroxyapatite and fluorapatite, especially for F-. We concluded that TOF-SIMS exhibited distinct advantages compared with other methods of analysis.

  18. A-10/TF34 Turbine Engine Monitoring System (TEMS)

    Science.gov (United States)

    Christopher, R. G.

    1981-01-01

    The hardware and software development of the A-10/TF34 turbine engine monitoring system (TEMS) is described. The operation and interfaces of the A-10/TF34 TEMS hardware are discussed with particular emphasis on function, capabilities, and limitations. The TEMS data types are defined and the various data acquisition modes are explained. Potential data products are also discussed.

  19. TEM microstructural analysis of creep deformed CM186LC single crystal Ni-base superalloy

    Energy Technology Data Exchange (ETDEWEB)

    Dubiel, B.; Czyrska-Filemonowicz, A. [AGH Univ. of Science and Technology, Krakow (Poland); Blackler, M. [Howmet Ltd., Exeter (United Kingdom); Barnard, P.M. [ALSTOM Power Turbo-Systems Technology Centre, Rugby (United Kingdom)

    2006-07-01

    The nickel based single crystal superalloy CM186LC was extensively investigated as a potential low cost material for industrial gas turbine vanes within the COST522 programme. The alloy exhibits inhomogeneous structure consisting of dendritic regions and eutectic colonies. In the present work attention is focused on microstructural changes observed in single crystal CM186LC following creep deformation at 750 C. Creep tests were conducted at 750 C with an applied stress of 560 or 675 MPa for up to 11440 hours. The microstructure o ruptured and terminated specimens was investigated by scanning (SEM) and transmission (TEM) electron microscopy. TEM analysis revealed the microstructural changes in the CM186LC at primary and secondary creep as well as after creep rupture. (orig.)

  20. Green synthesis of silver nanoparticles and their characterization by XRD

    Science.gov (United States)

    Mehta, B. K.; Chhajlani, Meenal; Shrivastava, B. D.

    2017-05-01

    A cost effective and environment friendly technique for green synthesis of silver nanoparticles has been reported. Silver nanoparticles have been synthesized using ethanol extract of fruits of Santalum album (Family Santalaceae), commonly known as East Indian sandalwood. Fruits of S.album were collected and crushed. Ethanol was added to the crushed fruits and mixture was exposed to microwave for few minutes. Extract was concentrated by Buchi rotavaporator. To this extract, 1mM aqueous solution of silver nitrate (AgNO3) was added. After about 24 hr incubation Ag+ ions in AgNO3 solution were reduced to Ag atoms by the extract. Silver nanoparticles were obtained in powder form. X-ray diffraction (XRD) pattern of the prepared sample of silver nanoparticles was recorded The diffractogram has been compared with the standard powder diffraction card of JCPDS silver file. Four peaks have been identified corresponding to (hkl) values of silver. The XRD study confirms that the resultant particles are silver nanoparticles having FCC structure. The average crystalline size D, the value of the interplanar spacing between the atoms, d, lattice constant and cell volume have been estimated. Thus, silver nanoparticles with well-defined dimensions could be synthesized by reduction of metal ions due to fruit extract of S.album.

  1. Suspended DNA structural characterization by TEM diffraction

    KAUST Repository

    Marini, Monica

    2017-12-01

    In this work, micro-fabrication, super-hydrophobic properties and a physiologically compatible preparation step are combined and tailored to obtain background free biological samples to be investigated by Transmission Electron Microscopy (TEM) diffraction technique. The validation was performed evaluating a well-known parameter such as the DNA interbases value. The diffraction spacing measured is in good agreement with those obtained by HRTEM direct metrology and by traditional X-Ray diffraction. This approach addresses single molecule studies in a simplified and reproducible straightforward way with respect to more conventional and widely used techniques. In addition, it overcomes the need of long and elaborated samples preparations: the sample is in its physiological environment and the HRTEM data acquisition occurs without any background interference, coating, staining or additional manipulation. The congruence in the results reported in this paper makes the application of this approach extremely promising towards those molecules for which crystallization remains a hurdle, such as cell membrane proteins and fibrillar proteins.

  2. Suspended DNA structural characterization by TEM diffraction

    KAUST Repository

    Marini, Monica; Allione, Marco; Lopatin, Sergei; Moretti, Manola; Giugni, Andrea; Torre, Bruno; Di Fabrizio, Enzo M.

    2017-01-01

    In this work, micro-fabrication, super-hydrophobic properties and a physiologically compatible preparation step are combined and tailored to obtain background free biological samples to be investigated by Transmission Electron Microscopy (TEM) diffraction technique. The validation was performed evaluating a well-known parameter such as the DNA interbases value. The diffraction spacing measured is in good agreement with those obtained by HRTEM direct metrology and by traditional X-Ray diffraction. This approach addresses single molecule studies in a simplified and reproducible straightforward way with respect to more conventional and widely used techniques. In addition, it overcomes the need of long and elaborated samples preparations: the sample is in its physiological environment and the HRTEM data acquisition occurs without any background interference, coating, staining or additional manipulation. The congruence in the results reported in this paper makes the application of this approach extremely promising towards those molecules for which crystallization remains a hurdle, such as cell membrane proteins and fibrillar proteins.

  3. A Combined XRD/XRF Instrument for Lunar Resource Assessment

    Science.gov (United States)

    Vaniman, D. T.; Bish, D. L.; Chipera, S. J.; Blacic, J. D.

    1992-01-01

    Robotic surface missions to the Moon should be capable of measuring mineral as well as chemical abundances in regolith samples. Although much is already known about the lunar regolith, our data are far from comprehensive. Most of the regolith samples returned to Earth for analysis had lost the upper surface, or it was intermixed with deeper regolith. This upper surface is the part of the regolith most recently exposed to the solar wind; as such it will be important to resource assessment. In addition, it may be far easier to mine and process the uppermost few centimeters of regolith over a broad area than to engage in deep excavation of a smaller area. The most direct means of analyzing the regolith surface will be by studies in situ. In addition, the analysis of the impact-origin regolith surfaces, the Fe-rich glasses of mare pyroclastic deposits, are of resource interest, but are inadequately known; none of the extensive surface-exposed pyroclastic deposits of the Moon have been systematically sampled, although we know something about such deposits from the Apollo 17 site. Because of the potential importance of pyroclastic deposits, methods to quantify glass as well as mineral abundances will be important to resource evaluation. Combined x ray diffraction (XRD) and x ray fluorescence (XRF) analysis will address many resource characterization problems on the Moon. XRF methods are valuable for obtaining full major-element abundances with high precision. Such data, collected in parallel with quantitative mineralogy, permit unambiguous determination of both mineral and chemical abundances where concentrations are high enough to be of resource grade. Collection of both XRD and XRF data from a single sample provides simultaneous chemical and mineralogic information. These data can be used to correlate quantitative chemistry and mineralogy as a set of simultaneous linear equations, the solution of which can lead to full characterization of the sample. The use of

  4. Electrochemical maps and movies of the hydrogen evolution reaction on natural crystals of molybdenite (MoS2): basal vs. edge plane activity† †Electronic supplementary information (ESI) available: Movies S1 to S4: spatially resolved LSV-SECCM movies obtained from the electrocatalytic HER on the surface of bulk MoS2. Fig. S1 to S14: XRD, XPS, Raman, SEM and OM characterization of MoS2; SEM images of the nanopipets; WCA measurements; LSVs and Tafel plots obtained from the HER on MoS2. See DOI: 10.1039/c7sc02545a Click here for additional data file. Click here for additional data file. Click here for additional data file. Click here for additional data file. Click here for additional data file.

    Science.gov (United States)

    Kang, Minkyung; Maddar, Faduma M.; Li, Fengwang; Walker, Marc; Zhang, Jie

    2017-01-01

    Two dimensional (2D) semiconductor materials, such as molybdenum disulfide (MoS2) have attracted considerable interest in a range of chemical and electrochemical applications, for example, as an abundant and low-cost alternative electrocatalyst to platinum for the hydrogen evolution reaction (HER). While it has been proposed that the edge plane of MoS2 possesses high catalytic activity for the HER relative to the “catalytically inert” basal plane, this conclusion has been drawn mainly from macroscale electrochemical (voltammetric) measurements, which reflect the “average” electrocatalytic behavior of complex electrode ensembles. In this work, we report the first spatially-resolved measurements of HER activity on natural crystals of molybdenite, achieved using voltammetric scanning electrochemical cell microscopy (SECCM), whereby pixel-resolved linear-sweep voltammogram (LSV) measurements have allowed the HER to be visualized at multiple different potentials to construct electrochemical flux movies with nanoscale resolution. Key features of the SECCM technique are that characteristic surface sites can be targeted and analyzed in detail and, further, that the electrocatalyst area is known with good precision (in contrast to many macroscale measurements on supported catalysts). Through correlation of the local voltammetric response with information from scanning electron microscopy (SEM) and atomic force microscopy (AFM) in a multi-microscopy approach, it is demonstrated unequivocally that while the basal plane of bulk MoS2 (2H crystal phase) possesses significant activity, the HER is greatly facilitated at the edge plane (e.g., surface defects such as steps, edges or crevices). Semi-quantitative treatment of the voltammetric data reveals that the HER at the basal plane of MoS2 has a Tafel slope and exchange current density (J 0) of ∼120 mV per decade and 2.5 × 10–6 A cm–2 (comparable to polycrystalline Co, Ni, Cu and Au), respectively, while the edge

  5. Study of archaeological objects by neutron imaging, xrd and xrf

    International Nuclear Information System (INIS)

    Dinca, M.; Dinu, A. D.; Stanciulescu, M. G.; Mandescu, D.

    2015-01-01

    Archaeological objects were borrowed from Arges County History Museum (ACHM) and investigated at the Institute for Nuclear Research (INR). Metallic objects made in iron, copper alloys and silver discovered in southern part of Romania, mostly Dacian and Roman origin, were investigated. For imaging was used the neutron and gamma imaging facility from tangential channel of the TRIGA ACPR to put in evidence the internal structure of the objects. For elemental and chemical composition, concentration levels in objects were performed investigations by X-ray fluorescence (XRF) and X-ray diffraction (XRD). These investigations offer valuable information in archaeological research about composition, structure of the bulk, presence of alteration, inclusions, typology of the location of material extraction, manufacturing techniques etc. This work is an example of application of neutron imaging and other radiation-based analytical methods for cultural heritage research that had the aim to involve some of the non-destructive investigation methods available at INR. (authors)

  6. High temperature XRD of Cu2GeSe3

    International Nuclear Information System (INIS)

    Premkumar, D. S.; Malar, P.; Chetty, Raju; Mallik, Ramesh Chandra

    2015-01-01

    The Cu 2 GeSe 3 is prepared by solid state synthesis method. The high temperature XRD has been done at different temperature from 30 °C to 450 °C. The reitveld refinement confirms Cu 2 GeSe 3 phase and orthorhombic crystal structure. The lattice constants are increasing with increase in the temperature and their rate of increase with respect to temperature are used for finding the thermal expansion coefficient. The calculation of the linear and volume coefficient of thermal expansion is done from 30 °C to 400 °C. Decrease in the values of linear expansion coefficients with temperature are observed along a and c axis. Since thermal expansion coefficient is the consequence of the distortion of atoms in the lattice; this can be further used to find the minimum lattice thermal conductivity at given temperature

  7. SEM probe of IC radiation sensitivity

    Science.gov (United States)

    Gauthier, M. K.; Stanley, A. G.

    1979-01-01

    Scanning Electron Microscope (SEM) used to irradiate single integrated circuit (IC) subcomponent to test for radiation sensitivity can localize area of IC less than .03 by .03 mm for determination of exact location of radiation sensitive section.

  8. Identification of unknown sample using NAA, EDXRF, XRD techniques

    International Nuclear Information System (INIS)

    Dalvi, Aditi A.; Swain, K.K.; Chavan, Trupti; Remya Devi, P.S.; Wagh, D.N.; Verma, R.

    2015-01-01

    Analytical Chemistry Division (ACD), Bhabha Atomic Research Centre (BARC) receives samples from law enforcement agencies such as Directorate of Revenue Intelligence, Customs for analysis. Five unknown grey powdered samples were received for identification and were suspected to be Iridium (Ir). Identification of unknown sample is always a challenging task and suitable analytical techniques have to be judiciously utilized for arriving at the conclusion. Qualitative analysis was carried out using Jordan Valley, EX-3600 M Energy dispersive X-ray fluorescence (EDXRF) spectrometer at ACD, BARC. A SLP series LEO Si (Li) detector (active area: 30 mm 2 ; thickness: 3.5 mm; resolution: 140 eV at 5.9 keV of Mn K X-ray) was used during the measurement and only characteristic X-rays of Ir (Lα: 9.17 keV and Lβ: 10.70 keV) was seen in the X-ray spectrum. X-ray diffraction (XRD) measurement results indicated that the Ir was in the form of metal. To confirm the XRD data, neutron activation analysis (NAA) was carried out by irradiating samples and elemental standards (as comparator) in graphite reflector position of Advanced Heavy Water Reactor Critical Facility (AHWR CF) reactor, BARC, Mumbai. After suitable decay period, gamma activity measurements were carried out using 45% HPGe detector coupled to 8 k multi channel analyzer. Characteristic gamma line at 328.4 keV of the activation product 194 Ir was used for quantification of iridium and relative method of NAA was used for concentration calculations. NAA results confirmed that all the samples were Iridium metal. (author)

  9. Analytical TEM investigations of nanoscale magnetic materials

    International Nuclear Information System (INIS)

    Meingast, A.

    2015-01-01

    Analytical transmission electron microscopy has been applied within this thesis to investigate several novel approaches to design and fabricate nanoscale magnetic materials. As the size of the features of interest rank in the sub-nanometer range, it is necessary to employ techniques with a resolution – both spatial and analytical – well below this magnitude. Only at this performance level it is possible to examine material properties, necessary for the further tailoring of materials. Within this work two key aspects have been covered: First, analytical TEM (transmission electron microscopy) investigations were carried out to get insight into novel magnetic materials with high detail. Second, new analytical and imaging possibilities enabled with the commissioning of the new ASTEM (Austrian scanning transmission electron microscope) were explored. The aberration corrected TITAN® microscope (© FEI Company) allows resolving features in scanning transmission mode (STEM) with 70 pm distance. Thereby, direct imaging of light elements in STEM mode by using the annular bright field method becomes possible. Facilitated through high beam currents within the electron probe, an increased acquisition speed of analytical signals is possible. For energy dispersive X-ray spectroscopy (EDXS) a new four detector disc geometry around the specimen was implemented, which increases the accessible collection angle. With the integration of the latest generation of image filter and electron spectrometer (GIF QuantumERS), electron energy loss spectroscopy (EELS) is boosted through the high acquisition speed and the dual spectroscopy mode. The high acquisition speed allows to record up to 1000 spectra per second and the possibility to record atomically resolved EELS maps is at hand. Hereby it is important to avoid beam damage and alteration of the material during imaging and analysis. With the simultaneous acquisition of the low and the high loss spectral region, an extended range for

  10. High resolution SEM characterization of nano-precipitates in ODS steels.

    Science.gov (United States)

    Jóźwik, Iwona; Strojny-Nędza, Agata; Chmielewski, Marcin; Pietrzak, Katarzyna; Kurpaska, Łukasz; Nosewicz, Szymon

    2018-05-01

    The performance of the present-day scanning electron microscopy (SEM) extends far beyond delivering electronic images of the surface topography. Oxide dispersion strengthened (ODS) steel is on of the most promising materials for the future nuclear fusion reactor because of its good radiation resistance, and higher operation temperature up to 750°C. The microstructure of ODS should not exceed tens of nm, therefore there is a strong need in a fast and reliable technique for their characterization. In this work, the results of low-kV SEM characterization of nanoprecipitates formed in the ODS matrix are presented. Application of highly sensitive photo-diode BSE detector in SEM imaging allowed for the registration of single nm-sized precipitates in the vicinity of the ODS alloys. The composition of the precipitates has been confirmed by TEM-EDS. © 2018 Wiley Periodicals, Inc.

  11. Comparison of multilayered nanowire imaging by SEM and Helium Ion Microscopy

    International Nuclear Information System (INIS)

    Inkson, B J; Peng, Y; Jepson, M A E; Rodenburg, C; Liu, X

    2010-01-01

    The helium ion microscope (HeIM) is capable of probe sizes smaller than SEM and, with intrinsically small ion/sample interaction volumes, may therefore potentially offer higher spatial resolution secondary electron (SE) imaging of nanostructures. Here 55 nm diameter CoPt/Pt multilayered nanowires have been imaged by HeIM, SEM and TEM. It is found that there is an increased resolution of nanowire surface topography in HeIM SE images compared to SEM, however there is a reduction of materials contrast of the alternating Pt and CoPt layers. This can be attributed to the increased contribution of surface contamination layers to the ion-induced SE signal, and carbon is also observed to grow on the nanowires under prolonged HeIM scanning.

  12. Advanced metrology by offline SEM data processing

    Science.gov (United States)

    Lakcher, Amine; Schneider, Loïc.; Le-Gratiet, Bertrand; Ducoté, Julien; Farys, Vincent; Besacier, Maxime

    2017-06-01

    Today's technology nodes contain more and more complex designs bringing increasing challenges to chip manufacturing process steps. It is necessary to have an efficient metrology to assess process variability of these complex patterns and thus extract relevant data to generate process aware design rules and to improve OPC models. Today process variability is mostly addressed through the analysis of in-line monitoring features which are often designed to support robust measurements and as a consequence are not always very representative of critical design rules. CD-SEM is the main CD metrology technique used in chip manufacturing process but it is challenged when it comes to measure metrics like tip to tip, tip to line, areas or necking in high quantity and with robustness. CD-SEM images contain a lot of information that is not always used in metrology. Suppliers have provided tools that allow engineers to extract the SEM contours of their features and to convert them into a GDS. Contours can be seen as the signature of the shape as it contains all the dimensional data. Thus the methodology is to use the CD-SEM to take high quality images then generate SEM contours and create a data base out of them. Contours are used to feed an offline metrology tool that will process them to extract different metrics. It was shown in two previous papers that it is possible to perform complex measurements on hotspots at different process steps (lithography, etch, copper CMP) by using SEM contours with an in-house offline metrology tool. In the current paper, the methodology presented previously will be expanded to improve its robustness and combined with the use of phylogeny to classify the SEM images according to their geometrical proximities.

  13. Transmission Electron Microscopy (TEM) Sample Preparation of Si(1-x)Gex in c-Plane Sapphire Substrate

    Science.gov (United States)

    Kim, Hyun Jung; Choi, Sang H.; Bae, Hyung-Bin; Lee, Tae Woo

    2012-01-01

    The National Aeronautics and Space Administration-invented X-ray diffraction (XRD) methods, including the total defect density measurement method and the spatial wafer mapping method, have confirmed super hetero epitaxy growth for rhombohedral single crystalline silicon germanium (Si1-xGex) on a c-plane sapphire substrate. However, the XRD method cannot observe the surface morphology or roughness because of the method s limited resolution. Therefore the authors used transmission electron microscopy (TEM) with samples prepared in two ways, the focused ion beam (FIB) method and the tripod method to study the structure between Si1-xGex and sapphire substrate and Si1?xGex itself. The sample preparation for TEM should be as fast as possible so that the sample should contain few or no artifacts induced by the preparation. The standard sample preparation method of mechanical polishing often requires a relatively long ion milling time (several hours), which increases the probability of inducing defects into the sample. The TEM sampling of the Si1-xGex on sapphire is also difficult because of the sapphire s high hardness and mechanical instability. The FIB method and the tripod method eliminate both problems when performing a cross-section TEM sampling of Si1-xGex on c-plane sapphire, which shows the surface morphology, the interface between film and substrate, and the crystal structure of the film. This paper explains the FIB sampling method and the tripod sampling method, and why sampling Si1-xGex, on a sapphire substrate with TEM, is necessary.

  14. Attempt of correlative observation of morphological synaptic connectivity by combining confocal laser-scanning microscope and FIB-SEM for immunohistochemical staining technique.

    Science.gov (United States)

    Sonomura, Takahiro; Furuta, Takahiro; Nakatani, Ikuko; Yamamoto, Yo; Honma, Satoru; Kaneko, Takeshi

    2014-11-01

    Ten years have passed since a serial block-face scanning electron microscopy (SBF-SEM) method was developed [1]. In this innovative method, samples were automatically sectioned with an ultramicrotome placed inside a scanning electron microscope column, and the block surfaces were imaged one after another by SEM to capture back-scattered electrons. The contrast-inverted images obtained by the SBF-SEM were very similar to those acquired using conventional TEM. SFB-SEM has made easy to acquire image stacks of the transmission electron microscopy (TEM) in the mesoscale, which is taken with the confocal laser-scanning microcopy(CF-LSM).Furthermore, serial-section SEM has been combined with the focused ion beam (FIB) milling method [2]. FIB-incorporated SEM (FIB-SEM) has enabled the acquisition of three-dimensional images with a higher z-axis resolution com- pared to ultramicrotome-equipped SEM.We tried immunocytochemistry for FIB-SEM and correlated this immunoreactivity with that in CF-LSM. Dendrites of neurons in the rat neostriatum were visualized using a recombinant viral vector. Moreover, the thalamostriatal afferent terminals were immunolabeled with Cy5 fluorescence for vesicular glutamate transporter 2 (VGluT2). After detection of the sites of terminals apposed to the dendrites by using CF-LSM, GFP and VGluT2 immunoreactivities were further developed for EM by using immunogold/silver enhancement and immunoperoxidase/diaminobenzidine (DAB) methods, respectively.We showed that conventional immuno-cytochemical staining for TEM was applicable to FIB-SEM. Furthermore, several synaptic contacts, which were thought to exist on the basis of CF-LSM findings, were confirmed with FIB-SEM, revealing the usefulness of the combined method of CF-LSM and FIB-SEM. © The Author 2014. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

  15. Experimental study on propagation properties of large size TEM antennas

    International Nuclear Information System (INIS)

    Zhang Guowei; Wang Haiyang; Chen Weiqing; Wang Wei; Zhu Xiangqin; Xie Linshen

    2014-01-01

    The propagation properties of large size TEM antennas were studied by experiment. The size of the TEM antennas is 60 m × 20 m × 10 m and the character Impedance is 120 Ω. A kind of dielectric foil switch is designed compactly with TEM antennas which can generate double exponential waveform with altitude of 10 kV and rise time of l.2 ns. The radiated field distribution was measured. The relationship between rise time/altitude and distance were provided, and the propagation properties of large size TEM antennas were summarized. (authors)

  16. Characterization of North American lignite fly ashes. II. XRD Mineralogy

    International Nuclear Information System (INIS)

    McCarthy, G.J.; Johansen, D.M.; Thedchanamoorthy, A.; Steinwand, S.J.; Swanson, K.D.

    1988-01-01

    X-ray powder diffraction has been used to determine the crystalline phase mineralogy in samples of fly ash from each of the lignite mining areas of North America. The characteristic phases of North Dakota lignite fly ashes were periclase, lime, merwinite and the sulfate phases anhydrite, thenardite and a sodalite-structure phase. Mullite was absent in these low-Al/sub 2/O/sub 3/ ashes. Montana lignite ash mineralogy had characteristics of ND lignite and MT subbituminous coal fly ashes; mullite and C/sub 3/A were present and the alkali sulfates were absent. Texas and Louisiana lignite fly ashes had the characteristic mineralogy of bituminous coal fly ash: quartz, mullite, ferrite-spinel (magnetite) and minor hematite. Even though their analytical CaO contents were 7-14%, all but one lacked crystalline CaO-containing phases. Lignite fly ashes from Saskatchewan were generally the least crystalline of those studied and had a mineralogy consisting of quartz, mullite, ferrite spinel and periclase. Quantitative XRD data were obtained. The position of the diffuse scattering maximum in the x-ray diffractograms was indicative of the glass composition of the lignite fly ash

  17. Oxford CyberSEM: remote microscopy

    International Nuclear Information System (INIS)

    Rahman, M; Kirkland, A; Cockayne, D; Meyer, R

    2008-01-01

    The Internet has enabled researchers to communicate over vast geographical distances, sharing ideas and documents. e-Science, underpinned by Grid and Web Services, has enabled electronic communications to the next level where, in addition to document sharing, researchers can increasingly control high precision scientific instruments over the network. The Oxford CyberSEM project developed a simple Java applet via which samples placed in a JEOL 5510LV Scanning Electron Microscope (SEM) can be manipulated and examined collaboratively over the Internet. Designed with schoolchildren in mind, CyberSEM does not require any additional hardware or software other than a generic Java-enabled web browser. This paper reflects on both the technical and social challenges in designing real-time systems for controlling scientific equipments in collaborative environments. Furthermore, it proposes potential deployment beyond the classroom setting.

  18. Partial Least Squares Strukturgleichungsmodellierung (PLS-SEM)

    DEFF Research Database (Denmark)

    Hair, Joseph F.; Hult, G. Tomas M.; Ringle, Christian M.

    (PLS-SEM) hat sich in der wirtschafts- und sozialwissenschaftlichen Forschung als geeignetes Verfahren zur Schätzung von Kausalmodellen behauptet. Dank der Anwenderfreundlichkeit des Verfahrens und der vorhandenen Software ist es inzwischen auch in der Praxis etabliert. Dieses Buch liefert eine...... anwendungsorientierte Einführung in die PLS-SEM. Der Fokus liegt auf den Grundlagen des Verfahrens und deren praktischer Umsetzung mit Hilfe der SmartPLS-Software. Das Konzept des Buches setzt dabei auf einfache Erläuterungen statistischer Ansätze und die anschauliche Darstellung zahlreicher Anwendungsbeispiele anhand...... einer einheitlichen Fallstudie. Viele Grafiken, Tabellen und Illustrationen erleichtern das Verständnis der PLS-SEM. Zudem werden dem Leser herunterladbare Datensätze, Aufgaben und weitere Fachartikel zur Vertiefung angeboten. Damit eignet sich das Buch hervorragend für Studierende, Forscher und...

  19. FIB-SEM tomography in biology.

    Science.gov (United States)

    Kizilyaprak, Caroline; Bittermann, Anne Greet; Daraspe, Jean; Humbel, Bruno M

    2014-01-01

    Three-dimensional information is much easier to understand than a set of two-dimensional images. Therefore a layman is thrilled by the pseudo-3D image taken in a scanning electron microscope (SEM) while, when seeing a transmission electron micrograph, his imagination is challenged. First approaches to gain insight in the third dimension were to make serial microtome sections of a region of interest (ROI) and then building a model of the object. Serial microtome sectioning is a tedious and skill-demanding work and therefore seldom done. In the last two decades with the increase of computer power, sophisticated display options, and the development of new instruments, an SEM with a built-in microtome as well as a focused ion beam scanning electron microscope (FIB-SEM), serial sectioning, and 3D analysis has become far easier and faster.Due to the relief like topology of the microtome trimmed block face of resin-embedded tissue, the ROI can be searched in the secondary electron mode, and at the selected spot, the ROI is prepared with the ion beam for 3D analysis. For FIB-SEM tomography, a thin slice is removed with the ion beam and the newly exposed face is imaged with the electron beam, usually by recording the backscattered electrons. The process, also called "slice and view," is repeated until the desired volume is imaged.As FIB-SEM allows 3D imaging of biological fine structure at high resolution of only small volumes, it is crucial to perform slice and view at carefully selected spots. Finding the region of interest is therefore a prerequisite for meaningful imaging. Thin layer plastification of biofilms offers direct access to the original sample surface and allows the selection of an ROI for site-specific FIB-SEM tomography just by its pronounced topographic features.

  20. TEM analysis and wear resistance of the ceramic coatings on Q235 steel prepared by hybrid method of hot-dipping aluminum and plasma electrolytic oxidation

    Energy Technology Data Exchange (ETDEWEB)

    Lu Lihong [State Key Laboratory of Metastable Materials Science and Technology, College of Materials Science and Engineering, Yanshan University, Qinhuangdao 066004 (China); Science and Research Department, Chinese People' s Armed Police Academy, Langfang 065000 (China); Zhang Jingwu [State Key Laboratory of Metastable Materials Science and Technology, College of Materials Science and Engineering, Yanshan University, Qinhuangdao 066004 (China); Shen Dejiu, E-mail: sdj217@ysu.edu.cn [State Key Laboratory of Metastable Materials Science and Technology, College of Materials Science and Engineering, Yanshan University, Qinhuangdao 066004 (China); Wu Lailei; Jiang Guirong [State Key Laboratory of Metastable Materials Science and Technology, College of Materials Science and Engineering, Yanshan University, Qinhuangdao 066004 (China); Li Liang [State Key Laboratory of Automotive Safety and Energy, Tsinghua University, Beijing 100084 (China)

    2012-01-25

    Highlights: Black-Right-Pointing-Pointer Transmission electron microscopy (TEM) was firstly used to analyze the phase composition of the ceramic coatings. Black-Right-Pointing-Pointer The phase composition of the ceramic coatings is mainly amorphous phase and crystal Al{sub 2}O{sub 3} oxides. Black-Right-Pointing-Pointer The cross-section micro-hardness of the treated samples was investigated, the hardness of the ceramic coatings is about HV1300. Black-Right-Pointing-Pointer The wear resistance of the PEO samples is about 3 times higher than that of the heat treated 45 steel. - Abstract: The hybrid method of PEO and hot-dipping aluminum (HDA) was employed to deposit composite ceramic coatings on the surface of Q235 steel. The composition of the composite coatings was investigated with X-ray diffraction (XRD) and transmission electron microscopy (TEM), respectively. The cross-section microstructure and micro-hardness of the treated specimens were investigated and analyzed with scanning electron microscopy (SEM) and microscopic hardness meter (MHM), respectively. The wear resistance of the ceramic coatings was investigated by a self-made rubbing wear testing machine. The results indicate that metallurgical bonding can be observed between the ceramic coatings and the steel substrate. There are many micro-pores and micro-cracks, which act as the discharge channels and result of quick and non-uniform cooling of melted sections in the plasma electrolytic oxidation ceramic coatings. The phase composition of the ceramic coatings is mainly composed of amorphous phase and crystal Al{sub 2}O{sub 3} oxides. The crystal Al{sub 2}O{sub 3} phase includes {kappa}-Al{sub 2}O{sub 3}, {theta}-Al{sub 2}O{sub 3} and {beta}-Al{sub 2}O{sub 3}. The grain size of the {kappa}-Al{sub 2}O{sub 3} crystal is quite non-uniform. The hardness of the ceramic coatings is about HV1300 and 10 times higher than that of the Q235 substrate, which was favorable to the better wear resistance of the ceramic

  1. 3D imaging of cells and tissues by focused ion beam/scanning electron microscopy (FIB/SEM).

    Science.gov (United States)

    Drobne, Damjana

    2013-01-01

    Integration of a scanning electron microscope (SEM) and focused ion beam (FIB) technology into a single FIB/SEM system permits use of the FIB as a nano-scalpel to reveal site-specific subsurface microstructures which can be examined in great detail by SEM. The FIB/SEM technology is widely used in the semiconductor industry and material sciences, and recently its use in the life sciences has been initiated. Samples for FIB/SEM investigation can be either embedded in a plastic matrix, the traditional means of preparation of transmission electron microscopy (TEM) specimens, or simply dried as in samples prepared for SEM imaging. Currently, FIB/SEM is used in the life sciences for (a) preparation by the lift-out technique of lamella for TEM analysis, (b) tomography of samples embedded in a matrix, and (c) in situ site-specific FIB milling and SEM imaging using a wide range of magnifications. Site-specific milling and imaging has attracted wide interest as a technique in structural research of single eukaryotic and prokaryotic cells, small animals, and different animal tissue, but it still remains to be explored more thoroughly. In the past, preparation of samples for site-specific milling and imaging by FIB/SEM has typically adopted the embedding techniques used for TEM samples, and which have been very well described in the literature. Sample preparation protocols for the use of dried samples in FIB/SEM have been less well investigated. The aim of this chapter is to encourage application of FIB/SEM on dried biological samples. A detailed description of conventional dried sample preparation and FIB/SEM investigation of dried biological samples is presented. The important steps are described and illustrated, and direct comparison between embedded and dried samples of same tissues is provided. The ability to discover links between gross morphology of the tissue or organ, surface characteristics of any selected region, and intracellular structural details on the nanometer

  2. In-situ TEM Studies : Heat-treatment and Corrosion

    NARCIS (Netherlands)

    Malladi, S.R.K.

    2014-01-01

    Transmission electron microscopy (TEM) has been well known as a powerful characterisation tool to understand the structure and composition of various materials down to the atomic level. Over the years, several TEM studies have been carried out to understand the compositional, structural and

  3. Focus-variation image reconstruction in field-emission TEM

    NARCIS (Netherlands)

    Coene, W.M.J.; Janssen, A.J.E.M.; Op de Beeck, M.; Van Dyck, D.; Van Zwet, E.J.; Zandbergen, H.W.; Bailey, G.W.; Rieder, C.L.

    1993-01-01

    The use of a field emission gun (FEG) in high resolution TEM (HRTEM) improves the information limit much below the point resolution. In the area between point and information resolution of the FEG-TEM, image interpretation is complicated by the lens aberrations and focus effects. Different

  4. XRD characterisation of nanoparticle size and shape distributions

    International Nuclear Information System (INIS)

    Armstrong, N.; Kalceff, W.; Cline, J.P.; Bonevich, J.

    2004-01-01

    Full text: The form of XRD lines and the extent of their broadening provide useful structural information about the shape, size distribution, and modal characteristics of the nanoparticles comprising the specimen. Also, the defect content of the nanoparticles can be determined, including the type, dislocation density, and stacking faults/twinning. This information is convoluted together and can be grouped into 'size' and 'defect' broadening contributions. Modern X-ray diffraction analysis techniques have concentrated on quantifying the broadening arising from the size and defect contributions, while accounting for overlapping of profiles, instrumental broadening, background scattering and noise components. We report on a combined Bayesian/Maximum Entropy (MaxEnt) technique developed for use in the certification of a NIST Standard Reference Material (SRM) for size-broadened line profiles. The approach used was chosen because of its generality in removing instrumental broadening from the observed line profiles, and its ability to determine not only the average crystallite size, but also the distribution of sizes and the average shape of crystallites. Moverover, this Bayesian/MaxEnt technique is fully quantitative, in that it also determines uncertainties in the crystallite-size distribution and other parameters. Both experimental and numerical simulations of size broadened line-profiles modelled on a range of specimens with spherical and non-spherical morphologies are presented to demonstrate how this information can be retrieved from the line profile data. The sensitivity of the Bayesian/MaxEnt method to determining the size distribution using varying a priori information are emphasised and discussed

  5. Accurate quantitative XRD phase analysis of cement clinkers

    International Nuclear Information System (INIS)

    Kern, A.

    2002-01-01

    Full text: Knowledge about the absolute phase abundance in cement clinkers is a requirement for both, research and quality control. Traditionally, quantitative analysis of cement clinkers has been carried out by theoretical normative calculation from chemical analysis using the so-called Bogue method or by optical microscopy. Therefore chemical analysis, mostly performed by X-ray fluorescence (XRF), forms the basis of cement plan control by providing information for proportioning raw materials, adjusting kiln and burning conditions, as well as cement mill feed proportioning. In addition, XRF is of highest importance with respect to the environmentally relevant control of waste recovery raw materials and alternative fuels, as well as filters, plants and sewage. However, the performance of clinkers and cements is governed by the mineralogy and not the elemental composition, and the deficiencies and inherent errors of Bogue as well as microscopic point counting are well known. With XRD and Rietveld analysis a full quantitative analysis of cement clinkers can be performed providing detailed mineralogical information about the product. Until recently several disadvantages prevented the frequent application of the Rietveld method in the cement industry. As the measurement of a full pattern is required, extended measurement times made an integration of this method into existing automation environments difficult. In addition, several drawbacks of existing Rietveld software such as complexity, low performance and severe numerical instability were prohibitive for automated use. The latest developments of on-line instrumentation, as well as dedicated Rietveld software for quantitative phase analysis (TOPAS), now make a decisive breakthrough possible. TOPAS not only allows the analysis of extremely complex phase mixtures in the shortest time possible, but also a fully automated online phase analysis for production control and quality management, free of any human interaction

  6. TEM sample preparation by FIB for carbon nanotube interconnects

    International Nuclear Information System (INIS)

    Ke, Xiaoxing; Bals, Sara; Romo Negreira, Ainhoa; Hantschel, Thomas; Bender, Hugo; Van Tendeloo, Gustaaf

    2009-01-01

    A powerful method to study carbon nanotubes (CNTs) grown in patterned substrates for potential interconnects applications is transmission electron microscopy (TEM). However, high-quality TEM samples are necessary for such a study. Here, TEM specimen preparation by focused ion beam (FIB) has been used to obtain lamellae of patterned samples containing CNTs grown inside contact holes. A dual-cap Pt protection layer and an extensive 5 kV cleaning procedure are applied in order to preserve the CNTs and avoid deterioration during milling. TEM results show that the inner shell structure of the carbon nanotubes has been preserved, which proves that focused ion beam is a useful technique to prepare TEM samples of CNT interconnects.

  7. TEM sample preparation by FIB for carbon nanotube interconnects

    Energy Technology Data Exchange (ETDEWEB)

    Ke, Xiaoxing, E-mail: xiaoxing.ke@ua.ac.be [EMAT, University of Antwerp, Groenenborgerlaan 171, B-2020 Antwerp (Belgium); Bals, Sara [EMAT, University of Antwerp, Groenenborgerlaan 171, B-2020 Antwerp (Belgium); Romo Negreira, Ainhoa [IMEC, Kapeldreef 75, B-3001 Leuven (Belgium); Metallurgy and Materials Engineering Department, KU Leuven, Kasteelpark Arenberg 44, Leuven B-3001 (Belgium); Hantschel, Thomas; Bender, Hugo [IMEC, Kapeldreef 75, B-3001 Leuven (Belgium); Van Tendeloo, Gustaaf [EMAT, University of Antwerp, Groenenborgerlaan 171, B-2020 Antwerp (Belgium)

    2009-10-15

    A powerful method to study carbon nanotubes (CNTs) grown in patterned substrates for potential interconnects applications is transmission electron microscopy (TEM). However, high-quality TEM samples are necessary for such a study. Here, TEM specimen preparation by focused ion beam (FIB) has been used to obtain lamellae of patterned samples containing CNTs grown inside contact holes. A dual-cap Pt protection layer and an extensive 5 kV cleaning procedure are applied in order to preserve the CNTs and avoid deterioration during milling. TEM results show that the inner shell structure of the carbon nanotubes has been preserved, which proves that focused ion beam is a useful technique to prepare TEM samples of CNT interconnects.

  8. Mechanical Conversion for High-Throughput TEM Sample Preparation

    International Nuclear Information System (INIS)

    Kendrick, Anthony B; Moore, Thomas M; Zaykova-Feldman, Lyudmila

    2006-01-01

    This paper presents a novel method of direct mechanical conversion from lift-out sample to TEM sample holder. The lift-out sample is prepared in the FIB using the in-situ liftout Total Release TM method. The mechanical conversion is conducted using a mechanical press and one of a variety of TEM coupons, including coupons for both top-side and back-side thinning. The press joins a probe tip point with attached TEM sample to the sample coupon and separates the complete assembly as a 3mm diameter TEM grid, compatible with commercially available TEM sample holder rods. This mechanical conversion process lends itself well to the high through-put requirements of in-line process control and to materials characterization labs where instrument utilization and sample security are critically important

  9. Crystallographic structure and grain size of polycrystalline Cu{sub 2}ZnSnS{sub 4} nanoparticles and thin films studied with XRD and SEM

    Energy Technology Data Exchange (ETDEWEB)

    Zutz, Folker; Chory, Christine; Riedel, Ingo; Parisi, Juergen [Thin Film Photovoltaics, Energy and Semiconductor Research Laboratory, University of Oldenburg, D-26111 Oldenburg (Germany)

    2011-07-01

    Cu{sub 2}ZnSnS{sub 4} (CZTS) is a compound semiconductor with an absorption coefficient of >10{sup 4} cm{sup -1} and energy gap of about 1.5 eV. Because CZTS is comprised of abundant and non-toxic precursor elements the semiconductor represents an attractive material for low-cost thin film solar cells. CZTS nanoparticles (NP) were prepared in a low-temperature colloidal synthesis yielding high amounts per synthesis cycle. For thin film deposition the NPs were converted to an ink which can be processed to thin films via printing techniques. Finally, the thin films were annealed in argon atmosphere at different temperatures in order to control the growth of microcrystallites. The photoelectrical quality of the semiconductor sensitively depends on the relative concentrations of the precursor elements (band gap, crystallographic phases) and the average grain size (charge transport). We report on structural investigations (X-ray diffraction, electron microscopy) of CZTS dried powders and thin films processed from inks with varying chemical compositions. Further, the evolution of the grain size was studied as function of the annealing temperature.

  10. The application of thermal analysis, XRD and SEM to study the hydration behavior of tricalcium silicate in the presence of a polycarboxylate superplasticizer

    International Nuclear Information System (INIS)

    Liu, Ming; Lei, Jiaheng; Guo, Liping; Du, Xiaodi; Li, Junsheng

    2015-01-01

    Highlights: • The initial hydration process of C 3 S is markedly retarded by PC. • The decomposition temperature of Ca(OH) 2 is slightly lower after PC modification. • The adsorption amount of PC on C 3 S increases progressively with the hydration time. • The size of Ca(OH) 2 crystals are changed due to the adsorption of PC. - Abstract: Hydration behavior of tricalcium silicate (C 3 S) in the presence of a polycarboxylate (PC) superplasticizer was investigated by means of isothermal calorimetry, differential thermal analysis and X-ray diffraction. In addition, the adsorption characteristics of PC and morphology change of Ca(OH) 2 crystals were also examined, respectively. The results showed that initial hydration process of C 3 S was markedly retarded by PC and the retardation effect depended on the dosage of PC. The decomposition temperature of the Ca(OH) 2 was slightly lower after PC modification. Moreover, the size of Ca(OH) 2 crystals were found to be changed due to the adsorption of PC. The results obtained in this research allowed us to gain insights into the interactions between PC and cement

  11. Study the chemical composition and biological outcomes resulting from the interaction of the hormone adrenaline with heavy elements: Infrared, Raman, electronic, 1H NMR, XRD and SEM studies

    Science.gov (United States)

    Ibrahim, Omar B.; Mohamed, Mahmoud A.; Refat, Moamen S.

    2014-01-01

    Heavy metal adrenaline complexes formed from the reaction of adrenaline with Al3+, Zn2+, Sn2+, Sb3+, Pb2+and Bi3+ ions in methanolic solvent at 60 °C. The final reaction products have been isolated and characterization using elemental analyses (% of carbon, hydrogen and nitrogen), conductivity measurements, mid infrared, Raman laser, UV-Vis, 1H NMR spectra, X-ray powder diffraction, scanning electron microscopy and energy-dispersive X-ray spectroscopy (EDX). Upon the spectroscopic, conductivity and elemental analyses, the stoichiometric reactions indicated that the data obtained refer to 1:2 (M:L) for Zn2+, Sn2+, Pb2+and Bi3+ complexes [Zn(Adr)2(Cl)2], [Sn(Adr)2]Cl2, [Pb(Adr)2](NO3)2 and [Bi(Adr)2(Cl)2]Cl, while the molar ratio 1:3 (M:L) for Al3+ and Sb3+ with formulas [Al(Adr)3](NO3)3 and [Sb(Adr)3]Cl3. The infrared and Raman laser spectra interpreted the mode of interactions which associated through the two phenolic groups of catechol moiety. The adrenaline chelates have been screened for their in vitro antibacterial activity against four bacteria, Gram-positive (Bacillus subtilis and Staphylococcus aureus) and Gram-negative (Escherichia coli and Pseudomonas aeruginosa) and two strains of fungus (Aspergillus flavus and Candida albicans). The metal chelates were shown to possess more antibacterial and antifungal activities than the free adrenaline chelate.

  12. Search Engine Marketing (SEM: Financial & Competitive Advantages of an Effective Hotel SEM Strategy

    Directory of Open Access Journals (Sweden)

    Leora Halpern Lanz

    2015-05-01

    Full Text Available Search Engine Marketing and Optimization (SEO, SEM are keystones of a hotels marketing strategy, in fact research shows that 90% of travelers start their vacation planning with a Google search. Learn five strategies that can enhance a hotels SEO and SEM strategies to boost bookings.

  13. Search Engine Marketing (SEM): Financial & Competitive Advantages of an Effective Hotel SEM Strategy

    OpenAIRE

    Leora Halpern Lanz

    2015-01-01

    Search Engine Marketing and Optimization (SEO, SEM) are keystones of a hotels marketing strategy, in fact research shows that 90% of travelers start their vacation planning with a Google search. Learn five strategies that can enhance a hotels SEO and SEM strategies to boost bookings.

  14. XRD measurement of mean crystallite thickness of illite and illite/smectite: Reappraisal of the Kubler index and the Scherrer equation

    Science.gov (United States)

    Drits, Victor A.; Środoń, Jan; Eberl, D.D.

    1997-01-01

    The standard form of the Scherrer equation, which has been used to calculate the mean thickness of the coherent scattering domain (CSD) of illite crystals from X-ray diffraction (XRD) full width data at half maximum (FWHM) intensity, employs a constant, Ksh, of 0.89. Use of this constant is unjustified, even if swelling has no effect on peak broadening, because this constant is valid only if all CSDs have a single thickness. For different thickness distributions, the Scherrer “constant” has very different values.Analysis of fundamental particle thickness data (transmission electron microscopy, TEM) for samples of authigenic illite and illite/smectite from diagenetically altered pyroclastics and filamentous illites from sandstones reveals a unique family of lognormal thickness distributions for these clays. Experimental relations between the distributions' lognormal parameters and mean thicknesses are established. These relations then are used to calculate the mean thickness of CSDs for illitic samples from XRD FWHM, or from integral XRD peak widths (integrated intensity/maximum intensity).For mixed-layer illite/smectite, the measured thickness of the CSD corresponds to the mean thickness of the mixed-layer crystal. Using this measurement, the mean thickness of the fundamental particles that compose the mixed-layer crystals can be calculated after XRD determination of percent smectitic interlayers. The effect of mixed layering (swelling) on XRD peak width for these samples is eliminated by using the 003 reflection for glycolated samples, and the 001, 002 or 003 reflection for dehydrated, K-saturated samples. If this technique is applied to the 001 reflection of air-dried samples (Kubler index measurement), mean CSD thicknesses are underestimated due to the mixed-layering effect.The technique was calibrated using NEW MOD©-simulated XRD profiles of illite, and then tested on well-characterized illite and illite/smectite samples. The XRD measurements are in good

  15. Does Sexually Explicit Media (SEM) Affect Me?

    DEFF Research Database (Denmark)

    Hald, Gert Martin; Træen, Bente; Noor, Syed W

    2015-01-01

    and understanding of one’s sexual orientation.First-person effects refer to self-perceived and self-reported effects of SEM consumptionas experienced by the consumer. In addition, the study examined and provided athorough validation of the psychometric properties of the seven-item PornographyConsumption Effect...

  16. SEM: A user's manual for materials science

    International Nuclear Information System (INIS)

    Gabriel, B.L.

    1985-01-01

    This book provides a reference of techniques used by the metallurgical microscopist. It contains an introduction to the instrumentation and methods of scanning electron microscopy with historical as well as state-of-the-art methodologies. Topics covered include: SEM instrumentation, photography, energy dispersive spectroscopy, introduction to sample preparation, polished samples, fracture surfaces, replicas and thin films

  17. Building a SEM Analytics Reporting Portfolio

    Science.gov (United States)

    Goff, Jay W.; Williams, Brian G.; Kilgore, Wendy

    2016-01-01

    Effective strategic enrollment management (SEM) efforts require vast amounts of internal and external data to ensure that meaningful reporting and analysis systems can assist managers in decision making. A wide range of information is integral for leading effective and efficient student recruitment and retention programs. This article is designed…

  18. XRD and HRTEM characterization of mechanosynthesized Ti{sub 0.9}W{sub 0.1}C cermet

    Energy Technology Data Exchange (ETDEWEB)

    Bandyopadhyay, S. [Department of Physics, The University of Burdwan, Golapbag, Burdwan 713104, West Bengal (India); Dutta, H. [Department of Physics, Vivekananda College, Burdwan 713103, West Bengal (India); Pradhan, S.K., E-mail: skp_bu@yahoo.com [Department of Physics, The University of Burdwan, Golapbag, Burdwan 713104, West Bengal (India)

    2013-12-25

    Highlights: •Cubic Ti{sub 0.9}W{sub 0.1}C is formed after 50 min of milling of α-Ti, W and graphite powders. •Nanocrystalline Ti{sub 0.9}W{sub 0.1}C with particle size ∼11 nm is obtained after 8 h milling. •Average particle size of Ti{sub 0.9}W{sub 0.1}C from XRD analysis and HRTEM is very close. •Formation of Ti{sub 0.9}W{sub 0.1}C is hindered as compared with TiC. -- Abstract: Elemental powder mixture of titanium, tungsten and graphite is milled by high energy planetary ball mill at a fixed ball to powder mass ratio (BPMR) for different duration to produce nanosized particles of Ti{sub 0.9}W{sub 0.1}C hard metal. Microstructure characterization in terms of lattice imperfections and phase quantification of ball-milled samples has been done primarily by analyzing the XRD pattern and employing Rietveld method of structure and microstructure refinement. After 8 h of ball-milling full formation of Ti{sub 0.9}W{sub 0.1}C is noticed without any contamination of other phase or milling media. TEM study of 8 h ball-milled sample gives direct supportive evidence of structural and microstructural evaluation by XRD pattern analysis. A comparative study of microstructural changes between TiC and Ti{sub 0.9}W{sub 0.1}C helps to understand the effect of addition of W as solute in Ti–C metal matrix.

  19. Synchrotron-based XRD from rat bone of different age groups

    Energy Technology Data Exchange (ETDEWEB)

    Rao, D.V., E-mail: dvrao_9@yahoo.com [Science Based Applications to Engineering (SBAI), Physics Division, University of Rome “La Sapienza”, Via Scarpa 10, 00161 Roma (Italy); Gigante, G.E. [Science Based Applications to Engineering (SBAI), Physics Division, University of Rome “La Sapienza”, Via Scarpa 10, 00161 Roma (Italy); Cesareo, R.; Brunetti, A. [Istituto di Matematica e Fisica, Università di Sassari, Via Vienna 2, 07100 Sassari (Italy); Schiavon, N. [Hercules Laboratory, University of Evora (Portugal); Akatsuka, T.; Yuasa, T. [Department of Bio-System Engineering, Faculty of Engineering, Yamagata University, Yonezawa-shi, Yamagata 992-8510 (Japan); Takeda, T. [Allied Health Science, Kitasato University, 1-15-1 Kitasato, Sagamihara, Kanagawa 228-8555 (Japan)

    2017-05-01

    Synchrotron-based XRD spectra from rat bone of different age groups (w, 56 w and 78w), lumber vertebra at early stages of bone formation, Calcium hydroxyapatite (HAp) [Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}] bone fill with varying composition (60% and 70%) and bone cream (35–48%), has been acquired with 15 keV synchrotron X-rays. Experiments were performed at Desy, Hamburg, Germany, utilizing the Resonant and Diffraction beamline (P9), with 15 keV X-rays (λ = 0.82666 A{sup 0}). Diffraction data were quantitatively analyzed using the Rietveld refinement approach, which allowed us to characterize the structure of these samples in their early stages. Hydroxyapatite, received considerable attention in medical and materials sciences, since these materials are the hard tissues, such as bone and teeth. Higher bioactivity of these samples gained reasonable interest for biological application and for bone tissue repair in oral surgery and orthopedics. The results obtained from these samples, such as phase data, crystalline size of the phases, as well as the degree of crystallinity, confirm the apatite family crystallizing in a hexagonal system, space group P6{sub 3}/m with the lattice parameters of a = 9.4328 Å and c = 6.8842 Å (JCPDS card #09-0432). Synchrotron-based XRD patterns are relatively sharp and well resolved and can be attributed to the hexagonal crystal form of hydroxyapatite. All the samples were examined with scanning electron microscope at an accelerating voltage of 15 kV. The presence of large globules of different sizes is observed, in small age groups of the rat bone (8w) and lumber vertebra (LV), as distinguished from, large age groups (56 and 78w) in all samples with different magnification, reflects an amorphous phase without significant traces of crystalline phases. Scanning electron microscopy (SEM) was used to characterize the morphology and crystalline properties of Hap, for all the samples, from 2 to 100 μm resolution. - Highlights: • For

  20. Synchrotron-based XRD from rat bone of different age groups.

    Science.gov (United States)

    Rao, D V; Gigante, G E; Cesareo, R; Brunetti, A; Schiavon, N; Akatsuka, T; Yuasa, T; Takeda, T

    2017-05-01

    Synchrotron-based XRD spectra from rat bone of different age groups (w, 56 w and 78w), lumber vertebra at early stages of bone formation, Calcium hydroxyapatite (HAp) [Ca 10 (PO 4 ) 6 (OH) 2 ] bone fill with varying composition (60% and 70%) and bone cream (35-48%), has been acquired with 15keV synchrotron X-rays. Experiments were performed at Desy, Hamburg, Germany, utilizing the Resonant and Diffraction beamline (P9), with 15keV X-rays (λ=0.82666 A 0 ). Diffraction data were quantitatively analyzed using the Rietveld refinement approach, which allowed us to characterize the structure of these samples in their early stages. Hydroxyapatite, received considerable attention in medical and materials sciences, since these materials are the hard tissues, such as bone and teeth. Higher bioactivity of these samples gained reasonable interest for biological application and for bone tissue repair in oral surgery and orthopedics. The results obtained from these samples, such as phase data, crystalline size of the phases, as well as the degree of crystallinity, confirm the apatite family crystallizing in a hexagonal system, space group P6 3 /m with the lattice parameters of a=9.4328Å and c=6.8842Å (JCPDS card #09-0432). Synchrotron-based XRD patterns are relatively sharp and well resolved and can be attributed to the hexagonal crystal form of hydroxyapatite. All the samples were examined with scanning electron microscope at an accelerating voltage of 15kV. The presence of large globules of different sizes is observed, in small age groups of the rat bone (8w) and lumber vertebra (LV), as distinguished from, large age groups (56 and 78w) in all samples with different magnification, reflects an amorphous phase without significant traces of crystalline phases. Scanning electron microscopy (SEM) was used to characterize the morphology and crystalline properties of Hap, for all the samples, from 2 to 100μm resolution. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. New constraints on deformation processes in serpentinite from sub-micron Raman Spectroscopy and TEM

    Science.gov (United States)

    Smith, S. A. F.; Tarling, M.; Rooney, J. S.; Gordon, K. C.; Viti, C.

    2017-12-01

    Extensive work has been performed to characterize the mineralogical and mechanical properties of the various serpentine minerals (i.e. antigorite, lizardite, chrysotile, polyhedral and polygonal serpentine). However, correct identification of serpentine minerals is often difficult or impossible using conventional analytical techniques such as optical- and SEM-based microscopy, X-ray diffraction and infrared spectroscopy. Transmission Electron Microscopy (TEM) is the best analytical technique to identify the serpentine minerals, but TEM requires complex sample preparation and typically results in very small analysis areas. Sub-micron confocal Raman spectroscopy mapping of polished thin sections provides a quick and relatively inexpensive way of unambiguously distinguishing the main serpentine minerals within their in-situ microstructural context. The combination of high spatial resolution (with a diffraction-limited system, 366 nm), large-area coverage (up to hundreds of microns in each dimension) and ability to map directly on thin sections allows intricate fault rock textures to be imaged at a sample-scale, which can then form the target of more focused TEM work. The potential of sub-micron Raman Spectroscopy + TEM is illustrated by examining sub-micron-scale mineral intergrowths and deformation textures in scaly serpentinites (e.g. dissolution seams, mineral growth in pressure shadows), serpentinite crack-seal veins and polished fault slip surfaces from a serpentinite-bearing mélange in New Zealand. The microstructural information provided by these techniques has yielded new insights into coseismic dehydration and amorphization processes and the interplay between creep and localised rupture in serpentinite shear zones.

  2. Novel sample preparation for operando TEM of catalysts

    International Nuclear Information System (INIS)

    Miller, Benjamin K.; Barker, Trevor M.; Crozier, Peter A.

    2015-01-01

    A new TEM sample preparation method is developed to facilitate operando TEM of gas phase catalysis. A porous Pyrex-fiber pellet TEM sample was produced, allowing a comparatively large amount of catalyst to be loaded into a standard Gatan furnace-type tantalum heating holder. The increased amount of catalyst present inside the environmental TEM allows quantitative determination of the gas phase products of a catalytic reaction performed in-situ at elevated temperatures. The product gas concentration was monitored using both electron energy loss spectroscopy (EELS) and residual gas analysis (RGA). Imaging of catalyst particles dispersed over the pellet at atomic resolution is challenging, due to charging of the insulating glass fibers. To overcome this limitation, a metal grid is placed into the holder in addition to the pellet, allowing catalyst particles dispersed over the grid to be imaged, while particles in the pellet, which are assumed to experience identical conditions, contribute to the overall catalytic conversion inside the environmental TEM cell. The gas within the cell is determined to be well-mixed, making this assumption reasonable. - Highlights: • High in-situ conversion of CO to CO 2 achieved by a novel TEM sample preparation method. • A 3 mm fiber pellet increases the TEM sample surface area by 50×. • Operando atomic resolution is maintained by also including a 3 mm grid in the sample. • Evidence for a well-mixed gas composition inside the ETEM cell is given

  3. Bases de Datos Semánticas

    Directory of Open Access Journals (Sweden)

    Irving Caro Fierros

    2016-12-01

    Full Text Available En 1992, cuando Tim Berners-Lee dio a conocer la primera  versión  de  la  Web,  su  visión  a  futuro  era  incorporar metadatos  con  información  semántica  en  las  páginas  Web.  Es precisamente   a   principios   de   este   siglo   que   inicia   el   auge repentino  de  la  Web  semántica  en  el  ambiente  académico  e Internet. El modelo de datos semántico se define como un modelo conceptual que permite definir el significado de los datos a través de  sus  relaciones  con  otros.  En  este  sentido,  el  formato  de representación  de  los  datos  es  fundamental  para  proporcionar información de carácter semántico. La tecnología enfocada en las bases de datos semánticas se encuentra actualmente en un punto de  inflexión,  al  pasar  del  ámbito  académico  y  de  investigación  a ser una opción comercial completa. En este artículo se realiza un análisis  del  concepto  de  base  de  datos  semántica.  También  se presenta  un  caso  de  estudio  donde  se  ejemplifican  operaciones básicas  que  involucran  la  gestión  de  la  información  almacenada en este tipo de base de datos.

  4. Morphology of Poly lactide/Polycaprolactone (PLA/PCL) Nano composite by Scanning Electron Microscopy (SEM)

    International Nuclear Information System (INIS)

    Siti Zulaiha Hairaldin; Wan Md Zin Wan Yunus; Norazowa Ibrahim

    2011-01-01

    In this study, Octadecylamine Modified Montmorillonites (ODAMMT) were used to prepare Poly lactide/ Polycaprolactone (PLA/ PCL) nano composites. PLA and PCL mix in 90:10 ratios, using an internal mixer by melt blending technique. The other sample was blend with Natrium Montmorillonite (NaMMT) and Octadecylamine Modified Montmorillonite (ODA-MMT) to produce PLA/ PCL-NaMMT and PLA/ PCL ODAMMT. To characterize the polymer nano composites, X-ray diffraction (XRD), FTIR and SEM analysis were conducted. Comparison of morphology were made up between PLA/ PCL, PLA/ PCL with presence of 7 % of Na-MMT and 7 % ODA-MMT respectively based on SEM micrograph by calculate the number-average diameter. (author)

  5. Local behavior of an AISI 304 stainless steel submitted to in situ biaxial loading in SEM

    Energy Technology Data Exchange (ETDEWEB)

    Caër, C., E-mail: celia.caer@gmail.com; Pesci, R.

    2017-04-06

    The microstructural response of a coarse grained AISI 304 stainless steel submitted to biaxial tensile loading was investigated using SEM and X-ray diffraction. The specimen geometry was designed to allow for biaxial stress state and incipient crack in the center of the active part under biaxial tensile loading. This complex loading was performed step by step by a micromachine fitting into a SEM chamber. At each loading step FSD pictures and EBSD measurements were carried out to study the microstructural evolution of the alloy, namely grain rotations and misorientations, stress-induced martensite formation and crack propagation. According to their initial orientation, grains are found to behave differently under loading. Approximately 60% of grains are shown to reorient to the [110] Z orientation under biaxial tensile loading, whereas the 40% left undergo high plastic deformation. EBSD and XRD measurements respectively performed under loading and on the post mortem specimen highlighted the formation of about 4% of martensite.

  6. SEM investigation of heart tissue samples

    Energy Technology Data Exchange (ETDEWEB)

    Saunders, R; Amoroso, M [Physics Department, University of the West Indies, St. Augustine, Trinidad and Tobago, West Indies (Trinidad and Tobago)

    2010-07-01

    We used the scanning electron microscope to examine the cardiac tissue of a cow (Bos taurus), a pig (Sus scrofa), and a human (Homo sapiens). 1mm{sup 3} blocks of left ventricular tissue were prepared for SEM scanning by fixing in 96% ethanol followed by critical point drying (cryofixation), then sputter-coating with gold. The typical ridged structure of the myofibrils was observed for all the species. In addition crystal like structures were found in one of the samples of the heart tissue of the pig. These structures were investigated further using an EDVAC x-ray analysis attachment to the SEM. Elemental x-ray analysis showed highest peaks occurred for gold, followed by carbon, oxygen, magnesium and potassium. As the samples were coated with gold for conductivity, this highest peak is expected. Much lower peaks at carbon, oxygen, magnesium and potassium suggest that a cystallized salt such as a carbonate was present in the tissue before sacrifice.

  7. SEM investigation of heart tissue samples

    International Nuclear Information System (INIS)

    Saunders, R; Amoroso, M

    2010-01-01

    We used the scanning electron microscope to examine the cardiac tissue of a cow (Bos taurus), a pig (Sus scrofa), and a human (Homo sapiens). 1mm 3 blocks of left ventricular tissue were prepared for SEM scanning by fixing in 96% ethanol followed by critical point drying (cryofixation), then sputter-coating with gold. The typical ridged structure of the myofibrils was observed for all the species. In addition crystal like structures were found in one of the samples of the heart tissue of the pig. These structures were investigated further using an EDVAC x-ray analysis attachment to the SEM. Elemental x-ray analysis showed highest peaks occurred for gold, followed by carbon, oxygen, magnesium and potassium. As the samples were coated with gold for conductivity, this highest peak is expected. Much lower peaks at carbon, oxygen, magnesium and potassium suggest that a cystallized salt such as a carbonate was present in the tissue before sacrifice.

  8. Viewing Integrated-Circuit Interconnections By SEM

    Science.gov (United States)

    Lawton, Russel A.; Gauldin, Robert E.; Ruiz, Ronald P.

    1990-01-01

    Back-scattering of energetic electrons reveals hidden metal layers. Experiment shows that with suitable operating adjustments, scanning electron microscopy (SEM) used to look for defects in aluminum interconnections in integrated circuits. Enables monitoring, in situ, of changes in defects caused by changes in temperature. Gives truer picture of defects, as etching can change stress field of metal-and-passivation pattern, causing changes in defects.

  9. Structuring Consumer Preferences with the SEM Method

    OpenAIRE

    Rosa, Franco

    2002-01-01

    Structuring preferences has been developed with econometric models using functional flexible parametric form and the exploring the perceptions about expressed and latent needs using different multivariate approaches. Purpose of this research is to explore the demand for a new drink using the mean-end chain (MEC) theory and multivariate SEM procedure. The first part is dedicated to description of specialty foods for their capacity to create new niche markets. The MEC theory is introduced to ex...

  10. Bases de Datos Semánticas

    OpenAIRE

    Irving Caro Fierros; Víctor Hugo Menéndez Domínguez; María Enriqueta Castellanos Bolaños

    2016-01-01

    En 1992, cuando Tim Berners-Lee dio a conocer la primera  versión  de  la  Web,  su  visión  a  futuro  era  incorporar metadatos  con  información  semántica  en  las  páginas  Web.  Es precisamente   a   principios   de   este   siglo   que   inicia   el   auge repentino  de  la  Web  semántica  en  el  ambiente  académico  e Internet. El modelo de datos semántico se define como un modelo conceptual que permite definir el significado de los datos a través de  sus  relaciones  con  otros.  E...

  11. NPP Multi-Biome: TEM Calibration Data, 1992, R1

    Data.gov (United States)

    National Aeronautics and Space Administration — This data set contains one data file (.csv format) that is known as the Terrestrial Ecosystem Model (TEM) data set. The data provide pool sizes and fluxes of carbon...

  12. NPP Multi-Biome: TEM Calibration Data, 1992, R1

    Data.gov (United States)

    National Aeronautics and Space Administration — ABSTRACT: This data set contains one data file (.csv format) that is known as the Terrestrial Ecosystem Model (TEM) data set. The data provide pool sizes and fluxes...

  13. Conservation through payments for an ecosys- tem service?

    African Journals Online (AJOL)

    tem service? In his Spotlights ... functions” and “ecosystem services” are being ridiculed by the developments in ... high price as legal marketing would avoid various middlemen. ... Diagnostic participatif de la gestion des ressources naturelles.

  14. Preparation of carbon-free TEM microgrids by metal sputtering

    International Nuclear Information System (INIS)

    Janbroers, S.; Kruijff, T.R. de; Xu, Q.; Kooyman, P.J.; Zandbergen, H.W.

    2009-01-01

    A new method for preparing carbon-free, temperature-stable Transmission Electron Microscope (TEM) grids is presented. An 80% Au/20% Pd metal film is deposited onto a 'holey' microgrid carbon supported on standard mixed-mesh Au TEM grids. Subsequently, the carbon film is selectively removed using plasma cleaning. In this way, an all-metal TEM film is made containing the 'same' microgrid as the original carbon film. Although electron transparency of the foil is reduced significantly, the open areas for TEM inspection of material over these areas are maintained. The metal foil can be prepared with various thicknesses and ensures good electrical conductivity. The new Au/Pd grids are stable to at least 775 K under vacuum conditions.

  15. Preparation of carbon-free TEM microgrids by metal sputtering

    Energy Technology Data Exchange (ETDEWEB)

    Janbroers, S., E-mail: stephan.janbroers@albemarle.com [Albemarle Catalysts B.V., Nieuwendammerkade 1-3, 1030 BE, Amsterdam (Netherlands); Kavli Institute of Nanoscience, Delft University of Technology, Lorentzweg 1, 2628 CJ Delft (Netherlands); Kruijff, T.R. de; Xu, Q. [Kavli Institute of Nanoscience, Delft University of Technology, Lorentzweg 1, 2628 CJ Delft (Netherlands); Kooyman, P.J. [DelftChemTech, Delft University of Technology, Julianalaan 136, 2628 BL, Delft (Netherlands); Kavli Institute of Nanoscience, Delft University of Technology, Lorentzweg 1, 2628 CJ Delft (Netherlands); Zandbergen, H.W. [Kavli Institute of Nanoscience, Delft University of Technology, Lorentzweg 1, 2628 CJ Delft (Netherlands)

    2009-08-15

    A new method for preparing carbon-free, temperature-stable Transmission Electron Microscope (TEM) grids is presented. An 80% Au/20% Pd metal film is deposited onto a 'holey' microgrid carbon supported on standard mixed-mesh Au TEM grids. Subsequently, the carbon film is selectively removed using plasma cleaning. In this way, an all-metal TEM film is made containing the 'same' microgrid as the original carbon film. Although electron transparency of the foil is reduced significantly, the open areas for TEM inspection of material over these areas are maintained. The metal foil can be prepared with various thicknesses and ensures good electrical conductivity. The new Au/Pd grids are stable to at least 775 K under vacuum conditions.

  16. Preparation of carbon-free TEM microgrids by metal sputtering.

    Science.gov (United States)

    Janbroers, S; de Kruijff, T R; Xu, Q; Kooyman, P J; Zandbergen, H W

    2009-08-01

    A new method for preparing carbon-free, temperature-stable Transmission Electron Microscope (TEM) grids is presented. An 80% Au/20% Pd metal film is deposited onto a 'holey' microgrid carbon supported on standard mixed-mesh Au TEM grids. Subsequently, the carbon film is selectively removed using plasma cleaning. In this way, an all-metal TEM film is made containing the 'same' microgrid as the original carbon film. Although electron transparency of the foil is reduced significantly, the open areas for TEM inspection of material over these areas are maintained. The metal foil can be prepared with various thicknesses and ensures good electrical conductivity. The new Au/Pd grids are stable to at least 775K under vacuum conditions.

  17. Regulation of ETG turbulence by TEM driven zonal flows

    Science.gov (United States)

    Asahi, Yuuichi; Ishizawa, Akihiro; Watanabe, Tomohiko; Tsutsui, Hiroaki; Tsuji-Iio, Shunji

    2013-10-01

    Anomalous heat transport driven by electron temperature gradient (ETG) turbulence is investigated by means of gyrokinetic simulations. It is found that the ETG turbulence can be suppressed by zonal flows driven by trapped electron modes (TEMs). The TEMs appear in a statistically steady state of ETG turbulence and generate zonal flows, while its growth rate is much smaller than those of ETGs. The TEM-driven zonal flows with lower radial wave numbers are more strongly generated than those driven by ETG modes, because of the higher zonal flow response to a density source term. An ExB shearing rate of the TEM-driven zonal flows is strong enough to suppress the long-wavelength ETG modes which make the main contribution to the turbulent transport.

  18. Indications and techniques of transanal endoscopic microsurgery (TEMS).

    Science.gov (United States)

    Qi, Yanjie; Stoddard, David; Monson, John R T

    2011-08-01

    Transanal endoscopic microsurgery (TEMS) has recently reemerged as a valuable technique for the management of rectal neoplasms - both benign and malignant. Since the original description of this technique in the early 1980s, TEMS has emerged as the approach of choice for most benign rectal tumors because of the excellent views provided and superior dissection techniques possible when compared to traditional transanal excision. Many published reports demonstrate that the lowest rates of recurrence are associated with TEMS probably because of full-thickness excision with negative margins. Increasingly, TEMS is being applied to primary rectal cancer when used alone as a full-thickness excision alone or in combination with additional therapies, depending on tumor stage. There is now a significant evidence base to suggest that this approach should be considered as part of a multidisciplinary approach to rectal cancer. This paper describes indications and techniques for this technology.

  19. Coordinated Isotopic and TEM Studies of Presolar Graphites from Murchison

    Science.gov (United States)

    Croat, T. K.; Stadermann, F. J.; Zinner, E.; Bernatowicz, T. J.

    2004-03-01

    TEM and NanoSIMS investigations of the same presolar Murchison KFC graphites revealed high Zr, Mo, and Ru content in refractory carbides within the graphites. Along with isotopically light carbon, these suggest a low-metallicity AGB source.

  20. Sol-gel route of synthesis of nanoparticles of MgFe2O4 and XRD, FTIR and VSM study

    International Nuclear Information System (INIS)

    Pradeep, A.; Priyadharsini, P.; Chandrasekaran, G.

    2008-01-01

    Nanoparticles of MgFe 2 O 4 are synthesized using sol-gel autocombustion method. Structural studies are carried out using X-ray diffraction (XRD). The XRD pattern of MgFe 2 O 4 provides information about single-phase formation of spinel structure with cubic symmetry. The grain size and lattice constant are obtained using XRD data. The cation distribution is also proposed theoretically. The change in site preference of cations in nano-MgFe 2 O 4 is compared with its bulk counterpart. The structural morphology of the nanoparticles is studied using Scanning Electron Microscopy (SEM). Formation of spinel structure is conformed using Fourier transform infrared spectroscopy (FTIR), which also lends support for the cation distribution proposed using XRD data. The effect of nanoregime on parameters such as bond length, vibration frequency and force constant are discussed with the help of FTIR data. The M-H loop of MgFe 2 O 4 has been traced using the Vibrating Sample Magnetometer (VSM) and magnetic parameters such as saturation magnetization (M S ), coercivity (H C ) and retentivity (M R ) are obtained from VSM data

  1. ToTem: a tool for variant calling pipeline optimization.

    Science.gov (United States)

    Tom, Nikola; Tom, Ondrej; Malcikova, Jitka; Pavlova, Sarka; Kubesova, Blanka; Rausch, Tobias; Kolarik, Miroslav; Benes, Vladimir; Bystry, Vojtech; Pospisilova, Sarka

    2018-06-26

    High-throughput bioinformatics analyses of next generation sequencing (NGS) data often require challenging pipeline optimization. The key problem is choosing appropriate tools and selecting the best parameters for optimal precision and recall. Here we introduce ToTem, a tool for automated pipeline optimization. ToTem is a stand-alone web application with a comprehensive graphical user interface (GUI). ToTem is written in Java and PHP with an underlying connection to a MySQL database. Its primary role is to automatically generate, execute and benchmark different variant calling pipeline settings. Our tool allows an analysis to be started from any level of the process and with the possibility of plugging almost any tool or code. To prevent an over-fitting of pipeline parameters, ToTem ensures the reproducibility of these by using cross validation techniques that penalize the final precision, recall and F-measure. The results are interpreted as interactive graphs and tables allowing an optimal pipeline to be selected, based on the user's priorities. Using ToTem, we were able to optimize somatic variant calling from ultra-deep targeted gene sequencing (TGS) data and germline variant detection in whole genome sequencing (WGS) data. ToTem is a tool for automated pipeline optimization which is freely available as a web application at  https://totem.software .

  2. Characterization of Yeast Biofilm by Cryo-SEM and FIB-SEM

    Czech Academy of Sciences Publication Activity Database

    Hrubanová, Kamila; Nebesářová, Jana; Růžička, F.; Dluhoš, J.; Krzyžánek, Vladislav

    2013-01-01

    Roč. 19, S2 (2013), s. 226-227 ISSN 1431-9276 R&D Projects: GA MŠk EE.2.3.20.0103; GA TA ČR TE01020118; GA ČR GAP205/11/1687 Institutional support: RVO:68081731 ; RVO:60077344 Keywords : yeast biofilm * cryo-SEM * FIB-SEM Subject RIV: BH - Optics, Masers, Lasers Impact factor: 1.757, year: 2013

  3. Novel Sample-handling Approach for XRD Analysis with Minimal Sample Preparation

    Science.gov (United States)

    Sarrazin, P.; Chipera, S.; Bish, D.; Blake, D.; Feldman, S.; Vaniman, D.; Bryson, C.

    2004-01-01

    Sample preparation and sample handling are among the most critical operations associated with X-ray diffraction (XRD) analysis. These operations require attention in a laboratory environment, but they become a major constraint in the deployment of XRD instruments for robotic planetary exploration. We are developing a novel sample handling system that dramatically relaxes the constraints on sample preparation by allowing characterization of coarse-grained material that would normally be impossible to analyze with conventional powder-XRD techniques.

  4. Cultivo sem solo do morangueiro Strawberry soilless cultivation

    Directory of Open Access Journals (Sweden)

    Gustavo Giménez

    2008-02-01

    Full Text Available O morangueiro é uma cultura importante em vários países, principalmente nos Estados Unidos e na Europa, por suas características sensoriais, propriedades nutritivas e por sua rentabilidade. O cultivo comercial sem solo de morangueiro está bem desenvolvido na Europa, onde tem permitido um aumento da produtividade e qualidade da produção assim como a ampliação da oferta do produto ao longo do ano. Predomina o sistema aberto, em sacolas ou vasos com diferentes tipos de substratos, utilizando-se densidades de 8 a 12plantas m-2. As produtividades obtidas estão entre 5 e 10kg m-2. Para isolar as plantas do solo e facilitar o manejo da cultura, os vasos ou sacolas são suspensos a uma altura entre 0,8 e 1m da superfície do solo. A composição da solução nutritiva é variável, refletindo as diferentes condições produtivas. As mudas são produzidas principalmente em bandejas com substrato, a partir de pontas de estolões obtidas da multiplicação de plantas matrizes provenientes da propagação in vitro. No Brasil, o cultivo sem solo de morangueiro é ainda incipiente e os resultados produtivos e econômicos têm sido insatisfatórios, principalmente por falta de informações de pesquisas capazes de indicar sistemas apropriados de cultivo para as condições locais. É necessário desenvolver sistemas sustentáveis, preferencialmente fechados, combinando alta produtividade e elevada eficiência de utilização da água e dos nutrientes. No presente trabalho, são revisados os principais aspectos da produção em sistemas de cultivo sem solo de mudas e fruta de morangueiro. São descritos a produção de mudas, os sistemas e as soluções nutritivas empregadas em diferentes países. Ao final, são feitas inferências sobre a possibilidade de adoção e geração do sistema de cultivo sem solo apropriado para as condições brasileiras.Strawberry is a very important crop in Europe and USA due to its nutritional and sensorial

  5. O ciberativismo sem bússola

    Directory of Open Access Journals (Sweden)

    Francisco Rüdiger

    2014-07-01

    Full Text Available Questiona-se no texto se uma abordagem que, no essencial, relata a trajetória do chamado ciberativismo de acordo com seus próprios termos se justifica academicamente ou, em vez disso, se mantém prisioneira de uma mitologia que o fenômeno, em si mesmo, já construiu e, por isso, autoriza seus sujeitos a dispensarem sem prejuízo eventual contribuição de origem universitária.

  6. Afasia global sem hemiparesia: relato de caso

    OpenAIRE

    SILVA,MARCUS TULIUS TEIXEIRA DA; CAVALCANTI,JOSÉ LUÍS DE SÁ; MOREIRA,DENISE MADEIRA

    2000-01-01

    Afasia global geralmente é acompanhada por hemiparesia direita devido à extensão da lesão subjacente. Recentemente têm sido registrados na literatura casos em que tal síndrome ou não se acompanha do déficit motor ou este é apenas transitório, sendo esta condição conhecida como afasia global sem hemiparesia (AGSH). Relatamos caso de AGSH devido a infarto cerebral embólico cardiogênico, corroborando a tese de que esta condição pode ter valor preditivo para o diagnóstico de infartos embólicos....

  7. Determination of the activation energy in a cast aluminium alloy by TEM and DSC

    International Nuclear Information System (INIS)

    Ovono Ovono, D.; Guillot, I.; Massinon, D.

    2007-01-01

    The precipitation behaviour and microstructure development of the A319 alloy during ageing were investigated by scanning electron microscopy (SEM), transmission electron microscopy (TEM and STEM). During T5 treatment, θ' precipitates with an average size of about 18 nm were observed by TEM. The precipitate sizes increased with ageing temperature and attained an average size of 107 nm. In addition, there was a linear relationship between precipitate growth temperature and the cube of the precipitate size. This indicates that precipitate growth of the A319 alloy belongs to a thermal activated process of the Arrhenius type. The activation energy for the precipitate growth was calculated to be 140.4 ± 13.3 kJ/mol. However, under continuous heating conditions, the activation energy for the precipitate growth obtained by Kissinger plot was determined to be 119.5 ± 8.3 kJ/mol. Allowing for experimental error, both values are comparable and are related to the diffusion of Cu and/or Si in Al

  8. Novel sample preparation for operando TEM of catalysts.

    Science.gov (United States)

    Miller, Benjamin K; Barker, Trevor M; Crozier, Peter A

    2015-09-01

    A new TEM sample preparation method is developed to facilitate operando TEM of gas phase catalysis. A porous Pyrex-fiber pellet TEM sample was produced, allowing a comparatively large amount of catalyst to be loaded into a standard Gatan furnace-type tantalum heating holder. The increased amount of catalyst present inside the environmental TEM allows quantitative determination of the gas phase products of a catalytic reaction performed in-situ at elevated temperatures. The product gas concentration was monitored using both electron energy loss spectroscopy (EELS) and residual gas analysis (RGA). Imaging of catalyst particles dispersed over the pellet at atomic resolution is challenging, due to charging of the insulating glass fibers. To overcome this limitation, a metal grid is placed into the holder in addition to the pellet, allowing catalyst particles dispersed over the grid to be imaged, while particles in the pellet, which are assumed to experience identical conditions, contribute to the overall catalytic conversion inside the environmental TEM cell. The gas within the cell is determined to be well-mixed, making this assumption reasonable. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Exploration of shallow subsurface resistivity structure using a portable TEM system: TEM-FAST prosystem; Kan`igata TEM ho sochi TEM-FAST prosystem ni yoru senbu hiteiko chosa

    Energy Technology Data Exchange (ETDEWEB)

    Miura, Y; Kumekawa, Y; Takasugi, S [GERD Geothermal Energy Research and Development Co. Ltd., Tokyo (Japan)

    1997-05-27

    Discussions were given on effectiveness of the TEM-FAST ProSystem which is a portable TEM system developed recently for use in exploration of shallow subsurface resistivity. The system consists of a loop type antenna, the TEM-FAST as the main equipment, and a host computer, the host computer controlling the entire system. The system acquires transient response data in secondary induced magnetic fields lasting 4 {mu} sec to 1 m sec. The number of data is 5490 stacks in one measurement, and the data acquisition time is about three minutes. Measurements were carried out by using the TEM-FAST in the vicinity of a well, whose results were compared with those of electric logging, and discussions were given on them. Although the electric logging results had no data available for depths shallower than 35 m, the measurement results from the TEM-FAST were found highly harmonious with those of the electric logging. In addition, there were transmission and telephone lines in locations about 10 m away from the well during the measurement, but extremely high data quality was discovered. 6 refs., 7 figs., 1 tab.

  10. A developed wedge fixtures assisted high precision TEM samples pre-thinning method: Towards the batch lamella preparation

    Directory of Open Access Journals (Sweden)

    Dandan Wang

    2017-04-01

    Full Text Available Ion milling, wedge cutting or polishing, and focused ion beam (FIB milling are widely-used techniques for the transmission electron microscope (TEM sample preparation. Especially, the FIB milling provides a site-specific analysis, deposition, and ablation of materials in the micrometer and nanometer scale. However, the cost of FIB tools has been always a significant concern. Since it is inevitable to use the FIB technique, the improvement of efficiency is a key point. Traditional TEM sample preparation with FIB was routinely implemented on a single sample each time. Aiming at cost efficiency, a new pre-thinning technique for batch sample preparation was developed in this paper. The present proposal combines the sample preparation techniques with multi-samples thinning, cross-section scanning electron microscopy (SEM, wedge cutting, FIB and other sample pre-thinning techniques. The new pre-thinning technique is to prepare an edge TEM sample on a grinding and polishing fixture with a slant surface. The thickness of the wedges sample can be measured to 1∼2 μm under optical microscope. Therefore, this fixture is superior to the traditional optical method of estimating the membrane thickness. Moreover, by utilizing a multi-sample holding fixture, more samples can be pre-thinned simultaneously, which significantly improved the productivity of TEM sample preparation.

  11. Remote In-Situ Quantitative Mineralogical Analysis Using XRD/XRF

    Science.gov (United States)

    Blake, D. F.; Bish, D.; Vaniman, D.; Chipera, S.; Sarrazin, P.; Collins, S. A.; Elliott, S. T.

    2001-01-01

    X-Ray Diffraction (XRD) is the most direct and accurate method for determining mineralogy. The CHEMIN XRD/XRF instrument has shown promising results on a variety of mineral and rock samples. Additional information is contained in the original extended abstract.

  12. Performance of a field emission gun TEM/STEM

    International Nuclear Information System (INIS)

    Carpenter, R.W.; Bentley, J.

    1979-01-01

    First experimental results on a Phillips EM 400 TEM/STEM fitted with a field-emission electron gun and objective twin lens are given here. Operation of the FEG is reliable up to maximum design voltage (120 kV). Highest resolution achieved in TEM was 1.9 A fringe. A wide variety of diffraction modes were demonstrated, ranging from CBDP from a small area (approx. 10 A dia) in STEM mode to SAD with angular resolution of 8 μrad in TEM mode. The EDS sensitivity is very high. STEM imaging performance to the highest magnifications examined (200 kx) is good. Work is in progress to evaluate the limits of STEM performance

  13. Tem holder for sample transfer under reaction conditions

    DEFF Research Database (Denmark)

    Damsgaard, Christian Danvad; Zandbergen, Henny W.; Wagner, Jakob Birkedal

    Environmental transmission electron microscopy (ETEM) studies are usually performed using conventional sample holders in a dedicated ETEM [1] or in a traditional TEM by use of a dedicated high-pressure cell sample holder [2]. In both cases, the setup defines the conditions regarding gas, pressure......]. Furthermore, dedicated transfer holders have been used to transfer catalyst samples between reactor set-ups and TEM at room temperature in inert atmosphere [5]. To take the full advantage of complementary in situ techniques, transfer under reactions conditions is essential. This study introduces the in situ...... transfer concept by use of a dedicated TEM transfer holder capable of enclosing the sample in a gaseous environment at temperatures up to approx. 900C. By oxidation and reduction experiments of Cu nanoparticles it is shown possible to keep the reaction conditions during transfer outside the microscope...

  14. SOFC anode reduction studied by in situ TEM

    DEFF Research Database (Denmark)

    Simonsen, Søren Bredmose; Wagner, Jakob Birkedal; Hansen, Thomas Willum

    The Solid Oxide Fuel Cell (SOFC) is a promising part of future energy approaches due to a relatively high energy conversion efficiency and low environmental pollution. SOFCs are typically composed of ceramic materials which are highly complex at the nanoscale. TEM is routinely applied ex situ...... for studying these nanoscale structures, but only few SOFC studies have applied in situ TEM to observe the ceramic nanostructures in a reactive gas environment at elevated temperatures. The present contribution focuses on the reduction of an SOFC anode which is a necessary process to form the catalytically...... active Ni surface before operating the fuel cells. The reduction process was followed in the TEM while exposing a NiO/YSZ (YSZ = Y2O3-stabilized ZrO2) model anode to H2 at T = 250-1000⁰C. Pure NiO was used in reference experiments. Previous studies have shown that the reduction of pure Ni...

  15. SIMS and TEM study on oxide characteristics of Zircaloy

    International Nuclear Information System (INIS)

    Jung, Y. H.; Baek, J. H.; Kim, S. J.; Kim, K. H.; Choi, B. K.; Jung, Y. H.

    1998-01-01

    Long-term corrosion test, SIMS analysis, and TEM study were carried out to investigate the corrosion characteristics and corrosion mechanism of Zircaloy-4 in LiOH solution. The corrosion tests were performed in alkali solutions at 350 deg C for 500days. SIMS analysis was performed for the specimens prepared to have an equal oxide thickness to measure the cation content. TEM studies on the samples formed in various alkali solutions were also conducted. Based on the corrosion test, SIMS analysis, and TEM study, the cation is considered to control the corrosion in LiOH solution and its effect is dependent on the concentration of alkali and the oxide thickness. The slight acceleration of corrosion rate at a low concentration is thought to be caused by the cation incorporation into oxide while the significant acceleration at a high concentration is due to the transformation of oxide microstructure that would be induced by the cation incorporation

  16. Complete Tem-Tomography: 3D Structure of Gems Cluster

    Science.gov (United States)

    Matsuno, J.; Miyake, A.; Tsuchiyama, A.; Messenger, S.; Nakamura-Messenger, K.

    2015-01-01

    GEMS (glass with embedded metal and sulfide) grains in interplanetary dust particles (IDPs) are considered to be one of the ubiquitous and fundamental building blocks of solids in the Solar System. They have been considered to be interstellar silicate dust that survived various metamorphism or alteration processes in the protoplanetary disk but the elemental and isotopic composition measurements suggest that most of them have been formed in the protoplanetary disk as condensates from high temperature gas. This formation model is also supported by the formation of GEMS-like grains with respect to the size, mineral assemblage, texture and infrared spectrum by condensation experiments from mean GEMS composition materials. Previous GEMS studies were performed only with 2D observation by transmission electron microscopy (TEM) or scanning TEM (STEM). However, the 3D shape and structure of GEMS grains and the spatial distribution of Fe/FeS's has critical information about their formation and origin. Recently, the 3D structure of GEMS grains in ultrathin sections of cluster IDPs was revealed by electron tomography using a TEM/STEM (JEM-2100F, JEOL). However, CT images of thin sections mounted on Cu grids acquired by conventional TEM-tomography are limited to low tilt angles (e. g., less than absolute value of 75 deg. In fact, previous 3D TEM observations of GEMS were affected by some artifacts related to the limited tilt range in the TEM used. Complete tomographic images should be acquired by rotating the sample tilt angle over a range of more than absolute value of 80 deg otherwise the CT images lose their correct structures. In order to constrain the origin and formation process of GEMS grains more clearly, we performed complete electron tomography for GEMS grains. Here we report the sample preparation method we have developed for this study, and the preliminary results.

  17. Moessbauer and XRD Characterization of the Mineral Matter of Coal from the Guachinte Mine in Colombia

    International Nuclear Information System (INIS)

    Reyes, F.; Perez Alcazar, G. A.; Barraza, J. M.; Bohorquez, A.; Tabares, J. A.; Speziali, N. L.

    2003-01-01

    The aim of this work was the characterization and differentiation, using Moessbauer spectroscopy (MS) and X-ray diffraction (XRD), of coal samples with different ash and sulfur contents obtained in three places corresponding at cuts in different seams from the Guachinte mine, Valle, Colombia. The mineral phases identified by XRD were in general kaolinite, quartz, pyrite and gypsum, and in particular dolomite and calcite. MS confirms the presence of pyrite and kaolinite, besides evidences the additional presence of jarosite which was not detected by the XRD results due their low amounts. In the high mineral matter ash sample quartz and hematite was identified by XRD, the last one confirmed by MS results. A second phase in this sample was detected by Moessbauer spectroscopy, which could be superparamagnetic hematite. Rietveld refinement for XRD pattern from a sample is reported.

  18. Microstructure and microanalysis (SEM/EDX determination of glasses from Mallorca and Menorca caves

    Directory of Open Access Journals (Sweden)

    Rincón, Jesús María

    1993-12-01

    Full Text Available In recent years a field of research of growing interest has been the application of physico-chemical characterization methods on modern materials to the study of ancient materials found by the archaeologists. This new field on Materials Science is known as Archaeometry. Many questions about the origin and manufacture of ancient glasses can be solved by using the same methods of analysis and microstructure characterization applied normally to special and advanced glasses. The islands of Mallorca and Menorca, located in the Balearic archipelago in the Mediterranean sea, has long been a crossing place of cultures. Transparent, opal and coloured glasses have been found in various archaeological investigations carried out in these islands. In order to know the composition and microstructure of some of these glasses, an archaeometric study has been carried out using X-ray diffraction (XRD, transmission electron microscopy (TEM, scanning electron microscopy and energy-dispersive X-ray analysis (SEM/EDX, differential thermal analysis (DTA, and hot stage optical microscopy (HSM methods. The SEM/EDX average microanalysis results show that these glasses are deficient in sodium and highly enriched in Al2O3 and Fe2O3, their composition being in the range: 0.5-1.5 K2O, 8-10 CaO, 6-8 Al2O3, 6-8 Fe2O3, 74-76 SiO2 (wt%. Some of these glasses also contain high percentages of lead. Small quantities of TiO2, CuO and SO3 (0.5 % have also been detected. Surface decoration and blue colour are other features of these ancient glasses, the surface of which, depicted by SEM, is highly altered with flaked and corroded microstructures.

    En los últimos años la aplicación de los métodos físicoquímicos de caracterización de materiales modernos al estudio de materiales antiguos es un campo de investigación de creciente interés para

  19. Location specific in situ TEM straining specimens made using FIB

    International Nuclear Information System (INIS)

    Field, R.D.; Papin, P.A.

    2004-01-01

    A method has been devised and demonstrated for producing in situ straining specimens for the transmission electron microscope (TEM) from specific locations in a sample using a dual-beam focused ion beam (FIB) instrument. The specimen is removed from a polished surface in the FIB using normal methods and then attached to a pre-fabricated substrate in the form of a modified TEM tensile specimen. In this manner, specific features of the microstructure of a polished optical mount can be selected for in situ tensile straining. With the use of electron backscattered diffraction (EBSD), this technique could be extended to select specific orientations of the specimen as well

  20. Developments in TEM Nanotomography of Calcium Silicate Hydrate

    KAUST Repository

    Taylor, Rae; Sakdinawat, Anne E.; Chae, Sejung R.; Wenk, Haz Rudolf; Levitz, Pierre E.; Sougrat, Rachid; Monteiro, Paulo José Meleragno

    2015-01-01

    This investigation was designed to explore the possibility of using transmission electron microscope (TEM) tomography on cement-based systems gain a greater understanding of their nanostructure and pore network. The preliminary results show a clearly a well-defined pore network at the nanoscale, with pore size approximately 1.7-2.4 nm in diameter and spaced around 5-8 nm apart. A comparison of small angle X-ray scattering data with 2-D TEM images analyzed with the Fourier slice theorem documents an excellent structural correlation. © 2015 The American Ceramic Society.

  1. Developments in TEM Nanotomography of Calcium Silicate Hydrate

    KAUST Repository

    Taylor, Rae

    2015-04-01

    This investigation was designed to explore the possibility of using transmission electron microscope (TEM) tomography on cement-based systems gain a greater understanding of their nanostructure and pore network. The preliminary results show a clearly a well-defined pore network at the nanoscale, with pore size approximately 1.7-2.4 nm in diameter and spaced around 5-8 nm apart. A comparison of small angle X-ray scattering data with 2-D TEM images analyzed with the Fourier slice theorem documents an excellent structural correlation. © 2015 The American Ceramic Society.

  2. Razvijmo sebe, druge in s tem svoj kraj

    Directory of Open Access Journals (Sweden)

    Dušana Findeisen

    1997-12-01

    Full Text Available Dušana Findeisen v tem prispevku obravnava vprašanje, kako spodbuditi ljudi k soodgovornosti za lasten razvoj in razvoj kraja. Preučuje tudi, kako naj prebivalci postanejo soodgovorni za zadostitev lastnih potreb in potreb njihovega kraja. V zvezi s tem se dotakne vloge izobraževalca odraslih - animatorja lokalnih projektov. Poudarja tudi pomen navezovanja novih odnosov in razmerij med lokalnimi skupnostmi in državo ter uvajanje “strukturalne politike”, kot jo imenuje avtorica, za sistemsko pomoč razvoju lokalnih projektov. Nazadnje pa obravnava vlogo lokalnih projektov z vidika razvoja kraja.

  3. El semáforo loco

    OpenAIRE

    González de Zachrisson, Hena

    2016-01-01

    El semáforo lo acababan de instalar en Vía Brasil y Calle 50 y estaba contento de poder mantener el orden del tránsito en tan importante calle. Sin embargo, pronto descubrió que su tarea no era fácil. Su territorio estaba atestado de muchachos que vendían frutas y vegetales y para escapar de ellos, los conductores hacían regatas para cruzar la calle antes de que la luz cambiara a rojo. —Todo a un dólar! —gritaban los chicos mostrando su bolsa de guineo, naranja, melón, maíz, papaya, c...

  4. In-situ SEM electrochemistry and radiolysis

    DEFF Research Database (Denmark)

    Møller-Nilsen, Rolf Erling Robberstad; Norby, Poul

    are backscattered and an image is reconstructed by the microscope. But the high energy electrons are a form of ionising radiation which can significantly affect the chemistry in liquid experiments. Ionising radiation can split water, produce radicals, reduce dissolved metal ions to metal particles, and more...... experiments. During the course of these studies it has also been possible to improve on the EC-SEM system. This has resulted in pyrolysed carbon electrodes, which offer the benefit of stability at 0.75 V higher potentials than traditional gold thin-film electrodes. With the quantitative insight...... microelectrodes on the windows to enable studies of electrohcemical processes. In this way it is possible to perform in-situ electrochemical experiments such as electroplating and charge and discharge analysis of battery electrodes. In a typical liquid cell, electrons are accelerated to sufficiently high energies...

  5. Interaction of selenite with reduced Fe and/or S species: An XRD and XAS study.

    Science.gov (United States)

    Finck, Nicolas; Dardenne, Kathy

    2016-05-01

    In this study, we investigated the interaction between selenite and either Fe((II))aq or S((-II))aq in solution, and the results were used to investigate the interaction between Se((IV))aq and FeS in suspension. The reaction products were characterized by a combination of methods (SEM, XRD and XAS) and the reaction mechanisms were identified. In a first experiment, Se((IV))aq was reduced to Se((0)) by interaction with Fe((II))aq which was oxidized to Fe((III)), but the reaction was only partial. Subsequently, some Fe((III)) produced akaganeite (β-FeOOH) and the release of proton during that reaction decreased the pH. The pH decrease changed the Se speciation in solution which hindered further Se((IV)) reduction by Fe((II))aq. In a second experiment, Se((IV))aq was quantitatively reduced to Se((0)) by S((-II))aq and the reaction was fast. Two sulfide species were needed to reduce one Se((IV)), and the observed pH increase was due to a proton consumption. For both experiments, experimental results are consistent with expectations based on the oxidation reduction potential of the various species. Upon interaction with FeS, Se((IV))aq was reduced to Se((0)) and minute amounts of pyrite were detected, a consequence of partial mackinawite oxidation at surface sulfur sites. These results are of prime importance with respect to safe deep disposal of nuclear waste which contains the long-lived radionuclide (79)Se. This study shows that after release of (79)Se((IV)) upon nuclear waste matrix corrosion, selenite can be reduced in the near field to low soluble Se((0)) by interaction with Fe((II))aq and/or S((-II))aq species. Because the solubility of Se((0)) species is significantly lower than that of Se((IV)), selenium will become much less (bio)available and its migration out of deep HLW repositories may be drastically hindered. Copyright © 2016. Published by Elsevier B.V.

  6. A short note on how to convert a conventional analytical TEM into an analytical Low Voltage TEM

    International Nuclear Information System (INIS)

    Stöger-Pollach, M.

    2014-01-01

    The present work is a short note on the performance of a conventional transmission electron microscope (TEM) being operated at very low beam energies (below 20 keV). We discuss the high tension stability and resolving power of this uncorrected TEM. We find out that the theoretical lens performance can nearly be achieved in practice. We also demonstrate that electron energy loss spectra can be recorded at these low beam energies with standard equipment. The signal-to-noise ratio is sufficiently good for further data treatment like multiple scattering deconvolution and Kramers–Kronig analysis. - Highlights: • TEM operation at very low beam energies (below 20 keV). • Testing of hardware performance at low beam energies. • EELS spectra recorded with 10 keV electrons

  7. TEM sample preparation by femtosecond laser machining and ion milling for high-rate TEM straining experiments

    Energy Technology Data Exchange (ETDEWEB)

    Voisin, Thomas; Grapes, Michael D. [Dept. of Materials Science and Engineering, Johns Hopkins University, Baltimore, MD 21218 (United States); Zhang, Yong [Dept. of Mechanical Engineering, Johns Hopkins University, Baltimore, MD 21218 (United States); Lorenzo, Nicholas; Ligda, Jonathan; Schuster, Brian [US Army Research Laboratory, Aberdeen Proving Ground, Aberdeen, MD 21005 (United States); Weihs, Timothy P. [Dept. of Materials Science and Engineering, Johns Hopkins University, Baltimore, MD 21218 (United States)

    2017-04-15

    To model mechanical properties of metals at high strain rates, it is important to visualize and understand their deformation at the nanoscale. Unlike post mortem Transmission Electron Microscopy (TEM), which allows one to analyze defects within samples before or after deformation, in situ TEM is a powerful tool that enables imaging and recording of deformation and the associated defect motion during mechanical loading. Unfortunately, all current in situ TEM mechanical testing techniques are limited to quasi-static strain rates. In this context, we are developing a new test technique that utilizes a rapid straining stage and the Dynamic TEM (DTEM) at the Lawrence Livermore National Laboratory (LLNL). The new straining stage can load samples in tension at strain rates as high as 4×10{sup 3}/s using two piezoelectric actuators operating in bending while the DTEM at LLNL can image in movie mode with a time resolution as short as 70 ns. Given the piezoelectric actuators are limited in force, speed, and displacement, we have developed a method for fabricating TEM samples with small cross-sectional areas to increase the applied stresses and short gage lengths to raise the applied strain rates and to limit the areas of deformation. In this paper, we present our effort to fabricate such samples from bulk materials. The new sample preparation procedure combines femtosecond laser machining and ion milling to obtain 300 µm wide samples with control of both the size and location of the electron transparent area, as well as the gage cross-section and length. - Highlights: • Tensile straining TEM specimens made by femtosecond laser machining and ion milling. • Accurate positioning of the electron transparent area within a controlled gauge region. • Optimization of femtosecond laser and ion milling parameters. • Fast production of numerous samples with a highly repeatable geometry.

  8. In situ TEM electromechanical testing of nanowires and nanotubes.

    Science.gov (United States)

    Espinosa, Horacio D; Bernal, Rodrigo A; Filleter, Tobin

    2012-11-05

    The emergence of one-dimensional nanostructures as fundamental constituents of advanced materials and next-generation electronic and electromechanical devices has increased the need for their atomic-scale characterization. Given its spatial and temporal resolution, coupled with analytical capabilities, transmission electron microscopy (TEM) has been the technique of choice in performing atomic structure and defect characterization. A number of approaches have been recently developed to combine these capabilities with in-situ mechanical deformation and electrical characterization in the emerging field of in-situ TEM electromechanical testing. This has enabled researchers to establish unambiguous synthesis-structure-property relations for one-dimensional nanostructures. In this article, the development and latest advances of several in-situ TEM techniques to carry out mechanical and electromechanical testing of nanowires and nanotubes are reviewed. Through discussion of specific examples, it is shown how the merging of several microsystems and TEM has led to significant insights into the behavior of nanowires and nanotubes, underscoring the significant role in-situ techniques play in the development of novel nanoscale systems and materials. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Scattering of a TEM wave from a time varying surface

    Science.gov (United States)

    Elcrat, Alan R.; Harder, T. Mark; Stonebraker, John T.

    1990-03-01

    A solution is given for reflection of a plane wave with TEM polarization from a planar surface with time varying properties. These properties are given in terms of the currents on the surface. The solution is obtained by numerically solving a system of differential-delay equations in the time domain.

  10. TEM studies of P+ implanted and subsequently laser annealed Si

    International Nuclear Information System (INIS)

    Sadana, D.K.; Wilson, M.C.; Booker, G.R.; Washburn, J.

    1979-05-01

    The present investigation is concerned with laser annealing of P + implanted Si. The aim of the work was to study the crystallization behavior of damage structure occurring due to high dose rate implantation using transmission electron microscopy (TEM) as the method of examination

  11. Correlation of simulated TEM images with irradiation induced damage

    International Nuclear Information System (INIS)

    Schaeublin, R.; Almeida, P. de; Almazouzi, A.; Victoria, M.

    2000-01-01

    Crystal damage induced by irradiation is investigated using transmission electron microscopy (TEM) coupled to molecular dynamics (MD) calculations. The displacement cascades are simulated for energies ranging from 10 to 50 keV in Al, Ni and Cu and for times of up to a few tens of picoseconds. Samples are then used to perform simulations of the TEM images that one could observe experimentally. Diffraction contrast is simulated using a method based on the multislice technique. It appears that the cascade induced damage in Al imaged in weak beam exhibits little contrast, which is too low to be experimentally visible, while in Ni and Cu a good contrast is observed. The number of visible clusters is always lower than the actual one. Conversely, high resolution TEM (HRTEM) imaging allows most of the defects contained in the sample to be observed, although experimental difficulties arise due to the low contrast intensity of the smallest defects. Single point defects give rise in HTREM to a contrast that is similar to that of cavities. TEM imaging of the defects is discussed in relation to the actual size of the defects and to the number of clusters deduced from MD simulations

  12. TEM specimen preparation of semiconductor-PMMA-metal interfaces

    International Nuclear Information System (INIS)

    Thangadurai, P.; Lumelsky, Yulia; Silverstein, Michael S.; Kaplan, Wayne D.

    2008-01-01

    Transmission electron microscopy (TEM) cross-section specimens of PMMA in contact with gold and Si were prepared by focused ion beam (FIB) and compared with plan-view PMMA specimens prepared by a dip-coating technique. The specimens were characterized by TEM and electron energy loss spectroscopy (EELS). In the cross-section specimens, the thin films of PMMA were located in a Si-PMMA-Au multilayer. Different thicknesses of PMMA films were spin-coated on the Si substrates. The thickness of the TEM specimens prepared by FIB was estimated using EELS to be 0.65 of the plasmon mean-free-path. Along the PMMA-Au interface, Au particle diffusion into the PMMA was observed, and the size of the Au particles was in the range of 2-4 nm. Dip-coating of PMMA directly on Cu TEM grids resulted in thin specimens with a granular morphology, with a thickness of 0.58 of the plasmon mean-free-path. The dip-coated specimens were free from ion milling induced artifacts, and thus serve as control specimens for comparison with the cross-sectioned specimens prepared by FIB

  13. TEM-turbulence in stellarators and its optimization

    Science.gov (United States)

    Proll, Josefine H. E.; Helander, Per; Lazerson, Samuel; Mynick, Harry; Xanthopoulos, Pavlos

    2014-10-01

    Quasi-isodynamic stellarators, which are especially optimized for neoclassical transport, have been shown to be resilient towards trapped-electrons modes (TEMs) in large regions of parameter space. In these configurations, all particles have average ``good curvature.'' It was shown analytically that, thanks to this property, particles that bounce faster than the mode in question draw energy from it near marginal stability, so that the ordinary density-gradient-driven TEM has to be stable in the electrostatic and collisionless limit.This has been confirmed in linear flux-tube simulations that were performed with the GENE code. Several magnetic field configurations were compared and it was found that the growth rates of the TEMs drop with increasing degree of quasi-isodynamicity. These findings can be used to optimize stellarators with respect to TEM turbulence by reducing the fraction of trapped particles with bounce averaged ``bad curvature.'' An appropriate proxy function has therefore been designed to be implemented in STELLOPT, a stellarator optimization tool that can now be used to further explore the configuration space of neoclassically optimized stellarators with the aim to extract designs with improved turbulent transport. This work was facilitated by the Max-Planck/Princeton Center for Plasma Physics.

  14. Applications of Real Space Crystallography in Characterization of Dislocations in Geological Materials in a Scanning Electron Microscope (SEM)

    Science.gov (United States)

    Kaboli, S.; Burnley, P. C.

    2017-12-01

    Imaging and characterization of defects in crystalline materials is of significant importance in various disciplines including geoscience, materials science, and applied physics. Linear defects such as dislocations and planar defects such as twins and stacking faults, strongly influence many of the properties of crystalline materials and also reflect the conditions and degree of deformation. Dislocations have been conventionally imaged in thin foils in a transmission electron microscope (TEM). Since the development of field emission scanning electron microscopes (FE-SEM) with high gun brightness and small spot size, extensive efforts have been dedicated to the imaging and characterization of dislocations in semi-conductors using electron channeling contrast imaging (ECCI) in the SEM. The obvious advantages of using SEM over TEM include easier and non-destructive sample preparation and a large field of view enabling statistical examination of the density and distribution of dislocations and other defects. In this contribution, we extend this technique to geological materials and introduce the Real Space Crystallography methodology for imaging and complete characterization of dislocations based on bend contour contrast obtained by ECCI in FE-SEM. Bend contours map out the distortion in the crystal lattice across a deformed grain. The contrast of dislocations is maximum in the vicinity of bend contours where crystal planes diffract at small and positive deviations from the Bragg positions (as defined by Bragg's law of electron diffraction). Imaging is performed in a commercial FE-SEM equipped with a standard silicon photodiode backscattered (BSE) detector and an electron backscatter diffraction (EBSD) system for crystal orientation measurements. We demonstrate the practice of this technique in characterization of a number of geological materials in particular quartz, forsterite olivine and corundum, experimentally deformed at high pressure-temperature conditions. This

  15. XRF, μ-XRD and μ-spectroscopic techniques for revealing the composition and structure of paint layers on polychrome sculptures after multiple restorations.

    Science.gov (United States)

    Franquelo, M L; Duran, A; Castaing, J; Arquillo, D; Perez-Rodriguez, J L

    2012-01-30

    This paper presents the novel application of recently developed analytical techniques to the study of paint layers on sculptures that have been restored/repainted several times across centuries. Analyses were performed using portable XRF, μ-XRD and μ-Raman instruments. Other techniques, such as optical microscopy, SEM-EDX and μ-FTIR, were also used. Pigments and other materials including vermilion, minium, red lac, ivory black, lead white, barium white, zinc white (zincite), titanium white (rutile and anatase), lithopone, gold and brass were detected. Pigments from both ancient and modern times were found due to the different restorations/repaintings carried out. μ-Raman was very useful to characterise some pigments that were difficult to determine by μ-XRD. In some cases, pigments identification was only possible by combining results from the different analytical techniques used in this work. This work is the first article devoted to the study of sculpture cross-section samples using laboratory-made μ-XRD systems. Copyright © 2011 Elsevier B.V. All rights reserved.

  16. Measuring topographies from conventional SEM acquisitions.

    Science.gov (United States)

    Shi, Qiwei; Roux, Stéphane; Latourte, Félix; Hild, François; Loisnard, Dominique; Brynaert, Nicolas

    2018-04-27

    The present study extends the stereoscopic imaging principle for estimating the surface topography to two orientations, namely, normal to the electron beam axis and inclined at 70° as suited for EBSD analyses. In spite of the large angle difference, it is shown that the topography can be accurately determined using regularized global Digital Image Correlation. The surface topography is compared to another estimate issued from a 3D FIB-SEM procedure where the sample surface is first covered by a Pt layer, and its initial topography is progressively revealed from successive FIB-milling. These two methods are successfully compared on a 6% strained steel specimen in an in situ mechanical test. This analysis is supplemented by a third approach estimating the change of topography from crystal rotations as measured from successive EBSD images. This last technique ignores plastic deformation, and thus only holds in an elastic regime. For the studied example, despite the large plastic flow, it is shown that crystal rotation already accounts for a significant part of the deformation-induced topography. Copyright © 2018 Elsevier B.V. All rights reserved.

  17. 2D Inversion of Transient Electromagnetic Method (TEM)

    Science.gov (United States)

    Bortolozo, Cassiano Antonio; Luís Porsani, Jorge; Acácio Monteiro dos Santos, Fernando

    2017-04-01

    A new methodology was developed for 2D inversion of Transient Electromagnetic Method (TEM). The methodology consists in the elaboration of a set of routines in Matlab code for modeling and inversion of TEM data and the determination of the most efficient field array for the problem. In this research, the 2D TEM modeling uses the finite differences discretization. To solve the inversion problem, were applied an algorithm based on Marquardt technique, also known as Ridge Regression. The algorithm is stable and efficient and it is widely used in geoelectrical inversion problems. The main advantage of 1D survey is the rapid data acquisition in a large area, but in regions with two-dimensional structures or that need more details, is essential to use two-dimensional interpretation methodologies. For an efficient field acquisition we used in an innovative form the fixed-loop array, with a square transmitter loop (200m x 200m) and 25m spacing between the sounding points. The TEM surveys were conducted only inside the transmitter loop, in order to not deal with negative apparent resistivity values. Although it is possible to model the negative values, it makes the inversion convergence more difficult. Therefore the methodology described above has been developed in order to achieve maximum optimization of data acquisition. Since it is necessary only one transmitter loop disposition in the surface for each series of soundings inside the loop. The algorithms were tested with synthetic data and the results were essential to the interpretation of the results with real data and will be useful in future situations. With the inversion of the real data acquired over the Paraná Sedimentary Basin (PSB) was successful realized a 2D TEM inversion. The results indicate a robust geoelectrical characterization for the sedimentary and crystalline aquifers in the PSB. Therefore, using a new and relevant approach for 2D TEM inversion, this research effectively contributed to map the most

  18. Analysis list: sem-4 [Chip-atlas[Archive

    Lifescience Database Archive (English)

    Full Text Available sem-4 Larvae + ce10 http://dbarchive.biosciencedbc.jp/kyushu-u/ce10/target/sem-4.1....tsv http://dbarchive.biosciencedbc.jp/kyushu-u/ce10/target/sem-4.5.tsv http://dbarchive.biosciencedbc.jp/kyushu-u/ce10/target/sem...-4.10.tsv http://dbarchive.biosciencedbc.jp/kyushu-u/ce10/colo/sem-4.Larvae.tsv http://dbarchive.biosciencedbc.jp/kyushu-u/ce10/colo/Larvae.gml ...

  19. Karakteristik Beberapa Jenis Antibiotik Berdasarkan Pola Difraksi Sinar-X (XRD Dan Spektrum FTIR

    Directory of Open Access Journals (Sweden)

    Mirzan T Razzak

    2017-03-01

    Full Text Available Telah dilakukan pengukuran karakteristik difraksi sinar-x (XRD terhadap beberapa jenisantibiotik. Penelitian ini bertujuan untuk memahami karakteristik difraksi sinar-x suatuantibiotik sebagai upaya untuk identifikasi antibiotik secara cepat. Dalam penelitian ini diamatikarakteristik difraksi sinar-x dari 15 (lima belas antibiotik yang tersedia di pasaran. SpektrumXRD diukur pada sudut 2 antara 5 – 75 untuk dibandingkan dan dievaluasi mengenai bentukkristalnya. Selanjutnya diukur pula spektrum XRD dari pencampuran antibiotik dengan tepungtapioka. Pengukuran spektrum infrared dengan FTIR juga dilakukan untuk menguji konsistensihasil evaluasi spektrum XRD. Hasil penelitian menunjukkan bahwa amoxicillin dan ampicillinmempunyai struktur kristal yang sama, yaitu orthorombic primitif. Sayangnya baik XRDmaupun FTIR, tidak memberikan nilai kuantitatif pada antibiotik. Oleh sebab itu, perbedaankonsentrasi dengan pencampuran tepung tapioka tidak dapat dideteksi. Walaupun demikian,metode ini terbukti dapat digunakan untuk membedakan komposisi zat penyusun antibiotiksecara cepat dan akurat.

  20. Mineralogical Composition of the Mexican Ordinary Chondrite Type Meteorite: A Raman, Infrared and XRD Study

    Science.gov (United States)

    Ostrooumov, M.

    2016-08-01

    The Raman microprobe (RMP), infrared (IR) and XRD analysis have been applied to the examination of mineralogical composition of seven mexican meteorites: Aldama, Cosina, El Pozo, Escalon, Nuevo Mercurio,Pacula, Zapotitlan Salinas.

  1. Stirling Energy Module (SEM) as Micro-CHP; Stirling Energy Module (SEM) als Mini-BHKW

    Energy Technology Data Exchange (ETDEWEB)

    Schlegel, A.

    2006-07-01

    Since many years, a lot of effort is being put into the development of combined heat and power units (CHP) for the decentralised production of electric power. For long time, the main focus was on fuel cells. In the meantime, the Stirling technology, which is based upon classical mechanical engineering and innovative technical concepts, proceeded in its development as well. The following article describes the technology and the actual state of the development of the Stirling Energy Module (SEM) for the application as Micro-CHP in one-family-houses. SEM is based on a free-piston engine with a linear power generator, producing electric power while heating. The Stirling engine is planned the be introduced into the market as a replacement for the conventional heating systems within a couple of years. (author)

  2. TEM Nanostructural Study of Al-6Si-3Cu-Mg Melt-Spun Ribbons

    Directory of Open Access Journals (Sweden)

    Ismeli Alfonso López

    2008-01-01

    Full Text Available Three quaternary Al-6Si-3Cu-xMg (x = 0.59, 3.80, and 6.78 wt.% alloys were produced by melt-spun and characterized using X-ray diffractometry (XRD, transmission electron microscopy (TEM, and microhardness techniques. Obtained second phases were Al2Cu( for the alloy with 0.59% Mg and Al5Cu2Mg8Si6 (Q for the alloys with 3.80 and 6.78% Mg. These phases are present as 30–50 nm or as 5–10 nm nanoparticles. Alloying elements content in solid solution increased, mainly for Si and Mg. The high alloying elements content in solid solution and the small -Al cell size for melt-spun alloys leads to microhardness values about 2 times higher than those of ingot counterparts. The microhardness increase for melt-spun alloys with 3.80 and 6.78% Mg depends on Mg content in solid solution.

  3. In situ TEM observation of solid-gas reactions

    International Nuclear Information System (INIS)

    Kishita, K; Kamino, T; Watabe, A; Kuroda, K; Saka, H

    2008-01-01

    Under a gaseous atmosphere at high temperatures, almost all the materials (metal, catalysts, etc.) change their structures and properties. For the research and development of materials, it is of vital importance to clarify mechanisms of solid-gas and liquid-gas reactions. Recently an in situ TEM system combined with an environmental holder, which has a gas injection nozzle close to a specimen-heating element, has been developed. The gas injection nozzle permits gas to flow around the specimens sitting on the heating element made of a fine W filament. The newly developed in situ TEM has a differential pumping system; therefore, the pressure in the specimen chamber is maintained in the range of higher than 1 Pa, while the pressure in the electron gun chamber can be kept in the range of 10 -5 Pa. This system was applied to in situ observation of chemical reactions of metals with gases: Observation of oxidation and reduction under a gas pressure ranging from 10 -5 Pa to 1 Pa at high temperatures (room temperature to ∼1473 K) were successfully carried out on pure metal and rare metal catalysts at near-atomic resolution. This in situ environmental TEM system is promising for clarifying mechanisms of many solid-gas and liquid-gas reactions that take place at high temperatures under a gas atmosphere.

  4. Preparation of TEM specimen by cross-section technique

    International Nuclear Information System (INIS)

    Hamada, Shozo

    1986-01-01

    Transmission electron microscopy (TEM) is applied to the direct observation of the depth dependent damage structure in ion-irradiated stainless steel by using the cross-section technique; obtaining the TEM specimen from a slice of the irradiated stainless steel with thick Ni plating. Here has been developed the specimen preparation method of cross-section technique without heat treatment, which was necessary in the conventional method to strengthen the bonding between Ni and stainless steel. Nickel plating with good bonding to stainless steel is enabled by the following manner. First, the irradiated stainless steel is immersed in the Wood's nickel solution at room temperature for 60s to activate the surface, followed by the stricking for 300s at a current density of 300 A/m 2 in the solution to make fine and homogeneous nucleation of Ni on the stainless steel. Then, the sample is plated with Ni in the Watt's nickel plating solution at 333 K with current density of 900 ∼ 1,000 A/m 2 . The TEM disc is obtained by mechanical slicing from the specimen with Ni plating of more than 3 mm thickness. Electropolishing is accomplished by using both Ballmann method and jet electropolishing to perforate the disc accurately at the aimed point for the observation of the damage structure. (author)

  5. Measurement and characterization of external oil in the fried waxy maize starch granules using ATR-FTIR and XRD.

    Science.gov (United States)

    Chen, Long; Tian, Yaoqi; Sun, Binghua; Cai, Canxin; Ma, Rongrong; Jin, Zhengyu

    2018-03-01

    Concerns regarding increased dietary oil uptake have prompted efforts to investigate the oil absorption and distribution in fried starchy foods. In the present study, attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy, together with a chloroform-methanol method, was used to analyze the external and internal oil contents in fried starchy samples. The micromorphology of fried starchy samples was further investigated using scanning electron microscope (SEM), polarized light microscope (PLM) and confocal laser scanning microscopy (CLSM). The results indicated that large amounts of oil were absorbed in or within waxy maize starch, but the majority of oil was located near the surface layer of the starch granules. After defatting, the internal oil was thoroughly removed, while a small amount of external oil remained. As evidenced by the changes of the crystalline characteristics with the help of X-ray diffraction (XRD), the interaction between starch and lipids on the surface was confirmed to form V-type complex compounds during frying at high moisture. Copyright © 2017 Elsevier Ltd. All rights reserved.

  6. Analysis of phase formation in Ni-rich alloys of the Ni-Ta-W system by calorimetry, DTA, SEM, and TEM

    Energy Technology Data Exchange (ETDEWEB)

    Witusiewicz, V.T.; Hecht, U.; Warnken, N.; Fries, S.G. [Access e.V., Aachen (Germany); Hu Weiping [Inst. fuer Metallkunde und Metallphysik der RWTH Aachen (Germany)

    2006-04-15

    The partial enthalpies of dissolution of pure Ni, W and Ta in liquid ternary Ni-Ta-W alloys have been determined at (1773 {+-} 5) K using a high temperature isoperibolic calorimeter. Measurements were performed in Ni-rich alloys (from 80 to 100 at.% Ni) along sections with constant Ta:W atomic ratios 1:0, 2:1, 1:2, and 0:1. The partial enthalpies and thereby the integral enthalpy of mixing of these ternary alloys are calculated from the partial enthalpies of dissolution using SGTE Gibbs energies for pure elements as reference. The obtained thermochemical data confirm that in the investigated Ni-rich alloys the binary interactions between Ta and W as well as the ternary Ni-Ta-W interactions are negligibly small. Due to this the variation of the integral enthalpy of mixing of the ternary alloys is well described as linear combination of the constituent Ni-Ta and Ni-W binaries. Such behaviour of the ternary liquid alloys is related to a very low probability of new ternary stable phases to occur in solid state. This prediction is confirmed by differential thermal analysis, scanning electron microscopy, and transmission electron microscopy of the as-solidified and annealed samples obtained as last alloy compositions in the series of calorimetric dissolution. (orig.)

  7. Characterization of natural photonic crystals in iridescent wings of damselfly Chalcopteryx rutilans by FIB/SEM, TEM, and TOF-SIMS.

    Science.gov (United States)

    Carr, David M; Ellsworth, Ashley A; Fisher, Gregory L; Valeriano, Wescley W; Vasco, Juan P; Guimarães, Paulo S S; de Andrade, Rodrigo R; da Silva, Elizabeth R; Rodrigues, Wagner N

    2018-02-05

    The iridescent wings of the Chalcopterix rutilans damselfly (Rambur) (Odonata, Polythoridae) are investigated with focused ion beam/scanning electron microscopy, transmission electron microscopy, and time-of-flight secondary ion mass spectrometry. The electron microscopy images reveal a natural photonic crystal as the source of the varying colors. The photonic crystal has a consistent number and thickness (∼195 nm) of the repeat units on the ventral side of the wing, which is consistent with the red color visible from the bottom side of the wing in all regions. The dorsal side of the wing shows strong color variations ranging from red to blue depending on the region. In the electron microscopy images, the dorsal side of the wing exhibits varied number and thicknesses of the repeat units. The repeat unit spacings for the red, yellow/green, and blue regions are approximately 195, 180, and 145 nm, respectively. Three-dimensional analysis of the natural photonic crystals by time-of-flight secondary ion mass spectrometry reveals that changes in the relative levels of Na, K, and eumelanin are responsible for the varying dielectric constant needed to generate the photonic crystal. The photonic crystal also appears to be assembled with a chemical tricomponent layer structure due to the enhancement of the CH 6 N 3 + species at every other interface between the high/low dielectric constant layers.

  8. Sem dança não tem força nenhuma: Creating indigenous spaces in São Paulo urban area

    Directory of Open Access Journals (Sweden)

    Sofia Venturoli

    2016-08-01

    Full Text Available L’articolo presenta alcune tappe fondamentali, politiche e culturali, del processo di formazione dell’associazione indigena Pankararé a San Paolo, Brasile. L’articolo si svolge attraverso le parole di uno dei protagonisti della costruzione del nucleo urbano Pankararé, la leader della associazione Alaìde Pereira Xavier Feitosa. Il racconto di Alaide si muove tra la zona urbana di San Paolo e la terra d’origine situata nello stato di Bahia, per ripercorrere il cammino di costruzione di spazi indigeni e rivendicazioni di cittadinanza differenziata che definiscono la loro legittimità nei percorsi della memoria e nelle pratiche rituali.

  9. A convenient method for X-ray analysis in TEM that measures mass thickness and composition

    Science.gov (United States)

    Statham, P.; Sagar, J.; Holland, J.; Pinard, P.; Lozano-Perez, S.

    2018-01-01

    We consider a new approach for quantitative analysis in transmission electron microscopy (TEM) that offers the same convenience as single-standard quantitative analysis in scanning electron microscopy (SEM). Instead of a bulk standard, a thin film with known mass thickness is used as a reference. The procedure involves recording an X-ray spectrum from the reference film for each session of acquisitions on real specimens. There is no need to measure the beam current; the current only needs to be stable for the duration of the session. A new reference standard with a large (1 mm x 1 mm) area of uniform thickness of 100 nm silicon nitride is used to reveal regions of X-ray detector occlusion that would give misleading results for any X-ray method that measures thickness. Unlike previous methods, the new X-ray method does not require an accurate beam current monitor but delivers equivalent accuracy in mass thickness measurement. Quantitative compositional results are also automatically corrected for specimen self-absorption. The new method is tested using a wedge specimen of Inconel 600 that is used to calibrate the high angle angular dark field (HAADF) signal to provide a thickness reference and results are compared with electron energy-loss spectrometry (EELS) measurements. For the new X-ray method, element composition results are consistent with the expected composition for the alloy and the mass thickness measurement is shown to provide an accurate alternative to EELS for thickness determination in TEM without the uncertainty associated with mean free path estimates.

  10. Clay pigment structure characterisation as a guide for provenance determination--a comparison between laboratory powder micro-XRD and synchrotron radiation XRD.

    Science.gov (United States)

    Švarcová, Silvie; Bezdička, Petr; Hradil, David; Hradilová, Janka; Žižak, Ivo

    2011-01-01

    Application of X-ray diffraction (XRD)-based techniques in the analysis of painted artworks is not only beneficial for indisputable identification of crystal constituents in colour layers, but it can also bring insight in material crystal structure, which can be affected by their geological formation, manufacturing procedure or secondary changes. This knowledge might be helpful for art historic evaluation of an artwork as well as for its conservation. By way of example of kaolinite, we show that classification of its crystal structure order based on XRD data is useful for estimation of its provenance. We found kaolinite in the preparation layer of a Gothic wall painting in a Czech church situated near Karlovy Vary, where there are important kaolin deposits. Comparing reference kaolin materials from eight various Czech deposits, we found that these can be differentiated just according to the kaolinite crystallinity. Within this study, we compared laboratory powder X-ray micro-diffraction (micro-XRD) with synchrotron radiation X-ray diffraction analysing the same real sample. We found that both techniques led to the same results.

  11. Recent improvement of a FIB-SEM serial-sectioning method for precise 3D image reconstruction - application of the orthogonally-arranged FIB-SEM.

    Science.gov (United States)

    Hara, Toru

    2014-11-01

    IntroductionWe installed the first "orthogonally-arranged" FIB-SEM in 2011. The most characteristic point of this instrument is that the FIB and SEM columns are perpendicularly mounted; this is specially designed to obtain a serial-sectioning dataset more accurately and precisely with higher contrast and higher spatial resolution compare to other current FIB-SEMs [1]. Since the installation in 2011, we have developed the hardware and methodology of the serial-sectioning based on this orthogonal FIB-SEM. In order to develop this technique, we have widely opened this instrument to every researcher of all fields. In the presentation, I would like to introduce some of application results that are obtained by users of this instrument. The characteristic points of the orthogonal systemFigure 1 shows a difference between the standard and the orthogonal FIB-SEM systems: In the standard system, shown in Fig.1(a), optical axes of a FIB and a SEM crosses around 60deg., while in the orthogonal system (Fig.1(b)), they are perpendicular to each other. The standard arrangement (a) is certainly suitable for TEM lamellae preparation etc. because the FIB and the SEM can see the same position simultaneously. However, for a serial-sectioning, it is not to say the best arrangement. One of the reasons is that the sliced plane by the FIB is not perpendicular to the electron beam so that the background contrast is not uniform and observed plane is distorted. On the other hand, in case of the orthogonally-arranged system,(b), these problems are resolved. In addition, spatial resolution can keep high enough even in a low accelerating voltage (e.g. 500V) because a working distance is set very small, 2mm. From these special design, we can obtain the serial-sectioning dataset from rather wide area (∼100um) with high spatial resolution (Max. 2×2×2nm). As this system has many kinds of detectors: SE, ET, Backscatter Electron(Energy-selective), EDS, EBSD, STEM(BF&ADF), with Ar+ ion-gun and a

  12. Objective function analysis for electric soundings (VES), transient electromagnetic soundings (TEM) and joint inversion VES/TEM

    Science.gov (United States)

    Bortolozo, Cassiano Antonio; Bokhonok, Oleg; Porsani, Jorge Luís; Monteiro dos Santos, Fernando Acácio; Diogo, Liliana Alcazar; Slob, Evert

    2017-11-01

    Ambiguities in geophysical inversion results are always present. How these ambiguities appear in most cases open to interpretation. It is interesting to investigate ambiguities with regard to the parameters of the models under study. Residual Function Dispersion Map (RFDM) can be used to differentiate between global ambiguities and local minima in the objective function. We apply RFDM to Vertical Electrical Sounding (VES) and TEM Sounding inversion results. Through topographic analysis of the objective function we evaluate the advantages and limitations of electrical sounding data compared with TEM sounding data, and the benefits of joint inversion in comparison with the individual methods. The RFDM analysis proved to be a very interesting tool for understanding the joint inversion method of VES/TEM. Also the advantage of the applicability of the RFDM analyses in real data is explored in this paper to demonstrate not only how the objective function of real data behaves but the applicability of the RFDM approach in real cases. With the analysis of the results, it is possible to understand how the joint inversion can reduce the ambiguity of the methods.

  13. Canticum Novum: música sem palavras e palavras sem som no pensamento de Santo Agostinho

    Directory of Open Access Journals (Sweden)

    Lorenzo Mammì

    2000-04-01

    Full Text Available NO De Magistro, Santo Agostinho coloca a reza e o canto numa posição similar, à margem das funções imediatamente comunicativas da linguagem. A reflexão agostiniana sobre a reza se baseia nos hábitos cristãos da leitura, da oração e da meditação silenciosas. Há sobre o canto, na prática igualmente inovadora do jubilus, melodia sem palavra destinada aos momentos mais intensos e gaudiosos da liturgia. A oração silenciosa e o jubilus são temas recorrentes da literatura patrística, mas Agostinho os aborda de maneira original, desenhando, a partir das palavras sem som da oração e do som sem palavra do jubilus, o perfil de um discurso interior, que não se destina aos homens, mas a Deus.IN HIS De Magistro Saint Augustine places prayer and song on a similar level, alongside the language immediately communicative functions. His considerations on prayer are grounded on the Christian habits of silent reading, prayer and meditation; those on song, on the equally innovating practice called jubilus, which is melody without words designed for the intensest and most joyous liturgical moments. Silent prayer and jubilus are recurring topics in patristic literature, but Augustine deals with them in an original way, drawing from the soundless words of prayer and the wordless sound of jubilus an inner discourse, addressed not to men but to God.

  14. Quantifying Golgi structure using EM: combining volume-SEM and stereology for higher throughput.

    Science.gov (United States)

    Ferguson, Sophie; Steyer, Anna M; Mayhew, Terry M; Schwab, Yannick; Lucocq, John Milton

    2017-06-01

    Investigating organelles such as the Golgi complex depends increasingly on high-throughput quantitative morphological analyses from multiple experimental or genetic conditions. Light microscopy (LM) has been an effective tool for screening but fails to reveal fine details of Golgi structures such as vesicles, tubules and cisternae. Electron microscopy (EM) has sufficient resolution but traditional transmission EM (TEM) methods are slow and inefficient. Newer volume scanning EM (volume-SEM) methods now have the potential to speed up 3D analysis by automated sectioning and imaging. However, they produce large arrays of sections and/or images, which require labour-intensive 3D reconstruction for quantitation on limited cell numbers. Here, we show that the information storage, digital waste and workload involved in using volume-SEM can be reduced substantially using sampling-based stereology. Using the Golgi as an example, we describe how Golgi populations can be sensed quantitatively using single random slices and how accurate quantitative structural data on Golgi organelles of individual cells can be obtained using only 5-10 sections/images taken from a volume-SEM series (thereby sensing population parameters and cell-cell variability). The approach will be useful in techniques such as correlative LM and EM (CLEM) where small samples of cells are treated and where there may be variable responses. For Golgi study, we outline a series of stereological estimators that are suited to these analyses and suggest workflows, which have the potential to enhance the speed and relevance of data acquisition in volume-SEM.

  15. A new procedure for making TEM specimens of superconductor devices

    International Nuclear Information System (INIS)

    Huang, Y.; Merkle, K.L.

    1997-04-01

    A new procedure is developed for making TEM specimens of thin film devices. In this procedure the sample is flatly polished to an overall ion-mill-ready thickness so that any point in the 2-D sample pane can be thinned to an electron-transparent thickness by subsequent ion-milling. Using this procedure, small regions of interest can be easily reached in both cross-section and plan-view samples. This is especially useful in device studies. Applications of this procedure to the study of superconductor devices yield good results. This procedure, using commercially available equipment and relatively cheap materials, is simple and easy to realize

  16. Easy process to obtain suspended graphene flakes on TEM grids

    International Nuclear Information System (INIS)

    Gonçalves, Hugo; Fernandes, Joel; Moura, Cacilda; Schellenberg, Peter; Belsley, Michael; Alves, Luís

    2015-01-01

    Much of the ongoing research on graphene requires free-hanging (suspended) graphene to eliminate any influence from underlying substrates. Several methods have been developed for its preparation but they are either very complex or not completely reliable. Here, we describe a simple method for the transfer of graphene single layers from glass or silicon substrates onto TEM grids. The method uses a carrier film for the transfer process. By optimizing the process yields greater than 60% were achieved. The integrity of the transferred films was confirmed using Raman spectroscopy; successful suspension of both mono- and double-layer graphene sheets was obtained. (paper)

  17. In-situ TEM characterization of nanomaterials and devices

    KAUST Repository

    Kim, Moon; Park, Seongyong; Cha, Dong Kyu; Kim, Jiyoung; Floresca, Herman Carlo; Lu, Ning; Wang, Jinguo

    2011-01-01

    Electrical properties of nano size devices were directly measured by TEM. Real time observation of phase transition behavior in PRAM revealed that the volume of the crystalline phase is the main factor in determining cell resistance. In the transistor device, we have identified the doping type and area by measuring the I-V curve at the individual nano contact on the specimen. The evolution of the graphene edge structure was controlled and monitored at and up to 1200°C in-situ. © 2011 IEEE.

  18. TEM observations of HT-9 as-welded weldment microstructures

    International Nuclear Information System (INIS)

    Foulds, J.R.; Lechtenberg, T.A.

    1984-01-01

    TEM studies of different locations in an HT-9 weldment indicated delta-ferrite (delta) occurrence, M 23 C 6 precipitation at delta-martensite interfaces, fine carbide precipitation at prior austenite grain boundaries, and martensite lath and lath packet size to be the distinguishable microstructure features observed. Furthermore, retained austenite films were observed in the weld metal and the HAZ adjacent to the weld metal that reached the highest temperature during joining. The microstructures correlate well with the observed room temperature microhardness except for the fusion boundary in weld metal which exhibited a hardness drop and an unexpected minimum amount of delta-ferrite

  19. Microfabricated Nanofluidic cells for in situ liquid TEM

    DEFF Research Database (Denmark)

    Laganà, Simone

    Over the last decade, transmission electron microscopy (TEM) has been revolutionized not only by the introduction of new and very sophisticated hardware for improved resolution, such as aberration correctors and monochromators, but also by the improvement of new methods that have provided more than......, allowing quantitative and high-precision acquisition of liquid thickness maps, high resolution observations and meaningful information about synthesis of NPs from metal precursor solutions in confined space. Finally, a new concept device based on a Si3N4 membrane for plunge freezing fixation, which enables...

  20. TEM Imaging of Mass-selected Polymer Molecules

    International Nuclear Information System (INIS)

    Nasibulin, Albert G.; Kauppinen, Esko I.; Thomson, Bruce A.; Fernandez de la Mora, J.

    2002-01-01

    Polyethylene glycol (PEG) molecules with masses below 1300 amu are electrosprayed (ES) from solution, mobility-selected at high resolution in a differential mobility analyzer (DMA), collected on a grid and imaged by transmission electron microscopy (ES-DMA-TEM). The DMA resolves individual n-mers, and selects only one out of the many present in the original sample. Ion identity is established from parallel mass spectra (ES-MS). The images reveal spherical particles 1.46 nm in diameter, in good agreement with the known ion mass and bulk density. The DMA-selection technique opens new paths for the study of very small particles

  1. Shear Punch Testing of BOR-60 Irradiated TEM Specimens

    Energy Technology Data Exchange (ETDEWEB)

    Saleh, Tarik A. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Quintana, Matthew Estevan [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Romero, Tobias J. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2017-06-13

    As a part of the project “High Fidelity Ion Beam Simulation of High Dose Neutron Irradiation” an Integrated Research Program (IRP) project from the U.S. Department of Energy, Nuclear Energy University Programs (NEUP), TEM geometry samples of ferritic cladding alloys, Ni based super alloys and model alloys were irradiated in the BOR-60 reactor to ~16 dpa at ~370°C and ~400°C. Samples were sent to Los Alamos National Laboratory and subjected to shear punch testing. This report presents the results from this testing.

  2. TEM INVESTIGATIONS OF WC-Co ALLOYS AFTER CREEP EXPERIMENTS

    OpenAIRE

    Lay , S.; Osterstock , F.; Vicens , J.

    1986-01-01

    Carbide tungsten cobalt alloys were deformed in compression or in three point bending in a temperature range 1000-1350°C and in a stress domain 30-1000MPa. In these conditions, the stress exponent n of WC-Co alloys is a function of only the cobalt volumic ratio and tends towards n = 1 for pure carbide. The apparent activation energy is 550 kj mole-1. T.E.M. investigations on pure carbide deformed at 1450°C show an extensive intragranular deformation. Analysis of these defects have been perfor...

  3. In-situ TEM characterization of nanomaterials and devices

    KAUST Repository

    Kim, Moon

    2011-10-01

    Electrical properties of nano size devices were directly measured by TEM. Real time observation of phase transition behavior in PRAM revealed that the volume of the crystalline phase is the main factor in determining cell resistance. In the transistor device, we have identified the doping type and area by measuring the I-V curve at the individual nano contact on the specimen. The evolution of the graphene edge structure was controlled and monitored at and up to 1200°C in-situ. © 2011 IEEE.

  4. Stability of mineral fibres in contact with human cell cultures. An in situ μXANES, μXRD and XRF iron mapping study.

    Science.gov (United States)

    Pollastri, Simone; Gualtieri, Alessandro F; Vigliaturo, Ruggero; Ignatyev, Konstantin; Strafella, Elisabetta; Pugnaloni, Armanda; Croce, Alessandro

    2016-12-01

    Relevant mineral fibres of social and economic importance (chrysotile UICC, crocidolite UICC and a fibrous erionite from Jersey, Nevada, USA) were put in contact with cultured diploid human non-tumorigenic bronchial epithelial (Beas2B) and pleural transformed mesothelial (MeT5A) cells to test their cytotoxicity. Slides of each sample at different contact times up to 96 h were studied in situ using synchrotron XRF, μ-XRD and μ-XAS (I18 beamline, Diamond Light Source, UK) and TEM investigations. XRF maps of samples treated for 96 h evidenced that iron is still present within the chrysotile and crocidolite fibres and retained at the surface of the erionite fibres, indicating its null to minor mobilization in contact with cell media; this picture was confirmed by the results of XANES pre-edge analyses. μ-XRD and TEM data indicate greater morphological and crystallinity modifications occurring in chrysotile, whereas crocidolite and erionite show to be resistant in the biological environment. The contact of chrysotile with the cell cultures seems to lead to earlier amorphization, interpreted as the first dissolution step of these fibres. The formation of such silica-rich fibre skeleton may prompt the production of HO in synergy with surface iron species and could indicate that chrysotile may be much more reactive and cytotoxic in vitro in the (very) short term whereas the activity of crocidolite and erionite would be much more sluggish but persistent in the long term. Copyright © 2016 Elsevier Ltd. All rights reserved.

  5. Three-dimensional intracellular structure of a whole rice mesophyll cell observed with FIB-SEM.

    Science.gov (United States)

    Oi, Takao; Enomoto, Sakiko; Nakao, Tomoyo; Arai, Shigeo; Yamane, Koji; Taniguchi, Mitsutaka

    2017-07-01

    Ultrathin sections of rice leaf blades observed two-dimensionally using a transmission electron microscope (TEM) show that the chlorenchyma is composed of lobed mesophyll cells, with intricate cell boundaries, and lined with chloroplasts. The lobed cell shape and chloroplast positioning are believed to enhance the area available for the gas exchange surface for photosynthesis in rice leaves. However, a cell image revealing the three-dimensional (3-D) ultrastructure of rice mesophyll cells has not been visualized. In this study, a whole rice mesophyll cell was observed using a focused ion beam scanning electron microscope (FIB-SEM), which provides many serial sections automatically, rapidly and correctly, thereby enabling 3-D cell structure reconstruction. Rice leaf blades were fixed chemically using the method for conventional TEM observation, embedded in resin and subsequently set in the FIB-SEM chamber. Specimen blocks were sectioned transversely using the FIB, and block-face images were captured using the SEM. The sectioning and imaging were repeated overnight for 200-500 slices (each 50 nm thick). The resultant large-volume image stacks ( x = 25 μm, y = 25 μm, z = 10-25 μm) contained one or two whole mesophyll cells. The 3-D models of whole mesophyll cells were reconstructed using image processing software. The reconstructed cell models were discoid shaped with several lobes around the cell periphery. The cell shape increased the surface area, and the ratio of surface area to volume was twice that of a cylinder having the same volume. The chloroplasts occupied half the cell volume and spread as sheets along the cell lobes, covering most of the inner cell surface, with adjacent chloroplasts in close contact with each other. Cellular and sub-cellular ultrastructures of a whole mesophyll cell in a rice leaf blade are demonstrated three-dimensionally using a FIB-SEM. The 3-D models and numerical information support the hypothesis that rice mesophyll

  6. Response Time Measurements of the NIF DANTE XRD-31 X-Ray Diodes (Pre-print)

    International Nuclear Information System (INIS)

    Pellinen, Don; Griffin, Michael

    2009-01-01

    The XRD-31 is a fast, windowless X-ray vacuum photodiode developed by EG and G. It is currently the primary fast X-ray detector used to diagnose the X-rays on NIF and OMEGA on the multichannel DANTE spectrometer. The XRD-31 has a dynamic range of less than 1e-12 amps to more than 10 amps. A technique is described to measure the impulse response of the diodes to a 150 fs pulse of 200 nm laser light and a method to calculate the 'risetime' for a square pulse and compare it with the computed electron transit time from the photocathode to the anode. Measured response time for 5 XRD-31s assembled in early 2004 was 149.7 ps +-2.75 ps

  7. Definitive Mineralogical Analysis of Mars Analog Rocks Using the CheMin XRD/XRF Instrument

    Science.gov (United States)

    Blake, D. F.; Sarrazin, P.; Bish, D. L.; Feldman, S.; Chipera, S. J.; Vaniman, D. T.; Collins, S.

    2004-01-01

    Mineral identification is a critical component of Mars Astrobiological missions. Chemical or elemental data alone are not definitive because a single elemental or chemical composition or even a single bonding type can represent a range of substances or mineral assemblages. Minerals are defined as unique structural and compositional phases that occur naturally. There are about 15,000 minerals that have been described on Earth, all uniquely identifiable via diffraction methods. There are likely many minerals yet undiscovered on Earth, and likewise on Mars. If an unknown phase is identified on Mars, it can be fully characterized by structural (X-ray Diffraction, XRD) and elemental analysis (X-ray Fluorescence, XRF) without recourse to other data because XRD relies on the principles of atomic arrangement for its determinations. XRD is the principal means of identification and characterization of minerals on Earth.

  8. Stress-strain relationship and XRD line broadening in [0001] textured hexagonal polycrystalline materials

    International Nuclear Information System (INIS)

    Yokoyama, Ryouichi

    2011-01-01

    Stress analysis with X-ray diffraction (XRD) for hexagonal polycrystalline materials in the Laue classes 6/mmm and 6/m has been studied on the basis of the crystal symmetry of the constituent crystallites which was proposed by R. Yokoyama and J. Harada ['Re-evaluation of formulae for X-ray stress analysis in polycrystalline specimens with fibre texture', Journal of Applied Crystallography, Vol.42, pp.185-191 (2009)]. The relationship between the stress and strain observable by XRD in a hexagonal polycrystalline material with [0001] fibre texture was formulated in terms of the elastic compliance defined for its single crystal. As a result, it was shown that the average strains obtained in the crystallites for both symmetries of 6/mmm and 6/m are different from each other under the triaxial or biaxial stress field. Then, it turned out that the line width of XRD changes depending on the measurement direction. (author)

  9. The thermal behaviour of cuprite: An XRD-EXAFS combined approach

    International Nuclear Information System (INIS)

    Dapiaggi, M.; Tiano, W.; Artioli, G.; Sanson, A.; Fornasini, P.

    2003-01-01

    Cuprite (Cu 2 O) is a low thermal expansion material with a negative thermal expansion coefficient below room temperature. Its peculiar thermal behaviour encompasses the increase of the shear modulus with increasing temperature, and the presence of rather intense symmetry-forbidden eeo reflections below room temperature. The thermal expansion of cuprite was studied at low temperature (between 5 and 298 K) by means of high-resolution (10 -5 A) X-ray powder diffraction at European Synchrotron Radiation Facility (Grenoble, BM16) and extended X-ray absorption fine structure (EXAFS) (BM29). Negative thermal expansion is confirmed up to 200 K, by EXAFS as well as by XRD measurements, and no sign of transition was found in XRD data. The comparison between EXAFS and XRD results provides a valuable insight into vibrational behaviour of cuprite at low temperature

  10. SIZE OF BOEHMITE NANOPARTICLES BY TEM IMAGES ANALYSIS

    Directory of Open Access Journals (Sweden)

    Maxime Moreaud

    2011-05-01

    Full Text Available Transition aluminas, and especially the gamma type, are largely used as catalyst supports in refining and petrochemicals. Most studies focus on properties resulting from material texture and casting (specific surface, porous volume, pore shape and diameter. However, surface properties of alumina should be considered as well, as the catalytic activity is tightly related to the structure of exposed crystalline faces. As γ alumina results from controlled thermal treatment of boehmite γ-AlOOH by a topotactic transformation, the nature of exposed crystalline planes is related to the starting material. Therefore, the synthesis of the oxihydroxide γ-AlOOH, and especially size and shape of these particles, is critical in determining the relevant surface properties. Unlike often aggregated alumina, boehmite nanoparticles can be observed by TEM. Analysis of these TEM images can be performed to estimate the size of the boehmite nanoparticles. Information about morphology of the nanoparticles is obtained by the analysis of the covariance, modeling micrographs by a dilution model.

  11. Complications of transanal endoscopic microsurgery (TEMS): a prospective audit.

    Science.gov (United States)

    Bignell, M B; Ramwell, A; Evans, J R; Dastur, N; Simson, J N L

    2010-07-01

    The aim of this study was to determine the postoperative complications of Transanal Endoscopic Microsurgery (TEMS) excision of rectal lesions. A prospective audit of 262 consecutive TEMS procedures performed by a single surgeon between 1999 and 2008. The mean age of patients was 72 years. The mean area of the lesions excised was 17.5 cm(2) with a mean diameter of 4.5 cm at a mean distance of 7.4 cm from the dentate line. There were 201 full thickness excisions, 51 partial thickness excisions and nine were mixed or unclassified. Thirty-three (13%) patients developed 41 complications. There were two (0.8%) deaths within 30 days. Pelvic sepsis occurred in seven (3%) patients and was significantly more common after excision of low lesions within 2 cm of the dentate line. Postoperative haemorrhage occurred in seven (3%) patients and was significantly less common when dissection was performed with ultrasonic dissection than with diathermy. Fourteen (5%) patients developed acute urinary retention. Four (1.5%) patients developed rectal stenosis and four (1.5%) suffered uncomplicated surgical emphysema that required no treatment. Transanal endoscopic microsurgery is a safe operation with a low mortality and morbidity. Pelvic sepsis is more common after excision of lesions within 2 cm of the dentate line. Ultrasonic dissection is associated with less postoperative haemorrhage than diathermy.

  12. In-situ heating TEM observation of microscopic structural changes of size-controlled metallic copper/gelatin composite.

    Science.gov (United States)

    Narushima, Takashi; Hyono, Atsushi; Nishida, Naoki; Yonezawa, Tetsu

    2012-10-01

    Copper/gelatin composite particles with controlled sizes were prepared at room temperature from cupric sulfate pentahydrate in the presence of gelatin as a protective reagent by using hydrazine monohydrate as a reducing agent. The formed particles with the size between 190-940 nm were secondary aggregated particles which were composed of smaller nanosized particles ("particle-in-particle"), the presence of which was established by XRD patterns and a cross-sectional TEM image. The sintering behavior of these copper/gelatin composite particles was demonstrated by in-situ heating TEM under a high vacuum (approximately 10(-5) Pa) and separately with the oxygen partial pressure controlled at the 10(-4) Pa level. It was established that the particles began to sinter at about 330 degrees C with the oxygen and that they sublimate above 450 degrees C both in the vacuum and oxygen conditions. This result shows that the introduction of an adequate amount of oxygen was effective to remove the gelatin surrounding the particles. It can also be concluded that the sintering of the copper/gelatin composite particles occurred even in the absence of a reducing agent such as hydrogen gas.

  13. FIB/SEM study of AA2024 corrosion under a seawater drop, part II

    International Nuclear Information System (INIS)

    King, Peter C.; Cole, Ivan S.; Corrigan, Penny A.; Hughes, Anthony E.; Muster, Tim H.; Thomas, Sebastian

    2012-01-01

    Highlights: ► Dealloying has a directional nature, exhibits banding. ► Oxidation state of copper in sponge remnants found to be variable. ► Dissolution and breakdown of copper sponge structure observed. ► Crystalline defects imaged in dealloyed S-phase. - Abstract: The dissolution of S-phase clusters in aluminium alloy 2024 (AA2024) exposed to a 0.5 μl seawater droplet is presented. Foils for transmission electron microscopy (TEM) were made from local attack sites using a focussed ion beam/scanning electron microscope (FIB/SEM). The sections showed that clusters of S-phase particles underwent dealloying. The resulting copper sponge morphology, banding, preferred orientation and crystal defect structure as a result of plastic deformation have been characterised. With build-up of amorphous corrosion product, physical and electrical isolation of parts of the clusters developed, with the result of copper dissolution from the S-phase remnants.

  14. Using of XRD in Industrial Sample Analysis and TENORM in Nuclear Malaysia

    International Nuclear Information System (INIS)

    Paulus, W.; Nurhaslinda Ee Abdullah; Meor Yusoff Meor Sulaiman

    2011-01-01

    Industrial waste such as aluminium dross and TENORM waste, oil sludge has been used as sample in this research. Determination of main elements by using X-Ray Diffraction (XRD) in Material Technology Group, Malaysian Nuclear Agency. Results shows that main elements in these samples, aluminium hydroxide (gibbsite) and quartz low, respectively. Thereby, this research shows that XRD can be considered as one of the techniques that can be used in waste characterization and furthermore, it can help researchers and engineer in the research related to waste treatment especially radioactive waste. (author)

  15. Determination of Stress Profiles in Expanded Austenite by Combining Successive Layer Removal and GI-XRD

    DEFF Research Database (Denmark)

    Fernandes, Frederico Augusto Pires; Christiansen, Thomas Lundin; Somers, Marcel A. J.

    2014-01-01

    The present work deals with the evaluation of the residual-stress profile in expanded-austenite by successive removal steps using GI-XRD. Preliminary results indicate stresses of several GPa's from 111 and 200 diffraction lines. These stresses appear largest for the 200 reflection. The strain......-free lattice parameter decayed smoothly with depth, while for the compressive stress a maximum value is observed at some depth below the surface. Additionally a good agreement was found between the nitrogen profile determined with GDOES analysis and the strain-free lattice parameter from XRD....

  16. Description and calibration beamline SEM/Ion Chamber Current Digitizer

    International Nuclear Information System (INIS)

    Schoo, D.

    1994-05-01

    This report discusses the following on beamline SEM/ion chamber current digitizers: Module description; testing and calibration; common setup procedures; summary of fault indications and associated causes; summary of input and output connections; SEM conversion constant table; ion chamber conversion constant table; hexadecimal to decimal conversion table; and schematic diagram

  17. lsnjbhakta@gmail.com A Comparative SEM-EDS Elemental

    African Journals Online (AJOL)

    Michael Horsfall

    effect on food production in terrestrial and aquatic compartment in ... Processing and SEM-EDS analysis of mud: In the laboratory, the ... and for SEM image observation was 15 kV, applying .... by weathering in the Omi acid clay deposit, Japan.

  18. On the Nature of SEM Estimates of ARMA Parameters.

    Science.gov (United States)

    Hamaker, Ellen L.; Dolan, Conor V.; Molenaar, Peter C. M.

    2002-01-01

    Reexamined the nature of structural equation modeling (SEM) estimates of autoregressive moving average (ARMA) models, replicated the simulation experiments of P. Molenaar, and examined the behavior of the log-likelihood ratio test. Simulation studies indicate that estimates of ARMA parameters observed with SEM software are identical to those…

  19. Structural Equations and Causal Explanations: Some Challenges for Causal SEM

    Science.gov (United States)

    Markus, Keith A.

    2010-01-01

    One common application of structural equation modeling (SEM) involves expressing and empirically investigating causal explanations. Nonetheless, several aspects of causal explanation that have an impact on behavioral science methodology remain poorly understood. It remains unclear whether applications of SEM should attempt to provide complete…

  20. The influence of environment temperature on SEM image quality

    International Nuclear Information System (INIS)

    Chen, Li; Liu, Junshan

    2015-01-01

    As the structure dimension goes down to the nano-scale, it often requires a scanning electron microscope (SEM) to provide image magnification up to 100 000  ×. However, SEM images at such a high magnification usually suffer from high resolution value and low signal-to-noise ratio, which results in low quality of the SEM image. In this paper, the quality of the SEM image is improved by optimizing the environment temperature. The experimental results indicate that at 100 000  ×, the quality of the SEM image is influenced by the environment temperature, whereas at 50 000  × it is not. At 100 000  × the best SEM image quality can be achieved from the environment temperature ranging 292 from 294 K, and the SEM image quality evaluated by the double stimulus continuous quality scale method can increase from grade 1 to grade 5. It is expected that this image quality improving method can be used in routine measurements with ordinary SEMs to get high quality images by optimizing the environment temperature. (paper)

  1. Design and Use of the Simple Event Model (SEM)

    NARCIS (Netherlands)

    van Hage, W.R.; Malaisé, V.; Segers, R.H.; Hollink, L.

    2011-01-01

    Events have become central elements in the representation of data from domains such as history, cultural heritage, multimedia and geography. The Simple Event Model (SEM) is created to model events in these various domains, without making assumptions about the domain-specific vocabularies used. SEM

  2. Canticum Novum: música sem palavras e palavras sem som no pensamento de Santo Agostinho

    OpenAIRE

    Mammì, Lorenzo

    2000-01-01

    NO De Magistro, Santo Agostinho coloca a reza e o canto numa posição similar, à margem das funções imediatamente comunicativas da linguagem. A reflexão agostiniana sobre a reza se baseia nos hábitos cristãos da leitura, da oração e da meditação silenciosas. Há sobre o canto, na prática igualmente inovadora do jubilus, melodia sem palavra destinada aos momentos mais intensos e gaudiosos da liturgia. A oração silenciosa e o jubilus são temas recorrentes da literatura patrística, mas Agostinho o...

  3. Construcción de la microestructura y macroestructura semántica en textos expositivos producidos por estudiantes universitarios de LUZ

    OpenAIRE

    Fuenmayor, Gloria; Villasmil, Yeriling; Rincón, María

    2008-01-01

    El objetivo de esta investigación es analizar la construcción de la microestructura y macroestructura semántica  en textos expositivos producidos por estudiantes universitarios, a partir del uso de  procedimientos gramaticales como las proformas. La teoría se sustenta en los conceptos: Microestructrura y Macroestructura semántica, (van Dijk y Kintsch 1983, 1992); Mecanismos de cohesión y progresión temática (Calsamiglia y Tusón, 1999); El texto expositivo (Álvarez, 1996, 2001); Carácter socia...

  4. Transreceptor de faixa larga baseado em impulso de rádio para sensor sem fios de curta distância implementado em tecnologia CMOS

    OpenAIRE

    Rodrigues, David Manuel Cardoso

    2013-01-01

    Dissertação para obtenção do Grau de Mestre em Engenharia Electrotécnica e de Computadores O rápido desenvolvimento da microtecnologia e microelectrónica tem vindo a contribuir de forma decisiva para uma crescente utilização de sensores, sejam eles com ou sem fios, o que permitirá interagir mais eficientemente com o meio envolvente, em consequência de mais e melhor medição e atuação. Neste contexto, as redes de sensores sem fios (WSNs) estão a emergir como uma das grandes e mais impo...

  5. Application of low current intensity electrolytic treatment for the chlorides extraction in underwater archaeological objects of iron. Observation of the mineralogical phases evolution through XRD-Rietveld

    International Nuclear Information System (INIS)

    Bethencourt, M.; Gil, M. L. A.; Fernandez-Lorenzo, C.; Santos, A.

    2004-01-01

    With the purpose of optimising a suitable methodology for the conservation of an archaeological object of iron, a low current intensities electrolytic treatment has been applied, to a piece of cast iron, proving to be effective in the extraction of chloride ions from the structure of akaganeite, principal corrosion product of iron in the marine medium. The monitoring of the electrolytic treatment has been proven by applying the Rietveld method to the patterns XRD of samples extracted from the corroded surface before and after the treatment. This method has permitted the unequivocal determination of the akaganeite and its chemical composition. This identification has been corroborated by means of SEM and EDS. After the electrolytic treatment, akaganeite was not present in the sample. (Author) 9 refs

  6. Implementação de sistemas eólicos para redes de sensores sem fios

    OpenAIRE

    Mendonça, Fábio Rúben Silva

    2015-01-01

    O trabalho tem por objetivo principal estudar a utilização de aerogeradores para microprodução de energia (menor que 1 W) de forma a poderem alimentar os nós das redes de sensores sem fios. Para tal, analisaram-se dois tipos de aerogeradores, os de eixo vertical e os de eixo horizontal, tendo-se efetuado simulações de CFD (Computational Fluid Dynamics) para verificar o desempenho das turbinas, de forma a determinar qual é o mais adequado. Foi realizado o projeto dos dois sistemas e anali...

  7. A Defensoria Pública Como Instrumento Garantidor do Acesso à Justiça, Inclusive às Pessoas sem Moradia

    OpenAIRE

    Lima, Marcos Feitosa; Sant Anna, Marília Mendonça Morais

    2015-01-01

    O estudo presente tem por escopo demonstrar que a Defensoria Pública é instituição devidamente capitaneada na Constituição Federal incumbida de conferir acesso à justiça aos necessitados, que assim se declararem, e que não tenham condições de constituir advogado privado sem o comprometimento de sua própria subsistência, alcançando, por óbvio, as pessoas que vivem em situação de rua, que na maioria das vezes são ignoradas pela sociedade como um todo, passando-se por despercebidas ou chegando a...

  8. Custo de produção de goiabas para mesa produzidas com e sem ensacamento: estudo de caso

    OpenAIRE

    Tatiane de Oliveira Tokairin; Fernando Perez Cappello; Marcel Bellato Spósito

    2014-01-01

    O ensacamento de goiabas para mesa tem por finalidade proteger os frutos contra o ataque de pragas, reduzir a aplicações e os níveis de resíduo de agroquímicos. O objetivo deste trabalho foi avaliar a sustentabilidade econômica da produção de goiabas, por meio da comparação do custo de produção entre os sistemas de cultivo com e sem ensacamento dos frutos. Foi realizado um estudo de caso com dados obtidos de uma propriedade comercial de goiabas para mesa no município de Valinhos - SP. O custo...

  9. The effect of size-selective samplers (cyclones) on XRD response

    CSIR Research Space (South Africa)

    Pretorius, CJ

    2011-07-01

    Full Text Available The study evaluated five size-selective samplers used in the South African mining industry to determine how their performance affects the X-ray powder diffraction (XRD) response when respirable dust samples are analysed for quartz using direct...

  10. EPXMA survey of shelf sediments (Southern Bight, North Sea): A glance beyond the XRD-invisible

    NARCIS (Netherlands)

    De Maeyer-Worobiec, A.; Dekov, V.M.; Laane, R.W.P.M.; van Grieken, R.

    2009-01-01

    Shelf sediments of the southern North Sea, were studied with a microanalytical [electron probe X-ray microanalysis (EPXMA)] and two bulk [X-ray diffraction (XRD) and X-ray fluorescence (XRF)] techniques. The investigation proved that the promptness of the microanalytical method is combined with a

  11. Crystallographic Investigation of Ag (4 mol%) Doped ZnO (SZO) Thin Films by XRD

    International Nuclear Information System (INIS)

    Lwin Lwin Nwe; Sandar Dwe; Khant Khant Lin; Khin Thuzar; Than Than Win; Ko Ko Kyaw Soe

    2008-03-01

    Silver doped ZnO(SZO) thin films are prepared by sol-based method. The silver dopant concentration is 4 mol % in this case. XRD analysis carried out to determine, crystallographic properties such as lattice parameters and crystallite size of SZO thin films.

  12. Effect of sample moisture content on XRD-estimated cellulose crystallinity index and crystallite size

    Science.gov (United States)

    Umesh P. Agarwal; Sally A. Ralph; Carlos Baez; Richard S. Reiner; Steve P. Verrill

    2017-01-01

    Although X-ray diffraction (XRD) has been the most widely used technique to investigate crystallinity index (CrI) and crystallite size (L200) of cellulose materials, there are not many studies that have taken into account the role of sample moisture on these measurements. The present investigation focuses on a variety of celluloses and cellulose...

  13. Characterization of carbonated serpentine using XPS and TEM

    International Nuclear Information System (INIS)

    Schulze, Roland K.; Hill, Mary Ann; Field, Robert D.; Papin, Pallas A.; Hanrahan, Robert J.; Byler, Darrin D.

    2004-01-01

    With the increasing concentration volume of carbon dioxide in the atmosphere, there has been an increasing interest in carbon dioxide sequestration. One method is to store the carbon dioxide in mineral form, reacting solution dissolved CO 2 to precipitate carbonates. In order to understand whether or not such an endeavor is feasible, the carbonation reaction must first be understood. In this study, the surface of ground serpentine, untreated, heat treated and following a carbonation experiment, has been characterized using X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). The results indicate that the mechanism for the reaction involves dissolution of the serpentine through the formation of an amorphous phase and subsequent precipitation of magnesite. The rate limiting step appears to be the diffusion of Mg out of the amorphous phase

  14. Tourism Employment Module (TEM: Case of the Czech Republic

    Directory of Open Access Journals (Sweden)

    Zdeněk Lejsek

    2011-09-01

    Full Text Available Tourism Employment Module (TEM provides information on the significance and contribution of tourism for the national economy in terms of employment. It refers to a system of tables describing the main economic characteristics of tourism (i.e. number of jobs and people employed in tourism by industry, seasonality, working scheme,permanency of job, sex, age groups, level of education or nationality and classifying thereby tourism as one of branches in the system of national accounts. The article describes basic methodological concept and structure of this tool (and approaches to measuring employment in the tourist industry in general, exploited data sources and provides a brief information on the type and form of publishing of the results as well as the data on principalmacroeconomic indicators of tourism-related industries in the Czech Republic in 2003–2009.

  15. TEM examination of irradiated zircaloy-2 pressure tube material

    International Nuclear Information System (INIS)

    Srivastava, D.; Tewari, R.; Dey, G.K.; Sharma, B.P.; Sah, D.N.; Banerjee, Suparna; Sahoo, K.C.

    2005-09-01

    In the present work, microstructure of the zircaloy-2 pressure tube material irradiated in the Indian Pressurized Heavy Water RAPP-1. Reactor (PHWR) has been examined for the first time using transmission electron microscope (TEM). The samples were obtained from a zircaloy-2 pressure tube, which had been in operation in the high flux region of Rajasthan Atomic Power Station Unit -1, for a period for 6.77 effective full power years (EFPYs) and expected to have a cumulative radiation damage of about 3 dpa. In this study irradiated microstructure has been characterized and compared it with the microstructure of the unirradiated pressure tube samples. The effect of irradiation on the hydriding behaviour is also studied. (author)

  16. Water state and TEM analysis of Konjac irradiation copolymer

    International Nuclear Information System (INIS)

    Geng Shengrong; Xia Hezhou; Chen Xueling; Ye Lixiu; Hua Yuejin

    2012-01-01

    To study the absorption performance of Konjac-AA copolymer prepared by irradiation, the water absorbent capacity, sorbent speed and water keeping ability was determined and DSC and TEM analysis were used to explore the water content and structure characters. The results showed that on room temperature the largest water absorption speed was 16 g · g -1 · min -1 at, and the largest water absorption was 400 times at 60 min. The water absorption was affected by granularity, temperature, ion content and ion type, especially the ion type, the water keeping ability was affected by temperature and time, which was up to 35% while the fully water absorbed copolymer was kept under room temperature for 15 d. The free and bounder water content which was assimilated by the plants was 99.617%. The gel stale co polymer has a three-dimensional structure of spiral, which was constituted by spherical objects of varying sizes. (authors)

  17. TEM analysis of fine sulphides dissolution and precipitation in steel

    International Nuclear Information System (INIS)

    Garbarz, B.; Marcisz, J.; Wojtas, J.

    2003-01-01

    Results of transmission electron microscopy (TEM) investigation of morphology, size distribution and chemistry of nano-inclusions formed in 4 mm thick laboratory steel ingots in as-cast condition and after heat treatment are reported. The investigated steel contained 0.11-0.14 C, 0.6 Mn, 0.25 Si, 0.22 Cu, 0.025-0.037 S (wt.%), and 80-115 ppm O and solidified at an average cooling rate of 250 K s -1 . In the as-cast specimens most nano-inclusions had a diameter in the range 10-100 nm with an average size of 30 nm. They were identified by microanalysis in thin foils as sulphides: MnS, (Mn,Cu)S, CuS and Cu 2 S. After a solution treatment of the thin ingots the re-precipitation of nano-sulphides was investigated

  18. A tem investigation on intermetallic particles in zircaloy-2

    International Nuclear Information System (INIS)

    Sudarminto, Harini Sosiati; Kuwano, Noriyuki; Oki, Kensuke

    1996-01-01

    Tem investigation were conducted on the heat treated zircaloy-2 having the composition of Zr containing 1.6% Sn, 0.2% Fe, 0.1% Cr and 0.05% Ni (%wt) in order tostudy the characteristics of intermetallic particles related to the microstructural basis on the corrosion effect. Forged zircaloy-2 was annealed in the β-phase at 1050 C degrees for various isothermally in the α-phase region at 650 and 750 C degrees, followed by water quenching. The size precipates, the lower became their number. By increasing the annealing temperature, the growth of precipitates formed in this zircaloy-2 were of the Zr(Cr,Fe) 2 and Zr 2 (Fe,Cr,Ni) types. These kinds of precipitates and the ratios of Fe/Cr were independent of size and shape of precipitates and annealing time and temperature. (author), 16 refs, 2 tabs, 5 figs

  19. Properties of TEM standing waves with E||B

    Science.gov (United States)

    Zaghloul, H.; Buckmaster, H. A.

    This paper summarizes the known properties of E∥B TEM standing waves and shows that for such waves (i) E and B cannot be linearly polarized, (ii) E ≠ αB where α is a constant (iii) it is impossible to find a Lorentz frame where E>B, (iv) direction of the propagation vector cannot be inferred from the fields at one point of the space, (v) their behaviour under Lorentz, parity, time-reversal and gauge transformations is proper, (vi) both Lorentz invariants E2 - B2 and E·B are nonzero, (vii) the magnetic helicity may be nonzero, (viii) the magnetic field may be force-free, and (ix) kμFμv ≠ 0. It also shows how electromagnetic waves can be classified using Lorentz invariants. Cet article résume les qualités connues des ondes stationnaires E∥B TEM et montre que pour des ondes parallèles (i) E et B ne peuvent pas être polarisées linéairement, (ii) E ≠ αB où a est une constante, (iii) il est impossible de trouver une construction de Lorentz où E>B, (iv) la direction de propagation d'un vecteur ne peut pas être déduite des opérations à un point d'intervalle, (v) leur conduite sous Lorentz, parité, temps inverse et transformations de jauge est propre, (vi) les deux invariants de Lorentz E2 - B2 et E·B sont non nulles (vii) l'hélice magnétique peut être non nulle (viii) l'opération magnétique peut être de force libre et (ix) KμFμ v ≠ 0. Ceci montre aussi comment les ondes électromagnétiques peuvent être classifiées, en employant les invariants de Lorentz.

  20. An alternative to the TEM (Transformed Eulerian Mean) equations

    Science.gov (United States)

    Gaßmann, Almut

    2013-04-01

    The TEM equations constitute a powerful means to get access to the residual circulation. However, due to their foundation on the wave perspective, they deliver only a zonally averaged picture without access to the three-dimensional structure or the local origins of the residual circulation. Therefore it is worth to investigate whether there are alternatives. The pathway followed here is to perform a transformation of the momentum and the potential temperature equation before taking the zonal mean. This is done by removing the steady state ideal wind solution vid = ?×?B-(?±P) from the equations (? - potential temperature, B - Bernoulli function, P - Ertel's potential vorticity EPV, ?± - density). The advantage of that approach is that the total EPV-flux does no longer contain an explicitly visible 'do-nothing-flux'. This flux, ?? ×?B, does only vanish when averaging on isentropic surfaces, but not on other isosurfaces. Here we find the reason why the conventional zonal mean on isentropes delivers a direct overturning cell on each hemisphere, whereas on other isosurfaces we obtain the typical three-cell structure with Headley, Ferrel, and polar cells. It will be demonstrated and made visible through idealized climate experiments with the ICON-IAP model that the zonal averages of the nonideal wind components vnid = v - vid and wnid = w - wid constitute similar direct overturning cells on non-isentropic surfaces as obtained with the TEM-generated v* and w*. It is also interesting to inspect fields of local nonideal wind components, the very origin of the residual circulation.

  1. Mel de abelhas sem ferrão: proposta de regulamentação

    Directory of Open Access Journals (Sweden)

    Ricardo Costa Rodrigues de Camargo

    Full Text Available Resumo Os méis das abelhas sem ferrão são produtos únicos da biodiversidade brasileira, presentes e valorizados pela cultura popular desde os povos originais das Américas. Por ser mais ácido e apresentar maior teor de umidade, seu sabor é peculiar e sua viscosidade é menor quando comparada ao mel proveniente da espécie exótica Apis mellifera. Devido a essas diferenças, esse produto necessita do estabelecimento de parâmetros físico-químicos específicos que sejam referência tanto para controle de qualidade como para sua comercialização. Com base em pesquisas realizadas pela Embrapa, pelo Instituto de Tecnologia de Alimentos de Campinas e pelo levantamento bibliográfico de diversos estudos científicos realizados por outros institutos de ensino e pesquisa, esta comunicação tem como objetivo esclarecer as peculiaridades deste produto e apresentar uma proposta de Regulamento Técnico de Identidade e Padrão para o Mel das Abelhas Sem Ferrão, visando sua comercialização no Estado de São Paulo, contribuindo assim para a disponibilidade de um produto seguro e de qualidade para o consumidor final.

  2. Automated CD-SEM metrology for efficient TD and HVM

    Science.gov (United States)

    Starikov, Alexander; Mulapudi, Satya P.

    2008-03-01

    CD-SEM is the metrology tool of choice for patterning process development and production process control. We can make these applications more efficient by extracting more information from each CD-SEM image. This enables direct monitors of key process parameters, such as lithography dose and focus, or predicting the outcome of processing, such as etched dimensions or electrical parameters. Automating CD-SEM recipes at the early stages of process development can accelerate technology characterization, segmentation of variance and process improvements. This leverages the engineering effort, reduces development costs and helps to manage the risks inherent in new technology. Automating CD-SEM for manufacturing enables efficient operations. Novel SEM Alarm Time Indicator (SATI) makes this task manageable. SATI pulls together data mining, trend charting of the key recipe and Operations (OPS) indicators, Pareto of OPS losses and inputs for root cause analysis. This approach proved natural to our FAB personnel. After minimal initial training, we applied new methods in 65nm FLASH manufacture. This resulted in significant lasting improvements of CD-SEM recipe robustness, portability and automation, increased CD-SEM capacity and MT productivity.

  3. SEM-EBSP能知道些什么

    Institute of Scientific and Technical Information of China (English)

    张唯敏

    2003-01-01

    @@ 1 SEM-EBSP是什么 所谓SEM-EBSP是指采用在扫描电子显微镜(SEM)镜体中的反射电子菊池线衍射的结晶方位分析.被称为菊池图形的衍射图形可因结晶的稍许倾斜而大大地改变其位置,因此,通过解析菊池图形就能正确地知道结晶方位.

  4. Improvement of geometrical measurements from 3D-SEM reconstructions

    DEFF Research Database (Denmark)

    Carli, Lorenzo; De Chiffre, Leonardo; Horsewell, Andy

    2009-01-01

    The quantification of 3D geometry at the nanometric scale is a major metrological challenge. In this work geometrical measurements on cylindrical items obtained with a 3D-SEM were investigated. Two items were measured: a wire gauge having a 0.25 mm nominal diameter and a hypodermic needle having...... that the diameter estimation performed using the 3D-SEM leads to an overestimation of approx. 7% compared to the reference values obtained using a 1-D length measuring machine. Standard deviation of SEM measurements performed on the wire gauge is approx. 1.5 times lower than the one performed on the hypodermic...

  5. Improvement of CD-SEM mark position measurement accuracy

    Science.gov (United States)

    Kasa, Kentaro; Fukuhara, Kazuya

    2014-04-01

    CD-SEM is now attracting attention as a tool that can accurately measure positional error of device patterns. However, the measurement accuracy can get worse due to pattern asymmetry as in the case of image based overlay (IBO) and diffraction based overlay (DBO). For IBO and DBO, a way of correcting the inaccuracy arising from measurement patterns was suggested. For CD-SEM, although a way of correcting CD bias was proposed, it has not been argued how to correct the inaccuracy arising from pattern asymmetry using CD-SEM. In this study we will propose how to quantify and correct the measurement inaccuracy affected by pattern asymmetry.

  6. Molecular identification of TEM-116 beta-lactamase gene in isolates ...

    African Journals Online (AJOL)

    Keywords: P. aeruginosa, Clinical isolates, Sequencing, TEM-116, Antibiotic susceptibility. Tropical Journal of ... organisms produce a wide range of beta ... TEM-1 is the most commonly encountered beta-lactamase in Gram-negative bacteria.

  7. Novel field emission SEM column with beam deceleration technology

    Energy Technology Data Exchange (ETDEWEB)

    Jiruše, Jaroslav; Havelka, Miloslav; Lopour, Filip

    2014-11-15

    A novel field-emission SEM column has been developed that features Beam Deceleration Mode, high-probe current and ultra-fast scanning. New detection system in the column is introduced to detect true secondary electron signal. The resolution power at low energy was doubled for conventional SEM optics and moderately improved for immersion optics. Application examples at low landing energies include change of contrast, imaging of non-conductive samples and thin layers. - Highlights: • A novel field-emission SEM column has been developed. • Implemented beam deceleration improves the SEM resolution at 1 keV two times. • New column maintains high analytical potential and wide field of view. • Detectors integrated in the column allow gaining true SE and BE signal separately. • Performance of the column is demonstrated on low energy applications.

  8. Role of scanning electron microscope )SEM) in metal failure analysis

    International Nuclear Information System (INIS)

    Shaiful Rizam Shamsudin; Hafizal Yazid; Mohd Harun; Siti Selina Abd Hamid; Nadira Kamarudin; Zaiton Selamat; Mohd Shariff Sattar; Muhamad Jalil

    2005-01-01

    Scanning electron microscope (SEM) is a scientific instrument that uses a beam of highly energetic electrons to examine the surface and phase distribution of specimens on a micro scale through the live imaging of secondary electrons (SE) and back-scattered electrons (BSE) images. One of the main activities of SEM Laboratory at MINT is for failure analysis on metal part and components. The capability of SEM is excellent for determining the root cause of metal failures such as ductility or brittleness, stress corrosion, fatigue and other types of failures. Most of our customers that request for failure analysis are from local petrochemical plants, manufacturers of automotive components, pipeline maintenance personnel and engineers who involved in the development of metal parts and component. This paper intends to discuss some of the technical concepts in failure analysis associated with SEM. (Author)

  9. Quantitative approach on SEM images of microstructure of clay soils

    Institute of Scientific and Technical Information of China (English)

    施斌; 李生林; M.Tolkachev

    1995-01-01

    The working principles of Videolab Image Processing System (VIPS), the examining methods of orientation of microstructural units of clay soils and analysing results on SEM images of some typical microstructures of clay soils using the VIPS are introduced.

  10. semPLS: Structural Equation Modeling Using Partial Least Squares

    Directory of Open Access Journals (Sweden)

    Armin Monecke

    2012-05-01

    Full Text Available Structural equation models (SEM are very popular in many disciplines. The partial least squares (PLS approach to SEM offers an alternative to covariance-based SEM, which is especially suited for situations when data is not normally distributed. PLS path modelling is referred to as soft-modeling-technique with minimum demands regarding mea- surement scales, sample sizes and residual distributions. The semPLS package provides the capability to estimate PLS path models within the R programming environment. Different setups for the estimation of factor scores can be used. Furthermore it contains modular methods for computation of bootstrap confidence intervals, model parameters and several quality indices. Various plot functions help to evaluate the model. The well known mobile phone dataset from marketing research is used to demonstrate the features of the package.

  11. Novel field emission SEM column with beam deceleration technology

    International Nuclear Information System (INIS)

    Jiruše, Jaroslav; Havelka, Miloslav; Lopour, Filip

    2014-01-01

    A novel field-emission SEM column has been developed that features Beam Deceleration Mode, high-probe current and ultra-fast scanning. New detection system in the column is introduced to detect true secondary electron signal. The resolution power at low energy was doubled for conventional SEM optics and moderately improved for immersion optics. Application examples at low landing energies include change of contrast, imaging of non-conductive samples and thin layers. - Highlights: • A novel field-emission SEM column has been developed. • Implemented beam deceleration improves the SEM resolution at 1 keV two times. • New column maintains high analytical potential and wide field of view. • Detectors integrated in the column allow gaining true SE and BE signal separately. • Performance of the column is demonstrated on low energy applications

  12. Using the in situ lift-out technique to prepare TEM specimens on a single-beam FIB instrument

    International Nuclear Information System (INIS)

    Lekstrom, M; McLachlan, M A; Husain, S; McComb, D W; Shollock, B A

    2008-01-01

    Transmission electron microscope (TEM) specimens are today routinely prepared using focussed ion beam (FIB) instruments. Specifically, the lift-out method has become an increasingly popular technique and involves removing thin cross-sections from site-specific locations and transferring them to a TEM grid. This lift-out process can either be performed ex situ or in situ. The latter is mainly carried out on combined dual-beam FIB and scanning electron microscope (SEM) systems whereas conventional single-beam instruments often are limited to the traditional ex situ method. It is nevertheless desirable to enhance the capabilities of existing single-beam instruments to allow for in situ lift-out preparation to be performed since this technique offers a number of advantages over the older ex situ method. A single-beam FIB instrument was therefore modified to incorporate an in situ micromanipulator fitted with a tungsten needle, which can be attached to a cut-out FIB section using ion beam induced platinum deposition. This article addresses the issues of using an ion beam to monitor the in situ manipulation process as well as approaches that can be used to create stronger platinum welds between two objects, and finally, views on how to limit the extent of ion beam damage to the specimen surface.

  13. DETECTION OF DELAMINATION IN A COMPOSITE PLATE BY SEM

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    A numerical method of integration of Green's functi ons of strip element method (SEM) is proposed. The response of ultrasonic sourc e generated by a transducer on the surface of a multi-ply composite plate conta ining a delamination is analyzed by the use of SEM. The numerical results show that the scanning features of the ultrasonic waves may be used to identify the d elamination inside the composite plate .

  14. A methodological basis for SEM autoradiography: biosynthesis and radioligand binding

    International Nuclear Information System (INIS)

    Cheng, G.; Hodges, G.M.; Trejdosiewicz, L.K.

    1985-01-01

    A method is described for scanning electron microscope (SEM) autoradiography whereby preservation of high resolution cell surface details is retained together with degelatination of the emulsion without gross loss or redistribution of silver grains. This method should provide a convenient medium-sized marker for SEM (using secondary, backscattered electron and X-ray imaging) topographic studies of biosynthesized molecules, and of cell surface receptors and antigens, using indirect or direct labelling procedures with radio-labelled ligands. (author)

  15. In Situ Synchrotron XRD on a Capillary Li-O2 Battery Cell

    DEFF Research Database (Denmark)

    Storm, Mie Møller; Johnsen, Rune; Norby, Poul

    2014-01-01

    of a electrolyte filled capillary with anode and cathode in each end suspended on stainless steel wires, the oxygen in-let is placed on the cathode side of the capillary with a flushing system for oxygen in-let. In this study we present a flexible design of a capillary based Li-O2 battery with discharge and charge...... a stainless steel wire where the cathode is attached. The in situ XRD measurements show how the Li2O2 growth depend on current discharge rate and how the FWHM changes dependent on reflection and charge/discharge.Several cells were tested both ex situ and in situ, and in situ XRD for 1st discharge/charge and 2...

  16. TEM investigation of plant-irradiated NPP bolt material

    International Nuclear Information System (INIS)

    Pakarinen, J.; Ehrnsten, U.; Keinaenen, H.; Karlsen, W.; Karlsen, T.

    2015-01-01

    Analytical transmission electron microscopy (ATEM) was used to examine irradiation-induced damage in material removed from two different bolts from two different nuclear power plants. One section came from a French PWR, was made of CW AISI 316, and included a section of the bolt that had accumulated a dose of approximately 15 dpa during 19 operation cycles at 350 - 390 C. degrees. Another section came from a VVER bolt that was removed from the plant due to indications found in non-destructive examinations (NDE). The VVER bolt was made of solution annealed titanium stabilized 0X18H10T (corresponding to Type AISI 321) and had accumulated a fluence of 2.9 dpa. During the removal of that bolt, it was found that the bolt washer had been inappropriately spot welded to the shielding plate during assembly. Destructive investigations showed that the bolt had two large intergranular cracks, and the TEM samples were prepared from the material adjacent to those cracks. The PWR bolt had not failed, although cracks in the bolts with a similar history had been found previously. The fluence for the cold-worked AISI 316 PWR bolt was estimated to be about 15 dpa. Both the examined bolts showed a clear radiation induced segregation of alloying elements at the grain boundaries (GB-RIS), the presence of dislocation loops, the formation of precipitates, and linear deformation microstructures. Additionally, voids were found from the PWR bolt and the VVER bolt had a high density of dislocations. (authors)

  17. TEM study of impurity segregations in beryllium pebbles

    Energy Technology Data Exchange (ETDEWEB)

    Klimenkov, M., E-mail: michael.klimenkov@kit.edu [Institute for Applied Materials – Applied Materials Physics, Karlsruhe Institute of Technology, Hermann-von-Helmholz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany); Chakin, V.; Moeslang, A. [Institute for Applied Materials – Applied Materials Physics, Karlsruhe Institute of Technology, Hermann-von-Helmholz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany); Rolli, R. [Institute for Applied Materials – Materials and Biomechanics, Karlsruhe Institute of Technology, Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany)

    2014-12-15

    Beryllium is planned to be used as a neutron multiplier in the Helium-cooled Pebble Bed European concept of a breeding blanket of demonstration power reactor DEMO. In order to evaluate the irradiation performance, individual pebbles and constrained pebble beds were neutron-irradiated at temperatures typical of fusion blankets. Beryllium pebbles 1 mm in diameter produced by the rotating electrode method were subjected to a TEM study before and after irradiation at High Flux Reactor, Petten, Netherlands at 861 K. The grain size varied in a wide range from sub-micron size up to several tens of micrometers, which indicated formation bimodal grain size distribution. Based on the application of combined electron energy loss spectroscopy and energy dispersive X-ray spectroscopy methods, we suggest that impurity precipitates play an important role in controlling the mechanical properties of beryllium. The impurity elements were present in beryllium at a sub-percent concentration form beryllide particles of a complex (Fe/Al/Mn/Cr)B composition. These particles are often ordered along dislocations lines, forming several micron-long chains. It can be suggested that fracture surfaces often extended along these chains in irradiated material.

  18. X-ray diffraction (XRD) characterization of microstrain in some iron and uranium alloys

    International Nuclear Information System (INIS)

    Kimmel, G.; Dayan, D.; Frank, G.A.; Landau, A.

    1996-01-01

    The high linear attenuation coefficient of steel, uranium and uranium based alloys is associated with the small penetration depth of X-rays with the usual wavelength used for diffraction. Nevertheless, by using the proper surface preparation technique, it is possible of obtaining surfaces with bulk properties (free of residual mechanical microstrain). Taking advantage of the feasibility to obtain well prepared surfaces, extensive work has been conducted in studying XRD line broadening effects from flat polycrystalline samples of steel, uranium and uranium alloys

  19. In-situ high temperature XRD of calcium phosphate biomaterial using DEHPA as the starting material

    International Nuclear Information System (INIS)

    Meor Yusoff Meor Sulaiman; Masliana Muslim

    2009-01-01

    A process to produce calcium phosphate biomaterial was done using an organic based phosphoric acid (DEHPA) as its starting material. The gel obtained from this reaction was used to study calcium phosphate transformation using in-situ XRD with temperature ranges from room temperature to 1300 degree C. The results obtained from this analysis show the following phase transformation: Gel β-Ca 2 P 2 O 7 β-TCP + HA α-TCP + HA, β-Ca 2 P 2 O 7 forms at 400 degree C and as we heat the sample at 1000 degree C peaks belonging to β- TCP and HA appears showing the transformation of the β-Ca 2 P 2 O 7 phase. When the sample is heated up further to 1200 degree C, β-TCP is transform into α-TCP. In the cold in-situ study, XRD analysis was performed on the sample from room temperature to -140 degree C. At room the XRD diffractogram shows the sample as an amorphous material and as the temperature was further lowered sharp peaks begins to form indicating that the material had becomes crystalline. The peaks were identified to be that calcium hydrogen phosphate (Ca(H 2 PO 4 ) 2 ) and this indicates that there is no hydroxyl group removal during the cooling process. The relative crystallinity values obtained for the different cooling temperatures show a slow exponential increase on the initial cooling of 0 to -100 degree C and at further cooling temperatures resulted fast and linear process. Also unlike the in-situ XRD analysis performs at high temperature no phase transformation occurred at this low temperature. (Author)

  20. A Study on Factors Affecting Strength of Solidified Peat through XRD and FESEM Analysis

    Science.gov (United States)

    Rahman, J. A.; Napia, A. M. A.; Nazri, M. A. A.; Mohamed, R. M. S. R.; Al-Geethi, A. S.

    2018-04-01

    Peat is soft soil that often causes multiple problems to construction. Peat has low shear strength and high deformation characteristics. Thus, peat soil needs to be stabilized or treated. Study on peat stabilization has been conducted for decades with various admixtures and mixing formulations. This project intends to provide an overview of the solidification of peat soil and the factors that affecting the strength of solidified peat soil. Three types of peats which are fabric, hemic and sapric were used in this study to understand the differences on the effect. The understanding of the factors affecting strength of solidified peat in this study is limited to XRD and FESEM analysis only. Peat samples were collected at Pontian, Johor and Parit Raja, Johor. Peat soil was solidified using fly ash, bottom ash and Portland cement with two mixing formulation following literature review. The solidified peat were cured for 7 days, 14 days, 28 days and 56 days. All samples were tested using Unconfined Compressive Strength Test (UCS), X-ray diffraction (XRD) and Field Emission Scanning Electron Microscope (FESEM). The compressive strength test of solidified peat had shown consistently increase of sheer strength, qu for Mixing 1 while decrease of its compressive strength value for Mixing 2. All samples were tested and compared for each curing days. Through XRD, it is found that all solidified peat are dominated with pargasite and richterite. The highest qu is Fabric Mixing 1(FM1) with the value of 105.94 kPa. This sample were proven contain pargasite. Samples with high qu were observed to be having fly ash and bottom ash bound together with the help of pargasite. Sample with decreasing strength showed less amount of pargasite in it. In can be concluded that XRD and FESEM findings are in line with UCS values.

  1. Study the oxidation kinetics of uranium using XRD and Rietveld method

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Yanzhi; Guan Weijun; Wang Qinguo; Wang Xiaolin; Lai Xinchun; Shuai Maobing, E-mail: yanzhizh@163.com [China Academy of Engineering Physics, PO Box 919-71, Mianyang, Sichuan, 621900 (China)

    2010-03-15

    The surface oxidation of uranium metal has been studied by X-ray diffraction (XRD) and Rietveld method in the range of 50{approx}300deg. C in air. The oxidation processes are analyzed by XRD to determine the extent of surface oxidation and the oxide structure. The dynamics expression for the formation of UO{sub 2} was derived. At the beginning, the dynamic expression was nonlinear, but switched to linear subsequently for uranium in air and humid oxygen. That is, the growth kinetics of UO{sub 2} can be divided into two stages: nonlinear portion and linear portion. Using the kinetic data of linear portion, the activation energy of reaction between uranium and air was calculated about 46.0 kJ/mol. However the content of oxide as a function of time was linear in humid helium ambience. Contrast the dynamics results, it prove that the absence of oxygen would accelerate the corrosion rate of uranium in the humid gas. We can find that the XRD and Rietveld method are a useful convenient method to estimate the kinetics and thermodynamics of solid-gas reaction.

  2. Mineralogical composition of the meteorite El Pozo (Mexico): a Raman, infrared and XRD study.

    Science.gov (United States)

    Ostrooumov, Mikhail; Hernández-Bernal, Maria del Sol

    2011-12-01

    The Raman (RMP), infrared (IR) and XRD analysis have been applied to the examination of mineralogical composition of El Pozo meteorite (an ordinary chondrite L5 type; village Valle of Allende, founded in State of Chihuahua, Mexico: 26°56'N and 105°24'W, 1998). RMP measurements in the range of 100-3500 cm(-1) revealed principal characteristic bands of the major minerals: olivine, two polymorph modifications of pyroxene (OPx and CPx) and plagioclase. Some bands of the minor minerals (hematite and goethite) were also identified. All these minerals were clearly distinguished using IR and XRD techniques. XRD technique has shown the presence of some metallic phases such as kamacite and taenite as well as troilite and chromite. These minerals do not have characteristic Raman spectra because Fe-Ni metals have no active modes for Raman spectroscopy and troilite is a weak Raman scatterer. Raman mapping microspectroscopy was a key part in the investigation of El Pozo meteorite's spatial distribution of the main minerals because these samples are structurally and chemically complex and heterogeneous. The mineral mapping by Raman spectroscopy has provided information for a certain spatial region on which a spatial distribution coexists of the three typical mineral assemblages: olivine; olivine+orthopyroxene; and orthopyroxene. Copyright © 2011 Elsevier B.V. All rights reserved.

  3. Validation of enhanced stabilization of municipal solid waste under controlled leachate recirculation using FTIR and XRD.

    Science.gov (United States)

    Sethi, Sapna; Kothiyal, N C; Nema, Arvind K

    2012-07-01

    Leachate recirculation at neutral PH accompanied with buffer/nutrients addition has been used successfully in earlier stabilization of municipal solid waste in bioreactor landfills. In the present study, efforts were made to enhance the stabilization rate of municipal solid waste (MSW) and organic solid waste (OSW) in simulated landfill bioreactors by controlling the pH of recirculated leachate towards slightly alkaline side in absence of additional buffer and nutrients addition. Enhanced stabilization in waste samples was monitored with the help of analytical tools like Fourier Transform Infrared Spectroscopy (FTIR) and X-Ray Diffraction (XRD). Predominance of bands assigned to inorganic compounds and comparatively lower intensities of bands for organic compounds in the FTIR spectra of waste samples degraded with leachate recirculation under controlled pH confirmed higher rate of biodegradation and mineralization of waste than the samples degraded without controlled leachate recirculation. XRD spectra also confirmed to a greater extent of mineralization in the waste samples degraded under leachate recirculation with controlled pH. Comparison of XRD spectra of two types of wastes pointed out higher degree of mineralization in organic solid waste as compared to municipal solid waste.

  4. [Study on the vibrational spectra and XRD characters of Huanglong jade from Longling County, Yunnan Province].

    Science.gov (United States)

    Pei, Jing-cheng; Fan, Lu-wei; Xie, Hao

    2014-12-01

    Based on the conventional test methods, the infrared absorption spectrum, Raman spectrum and X-ray diffraction (XRD) were employed to study the characters of the vibration spectrum and mineral composition of Huanglong jade. The testing results show that Huanglong jade shows typical vibrational spectrum characteristics of quartziferous jade. The main infrared absorption bands at 1162, 1076, 800, 779, 691, 530 and 466 cm(-1) were induced by the asymmetric stretching vibration, symmetrical stretching vibration and bending vibration of Si-O-Si separately. Especially the absorption band near 800 cm(-1) is split, which indicates that Huanglong jade has good crystallinity. In Raman spectrum, the main strong vibration bands at 463 and 355 cm(-1) were attributed to bending vibration of Si-O-Si. XRD test confirmed that Quartz is main mineral composition of Huanglong jade and there is a small amount of hematite in red color samples which induced the red color of Huanglong jade. This is the first report on the infrared, Raman and XRD spectra feature of Huanglong jade. It will provide a scientific basis for the identification, naming and other research for huanglong jade.

  5. Matching 4.7-Å XRD spacing in amelogenin nanoribbons and enamel matrix.

    Science.gov (United States)

    Sanii, B; Martinez-Avila, O; Simpliciano, C; Zuckermann, R N; Habelitz, S

    2014-09-01

    The recent discovery of conditions that induce nanoribbon structures of amelogenin protein in vitro raises questions about their role in enamel formation. Nanoribbons of recombinant human full-length amelogenin (rH174) are about 17 nm wide and self-align into parallel bundles; thus, they could act as templates for crystallization of nanofibrous apatite comprising dental enamel. Here we analyzed the secondary structures of nanoribbon amelogenin by x-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) and tested if the structural motif matches previous data on the organic matrix of enamel. XRD analysis showed that a peak corresponding to 4.7 Å is present in nanoribbons of amelogenin. In addition, FTIR analysis showed that amelogenin in the form of nanoribbons was comprised of β-sheets by up to 75%, while amelogenin nanospheres had predominantly random-coil structure. The observation of a 4.7-Å XRD spacing confirms the presence of β-sheets and illustrates structural parallels between the in vitro assemblies and structural motifs in developing enamel. © International & American Associations for Dental Research.

  6. Study the oxidation kinetics of uranium using XRD and Rietveld method

    Science.gov (United States)

    Zhang, Yanzhi; Guan, Weijun; Wang, Qinguo; Wang, Xiaolin; Lai, Xinchun; Shuai, Maobing

    2010-03-01

    The surface oxidation of uranium metal has been studied by X-ray diffraction (XRD) and Rietveld method in the range of 50~300°C in air. The oxidation processes are analyzed by XRD to determine the extent of surface oxidation and the oxide structure. The dynamics expression for the formation of UO2 was derived. At the beginning, the dynamic expression was nonlinear, but switched to linear subsequently for uranium in air and humid oxygen. That is, the growth kinetics of UO2 can be divided into two stages: nonlinear portion and linear portion. Using the kinetic data of linear portion, the activation energy of reaction between uranium and air was calculated about 46.0 kJ/mol. However the content of oxide as a function of time was linear in humid helium ambience. Contrast the dynamics results, it prove that the absence of oxygen would accelerate the corrosion rate of uranium in the humid gas. We can find that the XRD and Rietveld method are a useful convenient method to estimate the kinetics and thermodynamics of solid-gas reaction.

  7. FIB-SEM cathodoluminescence tomography: practical and theoretical considerations.

    Science.gov (United States)

    De Winter, D A M; Lebbink, M N; Wiggers De Vries, D F; Post, J A; Drury, M R

    2011-09-01

    Focused ion beam-scanning electron microscope (FIB-SEM) tomography is a powerful application in obtaining three-dimensional (3D) information. The FIB creates a cross section and subsequently removes thin slices. The SEM takes images using secondary or backscattered electrons, or maps every slice using X-rays and/or electron backscatter diffraction patterns. The objective of this study is to assess the possibilities of combining FIB-SEM tomography with cathodoluminescence (CL) imaging. The intensity of CL emission is related to variations in defect or impurity concentrations. A potential problem with FIB-SEM CL tomography is that ion milling may change the defect state of the material and the CL emission. In addition the conventional tilted sample geometry used in FIB-SEM tomography is not compatible with conventional CL detectors. Here we examine the influence of the FIB on CL emission in natural diamond and the feasibility of FIB-SEM CL tomography. A systematic investigation establishes that the ion beam influences CL emission of diamond, with a dependency on both the ion beam and electron beam acceleration voltage. CL emission in natural diamond is enhanced particularly at low ion beam and electron beam voltages. This enhancement of the CL emission can be partly explained by an increase in surface defects induced by ion milling. CL emission enhancement could be used to improve the CL image quality. To conduct FIB-SEM CL tomography, a recently developed novel specimen geometry is adopted to enable sequential ion milling and CL imaging on an untilted sample. We show that CL imaging can be manually combined with FIB-SEM tomography with a modified protocol for 3D microstructure reconstruction. In principle, automated FIB-SEM CL tomography should be feasible, provided that dedicated CL detectors are developed that allow subsequent milling and CL imaging without manual intervention, as the current CL detector needs to be manually retracted before a slice can be milled

  8. Distinction between amorphous and healed planar deformation features in shocked quartz using composite color scanning electron microscope cathodoluminescence (SEM-CL) imaging

    Science.gov (United States)

    Hamers, Maartje F.; Pennock, Gill M.; Herwegh, Marco; Drury, Martyn R.

    2016-10-01

    Planar deformation features (PDFs) in quartz are one of the most reliable and most widely used forms of evidence for hypervelocity impact. PDFs can be identified in scanning electron microscope cathodoluminescence (SEM-CL) images, but not all PDFs show the same CL behavior: there are nonluminescent and red luminescent PDFs. This study aims to explain the origin of the different CL emissions in PDFs. Focused ion beam (FIB) thin foils were prepared of specific sample locations selected in composite color SEM-CL images and were analyzed in a transmission electron microscope (TEM). The FIB preparation technique allowed a direct, often one-to-one correlation between the CL images and the defect structure observed in TEM. This correlation shows that composite color SEM-CL imaging allows distinction between amorphous PDFs on one hand and healed PDFs and basal Brazil twins on the other: nonluminescent PDFs are amorphous, while healed PDFs and basal Brazil twins are red luminescent, with a dominant emission peak at 650 nm. We suggest that the red luminescence is the result of preferential beam damage along dislocations, fluid inclusions, and twin boundaries. Furthermore, a high-pressure phase (possibly stishovite) in PDFs can be detected in color SEM-CL images by its blue luminescence.

  9. New insights into the toxicity of mineral fibres: A combined in situ synchrotron μ-XRD and HR-TEM study of chrysotile, crocidolite, and erionite fibres found in the tissues of Sprague-Dawley rats.

    Science.gov (United States)

    Gualtieri, Alessandro F; Bursi Gandolfi, Nicola; Pollastri, Simone; Burghammer, Manfred; Tibaldi, Eva; Belpoggi, Fiorella; Pollok, Kilian; Langenhorst, Falko; Vigliaturo, Ruggero; Dražić, Goran

    2017-05-15

    Along the line of the recent research topic aimed at understanding the in vivo activity of mineral fibres and their mechanisms of toxicity, this work describes the morpho-chemical characteristics of the mineral fibres found in the tissues of Sprague-Dawley rats subjected to intraperitoneal/intrapleural injection of UICC chrysotile, UICC crocidolite and erionite-Na from Nevada (USA). The fibres are studied with in situ synchrotron powder diffraction and high resolution transmission electron microscopy to improve our understanding of the mechanisms of toxicity of these mineral fibres. In contact with the tissues of the rats, chrysotile fibres are prone to dissolve, with leaching of Mg and production of a silica rich relict. On the other hand, crocidolite and erionite-Na fibres are stable even for very long contact times within the tissues of the rats, showing just a thin dissolution amorphous halo. These findings support the model of a lower biopersistence of chrysotile with respect to crocidolite and erionite-Na but the formation of a silica-rich fibrous residue after the pseudo-amorphization of chrysotile may justify a higher cytotoxic potential and intense inflammatory activity of chrysotile in the short term in contact with the lung tissues. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Sparsity-Based Super Resolution for SEM Images.

    Science.gov (United States)

    Tsiper, Shahar; Dicker, Or; Kaizerman, Idan; Zohar, Zeev; Segev, Mordechai; Eldar, Yonina C

    2017-09-13

    The scanning electron microscope (SEM) is an electron microscope that produces an image of a sample by scanning it with a focused beam of electrons. The electrons interact with the atoms in the sample, which emit secondary electrons that contain information about the surface topography and composition. The sample is scanned by the electron beam point by point, until an image of the surface is formed. Since its invention in 1942, the capabilities of SEMs have become paramount in the discovery and understanding of the nanometer world, and today it is extensively used for both research and in industry. In principle, SEMs can achieve resolution better than one nanometer. However, for many applications, working at subnanometer resolution implies an exceedingly large number of scanning points. For exactly this reason, the SEM diagnostics of microelectronic chips is performed either at high resolution (HR) over a small area or at low resolution (LR) while capturing a larger portion of the chip. Here, we employ sparse coding and dictionary learning to algorithmically enhance low-resolution SEM images of microelectronic chips-up to the level of the HR images acquired by slow SEM scans, while considerably reducing the noise. Our methodology consists of two steps: an offline stage of learning a joint dictionary from a sequence of LR and HR images of the same region in the chip, followed by a fast-online super-resolution step where the resolution of a new LR image is enhanced. We provide several examples with typical chips used in the microelectronics industry, as well as a statistical study on arbitrary images with characteristic structural features. Conceptually, our method works well when the images have similar characteristics, as microelectronics chips do. This work demonstrates that employing sparsity concepts can greatly improve the performance of SEM, thereby considerably increasing the scanning throughput without compromising on analysis quality and resolution.

  11. Oil refinery dusts: morphological and size analysis by TEM.

    Science.gov (United States)

    Sielicki, Przemysław; Janik, Helena; Guzman, Agnieszka; Broniszewski, Mieczysław; Namieśnik, Jacek

    2011-03-01

    The objectives of this work were to develop a means of sampling atmospheric dusts on the premises of an oil refinery for electron microscopic study to carry out preliminary morphological analyses and to compare these dusts with those collected at sites beyond the refinery limits. Carbon and collodion membranes were used as a support for collection of dust particles straight on transmission electron microscopy (TEM) grids. Micrographs of the dust particles were taken at magnifications from ×4,000 to ×80,000 with a Tesla BS500 transmission electron microscope. Four parameters were defined on the basis of the micrographs: surface area, Feret diameter, circumference, and shape coefficient. The micrographs and literature data were used to classify the atmospheric dusts into six groups: particles with an irregular shape and rounded edges; particles with an irregular shape and sharp edges; soot and its aggregates; spherical particles; singly occurring, ultrafine dust particles; and particles not allocated to any of the previous five groups. The types of dusts found in all the samples were similar, although differences did exist between the various morphological parameters. Dust particles with the largest Feret diameter were present in sample 3 (mean, 0.739 μm)-these were collected near the refinery's effluent treatment plant. The particles with the smallest diameter were found in the sample that had been intended to be a reference sample for the remaining results (mean, 0.326 μm). The dust particles collected in the refinery had larger mean Feret diameters, even 100% larger, than those collected beyond it. Particles with diameters from 0.1 to 0.2 μm made up the most numerous group in all the samples collected in the refinery.

  12. Heliborne time-domain electromagnetic (TEM) surveys for uranium exploration

    International Nuclear Information System (INIS)

    Chaturvedi, A.K.

    2015-01-01

    Airborne geophysical surveys have been used extensively in petroleum, mineral exploration, and environmental mapping. Of all the geophysical methods, Electromagnetic (EM) methods, both ground and airborne are used to map the conductive ore bodies buried in the resistive bed rock. Mapping resistivity variations can help unravel complex geological problems and identify areas of hidden potential. Besides the traditional applications to ground water investigations and other natural resource exploration and geological mapping, a number of new applications have been reported. These include hazardous-waste characterization studies, precision agriculture applications, archaeological surveys etc. Airborne Electromagnetic (AEM) methods have undergone rapid improvements over the past few decades. Several new airborne Time Do-main EM (TDEM) systems appeared; existing systems were updated and/or enhanced. The use of natural field (passive) EM surveys continued to increase, with new or improved systems becoming available for both airborne and ground surveys. The number of large airborne survey systems with combined EM, magnetic, gravimetric and gamma-ray spectrometric capabilities also increased. Exploration of a mineral deposit is a multi-stage and multi-disciplinary approach that commences from regional investigations and concludes with establishing of a deposit. As economics play a major role in exploration, a proper integrated study is always beneficial in narrowing down the potential mineral target zones. Heliborne geophysical surveys are being conducted world-wide for exploration of base metals, gold, phosphorite, oil, uranium etc. that are very effective tool in identifying zones of interest accurately, economically and with less span of time. These surveys give a very good insight of surface and sub-surface geophysical signatures that can be attributed to geology with proper modeling. Heliborne Time - domain Electromagnetic (TEM) methods are well known for search of

  13. Oil refinery dusts: morphological and size analysis by TEM

    Energy Technology Data Exchange (ETDEWEB)

    Sielicki, Przemyslaw; Janik, Helena; Guzman, Agnieszka [Gdansk University of Technology, Department of Polymer Technology, Chemical Faculty, Gdansk (Poland); Broniszewski, Mieczyslaw [Environmental Protection Office, Lotos Group, Gdansk (Poland); Namiesnik, Jacek [Gdansk University of Technology, Department of Analytical Chemistry, Chemical Faculty, Gdansk (Poland)

    2011-03-15

    The objectives of this work were to develop a means of sampling atmospheric dusts on the premises of an oil refinery for electron microscopic study to carry out preliminary morphological analyses and to compare these dusts with those collected at sites beyond the refinery limits. Carbon and collodion membranes were used as a support for collection of dust particles straight on transmission electron microscopy (TEM) grids. Micrographs of the dust particles were taken at magnifications from x 4,000 to x 80,000 with a Tesla BS500 transmission electron microscope. Four parameters were defined on the basis of the micrographs: surface area, Feret diameter, circumference, and shape coefficient. The micrographs and literature data were used to classify the atmospheric dusts into six groups: particles with an irregular shape and rounded edges; particles with an irregular shape and sharp edges; soot and its aggregates; spherical particles; singly occurring, ultrafine dust particles; and particles not allocated to any of the previous five groups. The types of dusts found in all the samples were similar, although differences did exist between the various morphological parameters. Dust particles with the largest Feret diameter were present in sample 3 (mean, 0.739 {mu}m) - these were collected near the refinery's effluent treatment plant. The particles with the smallest diameter were found in the sample that had been intended to be a reference sample for the remaining results (mean, 0.326 {mu}m). The dust particles collected in the refinery had larger mean Feret diameters, even 100% larger, than those collected beyond it. Particles with diameters from 0.1 to 0.2 {mu}m made up the most numerous group in all the samples collected in the refinery. (orig.)

  14. Blocos semânticos: o movimento argumentativo na construção do sentido no discurso

    Directory of Open Access Journals (Sweden)

    Ernani Cesar de FREITAS

    2008-07-01

    Full Text Available Este trabalho tem por objetivo sistematizar e aplicar conceitos da Semântica Argumentativa de Oswald Ducrot e Marion Carel, no que diz respeito ao modelo teórico dos Blocos Semânticos, de modo que dêem conta da construção do sentido de unidades mais complexas como o texto e o discurso. A tese concebida como norteadora deste estudo, seguindo a metodologia proposta por Ducrot (1987, pressupõe que o texto é um bloco semântico inscrito no nível teórico da produção e realizado pelo encadeamento argumentativo complexo que é o discurso, orientado argumentativamente pelo uso de conectores tipo DC e/ ou PT. As análises discursivas realizadas, neste trabalho, demonstram que os encadeamentos dos enunciados estão bem marcados pelos conectores donc e pourtant que dão sentido ao discurso complexo, pelas conexões semânticas produzidas em suas AI e AE. Esse movimento argumentativo resulta da interdependência dos segmentos argumentativos, dos encadeamentos e por conseqüência dos blocos semânticos, todos interconectados e interdependentes nas relações de sentido que estabelecem entre si, processo que culmina na realização linguística de nível complexo constituído pelo texto, entidade abstrata subjacente aos discursos realizados, e pelo discurso, como seqüência de enunciados interligados, por isso, também entendido como entidade concreta, ou seja, a manifestação e realização do texto.

  15. Blocos semânticos: o movimento argumentativo na construção do sentido no discurso

    Directory of Open Access Journals (Sweden)

    Ernani Cesar de FREITAS

    2013-10-01

    Full Text Available Este trabalho tem por objetivo sistematizar e aplicar conceitos da Semântica Argumentativa de Oswald Ducrot e Marion Carel, no que diz respeito ao modelo teórico dos Blocos Semânticos, de modo que dêem conta da construção do sentido de unidades mais complexas como o texto e o discurso. A tese concebida como norteadora deste estudo, seguindo a metodologia proposta por Ducrot (1987, pressupõe que o texto é um bloco semântico inscrito no nível teórico da produção e realizado pelo encadeamento argumentativo complexo que é o discurso, orientado argumentativamente pelo uso de conectores tipo DC e/ ou PT. As análises discursivas realizadas, neste trabalho, demonstram que os encadeamentos dos enunciados estão bem marcados pelos conectores donc e pourtant que dão sentido ao discurso complexo, pelas conexões semânticas produzidas em suas AI e AE. Esse movimento argumentativo resulta da interdependência dos segmentos argumentativos, dos encadeamentos e por conseqüência dos blocos semânticos, todos interconectados e interdependentes nas relações de sentido que estabelecem entre si, processo que culmina na realização linguística de nível complexo constituído pelo texto, entidade abstrata subjacente aos discursos realizados, e pelo discurso, como seqüência de enunciados interligados, por isso, também entendido como entidade concreta, ou seja, a manifestação e realização do texto.

  16. An electron moiré method for a common SEM

    Institute of Scientific and Technical Information of China (English)

    Y.M.Xing; S.Kishimoto; Y.R.Zhao

    2006-01-01

    In the electron moiré method,a high-frequency grating is used to measure microscopic deformation,which promises significant potential applications for the method in the microscopic analysis of materials.However,a special beam scanning control device is required to produce a grating and generate a moiré fringe pattern for the scanning electron microscope (SEM).Because only a few SEMs used in the material science studies are equipped with this device,the use of the electron moiré method is limited.In this study,an electron moiré method for a common SEM without the beam control device is presented.A grating based on a multi-scanning concept is fabricated in any observing mode.A real-time moiré pattern can also be generated in the SEM or an optical filtering system.Without the beam control device being a prerequisite,the electron moiré method can be more widely used.The experimental results from three different types of SEMS show that high quality gratings with uniform lines and less pitch error can be fabricated by this method,and moiré patterns can also be correctly generated.

  17. SEM facility for examination of reactive and radioactive materials

    International Nuclear Information System (INIS)

    Downs, G.L.; Tucker, P.A.

    1977-01-01

    A scanning electron microscope (SEM) facility for the examination of tritium-containing materials is operational at Mound Laboratory. The SEM is installed with the sample chamber incorporated as an integral part of an inert gas glovebox facility to enable easy handling of radioactive and pyrophoric materials. A standard SEM (ETEC Model B-1) was modified to meet dimensional, operational, and safety-related requirements. a glovebox was designed and fabricated which permitted access with the gloves to all parts of the SEM sample chamber to facilitate director and accessory replacement and repairs. A separate console combining the electron optical column and specimen chamber was interfaced to the glovebox by a custom-made, neoprene bellows so that the vibrations normally associated with the blowers and pumps were damped. Photomicrographs of tritiated pyrophoric materials show the usefulness of this facility. Some of the difficulties involved in the investigation of these materials are also discussed. The SEM is also equipped with an energy dispersive x-ray detector (ORTEC) and a Secondary Ion Mass Spectrometer (3M) attachments. This latter attachment allows analysis of secondary ions with masses ranging from 1-300 amu. (Auth.)

  18. Recent advances in 3D SEM surface reconstruction.

    Science.gov (United States)

    Tafti, Ahmad P; Kirkpatrick, Andrew B; Alavi, Zahrasadat; Owen, Heather A; Yu, Zeyun

    2015-11-01

    The scanning electron microscope (SEM), as one of the most commonly used instruments in biology and material sciences, employs electrons instead of light to determine the surface properties of specimens. However, the SEM micrographs still remain 2D images. To effectively measure and visualize the surface attributes, we need to restore the 3D shape model from the SEM images. 3D surface reconstruction is a longstanding topic in microscopy vision as it offers quantitative and visual information for a variety of applications consisting medicine, pharmacology, chemistry, and mechanics. In this paper, we attempt to explain the expanding body of the work in this area, including a discussion of recent techniques and algorithms. With the present work, we also enhance the reliability, accuracy, and speed of 3D SEM surface reconstruction by designing and developing an optimized multi-view framework. We then consider several real-world experiments as well as synthetic data to examine the qualitative and quantitative attributes of our proposed framework. Furthermore, we present a taxonomy of 3D SEM surface reconstruction approaches and address several challenging issues as part of our future work. Copyright © 2015 Elsevier Ltd. All rights reserved.

  19. A methodology for extending domain coverage in SemRep.

    Science.gov (United States)

    Rosemblat, Graciela; Shin, Dongwook; Kilicoglu, Halil; Sneiderman, Charles; Rindflesch, Thomas C

    2013-12-01

    We describe a domain-independent methodology to extend SemRep coverage beyond the biomedical domain. SemRep, a natural language processing application originally designed for biomedical texts, uses the knowledge sources provided by the Unified Medical Language System (UMLS©). Ontological and terminological extensions to the system are needed in order to support other areas of knowledge. We extended SemRep's application by developing a semantic representation of a previously unsupported domain. This was achieved by adapting well-known ontology engineering phases and integrating them with the UMLS knowledge sources on which SemRep crucially depends. While the process to extend SemRep coverage has been successfully applied in earlier projects, this paper presents in detail the step-wise approach we followed and the mechanisms implemented. A case study in the field of medical informatics illustrates how the ontology engineering phases have been adapted for optimal integration with the UMLS. We provide qualitative and quantitative results, which indicate the validity and usefulness of our methodology. Published by Elsevier Inc.

  20. JST Thesaurus Headwords and Synonyms: XRD [MeCab user dictionary for science technology term[Archive

    Lifescience Database Archive (English)

    Full Text Available MeCab user dictionary for science technology term XRD 名詞 一般 * * * * X線回折 Xセンカイセツ エックスセンカイセツ Thesaurus2015 200906089250080619 C PA11/PA08 UNKNOWN_1 XRD

  1. SemGroup acquisition of central Alberta midstream : case study

    International Nuclear Information System (INIS)

    Purcell, T.

    2005-01-01

    A case study of SemGroup's acquisition of Central Alberta Midstream was presented. SemCAMS specializes in providing more efficient supply, storage, and distribution assets and services. Seminole Canada Gas is a leading independent natural gas marketing and energy asset management company that currently markets 369 MMbtu per day. The company purchases natural gas in western Canada for fee-based marketing services while also managing firm transportation contracts and providing gas storage for third party customers. SemCAMS owns the largest sour gas processor in Alberta as well as 3 sour gas processing plants, 600 miles of gathering pipeline, and a sweet gas processing plant. the company is also planning increased drilling and production activities and is now pursuing aggressive land acquisition policies. Over 25,000 square miles of land have been acquired. It was concluded that midstream companies should be customer-focused, provide reliability and guarantees, infrastructure investment and optimization. tabs., figs

  2. Critical factors in SEM 3D stereo microscopy

    DEFF Research Database (Denmark)

    Marinello, F.; Bariano, P.; Savio, E.

    2008-01-01

    This work addresses dimensional measurements performed with the scanning electron microscope (SEM) using 3D reconstruction of surface topography through stereo-photogrammetry. The paper presents both theoretical and experimental investigations, on the effects of instrumental variables and measure......This work addresses dimensional measurements performed with the scanning electron microscope (SEM) using 3D reconstruction of surface topography through stereo-photogrammetry. The paper presents both theoretical and experimental investigations, on the effects of instrumental variables...... factors are recognized: the first one is related to the measurement operation and the instrument set-up; the second concerns the quality of scanned images and represents the major criticality in the application of SEMs for 3D characterizations....

  3. Annual International DIC Society Conference and SEM Fall Conference

    CERN Document Server

    Reu, Phillip

    2017-01-01

    This collection represents a single volume of technical papers presented at the Annual International DIC Society Conference and SEM Fall Conference organized by the Society for Experimental Mechanics and Sandia National Laboratories and held in Philadelphia, PA, November 7-10, 2016. The volume presents early findings from experimental, standards development and various other investigations concerning digital image correlation - an important area within Experimental Mechanics. The area of Digital Image Correlation has been an integral track within the SEM Annual Conference spearheaded by Professor Michael Sutton from the University of South Carolina. In 2016, the SEM and Sandia joined their collaborative strengths to launch a standing fall meeting focusing specifically on developments in the area of Digital Image Correlation. The contributed papers within this volume span numerous technical aspects of DIC including standards development for the industry. .

  4. SemVisM: semantic visualizer for medical image

    Science.gov (United States)

    Landaeta, Luis; La Cruz, Alexandra; Baranya, Alexander; Vidal, María.-Esther

    2015-01-01

    SemVisM is a toolbox that combines medical informatics and computer graphics tools for reducing the semantic gap between low-level features and high-level semantic concepts/terms in the images. This paper presents a novel strategy for visualizing medical data annotated semantically, combining rendering techniques, and segmentation algorithms. SemVisM comprises two main components: i) AMORE (A Modest vOlume REgister) to handle input data (RAW, DAT or DICOM) and to initially annotate the images using terms defined on medical ontologies (e.g., MesH, FMA or RadLex), and ii) VOLPROB (VOlume PRObability Builder) for generating the annotated volumetric data containing the classified voxels that belong to a particular tissue. SemVisM is built on top of the semantic visualizer ANISE.1

  5. [Analysis of XRD spectral characteristics of soil clay mineral in two typical cultivated soils].

    Science.gov (United States)

    Zhang, Zhi-Dan; Luo, Xiang-Li; Jiang, Hai-Chao; Li, Qiao; Shen, Cong-Ying; Liu, Hang; Zhou, Ya-Juan; Zhao, Lan-Po; Wang, Ji-Hong

    2014-07-01

    The present paper took black soil and chernozem, the typical cultivated soil in major grain producing area of Northeast, as the study object, and determinated the soil particle composition characteristics of two cultivated soils under the same climate and location. Then XRD was used to study the composition and difference of clay mineral in two kinds of soil and the evolutionary mechanism was explored. The results showed that the two kinds of soil particles were composed mainly of the sand, followed by clay and silt. When the particle accumulation rate reached 50%, the central particle size was in the 15-130 microm interval. Except for black soil profile of Shengli Xiang, the content of clay showed converse sequence to the central particle in two soils. Clay accumulated under upper layer (18.82%) in black soil profile while under caliche layer (17.41%) in chernozem profile. Clay content was the least in parent material horizon except in black profile of Quanyanling. Analysis of clay XRD atlas showed that the difference lied in not only the strength of diffraction peak, but also in the mineral composition. The main contents of black soil and chernozem were both 2 : 1 clay, the composition of black soil was smectite/illite mixed layer-illite-vermiculite and that of chernozem was S/I mixture-illite-montmorillonite, and both of them contained little kaolinite, chlorite, quartz and other primary mineral. This paper used XRD to determine the characteristics of clay minerals comprehensively, and analyzed two kinds of typical cultivated soil comparatively, and it was a new perspective of soil minerals study.

  6. Quantitative XRD analysis: tools to investigate link between hydrous strain and clay mineral CEC

    International Nuclear Information System (INIS)

    Oueslati, W.; Ammar, M.; Ben Rhaiem, H.; Ben Haj Amara, A.

    2012-01-01

    Document available in extended abstract form only. This work aims at examining, by quantitative XRD analysis, the effect of an applied hydrous strain in the cationic exchange process of a di-octahedral smectite (Na-rich montmorillonite SWy-2). The hydrous constraint was created by a continuous, in situ, hydration-dehydration cycles using a variation of the %RH rate. Respectively, The starting, the intermediate and the final stressed samples was deposed in contact with saturated Me 2+ (i.e. Cd 2+ , Co 2+ , Zn 2+ and Ni 2+ ) chloride solutions respectively in order to examine the effect of the retained materials stress on the CEC of the host materials. An XRD profile modelling approach is adopted to describe all structural changes created by the environmental evolution of the %RH rate. This investigation allowed us to determine several structural parameters related to the nature, abundance, size, position and organization of exchangeable cation and water molecule in the inter-lamellar space along the c* axis. The obtained qualitative results show a considerable change in the hydration behaviour, versus the number of hydration - dehydration cycle, from homogeneous '2W' to heterogeneous '1W-2W' hydration state indicating an interstratified hydration phases and due probably to a new organization of the inter-lamellar space content. Quantitatively, the theoretical Mixed Layer Structure MLS suggest the coexistence of more one 'crystallite' species. Which are saturated by more than one exchangeable cations, indicating a partial saturation of all exchangeable sites. Using optimum structural parameter values, deduced from XRD modelling profile approach, some equations which described the evolution of exchangeable cation amount versus the applied hydrous strain were derived. (authors)

  7. Micro-XRD and temperature-modulated DSC investigation of nickel-titanium rotary endodontic instruments.

    Science.gov (United States)

    Alapati, Satish B; Brantley, William A; Iijima, Masahiro; Schricker, Scott R; Nusstein, John M; Li, Uei-Ming; Svec, Timothy A

    2009-10-01

    Employ Micro-X-ray diffraction and temperature-modulated differential scanning calorimetry to investigate microstructural phases, phase transformations, and effects of heat treatment for rotary nickel-titanium instruments. Representative as-received and clinically used ProFile GT and ProTaper instruments were principally studied. Micro-XRD analyses (Cu Kalpha X-rays) were performed at 25 degrees C on areas of approximately 50 microm diameter near the tip and up to 9 mm from the tip. TMDSC analyses were performed from -80 to 100 degrees C and back to -80 degrees C on segments cut from instruments, using a linear heating and cooling rate of 2 degrees C/min, sinusoidal oscillation of 0.318 degrees C, and period of 60s. Instruments were also heat treated 15 min in a nitrogen atmosphere at 400, 500, 600 and 850 degrees C, and analyzed. At all Micro-XRD analysis regions the strongest peak occurred near 42 degrees , indicating that instruments were mostly austenite, with perhaps some R-phase and martensite. Tip and adjacent regions had smallest peak intensities, indicative of greater work hardening, and the intensity at other sites depended on the instrument. TMDSC heating and cooling curves had single peaks for transformations between martensite and austenite. Austenite-finish (A(f)) temperatures and enthalpy changes were similar for as-received and used instruments. Heat treatments at 400, 500 and 600 degrees C raised the A(f) temperature to 45-50 degrees C, and heat treatment at 850 degrees C caused drastic changes in transformation behavior. Micro-XRD provides novel information about NiTi phases at different positions on instruments. TMDSC indicates that heat treatment might yield instruments with substantial martensite and improved clinical performance.

  8. SEM based overlay measurement between resist and buried patterns

    Science.gov (United States)

    Inoue, Osamu; Okagawa, Yutaka; Hasumi, Kazuhisa; Shao, Chuanyu; Leray, Philippe; Lorusso, Gian; Baudemprez, Bart

    2016-03-01

    With the continuous shrink in pattern size and increased density, overlay control has become one of the most critical issues in semiconductor manufacturing. Recently, SEM based overlay of AEI (After Etch Inspection) wafer has been used for reference and optimization of optical overlay (both Image Based Overlay (IBO) and Diffraction Based Overlay (DBO)). Overlay measurement at AEI stage contributes monitor and forecast the yield after formation by etch and calibrate optical measurement tools. however those overlay value seems difficult directly for feedback to a scanner. Therefore, there is a clear need to have SEM based overlay measurements of ADI (After Develop Inspection) wafers in order to serve as reference for optical overlay and make necessary corrections before wafers go to etch. Furthermore, to make the corrections as accurate as possible, actual device like feature dimensions need to be measured post ADI. This device size measurement is very unique feature of CDSEM , which can be measured with smaller area. This is currently possible only with the CD-SEM. This device size measurement is very unique feature of CD-SEM , which can be measured with smaller area. In this study, we assess SEM based overlay measurement of ADI and AEI wafer by using a sample from an N10 process flow. First, we demonstrate SEM based overlay performance at AEI by using dual damascene process for Via 0 (V0) and metal 1 (M1) layer. We also discuss the overlay measurements between litho-etch-litho stages of a triple patterned M1 layer and double pattern V0. Second, to illustrate the complexities in image acquisition and measurement we will measure overlay between M1B resist and buried M1A-Hard mask trench. Finally, we will show how high accelerating voltage can detect buried pattern information by BSE (Back Scattering Electron). In this paper we discuss the merits of this method versus standard optical metrology based corrections.

  9. Spectral studies of 2-pyrazoline derivatives: structural elucidation through single crystal XRD and DFT calculations.

    Science.gov (United States)

    Chinnaraja, D; Rajalakshmi, R; Srinivasan, T; Velmurugan, D; Jayabharathi, J

    2014-04-24

    A series of biologically active N-thiocarbamoyl pyrazoline derivatives have been synthesized using anhydrous potassium carbonate as the catalyst. All the synthesized compounds were characterized by FT-IR, (1)H NMR, (13)C NMR spectral studies, LCMS, CHN Analysis and X-ray diffraction analysis (compound 7). In order to supplement the XRD parameters, molecular modelling was carried out by Gaussian 03W. From the optimized structure, the energy, dipolemoment and HOMO-LUMO energies of all the systems were calculated. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. The XRD Amorphous Component in John Klein Drill Fines at Yellowknife Bay, Gale Crater, Mars

    Science.gov (United States)

    Morris, Richard V.; Ming,, Douglas W.; Blake, David; Vaniman, David; Bish, David L; Chipera, Steve; Downs, Robert; Morrison, Shaunna; Gellert, Ralf; Campbell, Iain; hide

    2013-01-01

    Drill fines of mudstone (targets John Klein and Cumberland) from the Sheepbed unit at Yel-lowknife Bay were analyzed by MSL payload elements including the Chemistry and Mineralogy (CheMin), APXS (Alpha Particle X-Ray Spectrometer), and Sample Analysis at Mars (SAM) instruments. CheMin XRD results show a variety of crystalline phases including feldspar, pyroxene, olivine, oxides, oxyhydroxides, sulfates, sulfides, a tri-octahedral smectite, and XRD amorphous material. The drill fines are distinctly different from corresponding analyses of the global soil (target Rocknest) in that the mudstone samples contained detectable phyllosilicate. Here we focus on John Klein and combine CheMin and APXS data to calculate the chemical composition and concentration of the amorphous component. The chemical composition of the amorphous plus smectite component for John Klein was calculated by subtracting the abundance-weighted chemical composition of the individual XRD crystalline components from the bulk composition of John Kline as measured by APXS. The chemical composition of individual crystalline components was determined either by stoichiometry (e.g., hematite and magnetite) or from their unit cell parameters (e.g., feldspar, olivine, and pyroxene). The chemical composition of the amorphous + smectite component (approx 71 wt.% of bulk sample) and bulk chemical composition are similar. In order to calculate the chemical composition of the amorphous component, a chemical composition for the tri-octahedral smectite must be assumed. We selected two tri-octahedral smectites with very different MgO/(FeO + Fe2O3) ratios (34 and 1.3 for SapCa1 and Griffithite, respectively). Relative to bulk sample, the concentration of amorphous and smectite components are 40 and 29 wt.% for SapCa1 and 33 and 36 wt.% for Griffithite. The amount of smectite was calculated by requiring the MgO concentration to be approx 0 wt.% in the amorphous component. Griffithite is the preferred smectite because

  11. Analytical electron microscopy of Mg-SiO smokes - A comparison with infrared and XRD studies

    Science.gov (United States)

    Rietmeijer, F. J. M.; Nuth, J. A.; Mackinnon, I. D. R.

    1986-01-01

    Analytical electron microscopy conducted for Mg-SiO smokes (experimentally obtained from samples previously characterized by IR spectroscopy) indicates that the microcrystallinity content of unannealed smokes increases with increased annealing for up to 30 hr. The growth of forsterite microcrystallites in the initially nonstoichiometric smokes may give rise to the contemporaneous growth of the SiO polymorph tridymite and MgO; after 4 hr of annealing, these react to form enstatite. It is suggested that XRD analysis and IR spectroscopy should be conducted in conjunction with detailed analytical electron microscopy for the detection of emerging crystallinity in vapor-phase condensates.

  12. Early Medieval ceramics from the Viile Tecii archaeological site (Romania: an optical and XRD study

    Directory of Open Access Journals (Sweden)

    Corina Ionescu

    2007-10-01

    Full Text Available Mineralogical and petrographic studies of Early Medieval potshards exhumed in the Viile Tecii archaeological site (North Transylvania, Romania show a ceramic body composed of a microcrystalline to amorphous matrix, various clasts and voids. The microscopical features and XRD patterns indicate that illitic-kaolinitic clays were used as raw materials, together with quartzitic sands as tempering material. The ceramic vessels were obtained with the potter’s wheel, but the fabric is only slightly oriented, due either to the fast modeling or to the coarseness of the clayish paste. The thermal alteration of mineral phases points to relatively high firing-temperatures, between 800 and 900°C.

  13. XRD analysis and microstructure of milled and sintered V, W, C, and Co powders

    CSIR Research Space (South Africa)

    Bolokang, AS

    2011-01-01

    Full Text Available on the starting compositions of pure elements, their lattice coherency according to Hume-Rothery rules on crystal structure and atomic size, and enough milling time that provides adequate kinetics. Keywords ? X-ray analysis; ? (V,W)C; ? Co15W8C6...-1 International Journal of Refractory Metals and Hard Materials Volume 29, Issue 1, January 2011, Pages 108?111 XRD analysis and microstructure of milled and sintered V, W, C, and Co powders ? A.S. Bolokang ? M.J. Phasha ? C. Oliphant ? D. Motaung ? a...

  14. XRD, lead equivalent and UV-VIS properties study of Ce and Pr lead silicate glasses

    International Nuclear Information System (INIS)

    Alias, Nor Hayati; Abdullah, Wan Shafie Wan; Isa, Norriza Mohd; Isa, Muhammad Jamal Md; Zali, Nurazila Mat; Abdullah, Nuhaslinda Ee; Muhammad, Azali

    2014-01-01

    In this work, Cerium (Ce) and Praseodymium (Pr) containing lead silicate glasses were produced with 2 different molar ratios low (0.2 wt%) and high (0.4wt%). These types of glasses can satisfy the characteristics required for radiation shielding glasses and minimize the lead composition in glass. The radiation shielding properties of the synthesized glasses is explained in the form of lead equivalent study. The XRD diffraction and UV-VIS analysis were performed to observe the structural changes of the synthesis glasses at 1.5 Gy gamma radiation exposures

  15. Protons, ions, electrons and the future of the SEM

    International Nuclear Information System (INIS)

    Joy, D C

    2010-01-01

    The Scanning Electron Microscope (SEM) is the most widely used high performance microscope in all fields of science but it is now reaching the theoretical limits of its performance. While advances in sources, optics, and detectors, can result in some improvement in performance the ultimate resolution is limited by fundamental physical constraints. One potential alternative is a scanning microscope utilizing light ions such as H+ and He+ . Such an instrument shares all of the benefits of the conventional SEM but is free from the constraints encountered when using electrons and could significantly extend the scope and success of scanning microscopy.

  16. What Determines Lean Manufacturing Implementation? A CB-SEM Model

    Directory of Open Access Journals (Sweden)

    Tan Ching Ng

    2018-02-01

    Full Text Available This research aims to ascertain the determinants of effective Lean Manufacturing (LM. In this research, Covariance-based Structural Equation Modeling (CB-SEM analysis will be used in order to analyze the determinants. Through CB-SEM analysis, the significant key determinants can be determined and the direct relationships among determinants can be analyzed. Thus, the findings of this research can act as guidelines for achievement of LM effectiveness, not only providing necessary steps for successful implementation of lean, but also helping lean companies to achieve higher level of lean cost and time savings.

  17. Characterization of TEM1/endosialin in human and murine brain tumors

    International Nuclear Information System (INIS)

    Carson-Walter, Eleanor B; Walter, Kevin A; Winans, Bethany N; Whiteman, Melissa C; Liu, Yang; Jarvela, Sally; Haapasalo, Hannu; Tyler, Betty M; Huso, David L; Johnson, Mahlon D

    2009-01-01

    TEM1/endosialin is an emerging microvascular marker of tumor angiogenesis. We characterized the expression pattern of TEM1/endosialin in astrocytic and metastatic brain tumors and investigated its role as a therapeutic target in human endothelial cells and mouse xenograft models. In situ hybridization (ISH), immunohistochemistry (IH) and immunofluorescence (IF) were used to localize TEM1/endosialin expression in grade II-IV astrocytomas and metastatic brain tumors on tissue microarrays. Changes in TEM1/endosialin expression in response to pro-angiogenic conditions were assessed in human endothelial cells grown in vitro. Intracranial U87MG glioblastoma (GBM) xenografts were analyzed in nude TEM1/endosialin knockout (KO) and wildtype (WT) mice. TEM1/endosialin was upregulated in primary and metastatic human brain tumors, where it localized primarily to the tumor vasculature and a subset of tumor stromal cells. Analysis of 275 arrayed grade II-IV astrocytomas demonstrated TEM1/endosialin expression in 79% of tumors. Robust TEM1/endosialin expression occurred in 31% of glioblastomas (grade IV astroctyomas). TEM1/endosialin expression was inversely correlated with patient age. TEM1/endosialin showed limited co-localization with CD31, αSMA and fibronectin in clinical specimens. In vitro, TEM1/endosialin was upregulated in human endothelial cells cultured in matrigel. Vascular Tem1/endosialin was induced in intracranial U87MG GBM xenografts grown in mice. Tem1/endosialin KO vs WT mice demonstrated equivalent survival and tumor growth when implanted with intracranial GBM xenografts, although Tem1/endosialin KO tumors were significantly more vascular than the WT counterparts. TEM1/endosialin was induced in the vasculature of high-grade brain tumors where its expression was inversely correlated with patient age. Although lack of TEM1/endosialin did not suppress growth of intracranial GBM xenografts, it did increase tumor vascularity. The cellular localization of TEM1

  18. A Data-Driven Approach to SEM Development at a Two-Year College

    Science.gov (United States)

    Pirius, Landon K.

    2014-01-01

    This article explores implementation of strategic enrollment management (SEM) at a two-year college and why SEM is critical to the long-term viability of an institution. This article also outlines the five initial steps needed to implement SEM, including identifying SEM leadership, building a SEM committee, developing a common understanding of…

  19. Effect of the weather in the aging of asphalts by XRD

    Energy Technology Data Exchange (ETDEWEB)

    Cardoso, Edson da R.; Braz, Delson; Lopes, Ricardo T., E-mail: ecardoso@lin.ufrj.b [Coordenacao dos Programas de Pos-graduacao de Engenharia (COPPE/UFRJ), Rio de Janeiro, RJ (Brazil). Programa de Engenharia Nuclear; Motta, Laura M.G. da, E-mail: Laura@coc.ufrj.b [Coordenacao dos Programas de Pos-graduacao de Engenharia (COPPE/UFRJ), Rio de Janeiro, RJ (Brazil). Programa de Construcao Civil/Geotecnia; Barroso, Regina C., E-mail: cely@uerj.b [Universidade do Estado do Rio de Janeiro (UERJ), RJ (Brazil). Inst. de Fisica

    2009-07-01

    Asphalt is a sticky, black and highly viscous liquid or semi-solid that is presented in most crude petroleum and in some natural deposits. As is well known, asphalt has been the preferential choice in pavement construction since excellent utility of pavement, however, as other organic substances, it is also subjected to aging phenomena evolving with time. Asphalt aging is one of the principal factors causing deterioration of asphalt pavements. The photodegradation of asphalts must be considered in the study of the performance of asphalt pavement, especially in geographical regions where high solar radiation intensity occurs. It has an important influence in asphalt aging in tropical places as Brazil. Many methods have been applied to simulate aging of bitumen. It was just a simulation but not real aging asphalt. In this study we submitted the asphalt to the weather as sun and rain. Periodically, during 430 days, the XRD profiles were done and the results analyzed. The scattering measurements were carried out in 0-20 reflection geometry using a powder diffractometer Shimadzu XRD-6000. Scans were typically done from 8 deg to 28 deg every 0.05 deg. The parameters FWHM and peak centroid were analyzed. From 0 until 180 days the aging was faster. The peaks were marked and analyzed with the pass of time. The crystallinity of asphalt increase with weather exposition. Some angles of profiles changed the position indicating change of atomics plans. (author)

  20. Effects of acid treatment on the clay palygorskite: XRD, surface area, morphological and chemical composition

    Energy Technology Data Exchange (ETDEWEB)

    Xavier, Katiane Cruz Magalhaes; Santos, Maria do Socorro Ferreira dos; Santos, Maria Rita Morais Chaves; Oliveira, Marilia Evelyn Rodrigues; Osajima, Josy Antevelli; Silva Filho, Edson Cavalcanti da [Universidade Federal do Piaui (UFPI), Teresina, PI (Brazil); Carvalho, Maria Wilma Nunes Cordeiro, E-mail: edsonfilho@ufpi.edu.br [Universidade Federal de Campina Grande (UFCG), PB (Brazil)

    2014-08-15

    The palygorskite is an aluminum-magnesium silicate that has a fibrous morphology. Their physicochemical characteristics are the result of high surface area, porosity and thermal resistance which make it an attractive adsorbent. Its adsorption capacity can be increased through chemical reactions and/or heat treatments. The objective of this work is to verify the effects of acid activation on the palygorskite, treated with HCl at 90 °C at concentrations of 2, 4 and 6 mol L{sup -1} in 2 and 4 hours, with clay/acid solution ratio 1 g 10 mL{sup -1} and characterized by techniques: XRF, XRD and surface area. A significant increase in specific surface area was observed in the sample treated with HCl at the concentration 6 mol L{sup -1}. The changes were more pronounced at stricter concentrations of acidity, with decreasing intensity of reflection of the clay indicated in the XRD. These changes were confirmed in the XRF with the leaching of some oxides and with increasing concentration of SiO{sub 2}. (author)

  1. Effect of the weather in the aging of asphalts by XRD

    International Nuclear Information System (INIS)

    Cardoso, Edson da R.; Braz, Delson; Lopes, Ricardo T.; Motta, Laura M.G. da; Barroso, Regina C.

    2009-01-01

    Asphalt is a sticky, black and highly viscous liquid or semi-solid that is presented in most crude petroleum and in some natural deposits. As is well known, asphalt has been the preferential choice in pavement construction since excellent utility of pavement, however, as other organic substances, it is also subjected to aging phenomena evolving with time. Asphalt aging is one of the principal factors causing deterioration of asphalt pavements. The photodegradation of asphalts must be considered in the study of the performance of asphalt pavement, especially in geographical regions where high solar radiation intensity occurs. It has an important influence in asphalt aging in tropical places as Brazil. Many methods have been applied to simulate aging of bitumen. It was just a simulation but not real aging asphalt. In this study we submitted the asphalt to the weather as sun and rain. Periodically, during 430 days, the XRD profiles were done and the results analyzed. The scattering measurements were carried out in 0-20 reflection geometry using a powder diffractometer Shimadzu XRD-6000. Scans were typically done from 8 deg to 28 deg every 0.05 deg. The parameters FWHM and peak centroid were analyzed. From 0 until 180 days the aging was faster. The peaks were marked and analyzed with the pass of time. The crystallinity of asphalt increase with weather exposition. Some angles of profiles changed the position indicating change of atomics plans. (author)

  2. Understanding changes in cellulose crystalline structure of lignocellulosic biomass during ionic liquid pretreatment by XRD.

    Science.gov (United States)

    Zhang, Jiafu; Wang, Yixun; Zhang, Liye; Zhang, Ruihong; Liu, Guangqing; Cheng, Gang

    2014-01-01

    X-ray diffraction (XRD) was used to understand the interactions of cellulose in lignocellulosic biomass with ionic liquids (ILs). The experiment was designed in such a way that the process of swelling and solubilization of crystalline cellulose in plant cell walls was followed by XRD. Three different feedstocks, switchgrass, corn stover and rice husk, were pretreated using 1-butyl-3-methylimidazolium acetate ([C4mim][OAc]) at temperatures of 50-130°C for 6h. At a 5 wt.% biomass loading, increasing pretreatment temperature led to a drop in biomass crystallinity index (CrI), which was due to swelling of crystalline cellulose. After most of the crystalline cellulose was swollen with IL molecules, a low-order structure was found in the pretreated samples. Upon further increasing temperature, cellulose II structure started to form in the pretreated biomass samples as a result of solubilization of cellulose in [C4mim][OAc] and subsequent regeneration. Copyright © 2013 Elsevier Ltd. All rights reserved.

  3. Trace elemental analysis of Indian natural moonstone gems by PIXE and XRD techniques.

    Science.gov (United States)

    Venkateswara Rao, R; Venkateswarulu, P; Kasipathi, C; Sivajyothi, S

    2013-12-01

    A selected number of Indian Eastern Ghats natural moonstone gems were studied with a powerful nuclear analytical and non-destructive Proton Induced X-ray Emission (PIXE) technique. Thirteen elements, including V, Co, Ni, Zn, Ga, Ba and Pb, were identified in these moonstones and may be useful in interpreting the various geochemical conditions and the probable cause of their inceptions in the moonstone gemstone matrix. Furthermore, preliminary XRD studies of different moonstone patterns were performed. The PIXE technique is a powerful method for quickly determining the elemental concentration of a substance. A 3MeV proton beam was employed to excite the samples. The chemical constituents of moonstones from parts of the Eastern Ghats geological formations of Andhra Pradesh, India were determined, and gemological studies were performed on those gems. The crystal structure and the lattice parameters of the moonstones were estimated using X-Ray Diffraction studies, trace and minor elements were determined using the PIXE technique, and major compositional elements were confirmed by XRD. In the present work, the usefulness and versatility of the PIXE technique for research in geo-scientific methodology is established. © 2013 Elsevier Ltd. All rights reserved.

  4. An Integrated XRF/XRD Instrument for Mars Exobiology and Geology Experiments

    Science.gov (United States)

    Koppel, L. N.; Franco, E. D.; Kerner, J. A.; Fonda, M. L.; Schwartz, D. E.; Marshall, J. R.

    1993-01-01

    By employing an integrated x-ray instrument on a future Mars mission, data obtained will greatly augment those returned by Viking; details characterizing the past and present environment on Mars and those relevant to the possibility of the origin and evolution of life will be acquired. A combined x-ray fluorescence/x-ray diffraction (XRF/XRD) instrument was breadboarded and demonstrated to accommodate important exobiology and geology experiment objectives outlined for MESUR and future Mars missions. Among others, primary objectives for the exploration of Mars include the intense study of local areas on Mars to establish the chemical, mineralogical, and petrological character of different components of the surface material; to determine the distribution, abundance, and sources and sinks of volatile materials, including an assessment of the biologic potential, now and during past epoches; and to establish the global chemical and physical characteristics of the Martian surface. The XRF/XRD breadboard instrument identifies and quantifies soil surface elemental, mineralogical, and petrological characteristics and acquires data necessary to address questions on volatile abundance and distribution. Additionally, the breadboard is able to characterize the biogenic element constituents of soil samples providing information on the biologic potential of the Mars environment. Preliminary breadboard experiments confirmed the fundamental instrument design approach and measurement performance.

  5. XRD- and infrared-probed anisotropic thermal expansion properties of an organic semiconducting single crystal.

    Science.gov (United States)

    Mohanraj, J; Capria, E; Benevoli, L; Perucchi, A; Demitri, N; Fraleoni-Morgera, A

    2018-01-17

    The anisotropic thermal expansion properties of an organic semiconducting single crystal constituted by 4-hydroxycyanobenzene (4HCB) have been probed by XRD in the range 120-300 K. The anisotropic thermal expansion coefficients for the three crystallographic axes and for the crystal volume have been determined. A careful analysis of the crystal structure revealed that the two different H-bonds stemming from the two independent, differently oriented 4HCB molecules composing the unit cell have different rearrangement patterns upon temperature variations, in terms of both bond length and bond angle. Linearly Polarized Mid InfraRed (LP-MIR) measurements carried out in the same temperature range, focused on the O-H bond spectral region, confirm this finding. The same LP-MIR measurements, on the basis of a semi-empirical relation and of geometrical considerations and assumptions, allowed calculation of the -CNH-O- hydrogen bond length along the a and b axes of the crystal. In turn, the so-calculated -CNH-O- bond lengths were used to derive the thermal expansion coefficients along the corresponding crystal axes, as well as the volumetric one, using just the LP-MIR data. Reasonable to good agreement with the same values obtained from XRD measurements was obtained. This proof-of-principle opens interesting perspectives about the possible development of a rapid, low cost and industry-friendly assessment of the thermal expansion properties of organic semiconducting single crystals (OSSCs) involving hydrogen bonds.

  6. Modeling and measurements of XRD spectra of extended solids under high pressure

    Science.gov (United States)

    Batyrev, I. G.; Coleman, S. P.; Stavrou, E.; Zaug, J. M.; Ciezak-Jenkins, J. A.

    2017-06-01

    We present results of evolutionary simulations based on density functional calculations of various extended solids: N-Si and N-H using variable and fixed concentration methods of USPEX. Predicted from the evolutionary simulations structures were analyzed in terms of thermo-dynamical stability and agreement with experimental X-ray diffraction spectra. Stability of the predicted system was estimated from convex-hull plots. X-ray diffraction spectra were calculated using a virtual diffraction algorithm which computes kinematic diffraction intensity in three-dimensional reciprocal space before being reduced to a two-theta line profile. Calculations of thousands of XRD spectra were used to search for a structure of extended solids at certain pressures with best fits to experimental data according to experimental XRD peak position, peak intensity and theoretically calculated enthalpy. Comparison of Raman and IR spectra calculated for best fitted structures with available experimental data shows reasonable agreement for certain vibration modes. Part of this work was performed by LLNL, Contract DE-AC52-07NA27344. We thank the Joint DoD / DOE Munitions Technology Development Program, the HE C-II research program at LLNL and Advanced Light Source, supported by BES DOE, Contract No. DE-AC02-05CH112.

  7. The chaotic points and XRD analysis of Hg-based superconductors

    Energy Technology Data Exchange (ETDEWEB)

    Aslan, Oe [Anatuerkler Educational Consultancy and Trading Company, Orhan Veli Kanik Cad., 6/1, Kavacik 34810 Beykoz, Istanbul (Turkey); Oezdemir, Z Gueven [Physics Department, Yildiz Technical University, Davutpasa Campus, Esenler 34210, Istanbul (Turkey); Keskin, S S [Department of Environmental Eng., University of Marmara, Ziverbey, 34722, Istanbul (Turkey); Onbasli, Ue, E-mail: ozdenaslan@yahoo.co [Physics Department, University of Marmara, Ridvan Pasa Cad. 3. Sok. 85/12 Goztepe, Istanbul (Turkey)

    2009-03-01

    In this article, high T{sub c} mercury based cuprate superconductors with different oxygen doping rates have been examined by means of magnetic susceptibility (magnetization) versus temperature data and X-ray diffraction pattern analysis. The under, optimally and over oxygen doping procedures have been defined from the magnetic susceptibility versus temperature data of the superconducting sample by extracting the Meissner critical transition temperature, T{sub c} and the paramagnetic Meissner temperature, T{sub PME}, so called as the critical quantum chaos points. Moreover, the optimally oxygen doped samples have been investigated under both a.c. and d.c. magnetic fields. The related a.c. data for virgin(uncut) and cut samples with optimal doping have been obtained under a.c. magnetic field of 1 Gauss. For the cut sample with the rectangular shape, the chaotic points have been found to occur at 122 and 140 K, respectively. The Meissner critical temperature of 140 K is the new world record for the high temperature oxide superconductors under normal atmospheric pressure. Moreover, the crystallographic lattice parameters of superconducting samples have a crucial importance in calculating Josephson penetration depth determined by the XRD patterns. From the XRD data obtained for under and optimally doped samples, the crystal symmetries have been found in tetragonal structure.

  8. Lupeol and its esters: NMR, powder XRD data and in vitro evaluation of cancer cell growth

    Directory of Open Access Journals (Sweden)

    Aline Teixeira Maciel e Silva

    2018-02-01

    Full Text Available ABSTRACT The triterpene lupeol (1 and some of its esters are secondary metabolites produced by species of Celastraceae family, which have being associated with cytotoxic activity. We report herein the isolation of 1, the semi-synthesis of eight lupeol esters and the evaluation of their in vitro activity against nine strains of cancer cells. The reaction of carboxylic acids with 1 and DIC/DMAP was used to obtain lupeol stearate (2, lupeol palmitate (3 lupeol miristate (4, and the new esters lupeol laurate (5, lupeol caprate (6, lupeol caprilate (7, lupeol caproate (8 and lupeol 3’,4’-dimethoxybenzoate (9, with high yields. Compounds 1-9 were identified using FT-IR, 1H, 13C-NMR, CHN analysis and XRD data and were tested in vitro for proliferation of human cancer cell activity. In these assays, lupeol was inactive (GI50> 250µg/mL while lupeol esters 2 -4 and 7 - 9 showed a cytostatic effect. The XRD method was a suitable tool to determine the structure of lupeol and its esters in solid state. Compound 3 showed a selective growth inhibition effect on erythromyeloblastoid leukemia (K-562 cells in a concentration-dependent way. Lupeol esters 4 and 9 showed a selective cytostatic effect with low GI50 values representing promising prototypes for the development of new anticancer drugs.

  9. Determination of equilibrium humidities using temperature and humidity controlled X-ray diffraction (RH-XRD)

    International Nuclear Information System (INIS)

    Linnow, Kirsten; Steiger, Michael

    2007-01-01

    Confined growth of crystals in porous building materials is generally considered to be a major cause of damage. We report on the use of X-ray diffraction under controlled conditions of temperature and relative humidity (RH-XRD) for the investigation of potentially deleterious phase transition reactions. An improved procedure based on rate measurements is used for the accurate and reproducible determination of equilibrium humidities of deliquescence and hydration reactions. The deliquescence humidities of NaCl (75.4 ± 0.5% RH) and Ca(NO 3 ) 2 .4H 2 O (50.8 ± 0.7% RH) at 25 deg. C determined with this improved RH-XRD technique are in excellent agreement with available literature data. Measurement of the hydration of anhydrous Ca(NO 3 ) 2 to form Ca(NO 3 ) 2 .2H 2 O revealed an equilibrium humidity of 10.2 ± 0.3%, which is also in reasonable agreement with available data. In conclusion, dynamic X-ray diffraction measurements are an appropriate method for the accurate and precise determination of equilibrium humidities with a number of interesting future applications

  10. Moessbauer and XRD study of pulse plated Fe-P and Fe-Ni thin layers

    Energy Technology Data Exchange (ETDEWEB)

    Miko, Annamaria [Bay Zoltan Institute for Material Science (Hungary); Kuzmann, Erno, E-mail: kuzmann@para.chem.elte.hu [Eoetvoes Lorand University, Research Group for Nuclear Methods in Structural Chemistry, Hungarian Academy of Sciences, Department of Nuclear Chemistry (Hungary); Lakatos-Varsanyi, Magda [Bay Zoltan Institute for Material Science (Hungary); Kakay, Attila [Research Institute for Solid State Physics and Optics (Hungary); Nagy, Ferenc [Eoetvoes Lorand University, Research Group for Nuclear Methods in Structural Chemistry, Hungarian Academy of Sciences, Department of Nuclear Chemistry (Hungary); Varga, Lajos Karoly [Research Institute for Solid State Physics and Optics (Hungary)

    2005-09-15

    {sup 57}Fe conversion electron Moessbauer spectroscopy, X-ray diffraction, electrochemical and magnetic measurements were used to study pulse electroplated Fe-P and Ni-Fe coatings. XRD and {sup 57}Fe CEMS measurements revealed the amorphous character of the novel pulse plated Fe-P alloys. CEM spectra indicated significant differences in the short range order and in the magnetic anisotropy between the Fe-P deposits pulse plated at medium long deposition time (t{sub on} = 2 ms), with short relaxation time (t{sub off} = 9 ms) and low current density (I{sub p} = 0.05 Acm{sup -2}) or at short deposition time (t{sub on} = 1 ms) with long relaxation time (t{sub off} = 250 ms) and high current density (I{sub p} = 1.0 Acm{sup -2}). The broad peaks centred around the fcc reflections in XRD of the pulse plated Ni-22 wt.% Fe deposit reflected a microcrystalline Ni-Fe alloy with a very fine, 5-8 nm, grain size. The CEM spectrum of the pulse plated Ni-22 wt.% Fe coating corresponded to a highly disordered solid solution alloy containing a minute amount of ferrihydrite. Extreme favourable soft magnetic properties were observed with these Ni-Fe and Fe-P pulse plated thin layers.

  11. Moessbauer and XRD study of pulse plated Fe-P and Fe-Ni thin layers

    International Nuclear Information System (INIS)

    Miko, Annamaria; Kuzmann, Erno; Lakatos-Varsanyi, Magda; Kakay, Attila; Nagy, Ferenc; Varga, Lajos Karoly

    2005-01-01

    57 Fe conversion electron Moessbauer spectroscopy, X-ray diffraction, electrochemical and magnetic measurements were used to study pulse electroplated Fe-P and Ni-Fe coatings. XRD and 57 Fe CEMS measurements revealed the amorphous character of the novel pulse plated Fe-P alloys. CEM spectra indicated significant differences in the short range order and in the magnetic anisotropy between the Fe-P deposits pulse plated at medium long deposition time (t on = 2 ms), with short relaxation time (t off = 9 ms) and low current density (I p = 0.05 Acm -2 ) or at short deposition time (t on = 1 ms) with long relaxation time (t off = 250 ms) and high current density (I p = 1.0 Acm -2 ). The broad peaks centred around the fcc reflections in XRD of the pulse plated Ni-22 wt.% Fe deposit reflected a microcrystalline Ni-Fe alloy with a very fine, 5-8 nm, grain size. The CEM spectrum of the pulse plated Ni-22 wt.% Fe coating corresponded to a highly disordered solid solution alloy containing a minute amount of ferrihydrite. Extreme favourable soft magnetic properties were observed with these Ni-Fe and Fe-P pulse plated thin layers.

  12. OSCE vs. TEM: Different approaches to assess clinical skills of nursing students

    Directory of Open Access Journals (Sweden)

    Prasuna Jelly

    2017-01-01

    Full Text Available Introduction: Nurses are trained with specific clinical skills, and objective structured clinical examination (OSCE could be a better approach to assess clinical skills of nursing students. Materials and Methods: A comparative study was conducted by observational checklist regarding antenatal care and opinionnaire on the usefulness of OSCE and tradition evaluation method (TEM was used to assess the clinical skills and to get opinion. Results: The mean score of OSCE was more than TEM and the difference was statistically significant (P < 0.001. The opinion of students regarding the usefulness of OSCE was higher than TEM. Conclusions: The study concluded that implementing OSCE will overweigh the advantages of the TEM.

  13. Retrofit implementation of Zernike phase plate imaging for cryo-TEM.

    Science.gov (United States)

    Marko, Michael; Leith, Ardean; Hsieh, Chyongere; Danev, Radostin

    2011-05-01

    In-focus phase-plate imaging is particularly beneficial for cryo-TEM because it offers a substantial overall increase in image contrast, without an electron dose penalty, and it simplifies image interpretation. We show how phase-plate cryo-TEM can be implemented with an appropriate existing TEM, and provide a basic practical introduction to use of thin-film (carbon) phase plates. We point out potential pitfalls of phase-plate operation, and discuss solutions. We provide information on evaluating a particular TEM for its suitability. Copyright © 2011 Elsevier Inc. All rights reserved.

  14. A simple algorithm for measuring particle size distributions on an uneven background from TEM images

    DEFF Research Database (Denmark)

    Gontard, Lionel Cervera; Ozkaya, Dogan; Dunin-Borkowski, Rafal E.

    2011-01-01

    Nanoparticles have a wide range of applications in science and technology. Their sizes are often measured using transmission electron microscopy (TEM) or X-ray diffraction. Here, we describe a simple computer algorithm for measuring particle size distributions from TEM images in the presence of a...... application to images of heterogeneous catalysts is presented.......Nanoparticles have a wide range of applications in science and technology. Their sizes are often measured using transmission electron microscopy (TEM) or X-ray diffraction. Here, we describe a simple computer algorithm for measuring particle size distributions from TEM images in the presence...

  15. Investigation of diversity of plasmids carrying the blaTEM-52 gene

    DEFF Research Database (Denmark)

    Bielak, Eliza Maria; Bergenholtz, Rikke D.; Jørgensen, Mikael Skaanning

    2011-01-01

    OBJECTIVES: To investigate the diversity of plasmids that carry blaTEM-52 genes among Escherichia coli and Salmonella enterica originating from animals, meat products and humans. METHODS: A collection of 22 blaTEM-52-encoding plasmids was characterized by restriction fragment length polymorphism...... of self-transfer to a plasmid-free E. coli recipient. CONCLUSIONS: The blaTEM-52 gene found in humans could have been transmitted on transferable plasmids originating from animal sources. Some of the blaTEM-52 plasmids carry replicons that differ from the classical ones. Two novel replicons were detected...

  16. Fast FIB-milled Electron-transparent Microchips for in situ TEM Investigations

    DEFF Research Database (Denmark)

    Lei, Anders; Petersen, Dirch Hjorth; Kallesøe, Christian

    In this work we present a fast approach to 50 nm resolution structures defined in a generic TEM-chip template in few minutes. While creating complex electrical and NEMS circuits for a specific insitu TEM experiment can be a cumbersome process, microchips with 100 nm thin flakes of single crystall......In this work we present a fast approach to 50 nm resolution structures defined in a generic TEM-chip template in few minutes. While creating complex electrical and NEMS circuits for a specific insitu TEM experiment can be a cumbersome process, microchips with 100 nm thin flakes of single...

  17. Identification of proangiogenic TIE2-expressing monocytes (TEMs) in human peripheral blood and cancer.

    Science.gov (United States)

    Venneri, Mary Anna; De Palma, Michele; Ponzoni, Maurilio; Pucci, Ferdinando; Scielzo, Cristina; Zonari, Erika; Mazzieri, Roberta; Doglioni, Claudio; Naldini, Luigi

    2007-06-15

    Tumor-infiltrating myeloid cells, including tumor-associated macrophages (TAMs), have been implicated in tumor progression. We recently described a lineage of mouse monocytes characterized by expression of the Tie2 angiopoietin receptor and required for the vascularization and growth of several tumor models. Here, we report that TIE2 expression in human blood identifies a subset of monocytes distinct from classical inflammatory monocytes and comprised within the less abundant "resident" population. These TIE2-expressing monocytes (TEMs) accounted for 2% to 7% of blood mononuclear cells in healthy donors and were distinct from rare circulating endothelial cells and progenitors. In human cancer patients, TEMs were observed in the blood and, intriguingly, within the tumors, where they represented the main monocyte population distinct from TAMs. Conversely, TEMs were hardly detected in nonneoplastic tissues. In vitro, TEMs migrated toward angiopoietin-2, a TIE2 ligand released by activated endothelial cells and angiogenic vessels, suggesting a homing mechanism for TEMs to tumors. Purified human TEMs, but not TEM-depleted monocytes, markedly promoted angiogenesis in xenotransplanted human tumors, suggesting a potentially critical role of TEMs in human cancer progression. Human TEMs may provide a novel, biologically relevant marker of angiogenesis and represent a previously unrecognized target of cancer therapy.

  18. Cuticle scale measurement of animal fibers by SEM and AFM

    CSIR Research Space (South Africa)

    Notayi, M

    2013-12-01

    Full Text Available -1 51st Microscopy Society of Southern Africa (MSSA) Conference, Farm Inn, Pretoria, 3-6 December 2013 Cuticle scale measurement of animal fibers by SEM and AFM Notayi M, Engelbrechts JAA, Lee ME, Goosen WE, Hunter L and Botha AF Abstract...

  19. Estudo comparativo entre histerectomia abdominal e vaginal sem prolapso uterino

    OpenAIRE

    Lisboa, Vânio Cardoso

    2002-01-01

    Dissertação (mestrado) - Universidade Federal de Santa Catarina, Centro de Ciências da Saúde. Programa de Pós-Graduação em Ciências Médicas. Objetivo: Comparar a histerectomia abdominal e vaginal sem prolapso uterino.

  20. SEM based CARMA time series modeling for arbitrary N

    NARCIS (Netherlands)

    Oud, J.H.L.; Völkle, M.C.; Driver, C.C.

    2018-01-01

    This article explains in detail the state space specification and estimation of first and higher-order autoregressive moving-average models in continuous time (CARMA) in an extended structural equation modeling (SEM) context for N = 1 as well as N > 1. To illustrate the approach, simulations will be

  1. DSS1/Sem1, a multifunctional and intrinsically disordered protein

    DEFF Research Database (Denmark)

    Kragelund, Birthe Brandt; Schenstrøm, Signe Marie; Rebula, Caio A.

    2016-01-01

    DSS1/Sem1 is a versatile intrinsically disordered protein. Besides being a bona fide subunit of the 26S proteasome, DSS1 associates with other protein complexes, including BRCA2-RPA, involved in homologous recombination; the Csn12-Thp3 complex, involved in RNA splicing; the integrator, involved...

  2. Continuous time modeling of panel data by means of SEM

    NARCIS (Netherlands)

    Oud, J.H.L.; Delsing, M.J.M.H.; Montfort, C.A.G.M.; Oud, J.H.L.; Satorra, A.

    2010-01-01

    After a brief history of continuous time modeling and its implementation in panel analysis by means of structural equation modeling (SEM), the problems of discrete time modeling are discussed in detail. This is done by means of the popular cross-lagged panel design. Next, the exact discrete model

  3. Processing a Biological Tissue from Cryo-SEM to Replica

    Czech Academy of Sciences Publication Activity Database

    Vaškovicová, Naděžda; Hrubanová, Kamila; Krzyžánek, Vladislav

    2016-01-01

    Roč. 22, S3 (2016), s. 236-237 ISSN 1431-9276 R&D Projects: GA MŠk(CZ) LO1212; GA MŠk ED0017/01/01 Institutional support: RVO:68081731 Keywords : Cryo-SEM * ACE600 Subject RIV: JA - Electronics ; Optoelectronics, Electrical Engineering Impact factor: 1.891, year: 2016

  4. A combined optical, SEM and STM study of growth spirals

    Indian Academy of Sciences (India)

    Some novel results of a combined sequential study of growth spirals on the basal surface of the richly polytypic CdI2 crystals by optical microscopy, scanning electron microscopy (SEM) and scanning tunneling microscopy (STM) are presented and discussed. In confirmation of the known structural data, the STM pictures ...

  5. SEM Analysis of Surface Impact on Biofilm Antibiotic Treatment.

    Science.gov (United States)

    Gomes, Luciana Calheiros; Mergulhão, Filipe José

    2017-01-01

    The aim of this work was to use scanning electron microscopy (SEM) to investigate the effect of ampicillin treatment on Escherichia coli biofilms formed on two surface materials with different properties, silicone (SIL) and glass (GLA). Epifluorescence microscopy (EM) was initially used to assess biofilm formation and killing efficiency on both surfaces. This technique showed that higher bacterial colonization was obtained in the hydrophobic SIL than in the hydrophilic GLA. It has also shown that higher biofilm inactivation was attained for GLA after the antibiotic treatment (7-log reduction versus 1-log reduction for SIL). Due to its high resolution and magnification, SEM enabled a more detailed analysis of the antibiotic effect on biofilm cells, complementing the killing efficiency information obtained by EM. SEM micrographs revealed that ampicillin-treated cells have an elongated form when compared to untreated cells. Additionally, it has shown that different materials induced different levels of elongation on cells exposed to antibiotic. Biofilms formed on GLA showed a 37% higher elongation than those formed on SIL. Importantly, cell elongation was related to viability since ampicillin had a higher bactericidal effect on GLA-formed biofilms. These findings raise the possibility of using SEM for understanding the efficacy of antimicrobial treatments by observation of biofilm morphology.

  6. SEM Investigation of Superheater Deposits from Biomass-Fired Boilers

    DEFF Research Database (Denmark)

    Jensen, Peter Arendt; Frandsen, Flemming; Hansen, Jørn

    2004-01-01

    , mature superheater deposit samples were extracted from two straw-fired boilers, Masnedø and Ensted, with fuel inputs of 33 MWth and 100 MWth, respectively. SEM (scanning electron microscopy) images and EDX (energy dispersive X-ray) analyses were performed on the deposit samples. Different strategies...

  7. Correlative SEM SERS for quantitative analysis of dimer nanoparticles.

    Science.gov (United States)

    Timmermans, F J; Lenferink, A T M; van Wolferen, H A G M; Otto, C

    2016-11-14

    A Raman microscope integrated with a scanning electron microscope was used to investigate plasmonic structures by correlative SEM-SERS analysis. The integrated Raman-SEM microscope combines high-resolution electron microscopy information with SERS signal enhancement from selected nanostructures with adsorbed Raman reporter molecules. Correlative analysis is performed for dimers of two gold nanospheres. Dimers were selected on the basis of SEM images from multi aggregate samples. The effect of the orientation of the dimer with respect to the polarization state of the laser light and the effect of the particle gap size on the Raman signal intensity is observed. Additionally, calculations are performed to simulate the electric near field enhancement. These simulations are based on the morphologies observed by electron microscopy. In this way the experiments are compared with the enhancement factor calculated with near field simulations and are subsequently used to quantify the SERS enhancement factor. Large differences between experimentally observed and calculated enhancement factors are regularly detected, a phenomenon caused by nanoscale differences between the real and 'simplified' simulated structures. Quantitative SERS experiments reveal the structure induced enhancement factor, ranging from ∼200 to ∼20 000, averaged over the full nanostructure surface. The results demonstrate correlative Raman-SEM microscopy for the quantitative analysis of plasmonic particles and structures, thus enabling a new analytical method in the field of SERS and plasmonics.

  8. Revolving SEM images visualising 3D taxonomic characters

    DEFF Research Database (Denmark)

    Akkari, Nesrine; Cheung, David Koon-Bong; Enghoff, Henrik

    2013-01-01

    images taken consecutively while rotating the SEM stage 360°, which allows the structure in question to be seen from all angles of view in one plane. Seven new species of the genus Ommatoiulus collected in Tunisia are described: O. chambiensis, O. crassinigripes, O. kefi, O. khroumiriensis, O. xerophilus...

  9. Ultrasonic-assisted synthesis of nano lead(II) coordination polymer as precursors for preparation of lead(II) oxide nano-structures: Thermal, optical properties and XRD studies.

    Science.gov (United States)

    Ghavidelaghdam, Elham; Shahverdizadeh, Gholam Hossein; Motameni Tabatabai, Javad; Mirtamizdoust, Babak

    2018-04-01

    Nano structure of a lead (II) coordination polymer [Pb 2 (C 2 Cl 3 O 2 ) 2 (NO 3 ) 2 (C l2 H 8 N 2 ) 2 ] n (1), has been synthesized by a sonochemical method in different concentrations. The nano particles were characterized by scanning electron microscopy (SEM) X-ray powder diffraction (XRD), FT-IR spectroscopy and elemental analyses. The thermal stability of nano structure is closely investigated via thermal gravimetric (TGA), and compared with crystalline structure. The compounds are then heated to 600 °C to produce PbO nano particles. The resulting PbO is characterized through XRD and SEM analyses. Concentration of initial reagents effects on size and morphology of nano-structured compound 1 have been studied and show that low concentrations of initial reagents decreased particles size and leaded to uniform nano particles morphology. The photoluminescence properties of the prepared compound, as crystalline and as nanoparticles, have been investigated. The result showed a good correlation between the size and emission wavelength. Copyright © 2017. Published by Elsevier B.V.

  10. Structural, electronic and optical properties of monoclinic Na2Ti3O7 from density functional theory calculations: A comparison with XRD and optical absorption measurements

    International Nuclear Information System (INIS)

    Araújo-Filho, Adailton A.; Silva, Fábio L.R.; Righi, Ariete; Silva, Mauricélio B. da; Silva, Bruno P.; Caetano, Ewerton W.S.; Freire, Valder N.

    2017-01-01

    Powder samples of bulk monoclinic sodium trititanate Na 2 Ti 3 O 7 were prepared carefully by solid state reaction, and its monoclinic P2 1 /m crystal structure and morphology were characterized by X-ray powder diffraction (XRD) and scanning electron microscopy (SEM), respectively. Moreover, the sodium trititanate main energy band gap was estimated as E g =3.51±0.01 eV employing UV–Vis spectroscopy, which is smaller than the measured 3.70 eV energy gap published previously by other authors. Aiming to achieve a better understanding of the experimental data, density functional theory (DFT) computations were performed within the local density and generalized gradient approximations (LDA and GGA, respectively) taking into account dispersion effects through the scheme of Tkatchenko and Scheffler (GGA+TS). Optimal lattice parameters, with deviations relative to measurements Δa=−0.06 Å, Δb=0.02 Å, and Δc=−0.09 Å, were obtained at the GGA level, which was then used to simulate the sodium trititanate electronic and optical properties. Indirect band transitions have led to a theoretical gap energy value of about 3.25 eV. Our results, however, differ from pioneer DFT results with respect to the specific Brillouin zone vectors for which the indirect transition with smallest energy value occurs. Effective masses for electrons and holes were also estimated along a set of directions in reciprocal space. Lastly, our calculations revealed a relatively large degree of optical isotropy for the Na 2 Ti 3 O 7 optical absorption and complex dielectric function. - Graphical abstract: Monoclinic sodium trititanate Na2Ti3O7 was characterized by experiment and dispersion-corrected DFT calculations. An indirect gap of 3.5 eV is predicted, with heavy electrons and anisotropic holes ruling its conductivity. - Highlights: • Monoclinic Na2Ti3O7 was characterized by experiment (XRD, SEM, UV–Vis spectroscopy). • DFT GGA+TS optimized geometry and optoelectronic properties were

  11. FIB/SEM and SEM/EDS microstructural analysis of metal-ceramic and zirconia-ceramic interfaces.

    Science.gov (United States)

    Massimi, F; Merlati, G; Sebastiani, M; Battaini, P; Menghini, P; Bemporad, E

    2012-01-10

    Recently introduced FIB/SEM analysis in microscopy seems to provide a high-resolution characterization of the samples by 3D (FIB) cross-sectioning and (SEM) high resolution imaging. The aim of this study was to apply the FIB/SEM and SEM/EDS analysis to the interfaces of a metal-ceramic vs. two zirconia-ceramic systems. Plate samples of three different prosthetic systems were prepared in the dental lab following the manufacturers' instructions, where metal-ceramic was the result of a ceramic veneering (porcelain-fused-to-metal) and the two zirconia-ceramic systems were produced by the dedicated CAD-CAM procedures of the zirconia cores (both with final sintering) and then veneered by layered or heat pressed ceramics. In a FIB/SEM equipment (also called DualBeam), a thin layer of platinum (1 μm) was deposited on samples surface crossing the interfaces, in order to protect them during milling. Then, increasingly deeper trenches were milled by a focused ion beam, first using a relatively higher and later using a lower ion current (from 9 nA to 0.28 nA, 30KV). Finally, FEG-SEM (5KV) micrographs (1000-50,000X) were acquired. In a SEM the analysis of the morphology and internal microstructure was performed by 13KV secondary and backscattered electrons signals (in all the samples). The compositional maps were then performed by EDS probe only in the metal-ceramic system (20kV). Despite the presence of many voids in all the ceramic layers, it was possible to identify: (1) the grain structures of the metallic and zirconia substrates, (2) the thin oxide layer at the metal-ceramic interface and its interactions with the first ceramic layer (wash technique), (3) the roughness of the two different zirconia cores and their interactions with the ceramic interface, where the presence of zirconia grains in the ceramic layer was reported in two system possibly due to sandblasting before ceramic firing.

  12. Investigation of synthetic spider silk crystallinity and alignment via electrothermal, pyroelectric, literature XRD, and tensile techniques.

    Science.gov (United States)

    Munro, Troy; Putzeys, Tristan; Copeland, Cameron G; Xing, Changhu; Lewis, Randolph V; Ban, Heng; Glorieux, Christ; Wubbenhorst, Michael

    2017-04-01

    The processes used to create synthetic spider silk greatly affect the properties of the produced fibers. This paper investigates the effect of process variations during artificial spinning on the thermal and mechanical properties of the produced silk. Property values are also compared to the ones of the natural dragline silk of the N. clavipes spider, and to unprocessed (as-spun) synthetic silk. Structural characterization by scanning pyroelectric microscopy is employed to provide insight into the axial orientation of the crystalline regions of the fiber and is supported by XRD data. The results show that stretching and passage through liquid baths induce crystal formation and axial alignment in synthetic fibers, but with different structural organization than natural silks. Furthermore, an increase in thermal diffusivity and elastic modulus is observed with decreasing fiber diameter, trending towards properties of natural fiber. This effect seems to be related to silk fibers being subjected to a radial gradient during production.

  13. Laboratory Detection and Analysis of Organic Compounds in Rocks Using HPLC and XRD Methods

    Science.gov (United States)

    Dragoi, D.; Kanik, I.; Bar-Cohen, Y.; Sherrit, S.; Tsapin, A.; Kulleck, J.

    2004-01-01

    In this work we describe an analytical method for determining the presence of organic compounds in rocks, limestone, and other composite materials. Our preliminary laboratory experiments on different rocks/limestone show that the organic component in mineralogical matrices is a minor phase on order of hundreds of ppm and can be better detected using high precision liquid chromatography (HPLC). The matrix, which is the major phase, plays an important role in embedding and protecting the organic molecules from the harsh Martian environment. Some rocks bear significant amounts of amino acids therefore, it is possible to identify these phases using powder x-ray diffraction (XRD) by crystallizing the organic. The method of detection/analysis of organics, in particular amino acids, that have been associated with life will be shown in the next section.

  14. XRD analysis of undoped and Fe doped TiO2 nanoparticles by Williamson Hall method

    International Nuclear Information System (INIS)

    Bharti, Bandna; Barman, P. B.; Kumar, Rajesh

    2015-01-01

    Undoped and Fe doped titanium dioxide (TiO 2 ) nanoparticles were synthesized by sol-gel method at room temperature. The synthesized samples were annealed at 500°C. For structural analysis, the prepared samples were characterized by X-ray diffraction (XRD). The crystallite size of TiO 2 and Fe doped TiO 2 nanoparticles were calculated by Scherer’s formula, and was found to be 15 nm and 11 nm, respectively. Reduction in crystallite size of TiO 2 with Fe doping was observed. The anatase phase of Fe-doped TiO 2 nanoparticles was also confirmed by X-ray diffraction. By using Williamson-Hall method, lattice strain and crystallite size were also calculated. Williamson–Hall plot indicates the presence of compressive strain for TiO 2 and tensile strain for Fe-TiO 2 nanoparticles annealed at 500°C

  15. XRD total scattering of the CZTS nanoparticle absorber layer for the thin film solar cells

    DEFF Research Database (Denmark)

    Symonowicz, Joanna; Jensen, Kirsten M. Ø.; Engberg, Sara Lena Josefin

    Cu2ZnSnS4 (CZTS) thin film solar cells are cheap, non-toxic and present an efficiency up to 9,2% [1]. They can be easily manufactured by the deposition of the nanoparticle ink as a thin film followed by a thermal treatment to obtain large grains [2]. Therefore, CZTS has the potential...... to revolutionize the solar energy market. However, to commercialize CZTS nanoparticle thin films, the efficiency issues must yet be resolved. In order to do so, it is vital to understand in detail their nanoscale atomic structure. CZTS crystallize in the kesterite structure, where Cu and Zn is distributed between......-ray Diffraction data with X-ray total scattering with Pair Distribution Function analysis. Powder neutron diffraction will furthermore allow characterization of the cation disorder on the metal sites in the kesterite structure. The nanoparticle ink is also characterized by XRD, EDS, and Raman spectroscopy...

  16. Different β-alanine dimeric forms in trifluoromethanesulfonic acid salts. XRD and vibrational studies

    Science.gov (United States)

    Wołoszyn, Łukasz; Ilczyszyn, Maria M.

    2018-03-01

    Two new crystalline salts: β-alaninium trifluoromethanesulfonate (β-AlaOTf) and bis(β-alanine) trifluoromethanesulfonate (β-2AlaOTf) were obtained. The former one contains diprotonated β-alanine dimer, the latter one monoprotonated β-alanine dimer. Both compounds were studied by single crystal XRD, vibrational (IR and Raman) spectroscopy and calorimetric method. The quantum-mechanical calculations (DFT/B3LYP/6-311 ++G(2d,2p)) for the diprotonated dimer were carried out. The β-AlaOTf salt crystallizes in the P 1 bar space group of triclinic system (Z = 2), the β-2AlaOTf in the P21/m space group of monoclinic system (Z = 2). The vibrational data for the studied compounds are discussed in relation to their crystal structure, and provide insight into the character of hydrogen bonds and β-alanine protonation. The studied crystals do not exhibit phase transitions in the solid state.

  17. Crystal imperfection studies of pure and silicon substituted hydroxyapatite using Raman and XRD.

    Science.gov (United States)

    Zou, Shuo; Huang, Jie; Best, Serena; Bonfield, William

    2005-12-01

    Hydroxyapatite (HA) is important in biomedical applications because of its chemical similarity to the mineral content of bone and its consequent bioactivity. Silicon substitution into the hydroxyapatite crystal lattice was found to enhance its bioactivity both in vitro and in vivo [1, 2]. However, the mechanism for the enhancement is still not well understood. In this paper, the crystal imperfections introduced by silicon substitution were studied using XRD and Raman spectroscopy. It was found that silicon substitution did not introduce microstrain, but deceased the crystal size in the hk0 direction. Three new vibration modes and peak broadening were observed in Raman spectra following silicon incorporation. The imperfections introduced by silicon substitution may play a role in enhancing bioactivity. A phenomenological relationship between the width of the PO4 v1 peak and crystal size was established.

  18. Self-assembled silver nanoparticles monolayers on mica-AFM, SEM, and electrokinetic characteristics

    International Nuclear Information System (INIS)

    Oćwieja, Magdalena; Morga, Maria; Adamczyk, Zbigniew

    2013-01-01

    A monodisperse silver particle suspension was produced by a chemical reduction method in an aqueous medium using sodium citrate. The average particle size determined by dynamic light scattering (DLS), transmission electron microscopy (TEM), and atomic force microscopy (AFM) was 28.5 nm. The DLS measurements confirmed that the suspension was stable for the ionic strength up to 3 × 10 −2 M NaCl. The electrophoretic mobility measurements revealed that the electrokinetic charge of particles was negative for pH range 3–10, assuming −50 e for pH = 9 and 0.01 M NaCl. Using the suspension, silver particle monolayers on mica modified by poly(allylamine hydrochloride) were produced under diffusion-controlled transport. Monolayer coverage, quantitatively determined by AFM and SEM, was regulated within broad limits by adjusting the nanoparticle deposition time. This allowed one to uniquely express the zeta potential of silver monolayers, determined by the in situ streaming potential measurements, in terms of particle coverage. Such dependencies obtained for various ionic strengths and pH, were successfully interpreted in terms of the 3D electrokinetic model. A universal calibrating graph was produced in this way, enabling one to determine silver monolayer coverage from the measured value of the streaming potential. Our experimental data prove that it is feasible to produce uniform and stable silver particle monolayers of well-controlled coverage and defined electrokinetic properties.

  19. Self-assembled silver nanoparticles monolayers on mica-AFM, SEM, and electrokinetic characteristics.

    Science.gov (United States)

    Oćwieja, Magdalena; Morga, Maria; Adamczyk, Zbigniew

    2013-03-01

    A monodisperse silver particle suspension was produced by a chemical reduction method in an aqueous medium using sodium citrate. The average particle size determined by dynamic light scattering (DLS), transmission electron microscopy (TEM), and atomic force microscopy (AFM) was 28.5 nm. The DLS measurements confirmed that the suspension was stable for the ionic strength up to 3 × 10 -2  M NaCl. The electrophoretic mobility measurements revealed that the electrokinetic charge of particles was negative for pH range 3-10, assuming -50  e for pH = 9 and 0.01 M NaCl. Using the suspension, silver particle monolayers on mica modified by poly(allylamine hydrochloride) were produced under diffusion-controlled transport. Monolayer coverage, quantitatively determined by AFM and SEM, was regulated within broad limits by adjusting the nanoparticle deposition time. This allowed one to uniquely express the zeta potential of silver monolayers, determined by the in situ streaming potential measurements, in terms of particle coverage. Such dependencies obtained for various ionic strengths and pH, were successfully interpreted in terms of the 3D electrokinetic model. A universal calibrating graph was produced in this way, enabling one to determine silver monolayer coverage from the measured value of the streaming potential. Our experimental data prove that it is feasible to produce uniform and stable silver particle monolayers of well-controlled coverage and defined electrokinetic properties.

  20. FIB/SEM technology and high-throughput 3D reconstruction of dendritic spines and synapses in GFP-labeled adult-generated neurons

    Directory of Open Access Journals (Sweden)

    Carles eBosch

    2015-05-01

    Full Text Available The fine analysis of synaptic contacts is usually performed using transmission electron microscopy (TEM and its combination with neuronal labeling techniques. However, the complex 3D architecture of neuronal samples calls for their reconstruction from serial sections. Here we show that focused ion beam/scanning electron microscopy (FIB/SEM allows efficient, complete, and automatic 3D reconstruction of identified dendrites, including their spines and synapses, from GFP/DAB-labeled neurons, with a resolution comparable to that of TEM. We applied this technology to analyze the synaptogenesis of labeled adult-generated granule cells (GCs in mice. 3D reconstruction of spines in GCs aged 3–4 and 8–9 weeks revealed two different stages of spine development and unexpected features of synapse formation, including vacant and branched spines and presynaptic terminals establishing synapses with up to 10 spines. Given the reliability, efficiency, and high resolution of FIB/SEM technology and the wide use of DAB in conventional EM, we consider FIB/SEM fundamental for the detailed characterization of identified synaptic contacts in neurons in a high-throughput manner.

  1. Spectroscopic, DFT, and XRD Studies of Hydrogen Bonds in N-Unsubstituted 2-Aminobenzamides.

    Science.gov (United States)

    Mphahlele, Malose Jack; Maluleka, Marole Maria; Rhyman, Lydia; Ramasami, Ponnadurai; Mampa, Richard Mokome

    2017-01-04

    The structures of the mono- and the dihalogenated N -unsubstituted 2-aminobenzamides were characterized by means of the spectroscopic (¹H-NMR, UV-Vis, FT-IR, and FT-Raman) and X-ray crystallographic techniques complemented with a density functional theory (DFT) method. The hindered rotation of the C(O)-NH₂ single bond resulted in non-equivalence of the amide protons and therefore two distinct resonances of different chemical shift values in the ¹H-NMR spectra of these compounds were observed. 2-Amino-5-bromobenzamide ( ABB ) as a model confirmed the presence of strong intramolecular hydrogen bonds between oxygen and the amine hydrogen. However, intramolecular hydrogen bonding between the carbonyl oxygen and the amine protons was not observed in the solution phase due to a rapid exchange of these two protons with the solvent and fast rotation of the Ar-NH₂ single bond. XRD also revealed the ability of the amide unit of these compounds to function as a hydrogen bond donor and acceptor simultaneously to form strong intermolecular hydrogen bonding between oxygen of one molecule and the NH moiety of the amine or amide group of the other molecule and between the amine nitrogen and the amide hydrogen of different molecules. DFT calculations using the B3LYP/6-311++G(d,p) basis set revealed that the conformer ( A ) with oxygen and 2-amine on the same side predominates possibly due to the formation of a six-membered intramolecular ring, which is assisted by hydrogen bonding as observed in the single crystal XRD structure.

  2. Reduction of mixed Mn-Zr oxides: in situ XPS and XRD studies.

    Science.gov (United States)

    Bulavchenko, O A; Vinokurov, Z S; Afonasenko, T N; Tsyrul'nikov, P G; Tsybulya, S V; Saraev, A A; Kaichev, V V

    2015-09-21

    A series of mixed Mn-Zr oxides with different molar ratios Mn/Zr (0.1-9) have been prepared by coprecipitation of manganese and zirconium nitrates and characterized by X-ray diffraction (XRD) and BET methods. It has been found that at concentrations of Mn below 30 at%, the samples are single-phase solid solutions (MnxZr1-xO2-δ) based on a ZrO2 structure. X-ray photoelectron spectroscopy (XPS) measurements showed that manganese in these solutions exists mainly in the Mn(4+) state on the surface. An increase in Mn content mostly leads to an increase in the number of Mn cations in the structure of solid solutions; however, a part of the manganese cations form Mn2O3 and Mn3O4 in the crystalline and amorphous states. The reduction of these oxides with hydrogen was studied by a temperature-programmed reduction technique, in situ XRD, and near ambient pressure XPS in the temperature range from 100 to 650 °C. It was shown that the reduction of the solid solutions MnxZr1-xO2-δ proceeds via two stages. During the first stage, at temperatures between 100 and 500 °C, the Mn cations incorporated into the solid solutions MnxZr1-xO2-δ undergo partial reduction. During the second stage, at temperatures between 500 and 700 °C, Mn cations segregate on the surface of the solid solution. In the samples with more than 30 at% Mn, the reduction of manganese oxides was observed: Mn2O3 → Mn3O4 → MnO.

  3. Thermal decomposition of dolomite under CO2: insights from TGA and in situ XRD analysis.

    Science.gov (United States)

    Valverde, Jose Manuel; Perejon, Antonio; Medina, Santiago; Perez-Maqueda, Luis A

    2015-11-28

    Thermal decomposition of dolomite in the presence of CO2 in a calcination environment is investigated by means of in situ X-ray diffraction (XRD) and thermogravimetric analysis (TGA). The in situ XRD results suggest that dolomite decomposes directly at a temperature around 700 °C into MgO and CaO. Immediate carbonation of nascent CaO crystals leads to the formation of calcite as an intermediate product of decomposition. Subsequently, decarbonation of this poorly crystalline calcite occurs when the reaction is thermodynamically favorable and sufficiently fast at a temperature depending on the CO2 partial pressure in the calcination atmosphere. Decarbonation of this dolomitic calcite occurs at a lower temperature than limestone decarbonation due to the relatively low crystallinity of the former. Full decomposition of dolomite leads also to a relatively low crystalline CaO, which exhibits a high reactivity as compared to limestone derived CaO. Under CO2 capture conditions in the Calcium-Looping (CaL) process, MgO grains remain inert yet favor the carbonation reactivity of dolomitic CaO especially in the solid-state diffusion controlled phase. The fundamental mechanism that drives the crystallographic transformation of dolomite in the presence of CO2 is thus responsible for its fast calcination kinetics and the high carbonation reactivity of dolomitic CaO, which makes natural dolomite a potentially advantageous alternative to limestone for CO2 capture in the CaL technology as well as SO2in situ removal in oxy-combustion fluidized bed reactors.

  4. Spectroscopic, DFT, and XRD Studies of Hydrogen Bonds in N-Unsubstituted 2-Aminobenzamides

    Directory of Open Access Journals (Sweden)

    Malose Jack Mphahlele

    2017-01-01

    Full Text Available The structures of the mono- and the dihalogenated N-unsubstituted 2-aminobenzamides were characterized by means of the spectroscopic (1H-NMR, UV-Vis, FT-IR, and FT-Raman and X-ray crystallographic techniques complemented with a density functional theory (DFT method. The hindered rotation of the C(O–NH2 single bond resulted in non-equivalence of the amide protons and therefore two distinct resonances of different chemical shift values in the 1H-NMR spectra of these compounds were observed. 2-Amino-5-bromobenzamide (ABB as a model confirmed the presence of strong intramolecular hydrogen bonds between oxygen and the amine hydrogen. However, intramolecular hydrogen bonding between the carbonyl oxygen and the amine protons was not observed in the solution phase due to a rapid exchange of these two protons with the solvent and fast rotation of the Ar–NH2 single bond. XRD also revealed the ability of the amide unit of these compounds to function as a hydrogen bond donor and acceptor simultaneously to form strong intermolecular hydrogen bonding between oxygen of one molecule and the NH moiety of the amine or amide group of the other molecule and between the amine nitrogen and the amide hydrogen of different molecules. DFT calculations using the B3LYP/6-311++G(d,p basis set revealed that the conformer (A with oxygen and 2-amine on the same side predominates possibly due to the formation of a six-membered intramolecular ring, which is assisted by hydrogen bonding as observed in the single crystal XRD structure.

  5. Molecular identification of TEM-116 beta-lactamase gene in isolates ...

    African Journals Online (AJOL)

    Purpose: Purpose: To determine TEM-116 beta-lactamase gene prevalence in drug-resistant Pseudomonas aeruginosa isolates from Pakistan. Methods: Sequence analysis of TEM beta-lactamase isolates and their antibiotic susceptibility patterns were carried out. Quantitative bacteriostatic concentrations for commonly ...

  6. Use of the TEM Cell for Compliance Testing of Emissions and Immunity, an IEC Perspective

    DEFF Research Database (Denmark)

    Bentz, Sigurd

    1996-01-01

    The current work of the IEC on preparing a standard for the use of TEM cells for compliance testing of emissions and immunity is reviewed. The requirements of TEM cells are related to the established procedures: “open area test site” and “shielded enclosure with area of uniform field”, respective...

  7. Pilot production of track etch membranes (TEMS) using heavy ion beam scanner

    International Nuclear Information System (INIS)

    Nair, J.P.; Surendran, P.; Sparrow, Hillary; Ninawe, N.G.; Bhagwat, P.V.; Acharya, N.; Kulshreshta, V.; Rajesh Kumar; Vijay, Y.K.; Kurup, M.B.

    2005-01-01

    Various methods for making TEMs were conducted at Pelletron Accelerator Facility. The technique for production using ion beam scattering was also established. This is an effort to make TEMs on pilot basis at BARC- TIFR Pelletron Accelerator using Heavy Ion Beam Scanner till large rolling mechanism is implemented

  8. ANALISIS JARINGAN UMTS PADA MENARA ROOFTOP DENGAN MENGGUNAKAN SOFTWARE TEMS INVESTIGATION DAN G-NETTRACK PRO

    OpenAIRE

    Pande Putu Wahyu Pramanda; Pande Ketut Sudiarta; Ngurah Indra ER.

    2016-01-01

    Berkembangnya dunia teknologi telekomunikasi dan informasi sejalan dengan kebutuhan akan kecepatan dan kestabilan akses internet teknologi UMTS. Metode drive test adalah metode yang biasanya digunakan untuk pengukuran kualitas sebuah site. Pihak provider umumnya menggunakan software TEMS Investigation dalam melakukan drive test. Melakukan drive test dengan TEMS Investigation sangatlah tidak praktis dan memerlukan biaya yang besar. Berkembangnya teknologi smartphone membuat drive test dapat di...

  9. Oxidation in ceria infiltrated metal supported SOFCs – A TEM investigation

    DEFF Research Database (Denmark)

    Knibbe, Ruth; Wang, Hsiang-Jen; Blennow Tullmar, Peter

    2013-01-01

    electron microscopy (TEM) techniques including energy-dispersive X-ray spectroscopy and electron energy-loss spectroscopy of focus ion beamed TEM samples. The infiltrated CGO is predominately converted into CeFeO3 after high temperature processing, protecting the alloy. A thin layer of Cr-oxide is observed...

  10. Critical factors in SEM 3D stereo microscopy

    International Nuclear Information System (INIS)

    Marinello, F; Savio, E; Bariani, P; Horsewell, A; De Chiffre, L

    2008-01-01

    This work addresses dimensional measurements performed with the scanning electron microscope (SEM) using 3D reconstruction of surface topography through stereo-photogrammetry. The paper presents both theoretical and experimental investigations, on the effects of instrumental variables and measurement parameters on reconstruction accuracy. Investigations were performed on a novel sample, specifically developed and implemented for the tests. The description is based on the model function introduced by Piazzesi and adapted for eucentrically tilted stereopairs. Two main classes of influencing factors are recognized: the first one is related to the measurement operation and the instrument set-up; the second concerns the quality of scanned images and represents the major criticality in the application of SEMs for 3D characterizations

  11. Three dimensional imaging of surface geometry in SEM

    International Nuclear Information System (INIS)

    Slowko, W.

    1997-01-01

    A great advantage of scanning electron microscopy (SEM) is its ability of the surface topography in the way as a human eye is accustomed to see lights and shadows on macroobjects. However, SEM's can hardly display vertical dimensions of the structures. One of possible solutions is reconstruction of the surface profiles by directional detection of secondary electrons and proper signal processing. However, the surface profile still gives two dimensional information and the method should be extended to obtain fully three dimensional imaging. The extension consists in a simultaneous reconstruction of the surface profiles in two perpendicular directions (x and y) and their superposition. The solution proposed is based on a quadrupole detector system and a computer or analogue system for signal processing. Quantitative data of the surface topography can be displayed in many manners in the system of two or three co-ordinates with use of pseudo-colour for the altitude coding. (author)

  12. SEM and Raman studies of CNT films on porous Si

    Science.gov (United States)

    Belka, R.; Keczkowska, J.; Suchańska, M.; Firek, P.; Wronka, H.; Kozłowski, M.; Radomska, J.; Czerwosz, E.; Craciunoiu, F.

    2017-08-01

    Carbon nanotube (CNT) films deposited on different porous silica substrates were studied by Scanning Electron Microscopy (SEM) and Raman Spectroscopy (RS). The films samples were prepared by a two-step method consisting of PVD and CVD processes. In the first step the nanocomposite Ni-C film was obtained by evaporation in dynamic vacuum from two separated sources of fullerenes and nickel acetate. Those films were deposited on porous silica and DLC/porous silica substrates. Analysis of SEM imaging showed that the obtained film are composed of carbon nanotubes, the distribution, size and quality of which depend on the type of substrate. The CNT films were studied by RS method to determine the influence of the substrate type on disordering of carbonaceous structure and quality of CNT in deposited films.

  13. Repetitive Observation of Coniferous Samples in ESEM and SEM

    Czech Academy of Sciences Publication Activity Database

    Tihlaříková, Eva; Neděla, Vilém

    2015-01-01

    Roč. 21, S3 (2015), s. 1695-1696 ISSN 1431-9276 R&D Projects: GA ČR(CZ) GA14-22777S; GA MŠk(CZ) LO1212; GA MŠk ED0017/01/01 Institutional support: RVO:68081731 Keywords : SEM * ESEM * biological samples * repetitive observation Subject RIV: JA - Electronics ; Optoelectronics, Electrical Engineering Impact factor: 1.730, year: 2015

  14. Surface characteristics of isopod digestive gland epithelium studied by SEM.

    Science.gov (United States)

    Millaku, Agron; Leser, Vladka; Drobne, Damjana; Godec, Matjaz; Torkar, Matjaz; Jenko, Monika; Milani, Marziale; Tatti, Francesco

    2010-05-01

    The structure of the digestive gland epithelium of a terrestrial isopod Porcellio scaber has been investigated by conventional scanning electron microscopy (SEM), focused ion beam-scanning electron microscopy (FIB/SEM), and light microscopy in order to provide evidence on morphology of the gland epithelial surface in animals from a stock culture. We investigated the shape of cells, extrusion of lipid droplets, shape and distribution of microvilli, and the presence of bacteria on the cell surface. A total of 22 animals were investigated and we found some variability in the appearance of the gland epithelial surface. Seventeen of the animals had dome-shaped digestive gland "normal" epithelial cells, which were densely and homogeneously covered by microvilli and varying proportions of which extruded lipid droplets. On the surface of microvilli we routinely observed sparsely distributed bacteria of different shapes. Five of the 22 animals had "abnormal" epithelial cells with a significantly altered shape. In three of these animals, the cells were much smaller, partly or completely flat or sometimes pyramid-like. A thick layer of bacteria was detected on the microvillous border, and in places, the shape and size of microvilli were altered. In two animals, hypertrophic cells containing large vacuoles were observed indicating a characteristic intracellular infection. The potential of SEM in morphological investigations of epithelial surfaces is discussed.

  15. Analysis of microtraces in invasive traumas using SEM/EDS.

    Science.gov (United States)

    Vermeij, E J; Zoon, P D; Chang, S B C G; Keereweer, I; Pieterman, R; Gerretsen, R R R

    2012-01-10

    Scanning electron microscopy in combination with energy-dispersive X-ray spectrometry (SEM/EDS) is a proven forensic tool and has been used to analyze several kinds of trace evidence. A forensic application of SEM/EDS is the examination of morphological characteristics of tool marks that tools and instruments leave on bone. The microtraces that are left behind by these tools and instruments on the bone are, however, often ignored or not noticed at all. In this paper we will describe the use of SEM/EDS for the analysis of microtraces in invasive sharp-force, blunt-force and bone-hacking traumas in bone. This research is part of a larger multi-disciplinary approach in which pathologists, forensic anthropologists, toolmark and microtrace experts work together to link observed injuries to a suspected weapon or, in case of an unknown weapon, to indicate a group of objects that could have been used as a weapon. Although there are a few difficulties one have to consider, the method itself is rather simple and straightforward to apply. A sample of dry and clean bone is placed into the SEM sample chamber and brightness and contrast are set such that bone appears grey, metal appears white and organic material appears black. The sample is then searched manually to find relevant features. Once features are found their elemental composition is measured by an energy dispersive X-ray spectrometer (EDS). This method is illustrated using several cases. It is shown that SEM/EDS analysis of microtraces in bone is a valuable tool to get clues about an unknown weapon and can associate a specific weapon with injuries on the basis of appearance and elemental composition. In particular the separate results from the various disciplines are complementary and may be combined to reach a conclusion with a stronger probative value. This is not only useful in the courtroom but above all in criminal investigations when one have to know for what weapon or object to look for. Copyright © 2011

  16. Análisis de ítems y evidencias de fiabilidad de la Escala sobre Representación Cognitiva de la Enfermedad (ERCE

    Directory of Open Access Journals (Sweden)

    Macarena De los Santos-Roig

    2014-05-01

    Full Text Available La Escala sobre Representación Cognitiva de la Enfermedad, ERCE (De los Santos-Roig, 2009 ha sido elaborada para evaluar las creencias de los pacientes sobre su enfermedad. El modelo de Sentido Común, donde se inserta el constructo, ha sido puesto a prueba en numerosas ocasiones, encontrándose evidencia sobre la importancia de la Representación Cognitiva en los procesos de adaptación a la enfermedad (Hagger y Orbell, 2003; Leventhal et al., 1997. Su medida en nuestro ámbito cultural es necesaria, tanto desde un punto de vista teórico, como desde una perspectiva aplicada. Lo que aquí se muestra es la continuación a un trabajo previo (De los Santos-Roig, 2009; De los Santos-Roig y Pérez-Meléndez, 2013 donde se concretó la definición semántica del constructo RCE y las Tablas de Especificaciones del Test y de los Ítems, que finalmente culminó con la presentación de los primeros ítems construidos. Siguiendo con lo establecido en los estándares (AERA, APA y NCME, 1999, se muestran ahora los resultados del análisis estadístico de los ítems correspondientes a las cinco escalas que componen la ERCE, así como los obtenidos sobre sus evidencias de fiabilidad. Al final, se concluye sobre la idoneidad de los ítems que conforman la escala.

  17. Geoelectrical characterization by joint inversion of VES/TEM in Paraná basin, Brazil

    Science.gov (United States)

    Bortolozo, C. A.; Couto, M. A.; Almeida, E. R.; Porsani, J. L.; Santos, F. M.

    2012-12-01

    For many years electrical (DC) and transient electromagnetic (TEM) soundings have been used in a great number of environmental, hydrological and mining exploration studies. The data of both methods are interpreted usually by individual 1D models resulting in many cases in ambiguous models. This can be explained by how the two different methodologies sample the subsurface. The vertical electrical sounding (VES) is good on marking very resistive structures, while the transient electromagnetic sounding (TEM) is very sensitive to map conductive structures. Another characteristic is that VES is more sensitive to shallow structures, while TEM soundings can reach deeper structures. A Matlab program for joint inversion of VES and TEM soundings, by using CRS algorithm was developed aiming explore the best of the both methods. Initially, the algorithm was tested with synthetic data and after it was used to invert experimental data from Paraná sedimentary basin. We present the results of a re-interpretation of 46 VES/TEM soundings data set acquired in Bebedouro region in São Paulo State - Brazil. The previous interpretation was based in geoelectrical models obtained by single inversion of the VES and TEM soundings. In this work we present the results with single inversion of VES and TEM sounding inverted by the Curupira Program and a new interpretation based in the joint inversion of both methodologies. The goal is increase the accuracy in determining the underground structures. As a result a new geoelectrical model of the region is obtained.

  18. In situ TEM-tandem/implanter interface facility in Wuhan University for investigation of radiation effects

    International Nuclear Information System (INIS)

    Guo Liping; Li Ming; Liu Chuansheng; Song Bo; Ye Mingsheng; Fan Xiangjun; Fu Dejun

    2007-01-01

    Transmission electron microscope (TEM) interfaced to one or more ion implanters and/or accelerators, i.e. in situ TEM, provides effective tools to observe microstructural changes of studied samples during the ion irradiation. Evolution of both radiation damages and irradiation-induced nano-sized microstructures can be investigated with this technique, much more convenient than conventional ex situ techniques. In situ TEM technique has been widely applied in various fields, especially in the study of radiation damages of structural materials of fission and fusion nuclear reactors, and in evaluation and qualification of radioactive waste forms. Nowadays there are more than a dozen such facilities located in Japan, France, and the United States. Recently, we have constructed the first TEM-Tandem/Implanter interface facility of China in Wuhan University. A modified Hitachi H800 TEM was interfaced to a 200 kV ion implanter and a 2 x 1.7 MV tandem accelerator. Effective steps were taken to isolate the TEM from mechanical vibration from the ion beam line, and no obvious wobbling of the TEM image was observed during the ion implantation. The amorphization process of Si crystal irradiated by 115 keV N + ion beam was observed in the primary experiments, demonstrating that this interface facility is capable of in situ study of radiation effects. An online low energy gaseous ion source which may provide 1-20 keV H + and He + is under construction. (authors)

  19. Correlating TEM images of damage in irradiated materials to molecular dynamics simulations

    International Nuclear Information System (INIS)

    Schaeublin, R.; Caturla, M.-J.; Wall, M.; Felter, T.; Fluss, M.; Wirth, B.D.; Diaz de la Rubia, T.; Victoria, M.

    2002-01-01

    TEM image simulations are used to couple the results from molecular dynamics (MD) simulations to experimental TEM images. In particular we apply this methodology to the study of defects produced during irradiation. MD simulations have shown that irradiation of FCC metals results in a population of vacancies and interstitials forming clusters. The limitation of these simulations is the short time scales available, on the order of 100 s of picoseconds. Extrapolation of the results from these short times to the time scales of the laboratory has been difficult. We address this problem by two methods: we perform TEM image simulations of MD simulations of cascades with an improved technique, to relate defects produced at short time scales with those observed experimentally at much longer time scales. On the other hand we perform in situ TEM experiments of Au irradiated at liquid-nitrogen temperatures, and study the evolution of the produced damage as the temperature is increased to room temperature. We find that some of the defects observed in the MD simulations at short time scales using the TEM image simulation technique have features that resemble those observed in laboratory TEM images of irradiated samples. In situ TEM shows that stacking fault tetrahedra are present at the lowest temperatures and are stable during annealing up to room temperature, while other defect clusters migrate one dimensionally above -100 deg. C. Results are presented here

  20. Data from the Mars Science Laboratory CheMin XRD/XRF Instrument

    Science.gov (United States)

    Vaniman, David; Blake, David; Bristow, Tom; DesMarais, David; Achilles, Cherie; Anderson, Robert; Crips, Joy; Morookian, John Michael; Spanovich, Nicole; Vasavada, Ashwin; hide

    2013-01-01

    The CheMin instrument on the Mars Science Laboratory (MSL) rover Curiosity uses a Co tube source and a CCD detector to acquire mineralogy from diffracted primary X-rays and chemical information from fluoresced X-rays. CheMin has been operating at the MSL Gale Crater field site since August 5, 2012 and has provided the first X-ray diffraction (XRD) analyses in situ on a body beyond Earth. Data from the first sample collected, the Rocknest eolian soil, identify a basaltic mineral suite, predominantly plagioclase (approx.An50), forsteritic olivine (approx.Fo58), augite and pigeonite, consistent with expectation that detrital grains on Mars would reflect widespread basaltic sources. Minor phases (each XRD. This amorphous component is attested to by a broad rise in background centered at approx.27deg 2(theta) (Co K(alpha)) and may include volcanic glass, impact glass, and poorly crystalline phases including iron oxyhydroxides; a rise at lower 2(theta) may indicate allophane or hisingerite. Constraints from phase chemistry of the crystalline components, compared with a Rocknest bulk composition from the APXS instrument on Curiosity, indicate that in sum the amorphous or poorly crystalline components are relatively Si, Al, Mg-poor and enriched in Ti, Cr, Fe, K, P, S, and Cl. All of the identified crystalline phases are volatile-free; H2O, SO2 and CO2 volatile releases from a split of this sample analyzed by the SAM instrument on Curiosity are associated with the amorphous or poorly ordered materials. The Rocknest eolian soil may be a mixture of local detritus, mostly crystalline, with a regional or global set of dominantly amorphous or poorly ordered components. The Rocknest sample was targeted by MSL for "first time analysis" to demonstrate that a loose deposit could be scooped, sieved to <150 microns, and delivered to instruments in the body of the rover. A drilled sample of sediment in outcrop is anticipated. At the time of writing this abstract, promising outcrops are

  1. XRD monitoring of α self-irradiation in uranium-americium mixed oxides.

    Science.gov (United States)

    Horlait, Denis; Lebreton, Florent; Roussel, Pascal; Delahaye, Thibaud

    2013-12-16

    The structural evolution under (241)Am self-irradiation of U(1-x)Am(x)O(2±δ) transmutation fuels (with x ≤ 0.5) was studied by X-ray diffraction (XRD). Samples first underwent a preliminary heat treatment performed under a reducing atmosphere (Ar/H2(4%)) aiming to recover the previously accumulated structural defects. Over all measurements (carried out over up to a full year and for integrated doses up to 1.5 × 10(18) α-decay events·g(-1)), only fluorite U(1-x)Am(x)O(2±δ) solid solutions were observed. Within a few days after the end of the heat treatment, each of the five studied samples was slowly oxidized as a consequence of their move to air atmosphere, which is evidenced by XRD by an initial sharp decrease of the unit cell parameter. For the compounds with x ≤ 0.15, this oxidation occurred without any phase transitions, but for U0.6Am0.4O(2±δ) and U0.5Am0.5O(2±δ), this process is accompanied by a transition from a first fluorite solid solution to a second oxidized one, as the latter is thermodynamically stable in ambient conditions. In the meantime and after the oxidation process, (241)Am α self-irradiation caused a structural swelling up to ∼0.8 vol %, independently of the sample composition. The kinetic constants of swelling were also determined by regression of experimental data and are, as expected, dependent on x and thus on the dose rate. The normalization of these kinetic constants by sample α-activity, however, leads to very close swelling rates among the samples. Finally, evolutions of microstrain and crystallite size were also monitored, but for the considered dose rates and cumulated doses, α self-irradiation was found, within the limits of the diffractometer used, to have almost no impact on these characteristics. Microstrain was found to be influenced instead by the americium content in the materials (i.e., by the impurities associated with americium starting material and the increase of cationic charge heterogeneity with

  2. Evaluation of Rock Powdering Methods to Obtain Fine-grained Samples for CHEMIN, a Combined XRD/XRF Instrument

    Science.gov (United States)

    Chipera, S. J.; Vaniman, D. T.; Bish, D. L.; Sarrazin, P.; Feldman, S.; Blake, D. F.; Bearman, G.; Bar-Cohen, Y.

    2004-01-01

    A miniature XRD/XRF (X-ray diffraction / X-ray fluorescence) instrument, CHEMIN, is currently being developed for definitive mineralogic analysis of soils and rocks on Mars. One of the technical issues that must be addressed to enable remote XRD analysis is how best to obtain a representative sample powder for analysis. For powder XRD analyses, it is beneficial to have a fine-grained sample to reduce preferred orientation effects and to provide a statistically significant number of crystallites to the X-ray beam. Although a two-dimensional detector as used in the CHEMIN instrument will produce good results even with poorly prepared powder, the quality of the data will improve and the time required for data collection will be reduced if the sample is fine-grained and randomly oriented. A variety of methods have been proposed for XRD sample preparation. Chipera et al. presented grain size distributions and XRD results from powders generated with an Ultrasonic/Sonic Driller/Corer (USDC) currently being developed at JPL. The USDC was shown to be an effective instrument for sampling rock to produce powder suitable for XRD. In this paper, we compare powder prepared using the USDC with powder obtained with a miniaturized rock crusher developed at JPL and with powder obtained with a rotary tungsten carbide bit to powders obtained from a laboratory bench-scale Retsch mill (provides benchmark mineralogical data). These comparisons will allow assessment of the suitability of these methods for analysis by an XRD/XRF instrument such as CHEMIN.

  3. Influence of gamma irradiation on the surface morphology, XRD and thermophysical properties of silicide hexoboride

    Science.gov (United States)

    Mirzayev, Matlab N.; Mehdiyeva, Ravan N.; Garibov, Ramin G.; Ismayilova, Narmin A.; Jabarov, Sakin H.

    2018-05-01

    In this study, compounds of B6Si were irradiated using a 60Co gamma source that have an energy line of 1.25 MeV at the absorbed dose rates from 14.6 kGy to 194.4 kGy. Surface morphology images of the sample obtained by Scanning Electron Microscope (SEM) show that the crystal structure at a high absorbed doses (D ≥ 145.8kGy) starts to be destroyed. X-ray diffraction studies revealed that with increasing radiation absorption dose, the spectrum intensity of the sample was decreased 1.96 times compared with the initial value. Thermal properties were studied by Differential scanning calorimetry (DSC) method in the temperature range of 30-1000∘C.

  4. In situ TEM observations of unusual nanocrystallization in a Ti-based bulk metallic glass

    International Nuclear Information System (INIS)

    Yan, M.; Wang, D.J.; Shen, J.; Qian, M.

    2011-01-01

    In situ transmission electron microscopy (TEM) has been used to witness the nanocrystallization of amorphous Ti 42.5 Cu 40 Zr 10 Ni 5 Sn 2.5 . A crystallization front exists to separate the TEM sample into two parts with different thermal stabilities. The number density of the crystallization products varies significantly, with the precipitate sizes ranging from a few nanometres to ∼100 nm. Detailed TEM analysis suggests that oxygen is the most likely reason for realizing the unusual nanocrystallization. External thermal analysis also indicates that oxygen affects the crystallization.

  5. Development of a versatile TEM specimen holder for the characterization of photocatalytic materials

    DEFF Research Database (Denmark)

    Cavalca, Filippo; Langhammer, C.; Hansen, Thomas Willum

    2011-01-01

    conventional TEM analysis on photocatalysts with several in situ TEM techniques including environmental TEM (ETEM), in situ photo activation and localized surface plasmon resonance (LSPR) spectroscopy [3-4]. These experiments are facilitated by the construction of a specimen holder capable of illuminating....../on nanomaterials and thin films. We present results from combined ETEM-LSPR studies of thermally-induced catalytic phenomena and on metal nanoparticle sintering, an important process in catalysis, which we study in situ in both real and model systems by means of indirect nanoplasmonic sensing and ETEM....

  6. TEM investigation of the microstructural evolution in nickel during MeV helium implantation

    International Nuclear Information System (INIS)

    Gadalla, A.A.; Jaeger, W.; Ehrhart, P.

    1986-01-01

    In a recent TEM investigation of high energy He-implanted copper the low average helium density could be understood by the observation of the coexistence of two types of vacancy agglomerates i.e. relaxed vacancy agglomerates in the form of stacking fault tetrahedra (SFT) and small bubbles. In order to arrive at a more systematic understanding of the evolution of the microstructure during high energy helium implantation we extended these TEM investigations to nickel. Of particular interest was also the minimum implantation dose necessary to precipitate bubbles that are large enough to be visible in the TEM. (orig./RK)

  7. Tie2-expressing monocytes (TEMs): novel targets and vehicles of anticancer therapy?

    Science.gov (United States)

    De Palma, Michele; Naldini, Luigi

    2009-08-01

    There is a growing interest in understanding the complex interactions between bone marrow-derived myeloid-lineage cells and angiogenesis in tumors. Such interest has been revived recently by the observation that tumor-infiltrating myeloid cells convey proangiogenic programs that can counteract the activity of antiangiogenic drugs in mouse tumor models. Among myeloid cells, Tie2-expressing monocytes (TEMs) appear to have nonredundant function in promoting tumor angiogenesis and growth in mouse models. The identification and functional characterization of TEMs in mice and humans may provide novel molecular targets for anticancer therapy. Moreover, TEMs may be exploited to deliver antitumor drugs specifically to the tumor microenvironment.

  8. A accountability nas organizações sem fins lucrativos: o caso particular de algumas fundações em Portugal

    OpenAIRE

    Costa, Ana Lúcia de Jesus

    2011-01-01

    Mestrado em Contabilidade A crescente importância das Organizações Sem Fins Lucrativos (OSFL) na actividade económica das sociedades modernas tem levado a um aumento da procura de informação financeira e não financeira sobre estas entidades. Cada vez mais as OSFL devem dar ênfase à accountability, atendendo às especificidades da sua actividade, de modo a que os seus documentos de prestação de contas garantam uma imagem fidedigna e apropriada do seu desempenho, devendo, portanto, afastar...

  9. Classification and printability of EUV mask defects from SEM images

    Science.gov (United States)

    Cho, Wonil; Price, Daniel; Morgan, Paul A.; Rost, Daniel; Satake, Masaki; Tolani, Vikram L.

    2017-10-01

    Classification and Printability of EUV Mask Defects from SEM images EUV lithography is starting to show more promise for patterning some critical layers at 5nm technology node and beyond. However, there still are many key technical obstacles to overcome before bringing EUV Lithography into high volume manufacturing (HVM). One of the greatest obstacles is manufacturing defect-free masks. For pattern defect inspections in the mask-shop, cutting-edge 193nm optical inspection tools have been used so far due to lacking any e-beam mask inspection (EBMI) or EUV actinic pattern inspection (API) tools. The main issue with current 193nm inspection tools is the limited resolution for mask dimensions targeted for EUV patterning. The theoretical resolution limit for 193nm mask inspection tools is about 60nm HP on masks, which means that main feature sizes on EUV masks will be well beyond the practical resolution of 193nm inspection tools. Nevertheless, 193nm inspection tools with various illumination conditions that maximize defect sensitivity and/or main-pattern modulation are being explored for initial EUV defect detection. Due to the generally low signal-to-noise in the 193nm inspection imaging at EUV patterning dimensions, these inspections often result in hundreds and thousands of defects which then need to be accurately reviewed and dispositioned. Manually reviewing each defect is difficult due to poor resolution. In addition, the lack of a reliable aerial dispositioning system makes it very challenging to disposition for printability. In this paper, we present the use of SEM images of EUV masks for higher resolution review and disposition of defects. In this approach, most of the defects detected by the 193nm inspection tools are first imaged on a mask SEM tool. These images together with the corresponding post-OPC design clips are provided to KLA-Tencor's Reticle Decision Center (RDC) platform which provides ADC (Automated Defect Classification) and S2A (SEM

  10. {mu}-XRF/{mu}-RS vs. SR {mu}-XRD for pigment identification in illuminated manuscripts

    Energy Technology Data Exchange (ETDEWEB)

    Snickt, G. van der; Nolf, W. de; Vekemans, B.; Janssens, K. [University of Antwerp, Department of Chemistry, Antwerp (Belgium)

    2008-07-15

    For the non-destructive identification of pigments and colorants in works of art, in archaeological and in forensic materials, a wide range of analytical techniques can be used. Bearing in mind that every method holds particular limitations, two complementary spectroscopic techniques, namely confocal {mu}-Raman spectroscopy ({mu}-RS) and {mu}-X-ray fluorescence spectroscopy ({mu}-XRF), were joined in one instrument. The combined {mu}-XRF and {mu}-RS device, called PRAXIS unites both complementary techniques in one mobile setup, which allows {mu}- and in situ analysis. {mu}-XRF allows one to collect elemental and spatially-resolved information in a non-destructive way on major and minor constituents of a variety of materials. However, the main disadvantages of {mu}-XRF are the penetration depth of the X-rays and the fact that only elements and not specific molecular combinations of elements can be detected. As a result {mu}-XRF is often not specific enough to identify the pigments within complex mixtures. Confocal Raman microscopy ({mu}-RS) can offer a surplus as molecular information can be obtained from single pigment grains. However, in some cases the presence of a strong fluorescence background limits the applicability. In this paper, the concrete analytical possibilities of the combined PRAXIS device are evaluated by comparing the results on an illuminated sheet of parchment with the analytical information supplied by synchrotron radiation {mu}-X-ray diffraction (SR {mu}-XRD), a highly specific technique. (orig.)

  11. Mössbauer, XRD, and Complex Thermal Analysis of the Hydration of Cement with Fly Ash

    Directory of Open Access Journals (Sweden)

    Vili Lilkov

    2013-01-01

    Full Text Available Hydration of cement with and without fly ash is studied with Mössbauer spectroscopy, XRD, and thermal analysis. Iron in cement is present as Fe3+-ions and occupies two octahedral positions, with close isomer shifts and quadrupole splittings. Iron in fly ash is present as Fe2+ and Fe3+, and the Mössbauer spectra display three doublets—two for Fe3+ in octahedral coordination and one for Fe2+. A third doublet was registered in the hydrating plain cement pastes after the 5th day, due to Fe3+ in tetrahedral coordination in the structure of the newly formed monosulphate aluminate. In cement pastes with fly ash, the doublet of tetrahedral iron is formed earlier because the quantity of ettringite and portlandite is low and more monosulphate crystallizes. No Fe(OH3 phase forms during hydration of C4AF. The fly ash displays pozzolanic properties, which lead to lowering of the portlandite quantity in the cement mixtures and increasing of the high temperature products.

  12. Size distribution of magnetic iron oxide nanoparticles using Warren-Averbach XRD analysis

    Science.gov (United States)

    Mahadevan, S.; Behera, S. P.; Gnanaprakash, G.; Jayakumar, T.; Philip, J.; Rao, B. P. C.

    2012-07-01

    We use the Fourier transform based Warren-Averbach (WA) analysis to separate the contributions of X-ray diffraction (XRD) profile broadening due to crystallite size and microstrain for magnetic iron oxide nanoparticles. The profile shape of the column length distribution, obtained from WA analysis, is used to analyze the shape of the magnetic iron oxide nanoparticles. From the column length distribution, the crystallite size and its distribution are estimated for these nanoparticles which are compared with size distribution obtained from dynamic light scattering measurements. The crystallite size and size distribution of crystallites obtained from WA analysis are explained based on the experimental parameters employed in preparation of these magnetic iron oxide nanoparticles. The variation of volume weighted diameter (Dv, from WA analysis) with saturation magnetization (Ms) fits well to a core shell model wherein it is known that Ms=Mbulk(1-6g/Dv) with Mbulk as bulk magnetization of iron oxide and g as magnetic shell disorder thickness.

  13. Different β-alanine dimeric forms in trifluoromethanesulfonic acid salts. XRD and vibrational studies.

    Science.gov (United States)

    Wołoszyn, Łukasz; Ilczyszyn, Maria M

    2018-03-15

    Two new crystalline salts: β-alaninium trifluoromethanesulfonate (β-AlaOTf) and bis(β-alanine) trifluoromethanesulfonate (β-2AlaOTf) were obtained. The former one contains diprotonated β-alanine dimer, the latter one monoprotonated β-alanine dimer. Both compounds were studied by single crystal XRD, vibrational (IR and Raman) spectroscopy and calorimetric method. The quantum-mechanical calculations (DFT/B3LYP/6-311++G(2d,2p)) for the diprotonated dimer were carried out. The β-AlaOTf salt crystallizes in the P1¯ space group of triclinic system (Z=2), the β-2AlaOTf in the P2 1 /m space group of monoclinic system (Z=2). The vibrational data for the studied compounds are discussed in relation to their crystal structure, and provide insight into the character of hydrogen bonds and β-alanine protonation. The studied crystals do not exhibit phase transitions in the solid state. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. Synchrotron Radiation XRD Analysis of Indialite in Y-82094 Ungrouped Carbonaceous Chondrite

    Science.gov (United States)

    Mikouchi, T.; Hagiya, K.; Sawa, N.; Kimura, M.; Ohsumi, K.; Komatsu, M.; Zolensky, M.

    2016-01-01

    Y-82094 is an ungrouped type 3.2 carbonaceous chondrite, with abundant chondrules making 78 vol.% of the rock. Among these chondrules, an unusual porphyritic Al-rich magnesian chondrule is reported that consists of a cordierite-like phase, Al-rich orthopyroxene, cristobalite, and spinel surrounded by an anorthitic mesostasis. The reported chemical formula of the cordierite-like phase is Na(0.19)Mg(1.95)Fe(0.02)Al(3.66)Si(5.19)O18, which is close to stoichiometric cordierite (Mg2Al3[AlSi5O18]). Although cordierite can be present in Al-rich chondrules, it has a high temperature polymorph (indialite) and it is therefore necessary to determine whether it is cordierite or indialite in order to better constrain its formation conditions. In this abstract we report on our synchrotron radiation X-ray diffraction (SR-XRD) study of the cordierite-like phase in Y-82094.

  15. In situ synchrotron XRD analysis of the kinetics of spodumene phase transitions.

    Science.gov (United States)

    L Moore, Radhika; Mann, Jason P; Montoya, Alejandro; Haynes, Brian S

    2018-04-25

    The phase transition by thermal activation of natural α-spodumene was followed by in situ synchrotron XRD in the temperature range 896 to 940 °C. We observed both β- and γ-spodumene as primary products in approximately equal proportions. The rate of the α-spodumene inversion is first order and highly sensitive to temperature (apparent activation energy ∼800 kJ mol-1). The γ-spodumene product is itself metastable, forming β-spodumene, with the total product mass fraction ratio fγ/fβ decreasing as the conversion of α-spodumene continues. We found the relationship between the product yields and the degree of conversion of α-spodumene to be the same at all temperatures in the range studied. A model incorporating first order kinetics of the α- and γ-phase inversions with invariant rate constant ratio describes the results accurately. Theoretical phonon analysis of the three phases indicates that the γ phase contains crystallographic instabilities, whilst the α and β phases do not.

  16. A 4-(o-chlorophenyl)-2-aminothiazole: Microwave assisted synthesis, spectral, thermal, XRD and biological studies

    Science.gov (United States)

    Rajmane, S. V.; Ubale, V. P.; Lawand, A. S.; Nalawade, A. M.; Karale, N. N.; More, P. G.

    2013-11-01

    A 4-(o-chlorophenyl)-2-aminothiazole (CPAT) has been synthesized by reacting o-chloroacetophenone, iodine and thiourea under microwave irradiation as a green chemistry approach. The reactions proceed selectively and within a couple of minutes giving high yields of the products. The compound was characterized by elemental, spectral (UV-visible, IR, NMR and GC-MS), XRD and thermal analyses. The TG curve of the compound was analyzed to calculate various kinetic parameters (n, E, Z, ΔS and ΔG) by using Coats-Redfern (C.R.), MacCallum-Tanner (M.T.) and Horowitz-Metzger (H.M.) method. The compound was tested for the evaluation of antibacterial activity against B. subtilis and E. coli and antifungal activity against A. niger and C. albicans. The compound was evaluated for their in vitro nematicidal activity on plant parasitic nematode Meloidogyne javanica and molluscicidal activity on fresh water helminthiasis vector snail Lymnea auricularia. The compound is biologically active in very low concentration. X-ray diffraction study suggests a triclinic crystal system for the compound.

  17. Application of XRF and XRD in the study of ceramics and pottery

    International Nuclear Information System (INIS)

    Meor Yusoff Meor Sulaiman

    2004-01-01

    Ceramic artefacts are made from clay-based mineral and their elemental and mineral compositions tend to vary from one locality to another. The elemental and mineral composition data's besides able to verify the originality of the artifact also helps in regard to provenance, fabrication technology and also manufacturing technique. X-ray fluorescence XRF is a non-destructive technique to identify and quantify elements ranging from sodium (atomic number = 11 to uranium atomic number = 92). The paper also looks into recent advances of this technique in the study of ceramics and pottery. Microfocus XRF, besides able to do qualitative and quantitative elemental analysis, it also can perform accurate elemental mapping. Another aspect there is important in this study is the capability to do in-situ analysis. With the recent introduction of the peltiered-cooled silicon detector, in-situ analysis had become more easily available. X-ray diffraction (XRD) analysis on the other hand, helps to identify correctly the different mineral composition present in the ceramic artifact. This could also help in identifying the type of clay that is used in the manufacturing of these ceramic artifacts as well as its origin. Both x-ray techniques complement each other and are very important tool in the archaeological study of ceramic and pottery samples. (Author)

  18. EXAFS and XRD studies of nanocrystalline cerium oxide: the effect of preparation method on the microstructure

    International Nuclear Information System (INIS)

    Savin, S.L.P.; Chadwick, A.V.; Smith, M.E.; O'Dell, L.A.

    2007-01-01

    There is considerable interest in nanocrystalline materials due to their unusual properties, such as enhanced ionic conductivity in the case of nanocrystalline ionic solids. This has potential commercial applications, particularly for oxide ion conductors. However, a detailed knowledge of the microstructure is important in fully understanding the novel properties exhibited by nanocrystalline materials. The final microstructure of a material is dependent on the preparation method used, for example, sol-gel and ball-milling methods are commonly used in the preparation of nanocrystalline oxides. Additionally, there is a problem in maintaining the materials in nanocrystalline form when they are subjected to elevated temperatures. We have been exploring strategies to restrict the growth of nanocrystalline oxides and have found that adding a small amount of an inert material, e.g. SiO 2 or Al 2 O 3 , is particularly effective. We will report XRD and EXAFS studies of nanocrystalline ceria prepared by sol-gel, sol-gel pinned and ball-milling methods and the effect of preparation method on the final microstructure. (copyright 2007 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  19. Multielemental analyses of isomorphous Indian garnet gemstones by XRD and external pixe techniques.

    Science.gov (United States)

    Venkateswarulu, P; Srinivasa Rao, K; Kasipathi, C; Ramakrishna, Y

    2012-12-01

    Garnet gemstones were collected from parts of Eastern Ghats geological formations of Andhra Pradesh, India and their gemological studies were carried out. Their study of chemistry is not possible as they represent mixtures of isomorphism nature, and none of the individual specimens indicate independent chemistry. Hence, non-destructive instrumental methodology of external PIXE technique was employed to understand their chemistry and identity. A 3 MeV proton beam was employed to excite the samples. In the present study geochemical characteristics of garnet gemstones were studied by proton induced X-ray emission. Almandine variety of garnet is found to be abundant in the present study by means of their chemical contents. The crystal structure and the lattice parameters were estimated using X-Ray Diffraction studies. The trace and minor elements are estimated using PIXE technique and major compositional elements are confirmed by XRD studies. The technique is found very useful in characterizing the garnet gemstones. The present work, thus establishes usefulness and versatility of the PIXE technique with external beam for research in Geo-scientific methodology. Copyright © 2012 Elsevier Ltd. All rights reserved.

  20. A simplified method for scanning electron microscopy (SEM) autoradiography

    International Nuclear Information System (INIS)

    Shahar, A.; Lasher, R.

    1980-01-01

    The combination of autoradiography with SEM provides a valuable tool for the study of labeled biological materials, but the previously described methods are complicated because they call first for the removal of gelatin from the film emulsion and this is then followed by deposition of gold vapor on the specimen. The authors describe a much simpler method which can easily be adapted to routine examination of cell cultures. In this method, gelatin is not removed; the film is coated with vaporized carbon only. This procedure permits visualization of both cellular image and distribution of silver grains. (Auth.)

  1. La semántica en la Web

    OpenAIRE

    Roger, Sandra

    2004-01-01

    El propósito de este trabajo es presentar la motivación de nuestra línea de investigación, metas y desarrollos futuros. Fundamentalmente, nuestro interés se centrará en poder capturar el potencial de las técnicas y paradigmas basadas en conocimiento semántico para la representación de conocimiento, la localización, compartición e integración de recursos a mediante la WWW.

  2. [Study of the phase transformation of TiO2 with in-situ XRD in different gas].

    Science.gov (United States)

    Ma, Li-Jing; Guo, Lie-Jin

    2011-04-01

    TiO2 sample was prepared by sol-gel method from chloride titanium. The phase transformation of the prepared TiO2 sample was studied by in-situ XRD and normal XRD in different gas. The experimental results showed that the phase transformation temperatures of TiO2 were different under in-situ or normal XRD in different kinds of gas. The transformation of amorphous TiO2 to anatase was controlled by kinetics before 500 degrees C. In-situ XRD showed that the growth of anatase was inhibited, but the transformation of anatase to rutile was accelerated under inactive nitrogen in contrast to air. Also better crystal was obtained under hydrogen than in argon. These all showed that external oxygen might accelerate the growth of TiO2, but reduced gas might partly counteract the negative influence of lack of external oxygen. The mechanism of phase transformation of TiO2 was studied by in-situ XRD in order to control the structure in situ.

  3. Transmission X-ray Diffraction (XRD) Patterns Relevant to the MSL Chemin Amorphous Component: Sulfates And Silicates

    Science.gov (United States)

    Morris, R. V.; Rampe, E. B.; Graff, T. G.; Archer, P. D., Jr.; Le, L.; Ming, D. W.; Sutter, B.

    2015-01-01

    The Mars Science Laboratory (MSL) CheMin instrument on the Curiosity rover is a transmission X-ray diffractometer (Co-Kalpha radiation source and a approx.5deg to approx.52deg 2theta range) where the analyzed powder samples are constrained to have discrete particle diameters XRD amorphous component. Estimates of amorphous component abundance, based on the XRD data itself and on mass-balance calculations using APXS data crystalline component chemistry derived from XRD data, martian meteorites, and/or stoichiometry [e.g., 6-9], range from approx.20 wt.% to approx.50 wt.% of bulk sample. The APXSbased calculations show that the amorphous component is rich in volatile elements (esp. SO3) and is not simply primary basaltic glass, which was used as a surrogate to model the broad band in the RN CheMin pattern. For RN, the entire volatile inventory (except minor anhydrite) is assigned to the amorphous component because no volatile-bearing crystalline phases were reported within detection limits [2]. For JK and CB, Fesaponite, basanite, and akaganeite are volatile-bearing crystalline components. Here we report transmission XRD patterns for sulfate and silicate phases relevant to interpretation of MSL-CheMin XRD amorphous components.

  4. S tudies on the phase transitions and properties of tungsten (VI oxide nanoparticles by X - Ray diffraction (XRD and thermal analysis

    Directory of Open Access Journals (Sweden)

    S.F. Abdullah

    2017-11-01

    Full Text Available Tungsten (VI oxide, WO3nanoparticles were synthesized by colloidal gas aphrons(CGAs technique.The resultant WO3nanoparticleswere characterized by thermogravimetric-differential thermal analysis (TG-DTA and X-Ray diffraction (XRD measurements in order to determine the phase transitions, the crystallinity and the size of theWO3nanoparticles. As a comparison, transmission electron microscope (TEM was used to investigate the size of the WO3nanoparticles. The result from XRD and DTA show that the formation of polymorphsWO3nanoparticles have the following sequence: orthorhombic (b-WO3®monoclinic (g-WO3 ®triclinic (d-WO3 ®monoclinic (e-WO3 with respect to the calcination temperature of 400, 500, 600 and 700°C. No diffraction peaks were found in the X-Ray diffraction measurements for the sample heat treated at 300°C (as-prepared, suggesting that an amorphous structure was obtained at this temperature whereas the crystallinity had been obtained by the other samples of theWO3nanoparticles at the calcination temperatures of 400, 500, 600 and 700°C. It is also found that the X-Ray diffraction measurements produced an average diameter of (30 ±5, (50 ±5, (150 ±10 and (200 ±10 nm at calcination temperatures of 400, 500, 600 and 700°C respectively by using Debye-Scherrer formula. The TG curve revealed that the WO3nanoparticles is purely anhydrous since the weight loss is insignificant (0.3 –1.4 % from 30 until 600°C for the WO3nanoparticles calcined at 400°C. Finally, the composition and the purity of the WO3nanoparticleshave been examined by X-Ray photoelectron spectroscopy (XPS. Theresults indicate no significant changes to the composition and the purity of the WO3nanoparticle produced due to the temperature variations

  5. Sexual Arousal and Sexually Explicit Media (SEM): Comparing Patterns of Sexual Arousal to SEM and Sexual Self-Evaluations and Satisfaction Across Gender and Sexual Orientation.

    Science.gov (United States)

    Hald, Gert Martin; Stulhofer, Aleksandar; Lange, Theis

    2018-03-01

    Investigations of patterns of sexual arousal to certain groups of sexually explicit media (SEM) in the general population in non-laboratory settings are rare. Such knowledge could be important to understand more about the relative specificity of sexual arousal in different SEM users. (i) To investigate whether sexual arousal to non-mainstream vs mainstream SEM contents could be categorized across gender and sexual orientation, (ii) to compare levels of SEM-induced sexual arousal, sexual satisfaction, and self-evaluated sexual interests and fantasies between non-mainstream and mainstream SEM groups, and (iii) to explore the validity and predictive accuracy of the Non-Mainstream Pornography Arousal Scale (NPAS). Online cross-sectional survey of 2,035 regular SEM users in Croatia. Patterns of sexual arousal to 27 different SEM themes, sexual satisfaction, and self-evaluations of sexual interests and sexual fantasies. Groups characterized by sexual arousal to non-mainstream SEM could be identified across gender and sexual orientation. These non-mainstream SEM groups reported more SEM use and higher average levels of sexual arousal across the 27 SEM themes assessed compared with mainstream SEM groups. Only few differences were found between non-mainstream and mainstream SEM groups in self-evaluative judgements of sexual interests, sexual fantasies, and sexual satisfaction. The internal validity and predictive accuracy of the NPAS was good across most user groups investigated. The findings suggest that in classified non-mainstream SEM groups, patterns of sexual arousal might be less fixated and category specific than previously assumed. Further, these groups are not more judgmental of their SEM-related sexual arousal patterns than groups characterized by patterns of sexual arousal to more mainstream SEM content. Moreover, accurate identification of non-mainstream SEM group membership is generally possible across gender and sexual orientation using the NPAS. Hald GM

  6. Size Determination of Au Aerosol Nanoparticles by Off-Line TEM/STEM Observations

    Science.gov (United States)

    Karlsson, Lisa S.; Deppert, Knut; Malm, Jan-Olle

    2006-12-01

    Determination of particle size distributions of Au aerosol nanoparticles has been performed by a TEM/STEM investigation. The particles are generated by an evaporation/condensation method and are size-selected by differential mobility analyzers (DMA) based on their electrical mobility. Off-line TEM measurements resulted in equivalent projected area diameters assuming that the particles are spherical in shape. In this paper critical factors such as magnification calibration, sampling, image analysis, beam exposure and, particle shape are treated. The study shows that the measures of central tendency; mean, median and mode, are equal as expected from a narrow size distribution. Moreover, the correlation between TEM/STEM and DMA are good, in practice 1:1. Also, STEM has the advantage over TEM due to enhanced contrast and is proposed as an alternative route for determination of particle size distributions of nanoparticles with lower contrast.

  7. Size Determination of Au Aerosol Nanoparticles by Off-Line TEM/STEM Observations

    International Nuclear Information System (INIS)

    Karlsson, Lisa S.; Deppert, Knut; Malm, Jan-Olle

    2006-01-01

    Determination of particle size distributions of Au aerosol nanoparticles has been performed by a TEM/STEM investigation. The particles are generated by an evaporation/condensation method and are size-selected by differential mobility analyzers (DMA) based on their electrical mobility. Off-line TEM measurements resulted in equivalent projected area diameters assuming that the particles are spherical in shape. In this paper critical factors such as magnification calibration, sampling, image analysis, beam exposure and, particle shape are treated. The study shows that the measures of central tendency; mean, median and mode, are equal as expected from a narrow size distribution. Moreover, the correlation between TEM/STEM and DMA are good, in practice 1:1. Also, STEM has the advantage over TEM due to enhanced contrast and is proposed as an alternative route for determination of particle size distributions of nanoparticles with lower contrast

  8. TEM characterization of UO2-Gd2O3 nuclear fuels synthesized by coprecipitation method

    International Nuclear Information System (INIS)

    Soldati, A.; Gana Watkins, I.; Menghini, J.; Prado, M.

    2013-01-01

    We present a micro and nano structural characterization of 4% weight doped Gd 2 O 3 -UO 2 pellet using Transmission Electron Microscopy (TEM). Agglomerate morphology and crystallite sizes were determined using light/dark field and high resolution (HR-TEM) images. Convergent beam Energy Dispersive Spectroscopy (EDS) and Electron Diffraction (ED) were used to evaluate sample composition and homogeneity, even at the nanometer scale. We obtained an average crystallite size of 90±20 nm. Moreover, from TEM-EDS analyses we determined the presence of Gadolinium in all the analyzed crystallites but with 25% variation among their concentrations. These results show the capability of TEM analysis to characterize a nuclear fuel pellet with burnable poisons nano structure and homogeneity.(author)

  9. ANALISIS JARINGAN UMTS PADA MENARA ROOFTOP DENGAN MENGGUNAKAN SOFTWARE TEMS INVESTIGATION DAN G-NETTRACK PRO

    Directory of Open Access Journals (Sweden)

    Pande Putu Wahyu Pramanda

    2016-03-01

    Full Text Available Berkembangnya dunia teknologi telekomunikasi dan informasi sejalan dengan kebutuhan akan kecepatan dan kestabilan akses internet teknologi UMTS. Metode drive test adalah metode yang biasanya digunakan untuk pengukuran kualitas sebuah site. Pihak provider umumnya menggunakan software TEMS Investigation dalam melakukan drive test. Melakukan drive test dengan TEMS Investigation sangatlah tidak praktis dan memerlukan biaya yang besar. Berkembangnya teknologi smartphone membuat drive test dapat dilakukan dengan menggunakan handphone yaitu dengan G-NetTrack Pro. Namun G-NetTrack Pro tidak memiliki kemampuan yang sama dengan TEMS Investigation. Software G-NetTrack Pro dapat digunakan sebagai bahan pembelajaran yaitu untuk pengenalan drivetest namun belum cocok digunakan secara profesional. G-NetTrack Pro dapat menampilkan data yang dibutuhkan dalam drive test namun tidak sedetail TEMS Investigation, sehingga dalam proses pembelajaran dapat digunakan untuk pengenalan karena efisien dan dapat di install pada handphone mahasiswa namun tidak dapat digunakan melakukan drive test misalnya dalam dunia kerja atau secara professional.

  10. Interpretation of interfacial structures in X-ray multilayers by TEM Fresnel fringe effects

    OpenAIRE

    Nguyen, Tai D.; O'Keefe, Michael A.; Kilaas, Roar; Gronsky, Ronald; Kortright, Jeffrey B.

    1991-01-01

    Assessment of interfacial structures from high-resolution TEM images of cross-sectional specimens is difficult due to Fresnel fringe effects producing different apparent structures in the images. The effects of these fringes have been commonly over-looked in efforts of making quantitative interpretation of interfacial profiles. In this report, we present the observations of the Fresnel fringes in nanometer period Mo/Si, W/C, and WC/C multilayers in through-focus-series TEM images. Calculation...

  11. Maredata: red temática sobre datos de investigación en abierto

    OpenAIRE

    Abadal Falgueras, Ernest; Aleixandre, Rafael; Canals, Agustí; Ferrer, Antonia; Garrigós, Irene; Hernández, Tony; López-Borrull, Alexandre; Mazón, José N.; Melero Melero, Remedios; Méndez Rodríguez, Eva María; Ollé, Eva; Peset Mancebo, María Fernanda

    2017-01-01

    [ES]El objetivo central de la red temática MAREDATA es aglutinar y consolidar la colaboración entre grupos de investigación españoles centrados en el estudio de los datos científicos y también establecer relación con aquellos sectores y disciplinas interesados en esta temática.

  12. Recent advances in cryo-TEM imaging of soft lipid nanoparticles

    DEFF Research Database (Denmark)

    Helvig, Shen Yu; Mat Azmi, Intan Diana Binti; Moghimi, Seyed Moien

    2015-01-01

    Cryo-transmission electron microscopy (Cryo-TEM), and its technological variations thereof, have become a powerful tool for detailed morphological characterization and 3D tomography of soft lipid and polymeric nanoparticles as well as biological materials such as viruses and DNA without chemical...... fixation. Here, we review and discuss recent advances in Cryo-TEM analysis of lipid-based drug nanocarriers with particular emphasis on morphological and internal nanostructure characterization of lyotropic liquid crystalline nanoparticles such as cubosomes and hexosomes....

  13. Sem-edx and ftir studies of chlorinated rubber coating

    International Nuclear Information System (INIS)

    Bano, H.; Khan, M.I.

    2013-01-01

    Summary: Anticorrosive performance of chlorinated rubber coating has been investigated by visual examination, Scanning electron microscopy (SEM)/Energy dispersive X-ray (EDX) analysis and Fourier transform infrared (FTIR) spectroscopy. After surface preparation, commercially available coating system based on chlorinated rubber (primer)/chlorinated rubber (topcoat) formulation was applied on mild steel test panels (10cm x 15cm sizes). Prepared coated panels were exposed at marine, industrial and urban test sites located in Karachi, Pakistan according to ISO 8565 norm. Accelerated testing was performed by using a salt spray chamber (ASTM B117 norm). Accelerated weathering methods are the methods in which the factors responsible for the degradation of coatings are artificially intensified in order to achieve the rapid degradation of coatings. Visual examination of blistering and rusting as well as SEM micrographs indicated a more severe degradation of the coating surface characteristics at natural exposure testing sites (particularly at marine test site) than for accelerated (salt spray) testing. EDX determination of the Oxygen/Carbon (O/C) ratios also indicated increased degradation at natural test sites compared to the accelerated (salt spray) testing. Photooxidation of the binder results in the formation of carbonyl compounds as revealed by FTIR spectroscopy which also indicated dehydrochlorination. (author)

  14. Comparative SEM analysis of nine F22 aligner cleaning strategies.

    Science.gov (United States)

    Lombardo, Luca; Martini, Marco; Cervinara, Francesca; Spedicato, Giorgio Alfredo; Oliverio, Teresa; Siciliani, Giuseppe

    2017-12-01

    The orthodontics industry has paid great attention to the aesthetics of orthodontic appliances, seeking to make them as invisible as possible. There are several advantages to clear aligner systems, including aesthetics, comfort, chairside time reduction, and the fact that they can be removed for meals and oral hygiene procedures. Five patients were each given a series of F22 aligners, each to be worn for 14 days and nights, with the exception of meal and brushing times. Patients were instructed to clean each aligner using a prescribed strategy, and sections of the used aligners were observed under SEM. One grey-scale SEM image was saved per aligner in JPEG format with an 8-bit colour depth, and a total of 45 measurements on the grey scale ("Value" variable) were made. This dataset was analysed statistically via repeated measures ANOVA to determine the effect of each of the nine cleaning strategies in each of the five patients. A statistically significant difference in the efficacy of the cleaning strategies was detected. Specifically, rinsing with water alone was significantly less efficacious, and a combination of cationic detergent solution and ultrasonication was significantly more efficacious than the other methods (p aligners.

  15. O sistema "UFSC sem papel” sob a perspectiva da inovação

    Directory of Open Access Journals (Sweden)

    Naira Silva

    2013-04-01

    Full Text Available DOI: http://dx.doi.org/10.5007/2175-8077.2013v15n35p11   O presente artigo tem como objetivo analisar o sistema de informação “UFSC sem papel” sob a ótica da inovação. Para tanto, fez-se uso da pesquisa descritiva e do estudo de caso, com abordagem qualitativa. Apresenta uma perspectiva de estudo transversal, considerando-se o período compreendido entre outubro de 2011 a novembro de 2011. Trata-se, ainda, de uma pesquisa de campo, bibliográfica. O sujeito da pesquisa, escolhido por tipicidade, foi o superintendente da Superintendência de Governança Eletrônica e Tecnologia da Informação e Comunicação (SeTIC, da Universidade Federal de Santa Catarina. Para a coleta de dados, foi utilizada a entrevista semi-estruturada, a partir de um roteiro, sendo os dados analisados por meio da técnica pattern-matching. O sistema analisado é uma inovação técnica e radical, com efeitos sobre o âmbito administrativo, sendo dividido em módulos para a gestão dos processos administrativos (protocolo, de compras e licitações, de patrimônio e de materiais e almoxarifado. A sua finalidade é modernizar as atividades administrativas, reduzindo o uso de papel e gerando maior rapidez na tramitação dos documentos, mais transparência e maior eficiência na execução dos processos da organização. Em termos de desenvolvimento e aquisição da citada inovação, a UFSC fez opção pela compra de um pacote pronto, mas a implantação foi acompanhada pela equipe da SeTIC. Há certa preocupação com relação à falta de habilidade das pessoas em utilizá-lo. Conclui-se sobre a necessidade de conduzir uma apurada análise do sistema “UFSC sem Papel”, para que tal inovação possa ser bem sucedida.

  16. A New Approach to Studying Biological and Soft Materials Using Focused Ion Beam Scanning Electron Microscopy (FIB SEM)

    International Nuclear Information System (INIS)

    Stokes, D J; Morrissey, F; Lich, B H

    2006-01-01

    Over the last decade techniques such as confocal light microscopy, in combination with fluorescent labelling, have helped biologists and life scientists to study biological architectures at tissue and cell level in great detail. Meanwhile, obtaining information at very small length scales is possible with the combination of sample preparation techniques and transmission electron microscopy (TEM) or scanning transmission electron microscopy (STEM). Scanning electron microscopy (SEM) is well known for the determination of surface characteristics and morphology. However, the desire to understand the three dimensional relationships of meso-scale hierarchies has led to the development of advanced microscopy techniques, to give a further complementary approach. A focused ion beam (FIB) can be used as a nano-scalpel and hence allows us to reveal internal microstructure in a site-specific manner. Whilst FIB instruments have been used to study and verify the three-dimensional architecture of man made materials, SEM and FIB technologies have now been brought together in a single instrument representing a powerful combination for the study of biological specimens and soft materials. We demonstrate the use of FIB SEM to study three-dimensional relationships for a range of length scales and materials, from small-scale cellular structures to the larger scale interactions between biomedical materials and tissues. FIB cutting of heterogeneous mixtures of hard and soft materials, resulting in a uniform cross-section, has proved to be of particular value since classical preparation methods tend to introduce artefacts. Furthermore, by appropriate selection, we can sequentially cross-section to create a series of 'slices' at specific intervals. 3D reconstruction software can then be used to volume-render information from the 2D slices, enabling us to immediately see the spatial relationships between microstructural components

  17. Present status and future prospects of spherical aberration corrected TEM/STEM for study of nanomaterials

    International Nuclear Information System (INIS)

    Tanaka, Nobuo

    2008-01-01

    The present status of Cs-corrected TEM/STEM is described from the viewpoint of the observation of nanomaterials. Characteristic features in TEM and STEM are explained using the experimental data obtained by our group and other research groups. Cs correction up to the 3rd-order aberration of an objective lens has already been established and research interest is focused on correcting the 5th-order spherical aberration and the chromatic aberration in combination with the development of a monochromator below an electron gun for smaller point-to-point resolution in optics. Another fundamental area of interest is the limitation of TEM and STEM resolution from the viewpoint of the scattering of electrons in crystals. The minimum size of the exit-wave function below samples undergoing TEM imaging is determined from the calculation of scattering around related atomic columns in the crystals. STEM does not have this limitation because the resolution is, in principle, determined by the probe size. One of the future prospects of Cs-corrected TEM/STEM is the possibility of extending the space around the sample holder by correcting the chromatic and spherical aberrations. This wider space will contribute to the ease of performing in situ experiments and various combinations of TEM and other analysis methods. High-resolution, in situ dynamic and 3D observations/analysis are the most important keywords in the next decade of high-resolution electron microscopy. (topical review)

  18. TEM in situ cube-corner indentation analysis using ViBe motion detection algorithm

    Science.gov (United States)

    Yano, K. H.; Thomas, S.; Swenson, M. J.; Lu, Y.; Wharry, J. P.

    2018-04-01

    Transmission electron microscopic (TEM) in situ mechanical testing is a promising method for understanding plasticity in shallow ion irradiated layers and other volume-limited materials. One of the simplest TEM in situ experiments is cube-corner indentation of a lamella, but the subsequent analysis and interpretation of the experiment is challenging, especially in engineering materials with complex microstructures. In this work, we: (a) develop MicroViBE, a motion detection and background subtraction-based post-processing approach, and (b) demonstrate the ability of MicroViBe, in combination with post-mortem TEM imaging, to carry out an unbiased qualitative interpretation of TEM indentation videos. We focus this work around a Fe-9%Cr oxide dispersion strengthened (ODS) alloy, irradiated with Fe2+ ions to 3 dpa at 500 °C. MicroViBe identifies changes in Laue contrast that are induced by the indentation; these changes accumulate throughout the mechanical loading to generate a "heatmap" of features in the original TEM video that change the most during the loading. Dislocation loops with b = ½ identified by post-mortem scanning TEM (STEM) imaging correspond to hotspots on the heatmap, whereas positions of dislocation loops with b = do not correspond to hotspots. Further, MicroViBe enables consistent, objective quantitative approximation of the b = ½ dislocation loop number density.

  19. VES/TEM 1D joint inversion by using Controlled Random Search (CRS) algorithm

    Science.gov (United States)

    Bortolozo, Cassiano Antonio; Porsani, Jorge Luís; Santos, Fernando Acácio Monteiro dos; Almeida, Emerson Rodrigo

    2015-01-01

    Electrical (DC) and Transient Electromagnetic (TEM) soundings are used in a great number of environmental, hydrological, and mining exploration studies. Usually, data interpretation is accomplished by individual 1D models resulting often in ambiguous models. This fact can be explained by the way as the two different methodologies sample the medium beneath surface. Vertical Electrical Sounding (VES) is good in marking resistive structures, while Transient Electromagnetic sounding (TEM) is very sensitive to conductive structures. Another difference is VES is better to detect shallow structures, while TEM soundings can reach deeper layers. A Matlab program for 1D joint inversion of VES and TEM soundings was developed aiming at exploring the best of both methods. The program uses CRS - Controlled Random Search - algorithm for both single and 1D joint inversions. Usually inversion programs use Marquadt type algorithms but for electrical and electromagnetic methods, these algorithms may find a local minimum or not converge. Initially, the algorithm was tested with synthetic data, and then it was used to invert experimental data from two places in Paraná sedimentary basin (Bebedouro and Pirassununga cities), both located in São Paulo State, Brazil. Geoelectric model obtained from VES and TEM data 1D joint inversion is similar to the real geological condition, and ambiguities were minimized. Results with synthetic and real data show that 1D VES/TEM joint inversion better recovers simulated models and shows a great potential in geological studies, especially in hydrogeological studies.

  20. Comparison between measured and predicted turbulence frequency spectra in ITG and TEM regimes

    Science.gov (United States)

    Citrin, J.; Arnichand, H.; Bernardo, J.; Bourdelle, C.; Garbet, X.; Jenko, F.; Hacquin, S.; Pueschel, M. J.; Sabot, R.

    2017-06-01

    The observation of distinct peaks in tokamak core reflectometry measurements—named quasi-coherent-modes (QCMs)—are identified as a signature of trapped-electron-mode (TEM) turbulence (Arnichand et al 2016 Plasma Phys. Control. Fusion 58 014037). This phenomenon is investigated with detailed linear and nonlinear gyrokinetic simulations using the Gene code. A Tore-Supra density scan is studied, which traverses through a linear (LOC) to saturated (SOC) ohmic confinement transition. The LOC and SOC phases are both simulated separately. In the LOC phase, where QCMs are observed, TEMs are robustly predicted unstable in linear studies. In the later SOC phase, where QCMs are no longer observed, ion-temperature-gradient (ITG) modes are identified. In nonlinear simulations, in the ITG (SOC) phase, a broadband spectrum is seen. In the TEM (LOC) phase, a clear emergence of a peak at the TEM frequencies is seen. This is due to reduced nonlinear frequency broadening of the underlying linear modes in the TEM regime compared with the ITG regime. A synthetic diagnostic of the nonlinearly simulated frequency spectra reproduces the features observed in the reflectometry measurements. These results support the identification of core QCMs as an experimental marker for TEM turbulence.