Dissolution and precipitation behaviors of silicon-containing ceramic coating on Mg-Zn-Ca alloy in simulated body fluid.

PubMed

Pan, Yaokun; Chen, Chuanzhong; Wang, Diangang; Huang, Danlan

2014-10-01

We prepared Si-containing and Si-free coatings on Mg-1.74Zn-0.55Ca alloy by micro-arc oxidation. The dissolution and precipitation behaviors of Si-containing coating in simulated body fluid (SBF) were discussed. Corrosion products were characterized by scanning electron microscope (SEM), X-ray diffractometer (XRD), fourier transform infrared spectrometer (FT-IR) and X-ray photoelectron spectrometer (XPS). Electrochemical workstation, inductively coupled plasma atomic emission spectrometer (ICP-AES), flame atomic absorption spectrophotometer (AAS) and pH meter were employed to detect variations of electrochemical parameter and ions concentration respectively. Results indicate that the fast formation of calcium phosphates is closely related to the SiOx(n-) groups, which induce the heterogeneous nucleation of amorphous hydroxyapatite (HA) by sorption of calcium and phosphate ions. Copyright © 2014 Elsevier B.V. All rights reserved.

Ab initio simulation of diffractometer instrumental function for high-resolution X-ray diffraction1

PubMed Central

Mikhalychev, Alexander; Benediktovitch, Andrei; Ulyanenkova, Tatjana; Ulyanenkov, Alex

2015-01-01

Modeling of the X-ray diffractometer instrumental function for a given optics configuration is important both for planning experiments and for the analysis of measured data. A fast and universal method for instrumental function simulation, suitable for fully automated computer realization and describing both coplanar and noncoplanar measurement geometries for any combination of X-ray optical elements, is proposed. The method can be identified as semi-analytical backward ray tracing and is based on the calculation of a detected signal as an integral of X-ray intensities for all the rays reaching the detector. The high speed of calculation is provided by the expressions for analytical integration over the spatial coordinates that describe the detection point. Consideration of the three-dimensional propagation of rays without restriction to the diffraction plane provides the applicability of the method for noncoplanar geometry and the accuracy for characterization of the signal from a two-dimensional detector. The correctness of the simulation algorithm is checked in the following two ways: by verifying the consistency of the calculated data with the patterns expected for certain simple limiting cases and by comparing measured reciprocal-space maps with the corresponding maps simulated by the proposed method for the same diffractometer configurations. Both kinds of tests demonstrate the agreement of the simulated instrumental function shape with the measured data. PMID:26089760

Electrochromic TiO2 Thin Film Prepared by Dip-Coating Technique

NASA Astrophysics Data System (ADS)

Suriani, S.; Kamisah, M. M.

2002-12-01

Titanium dioxide (TiO2) thin films were prepared by using sol-gel dip coating technique. The coating solutions were prepared by reacting titanium isopropoxide as precursors and ethanol as solvent. The films were formed on transparent ITO-coated glass by a dip coating technique and final dried at various temperatures up to 600 °C for 30 minutes. The films were characterized with the UV-Vis-NIR Spectrometer, Scanning Electron Microscopy (SEM) and X-ray diffractometer (XRD). XRD results show that the films dried at 600 °C form anatase structure. From the spectroscopic studies, the sample shows electrochromic property.

Crystal and Vibrational Structure of Energetic 3,5-dinitro 1,3,5-oxadiazinane (DOD) by Single Crystal X-ray Diffractometry and Raman Spectroscopy

DTIC Science & Technology

2018-03-19

calculations using a temperature of 298 K. 15. SUBJECT TERMS 3,5-dinitro-1,3,5-oxadiazinane (DOD), X-ray crystallography , Raman, energetic material...X-ray analysis. 2.2 Characterization X-ray Crystallography . DOD crystals were characterized with a SuperNova, Dualflex, EosS2 diffractometer using

Synthesis of K2O/Zeolite catalysts by KOH impregnation for biodiesel production from waste frying oil

NASA Astrophysics Data System (ADS)

Fitriana, N.; Husin, H.; Yanti, D.; Pontas, K.; Alam, P. N.; Ridho, M.; Iskandar

2018-03-01

K2O/Zeolite compounds were successfully synthesized using KOH as starting material and natural zeolite as support. The catalysts were calcined at 500°C for 3 h and then characterized by X-Ray Diffractometer (XRD) and Scanning Electron Microscopy (SEM). The SEM images reveal that the zeolite and K2O/zeolite particles are irregular in shape (100 to 400 nm). The independent variables were impregnated amounts of KOH (15 - 25%), catalyst to oil ratios of 1.0 - 6.0 wt.%, and reaction time of 2 h. The highest biodiesel yield of 95% was produced from the reaction with 2.1 wt.% catalyst of 25% KOH impregnated. The properties of produced biodiesel complied with SNI. The catalytic stability test showed that the 25% KOH impregnated catalyst was stable.

Microstructural, optical and electrical properties of LaFe0.5Cr0.5O3 perovskite nanostructures

NASA Astrophysics Data System (ADS)

Ali, S. Asad; Naseem, Swaleha; Khan, Wasi; Sharma, A.; Naqvi, A. H.

2016-05-01

Perovskite nanocrystalline powder of LaFe0.5Cr0.5O3 was synthesized by sol-gel combustion route and characterized by x-ray diffractometer (XRD), scanning electron microscopy (SEM) equipped with EDS, UV-visible and LCR meter at room temperature Rietveld refinement of the XRD data confirms that the sample is in single phase-rhombohedral structure with space group R-3C. SEM micrograph shows clear nanostructure of the sample and EDS ensures the presence of all elements in good stoichiometric. The optical absorption indicates the maximum absorption at 315 nm and optical band gap of 2.94 eV was estimated using Tauc's relation. Dielectric constant (ɛ') and loss were found to decrease with increase in frequencies. The dielectric behavior was explained on the basis of Maxwell-Wagner's two layer model.

Fabrication and characterization of environmental-friendly Ni1-xRxTiO3 nanopigments with high NIR reflectance

NASA Astrophysics Data System (ADS)

Tong, Yu-Ping; Chen, Zheng; Wang, Hui-Xian; Zhang, Xu-Fang; Ma, Jun-Tao; Chen, Xi

2015-04-01

A series of novel high dispersed environmental-friendly nanopigments based on NiTiO3 doped with rare earth ion such as Y, La, Eu, Sm have been developed. The products were characterized by X-ray diffractometer (XRD), scanning electron microscopy (SEM), commission internationale de l'Eclairage (CIE) 1976 L*α*b* color scales and UV-Vis-near-infrared radiation (NIR) reflectance spectroscopy. The substitution of R3+ for Ni2+ in NiTiO3 can improve the yellowness of pigments, especially for Eu3+ substitution. The sample with the substitution of Eu3+ for Ni2+ processes the highest NIR reflectance and enhances the NIR reflectance to 89.0%. SEM results revealed that the obtained pigments were composed of well-dispersed spherical-like particles with the range of 40-60 nm. EDS results indicated that the distribution of Ni, Ti, R, O element was considerably uniform with no chemical segregation phenomenon.

A Novel X-ray Diffractometer for the Florida Split Coil 25 Tesla Magnet

NASA Astrophysics Data System (ADS)

Wang, Shengyu; Kovalev, Alexey; Suslov, Alexey; Siegrist, Theo

2014-03-01

At National High Magnetic Field Laboratory (NHMFL), we are developing a unique X-ray diffractometer for the 25 Tesla Florida Split Coil Magnet for scattering experiments under extremely high static magnetic fields. The X-ray source is a sealed tube (copper or molybdenum anode), connected to the magnet by an evacuated beam tunnel. The detectors are either an image plate or a silicon drift detector, with the data acquisition system based on LabVIEW. Our preliminary experimental results showed that the performance of the detector electronics and the X-ray generator is reliable in the fringe magnetic fields produced at the highest field of 25 T. Using this diffractometer, we will make measurements on standard samples, such as LaB6, Al2O3 and Si, to calibrate the diffraction system. Magnetic samples, such as single crystal HoMnO3 and stainless steel 301 alloys will be measured subsequently. The addition of X-ray diffraction to the unique split coil magnet will significantly expand the NHMFL experimental capabilities. Therefore, external users will be able to probe spin - lattice interactions at static magnetic fields up to 25T. This project is supported by NSF-DMR Award No.1257649. NHMFL is supported by NSF Cooperative Agreement No. DMR-1157490, the State of Florida, and the U.S. DoE.

Deposition of magnesium nitride thin films on stainless steel-304 substrates by using a plasma focus device

NASA Astrophysics Data System (ADS)

Ramezani, Amir Hoshang; Habibi, Maryam; Ghoranneviss, Mahmood

2014-08-01

In this research, for the first time, we synthesize magnesium nitride thin films on 304-type stainless steel substrates using a Mather-type (2 kJ) plasma focus (PF) device. The films of magnesium nitride are coated with different number of focus shots (like 15, 25 and 35) at a distance of 8 cm from the anode tip and at 0° angular position with respect to the anode axis. For investigation of the structural properties and surface morphology of magnesium nitride films, we utilized the X-ray diffractometer (XRD), atomic force microscopy (AFM) and scanning electron microscopy (SEM) analysis, respectively. Also, the elemental composition is characterized by energy-dispersive X-ray (EDX) analysis. Furthermore, Vicker's microhardness is used to study the mechanical properties of the deposited films. The results show that the degree of crystallinity of deposited thin films (from XRD), the average size of particles and surface roughness (from AFM), crystalline growth of structures (from SEM) and the hardness values of the films depend on the number of focus shots. The EDX analysis demonstrates the existence of the elemental composition of magnesium in the deposited samples.

Morphological and Wear behaviour of new Al-SiCmicro-SiCnano hybrid nanocomposites fabricated through powder metallurgy

NASA Astrophysics Data System (ADS)

Arif, Sajjad; Tanwir Alam, Md; Aziz, Tariq; Ansari, Akhter H.

2018-04-01

In the present work, aluminium matrix composites reinforced with 10 wt% SiC micro particles along with x% SiC nano particles (x = 0, 1, 3, 5 and 7 wt%) were fabricated through powder metallurgy. The fabricated hybrid composites were characterized by x-ray diffractometer (XRD), scanning electron microscope (SEM), energy dispersive spectrum (EDS) and elemental mapping. The relative density, hardness and wear behaviour of all hybrid nanocomposites were studied. The influence of various control factors like SiC reinforcement, sliding distance (300, 600, 900 and 1200 m) and applied load (20, 30 and 40 N) were explored using pin-on-disc wear apparatus. The uniform distribution of micro and nano SiC particles in aluminium matrix is confirmed by elemental maps. The hardness and wear test results showed that properties of the hybrid composite containing 5 wt% nano SiC was better than other hybrid composites. Additionally, the wear loss of all hybrid nanocomposites increases with increasing sliding distance and applied load. The identification of wear phenomenon were studied through the SEM images of worn surface.

Remote analysis of planetary soils: X-ray diffractometer development

NASA Technical Reports Server (NTRS)

Gregory, J. C.

1973-01-01

A system is described suitable for remote low power mineralogical analysis of lunar, planetary, or asteroid soils. It includes an X-ray diffractometer, fluorescence spectrometer, and sample preparation system. A one Curie Fe-55 source provides a monochromatic X-ray beam of 5.9 keV. Seeman-Bohlin or focusing geometry is employed in the camera, allowing peak detection to proceed simultaneously at all angles and obviating the need for moving parts. The detector system is an array of 500-600 proportional counters with a wire-spacing of 1 mm. An electronics unit comprising preamplifier, postamplifier, window discriminators, and storage flipflops requiring only 3.5 milliwatts was designed and tested. Total instrument power is less than 5 watts. Powder diffraction patterns using a flat breadboard multiwire counter were recorded.

HA/Bioglass composite films deposited by pulsed laser with different substrate temperature

NASA Astrophysics Data System (ADS)

Wang, D. G.; Chen, C. Z.; Jin, Q. P.; Li, H. C.; Pan, Y. K.

2014-03-01

In this experiment, the HA/Bioglass composite films on Ti-6Al-4V were deposited by a pulsed laser at Ar atmosphere, and the influence of substrate temperature on the morphology, phase constitutions, bonding configurations and adhesive strength of the films was studied. The obtained films were characterized by an electron probe microanalyzer (EPMA), scanning electron microscope (SEM), X-ray diffractometer (XRD), Fourier transform infrared spectrometer (FTIR), scratch apparatus, and so on. The results show that the amount of the droplets, the crystallinity, and the critical load of the deposited films all increase with the increase of the substrate temperature; however, the substrate temperature has little influence on the functional groups of the films.

Microwave Absorption Properties of La0.8Ca0.2-xAgxMnO3 (x=0.05; x=0.15) Synthesized by Sol-Gel Method

NASA Astrophysics Data System (ADS)

Kurniawan, B.; Laksmi, W.; Sahara, N. A.

2018-04-01

Microwave absorption properties of La0.8Ca0.2-xAgxMnO3 (x= 0.05; 0.15) is reported in this paper. Lanthanum manganite materials was reported as a potential absorber material [1][2][3]. In this paper, the material was synthesized by sol-gel method, calcined at 550°C, and sintered at 900°C. The material was characterized by X-Ray Diffractometer (XRD), and we found that the materials were single phased. Through SEM-EDS characterization it is found that the materials have compositional purity. The resistivity of the materials is obtained by four point probe method, and it is shown that Ag doped decreases the resistivity of the materials. Reflection loss of La0.8Ca0.15Ag0.05MnO3 reaches -4.470 dB and La0.8Ca0.05Ag0.15MnO3 reaches - 7.953 dB.

Effect of oxidizer to fuel molar ratio on particle size and DC conductivity of CeO{sub 2} nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Harish, B. M.; Rajeeva, M. P.; Naveen, C. S.

2016-05-06

Cerium oxide nanoparticles were synthesized by solution combustion method with varying the oxidizer (cerium nitrate hexa hydrate) to fuel (Glycine) molar ratio. The prepared samples were characterized by UV-visible spectrometer, X-ray diffractometer (XRD), Scanning electron microscope (SEM) and Energy dispersive X-Ray analysis (EDAX). XRD pattern reveals the formation of cubic fluorite structure of CeO{sub 2}. It was observed that finest crystallites were found at extreme fuel-deficient condition and it is good enough to produce favorable powder characteristics. The average crystallite size was found to be 14.46 nm to 21.57 nm. The temperature dependent dc conductivity was carried out using Keithleymore » source meter between the temperature range from 300 K to 573 K. From this study it was found that the conductivity increases with increase of temperature due to semiconducting behavior of CeO{sub 2} and it decreases with particle size due to increase in the energy band gap.« less

Synthesis of BiOCl nanosheets with oxygen vacancies for the improved photocatalytic properties

NASA Astrophysics Data System (ADS)

Cai, Yujie; Li, Dongya; Sun, Jingyu; Chen, Mengdie; Li, Yirui; Zou, Zhongwei; Zhang, Hua; Xu, Haiming; Xia, Dongsheng

2018-05-01

The square-sharped BiOCl nanosheets with oxygen vacancies were successfully synthesized via a facile hydrothermal route using xylitol as surfactant. The as-prepared BiOCl samples were characterized by Powder X-ray Diffractometer (XRD), scanning electron microscope (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), UV-Vis diffuse reflectance spectra (DRS), Brunauer-Emmett-Teller (BET), X-ray photoelectron spectroscopy (XPS) and Electron spin resonance (ESR). The as-prepared samples were phase-pure with the width and the thickness were about 50-400 nm and 20-50 nm respectively. Besides, the photodegradation performances showed the BiOCl nanosheets with 0.1 g concentration of xylitol (BOC-1) had the best photocatalytic activity under visible light due to its special polycrystalline structure, grain boundary and an optimum concentration of oxygen vacancies. The h+ and radO2- were the two main active species during the photocatalytic process and the possible photocatalytic mechanism was proposed.

In situ surface/interface x-ray diffractometer for oxide molecular beam epitaxy

NASA Astrophysics Data System (ADS)

Lee, J. H.; Tung, I. C.; Chang, S.-H.; Bhattacharya, A.; Fong, D. D.; Freeland, J. W.; Hong, Hawoong

2016-01-01

In situ studies of oxide molecular beam epitaxy by synchrotron x-ray scattering has been made possible by upgrading an existing UHV/molecular beam epitaxy (MBE) six-circle diffractometer system. For oxide MBE growth, pure ozone delivery to the chamber has been made available, and several new deposition sources have been made available on a new 12 in. CF (ConFlat, a registered trademark of Varian, Inc.) flange. X-ray diffraction has been used as a major probe for film growth and structures for the system. In the original design, electron diffraction was intended for the secondary diagnostics available without the necessity of the x-ray and located at separate positions. Deposition of films was made possible at the two diagnostic positions. And, the aiming of the evaporation sources is fixed to the point between two locations. Ozone can be supplied through two separate nozzles for each location. Also two separate thickness monitors are installed. Additional features of the equipment are also presented together with the data taken during typical oxide film growth to illustrate the depth of information available via in situ x-ray techniques.

In situ surface/interface x-ray diffractometer for oxide molecular beam epitaxy.

PubMed

Lee, J H; Tung, I C; Chang, S-H; Bhattacharya, A; Fong, D D; Freeland, J W; Hong, Hawoong

2016-01-01

In situ studies of oxide molecular beam epitaxy by synchrotron x-ray scattering has been made possible by upgrading an existing UHV/molecular beam epitaxy (MBE) six-circle diffractometer system. For oxide MBE growth, pure ozone delivery to the chamber has been made available, and several new deposition sources have been made available on a new 12 in. CF (ConFlat, a registered trademark of Varian, Inc.) flange. X-ray diffraction has been used as a major probe for film growth and structures for the system. In the original design, electron diffraction was intended for the secondary diagnostics available without the necessity of the x-ray and located at separate positions. Deposition of films was made possible at the two diagnostic positions. And, the aiming of the evaporation sources is fixed to the point between two locations. Ozone can be supplied through two separate nozzles for each location. Also two separate thickness monitors are installed. Additional features of the equipment are also presented together with the data taken during typical oxide film growth to illustrate the depth of information available via in situ x-ray techniques.

Structural and optical properties of Na-doped ZnO films

NASA Astrophysics Data System (ADS)

Akcan, D.; Gungor, A.; Arda, L.

2018-06-01

Zn1-xNaxO (x = 0.0-0.05) solutions have been synthesized by the sol-gel technique using Zinc acetate dihydrate and Sodium acetate which were dissolved into solvent and chelating agent. Na-doped ZnO nanoparticles were obtained from solutions to find phase and crystal structure. Na-doped ZnO films have been deposited onto glass substrate by using sol-gel dip coating system. The effects of dopant concentration on the structure, morphology, and optical properties of Na-doped ZnO thin films deposited on glass substrate are investigated. Characterization of Zn1-xNaxO nanoparticles and thin films are examined using differential thermal analysis (DTA)/thermogravimetric analysis (TGA), Scanning electron microscope (SEM) and X-Ray diffractometer (XRD). Optical properties of Zn1-xNaxO thin films were obtained by using PG Instruments UV-Vis-NIR spectrophotometer in 190-1100 nm range. The structure, morphology, and optical properties of thin films are presented.

Portable X-ray diffractometer equipped with XRF for archaeometry

NASA Astrophysics Data System (ADS)

Uda, M.; Ishizaki, A.; Satoh, R.; Okada, K.; Nakajima, Y.; Yamashita, D.; Ohashi, K.; Sakuraba, Y.; Shimono, A.; Kojima, D.

2005-09-01

A portable X-ray diffractometer equipped with an X-ray fluorescence spectrometer was improved so as to get a diffraction pattern and a fluorescence spectrum simultaneously in air from one and the same small area on a specimen. Here, diffraction experiments were performed in two modes, i.e. an angle rotation mode and an energy dispersive mode. In the latter a diffraction pattern and a fluorescence spectrum were simultaneously recorded in a short time, 100 s or less, on one display. The diffractometer was tested in the field to confirm its performance. Targets chosen for this purpose were a bronze mirror from the Eastern Han Dynasty (25-220), and a stupa and its pedestal which are part of the painted statue of "Tamonten holding a stupa" from the Heian Period (794-1192), enshrined in the Engyouji temple founded in 996. The bronze mirror was identified as a product of the Han Dynasty from its chemical composition and the existence of the δ phase in the Cu-Sn alloy. The stupa and its pedestal were decorated with gold powder and gold leaf, respectively. From the XRF data of the pedestal, the underlying layer of gold leaf seems to have been painted with emerald green.

New software to model energy dispersive X-ray diffraction in polycrystalline materials

NASA Astrophysics Data System (ADS)

Ghammraoui, B.; Tabary, J.; Pouget, S.; Paulus, C.; Moulin, V.; Verger, L.; Duvauchelle, Ph.

2012-02-01

Detection of illicit materials, such as explosives or drugs, within mixed samples is a major issue, both for general security and as part of forensic analyses. In this paper, we describe a new code simulating energy dispersive X-ray diffraction patterns in polycrystalline materials. This program, SinFullscat, models diffraction of any object in any diffractometer system taking all physical phenomena, including amorphous background, into account. Many system parameters can be tuned: geometry, collimators (slit and cylindrical), sample properties, X-ray source and detector energy resolution. Good agreement between simulations and experimental data was obtained. Simulations using explosive materials indicated that parameters such as the diffraction angle or the energy resolution of the detector have a significant impact on the diffraction signature of the material inspected. This software will be a convenient tool to test many diffractometer configurations, providing information on the one that best restores the spectral diffraction signature of the materials of interest.

Mechanical properties of Al-Cu alloy-SiC composites

DOE Office of Scientific and Technical Information (OSTI.GOV)

Anggara, B. S., E-mail: anggorobs1960@yahoo.com; Handoko, E.; Soegijono, B.

The synthesis of aluminum (Al) alloys, Al-Cu, from mixture 96.2 % Al and 3.8 % Cu has been prepared by melting process at a temperature of 1200°C. The adding 12.5 wt% up to 20 wt% of SiC on Al-Cu alloys samples has been investigated. The structure analyses were examined by X-Ray Diffractometer (XRD) and scanning electron microscope (SEM). Moreover, the morphology of Al-Cu alloys has been seen as structure in micrometer range. The hardness was measured by hardness Vickers method. According to the results, it can be assumed that the 15 wt% of SiC content is prefer content to getmore » better quality of back to back hardness Vickers of Al-Cu alloys.« less

Mechanical properties of Al-Cu alloy-SiC composites

NASA Astrophysics Data System (ADS)

Anggara, B. S.; Handoko, E.; Soegijono, B.

2014-09-01

The synthesis of aluminum (Al) alloys, Al-Cu, from mixture 96.2 % Al and 3.8 % Cu has been prepared by melting process at a temperature of 1200°C. The adding 12.5 wt% up to 20 wt% of SiC on Al-Cu alloys samples has been investigated. The structure analyses were examined by X-Ray Diffractometer (XRD) and scanning electron microscope (SEM). Moreover, the morphology of Al-Cu alloys has been seen as structure in micrometer range. The hardness was measured by hardness Vickers method. According to the results, it can be assumed that the 15 wt% of SiC content is prefer content to get better quality of back to back hardness Vickers of Al-Cu alloys.

Structural and magnetic properties of Ga-substituted Co 2 ‑W hexaferrites

NASA Astrophysics Data System (ADS)

Mahmood, Sami H.; Al Sheyab, Qusai; Bsoul, Ibrahim; Mohsen, Osama; Awadallah, Ahmad

2018-05-01

Precursor powders of BaMg2-xCoxFe16O27 with (x = 0.0, 1.0, and 2.0) were prepared using high-energy ball milling, and the effects of chemical composition and sintering temperature on the structural and magnetic properties were investigated using x-ray diffractometer (XRD), scanning electron microscopy (SEM), and vibrating sample magnetometry (VSM). XRD patterns of the prepared samples indicated that crystallization of pure BaW hexaferrite phase was achieved at sintering temperature of 1300{\\deg} C, while BaM and cubic spinel phase intermediate phases were obtained at lower sintering temperatures of 1100{\\deg} C and 1200{\\deg} C. SEM images revealed improvement of the crystallization of the structural phases, and growth of the particle size with increasing the sintering temperature. The magnetic data of the samples sintered at 1300{\\deg} C revealed an increase of the saturation magnetization from 59.44 emu/g to 72.56 emu/g with increasing Co concentration (x) from 0.0 to 2.0. The coercive field Hc decreased from 0.07 kOe at x = 0.0, to 0.03 kOe at x = 1.0, and then increases to 0.09 kOe at x = 2.0. The thermomagnetic curves of the samples sintered at 1300{\\deg} C confirmed the existence of the W-type phase, and revealed spin reorientation transitions above room temperature.

Low dose radiation damage effects in silicon strip detectors

NASA Astrophysics Data System (ADS)

Wiącek, P.; Dąbrowski, W.

2016-11-01

The radiation damage effects in silicon segmented detectors caused by X-rays have become recently an important research topic driven mainly by development of new detectors for applications at the European X-ray Free Electron Laser (E-XFEL). However, radiation damage in silicon strip is observed not only after extreme doses up to 1 GGy expected at E-XFEL, but also at doses in the range of tens of Gy, to which the detectors in laboratory instruments like X-ray diffractometers or X-ray spectrometers can be exposed. In this paper we report on investigation of radiation damage effects in a custom developed silicon strip detector used in laboratory diffractometers equipped with X-ray tubes. Our results show that significant degradation of detector performance occurs at low doses, well below 200 Gy, which can be reached during normal operation of laboratory instruments. Degradation of the detector energy resolution can be explained by increasing leakage current and increasing interstrip capacitance of the sensor. Another observed effect caused by accumulation of charge trapped in the surface oxide layer is change of charge division between adjacent strips. In addition, we have observed unexpected anomalies in the annealing process.

Synthesis of Zinc Oxide Nanoparticles using Anthocyanin as a Capping Agent

NASA Astrophysics Data System (ADS)

Septiani, N. L. W.; Yuliarto, B.; Iqbal, M.; Nugraha

2017-05-01

Zinc Oxide nanoparticles have been successfully synthesized by utilizing anthocyanin as a capping agent by thermal decomposition of precursor route. The influence of the high and low concentrations of the anthocyanin to the shape and size of ZnO was investigated in this work. The anthocyanin was obtained from Indonesia black rice extract with methanol as a solvent. The crystallinity and morphology properties were characterized by X-Ray Diffractometer (XRD), and Scanning Electron Microscope (SEM), respectively. XRD result showed that ZnO was formed with good crystallinity without any second phase and had a hexagonal wurtzite crystal structure. SEM result revealed that ZnO with a low concentration of anthocyanin has a spherical shape with a uniform size of about 16 nm while ZnO with a high concentration of anthocyanin has a rod-like shape. The size of spherical ZnO in this work is smaller than ZnO from the same method of synthesis without anthocyanin (~30 nm).

Sizes of X-ray radiation coherent domains in thin SmS films and their visualization

NASA Astrophysics Data System (ADS)

Sharenkova, N. V.; Kaminskii, V. V.; Petrov, S. N.

2011-09-01

The size of X-ray radiation coherent domains (250 ± 20 Å) is determined in a thin polycrystalline SmS film using X-ray diffraction patterns (θ-2θ scanning, DRON-2 diffractometer, Cu K α radiation) and the Selyakov-Scherrer formula with allowance for the effect of microstrains. An image of this film is taken with a transmission electron microscope, and regions with a characteristic size of 240 Å are clearly visible in it. It is concluded that X-ray radiation coherent domains are visualized.

TiC Reinforcement Composite Coating Produced Using Graphite of the Cast Iron by Laser Cladding

PubMed Central

Liu, Yanhui; Qu, Weicheng; Su, Yu

2016-01-01

In this study, a TiC-reinforced composite coating was produced to improve the wear resistance of a pearlite matrix grey iron using a pre-placed Ti powder by laser cladding. Results of scanning electron microscopy (SEM), X-ray diffractometer (XRD), and energy dispersive X-ray spectroscopy (EDS) confirmed that the coating was composed of TiC particles and two kinds of α-Fe phase. The fine TiC particles were only a few microns in size and uniformly distributed on the matrix phase in the composite coating. The microstructure characteristic of the composite coating resulted in the microhardness rising to about 1000 HV0.3 (China GB/T 4342-1991) and the wear resistance significantly increased relative to the substrate. In addition, the fine and homogeneous solidification microstructure without graphite phase in the transition zone led to a good metallurgical bonding and transition between the coating and the substrate. It was of great significance for the cast iron to modify the surface and repair surface defects or surface damage. PMID:28773934

TiC Reinforcement Composite Coating Produced Using Graphite of the Cast Iron by Laser Cladding.

PubMed

Liu, Yanhui; Qu, Weicheng; Su, Yu

2016-09-30

In this study, a TiC-reinforced composite coating was produced to improve the wear resistance of a pearlite matrix grey iron using a pre-placed Ti powder by laser cladding. Results of scanning electron microscopy (SEM), X-ray diffractometer (XRD), and energy dispersive X-ray spectroscopy (EDS) confirmed that the coating was composed of TiC particles and two kinds of α -Fe phase. The fine TiC particles were only a few microns in size and uniformly distributed on the matrix phase in the composite coating. The microstructure characteristic of the composite coating resulted in the microhardness rising to about 1000 HV0.3 (China GB/T 4342-1991) and the wear resistance significantly increased relative to the substrate. In addition, the fine and homogeneous solidification microstructure without graphite phase in the transition zone led to a good metallurgical bonding and transition between the coating and the substrate. It was of great significance for the cast iron to modify the surface and repair surface defects or surface damage.

In situ surface/interface x-ray diffractometer for oxide molecular beam epitaxy

DOE PAGES

Lee, J. H.; Tung, I. C.; Chang, S. -H.; ...

2016-01-05

In situ studies of oxide molecular beam epitaxy by synchrotron x-ray scattering has been made possible by upgrading an existing UHV/molecular beam epitaxy (MBE) six-circle diffractometer system. For oxide MBE growth, pure ozone delivery to the chamber has been made available, and several new deposition sources have been made available on a new 12 in. CF (ConFlat, a registered trademark of Varian, Inc.) flange. X-ray diffraction has been used as a major probe for film growth and structures for the system. In the original design, electron diffraction was intended for the secondary diagnostics available without the necessity of the x-raymore » and located at separate positions. Deposition of films was made possible at the two diagnostic positions. And, the aiming of the evaporation sources is fixed to the point between two locations. Ozone can be supplied through two separate nozzles for each location. Also two separate thickness monitors are installed. Finally, additional features of the equipment are also presented together with the data taken during typical oxide film growth to illustrate the depth of information available via in situ x-ray techniques.« less

Titration of a Solid Acid Monitored by X-Ray Diffraction

ERIC Educational Resources Information Center

Dungey, Keenan E.; Epstein, Paul

2007-01-01

An experiment is described to introduce students to an important class of solid-state reactions while reinforcing concepts of titration by using a pH meter and a powder X-ray diffractometer. The experiment was successful in teaching students the abstract concepts of solid-state structure and diffraction by applying the diffraction concepts learned…

Dye-Sensitized Solar Cells (DSSCs) reengineering using TiO2 with natural dye (anthocyanin)

NASA Astrophysics Data System (ADS)

Subodro, Rohmat; Kristiawan, Budi; Ramelan, Ari Handono; Wahyuningsih, Sayekti; Munawaroh, Hanik; Hanif, Qonita Awliya; Saputri, Liya Nikmatul Maula Zulfa

2017-01-01

This research on Dye-Sensitized Solar Cells (DSSCs) reengineering was carried out using TiO2 with natural dye (anthocyanin). The fabrication of active carbon layer/TiO2 DSSC solar cell was based on natural dye containing anthocyanins such as mangosteen peel, red rose flower, black glutinous rice, and purple eggplant peel. DSSC was prepared with TiO2 thin layer doped with active carbon; Natural dye was analyzed using UV-Vis and TiO2 was analyzed using X-ray diffractometer (XRD), meanwhile scanning electron microscope (SEM) was used to obtain the size of the crystal. Keithley instrument test was carried out to find out I-V characteristics indicating that the highest efficiency occurred in DSSCs solar cell with 24-hour soaking with mangosteen peel 0.00047%.

Growing barium hexaferrite (BaFe{sub 12}O{sub 19}) thin films using chemical solution deposition

DOE Office of Scientific and Technical Information (OSTI.GOV)

Budiawanti, Sri, E-mail: awanty77@yahoo.com; Faculty of Teacher Training and Education, Sebelas Maret University; Soegijono, Bambang

Barium hexaferrite (BaFe{sub 12}O{sub 19}, or simply known as BaM) thin films has been recognized as a potential candidate for microwave-based devices, magnetic recording media and data storage. To grow BaM thin films, chemical solution deposition is conducted using the aqueous solution of metal nitrates, which involves spin coatings on Si substrates. Furthermore, Thermal Gravimeter Analysis (TGA), X-Ray Diffractometer (XRD), Scanning Electron Microscopy (SEM) and Vibrating Sample Magnetometer (VSM) are applied to evaluate the decomposition behavior, structure, morphology, and magnetic properties of BaM thin films. Additionally, the effects of number of layers variation are also investigated. Finally, magnetic properties analysismore » indicates the isotropic nature of the films.« less

High Rate Deposition of Thick CrN and Cr2N Coatings Using Modulated Pulse Power (MPP) Magnetron Sputtering

DTIC Science & Technology

2010-12-01

in the conventional Bragg-Bentano mode. The residual stress of the coatings was measured by glancing incident angle XRD (GIXRD) in the same X - ray ...micro-analysis (EPMA), x - ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), nanoindentation, scratch test, and ball-on...the coatings was determined by XRD using a SIEMENS X - ray diffractometer (Model KRISTALLOFLEX-810) operated with K-alpha Cu radiation (30 kV and 20 mA

The SPRING Nanoenergetics Hub at UTD

DTIC Science & Technology

2008-12-01

synthesis and processing of advanced nanostructured materials, the structure and property characterization needed for materials optimization, the...nano-particles into hexane solvent a deposited films. Here we are modeling that processes to see how the droplet evaporation progresses in time. What...nanofibers was determined by powder X-ray diffraction (XRD) (Scintag XDS 2000 X-ray diffractometer with Cu Ka radiation). The fiber morphology was

Experiment to Determine the Absorption Coefficient of Gamma Rays as a Function of Energy.

ERIC Educational Resources Information Center

Ouseph, P. J.; And Others

1982-01-01

Simpler than x-ray diffractometer experiments, the experiment described illustrates certain concepts regarding the interaction of electromagnetic rays with matter such as the exponential decrease in the intensity with absorber thickness, variation of the coefficient of absorption with energy, and the effect of the K-absorption edge on the…

An X-ray diffractometer using mirage diffraction

PubMed Central

Fukamachi, Tomoe; Jongsukswat, Sukswat; Ju, Dongying; Negishi, Riichirou; Hirano, Keiichi; Kawamura, Takaaki

2014-01-01

Some characteristics are reported of a triple-crystal diffractometer with a (+, −, +) setting of Si(220) using mirage diffraction. The first crystal is flat, while the second and third crystals are bent. Basically, the first crystal is used as a collimator, the second as a monochromator and the third as the sample. The third crystal also works as an analyzer. The advantages of this diffractometer are that its setup is easy, its structure is simple, the divergence angle from the second crystal is small and the energy resolution of the third crystal is high, of the order of sub-meV. PMID:25242911

Microstructure, ferromagnetic and photoluminescence properties of ITO and Cr doped ITO nanoparticles using solid state reaction

NASA Astrophysics Data System (ADS)

Babu, S. Harinath; Kaleemulla, S.; Rao, N. Madhusudhana; Rao, G. Venugopal; Krishnamoorthi, C.

2016-11-01

Indium-tin-oxide (ITO) (In0.95Sn0.05)2O3 and Cr doped indium-tin-oxide (In0.90Sn0.05Cr0.05)2O3 nanoparticles were prepared using simple low cost solid state reaction method and characterized by different techniques to study their structural, optical and magnetic properties. Microstructures, surface morphology, crystallite size of the nanoparticles were studied using X-ray diffractometer (XRD), field emission scanning electron microscope (FE-SEM). From these methods it was found that the particles were about 45 nm. Chemical composition and valence states of the nanoparticles were studied using energy dispersive analysis of X-rays (EDAX) and X-ray photoelectron spectroscopy (XPS). From these techniques it was observed that the elements of indium, tin, chromium and oxygen were present in the system in appropriate ratios and they were in +3, +4, +3 and -2 oxidation states. Raman studies confirmed that the nanoparticle were free from unintentional impurities. Two broad emission peaks were observed at 330 nm and 460 nm when excited wavelength of 300 nm. Magnetic studies were carried out at 300 K and 100 K using vibrating sample magnetometer (VSM) and found that the ITO nanoparticles were ferromagnetic at 100 K and 300 K. Where-as the room temperature ferromagnetism completely disappeared in Cr doped ITO nanoparticles at 100 K and 300 K.

Structural analysis of polymer thin films using GISAXS in the tender X-ray region: Concept and design of GISAXS experiments using the tender X-ray energy at BL-15A2 at the Photon Factory

DOE Office of Scientific and Technical Information (OSTI.GOV)

Takagi, H., E-mail: takagih@post.kek.jp; Igarashi, N.; Mori, T.

If small angle X-ray scattering (SAXS) utilizing the soft X-ray region is available, advanced and unique experiments, which differ from traditional SAXS methods, can be realized. For example, grazing-incidence small angle X-ray scattering (GISAXS) using hard X-ray is a powerful tool for understanding the nanostructure in both vertical and lateral directions of thin films, while GISAXS utilizing the tender X-ray region (SX-GISAXS) enables depth-resolved analysis as well as a standard GISAXS analysis in thin films. Thus, at BL-15A2 at the Photon Factory, a dedicated diffractometer for SX-GISAXS (above 2.1 keV) was constructed. This diffractometer is composed of four vacuum chambers andmore » can be converted into the vacuum state from the sample chamber in front of the detector surface. Diffractions are clearly observed until 12th peak when measuring collagen by SAXS with an X-ray energy of 2.40 keV and a camera length of 825 mm. Additionally, we conducted the model experiment using SX-GISAXS with an X-ray energy of 2.40 keV to confirm that a poly(methyl methacrylate)-poly(n-butyl acrylate) block copolymer thin film has a microphase-separated structure in the thin film, which is composed of lamellae aligned both parallel and perpendicular to the substrate surface. Similarly, in a polystyrene-poly(methyl methacrylate) block copolymer thin film, SX-GISAXS with 3.60 keV and 5.73 keV revealed that hexagonally packed cylinders are aligned parallel to the substrate surface. The incident angle dependence of the first order peak position of the q{sub z} direction obtained from experiments at various incident X-ray energies agrees very well with the theoretical one calculated from the distorted wave Born approximation.« less

Surface morphological properties of Ag-Al2O3 nanocermet layers using dip-coating technique

NASA Astrophysics Data System (ADS)

Muhammad, Nor Adhila; Suhaimi, Siti Fatimah; Zubir, Zuhana Ahmad; Daud, Sahhidan

2017-12-01

Ag-Al2O3 nanocermet layer was deposited on Cu coated glass substrate using dip-coating technique. The aim of this study was to observe the surface morphology properties of Ag-Al2O3 nanocermet layers after annealing process at 350°C in H2. The surface morphology of Ag-Al2O3 nanocermet will be characterized by Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM) and X-Ray Diffractometer (XRD), respectively. The results show that nearly isolated Ag particles having a large and small size were present in the Al2O3 dielectric matrix after annealing process. The face centered cubic crystalline structure of Ag nanoparticles inclusion in the amorphous alumina dielectric matrix was confirmed using XRD pattern and supported by EDX spectra analysis.

New hardware and software platform for experiments on a HUBER-5042 X-ray diffractometer with a DISPLEX DE-202 helium cryostat in the temperature range of 20-300 K

NASA Astrophysics Data System (ADS)

Dudka, A. P.; Antipin, A. M.; Verin, I. A.

2017-09-01

Huber-5042 diffractometer with a closed-cycle Displex DE-202 helium cryostat is a unique scientific instrument for carrying out X-ray diffraction experiments when studying the single crystal structure in the temperature range of 20-300 K. To make the service life longer and develop new experimental techniques, the diffractometer control is transferred to a new hardware and software platform. To this end, a modern computer; a new detector reader unit; and new control interfaces for stepper motors, temperature controller, and cryostat vacuum pumping system are used. The system for cooling the X-ray tube, the high-voltage generator, and the helium compressor and pump for maintaining the desired vacuum in the cryostat are replaced. The system for controlling the primary beam shutter is upgraded. A biological shielding is installed. The new program tools, which use the Linux Ubuntu operating system and SPEC constructor, include a set of drivers for control units through the aforementioned interfaces. A program for searching reflections from a sample using fast continuous scanning and a priori information about crystal is written. Thus, the software package for carrying out the complete cycle of precise diffraction experiment (from determining the crystal unit cell to calculating the integral reflection intensities) is upgraded. High quality of the experimental data obtained on this equipment is confirmed in a number of studies in the temperature range from 20 to 300 K.

Photoluminescent and Thermoluminescent Studies of Dy3+ and Eu3+ Doped Y2O3 Phosphors.

PubMed

Verma, Tarkeshwari; Agrawal, Sadhana

2018-01-01

Eu 3+ doped and Dy 3+ codoped yttrium oxide (Y 2 O 3 ) phosphors have been prepared using solid-state reaction technique (SSR). The prepared phosphors were characterized by X-ray diffractometer (XRD), energy dispersive X-ray (EDX) spectroscopy, scanning electron microscopy (SEM) and Fourier transforms infrared spectroscopy (FTIR) techniques. Photoluminescence (PL) and Thermoluminescence (TL) properties were studied in detail. PL emission spectra were recorded for prepared phosphors under excitation wavelength 254 nm, which show a high intense peak at 613 nm for Y 2 O 3 :Dy 3+ , Eu 3+ (1:1.5 mol %) phosphor. The correlated color temperature (CCT) and CIE analysis have been performed for the synthesized phosphors. TL glow curves were recorded for Eu 3+ doped and Dy 3+ codoped phosphors to study the heating rate effect and dose response. The kinetic parameters were calculated using peak shape method for UV and γ exposures through computerized glow curve deconvolution (CGCD) technique. The phosphors show second order kinetics and activation energies varying from 5.823 × 10 - 1 to 18.608 × 10 - 1  eV.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sharma, Rabindar K., E-mail: rkrksharma6@gmail.com; Reddy, G. B., E-mail: rkrksharma6@gmail.com

In this report, we synthesize vertically aligned molybdenum trioxide (α−MoO{sub 3}) nanoflakes (NFs) with high aspect ratio (height/thickness >15) on the cobalt coated glass substrates by the plasma assisted sublimation process, employing Mo metal strip as a sublimation source. The effect of substrate temperature, nature of substrate as well as the geometry of the sublimation source (Mo-strip) have been investigated on the morphological, structural and optical properties of the grown NFs, keeping plasma parameters as fixed. The surface morphology, crystalline structure and optical properties of MoO{sub 3} NFs have been studied systematically by using scanning electron microscope (SEM), transmission electronmore » microscope (TEM) with selected area electron diffraction (SAED), X-ray diffractometer, and IR- spectroscopy. The experimental observations endorse that the characteristics of MoO{sub 3} NFs are strongly depend on substrate temperature, substrate nature as well as geometry of Mo-strip. All the observed results are well in consonance with each other.« less

Thermal Conductivity on the Nanofluid of Graphene and Silver Nanoparticles Composite Material.

PubMed

Myekhlai, Munkhshur; Lee, Taejin; Baatar, Battsengel; Chung, Hanshik; Jeong, Hyomin

2016-02-01

The composite material consisted of graphene (GN) and silver nanoparticles (AgNPs) has been essential topic in science and industry due to its unique thermal, electrical and antibacterial proper- ties. However, there are scarcity studies based on their thermal properties of nanofluids. Therefore, GN-AgNPs composite material was synthesized using facile and environment friendly method and further nanofluids were prepared by ultrasonication in this study. The morphological and structural investigations were carried out using scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray diffractometer (XRD) as well as ultra violet (UV)-visible spectroscopy. Furthermore, thermal conductivity measurements were performed for as-prepared nanofluids. As a result of thermal conductivity study, GN-AgNPs composite material was considerably enhanced the thermal conductivity of base fluid (water) by to 6.59% for the nanofluid (0.2 wt% GN and 0.4 wt% AgNPs).

Microstructure and optical properties of nanocrystalline Cu2O thin films prepared by electrodeposition.

PubMed

Jiang, Xishun; Zhang, Miao; Shi, Shiwei; He, Gang; Song, Xueping; Sun, Zhaoqi

2014-01-01

Cuprous oxide (Cu2O) thin films were prepared by using electrodeposition technique at different applied potentials (-0.1, -0.3, -0.5, -0.7, and -0.9 V) and were annealed in vacuum at a temperature of 100°C for 1 h. Microstructure and optical properties of these films have been investigated by X-ray diffractometer (XRD), field-emission scanning electron microscope (SEM), UV-visible (vis) spectrophotometer, and fluorescence spectrophotometer. The morphology of these films varies obviously at different applied potentials. Analyses from these characterizations have confirmed that these films are composed of regular, well-faceted, polyhedral crystallites. UV-vis absorption spectra measurements have shown apparent shift in optical band gap from 1.69 to 2.03 eV as the applied potential becomes more cathodic. The emission of FL spectra at 603 nm may be assigned as the near band-edge emission.

Synthesis, characterization and color performance of novel Co²+-doped alumina/titania nanoceramic pigments.

PubMed

Hafez, Hoda S; El-Fadaly, E

2012-09-01

Blue-green nanoceramic pigments from Co(2+)-doped alumina-titania (xCo(2+)-Al(2)O(3)/TiO(2)) have been synthesized by alkoxide sol-gel route from a mixture of titania and boehmite sols that derived from titanium isopropoxide and aluminum nitrate precursors. The composition of the alumina/titania (AT) matrix is 3:1M ratio. A series of xCo(2+):3TiO(2):1Al(2)O(3) mixed oxides with different Co(2+)-dopant ion concentration has been prepared. The molar ratio of the Co(2+)-dopant ion in the Al(2)O(3)/TiO(2) matrix is from x=0 to 0.5M ratio relative to the titania composition. Characterizations of Co(2+)-doped alumina/titania nanocomposites are carried out using reflectance spectroscopy, transmission electron microscope (TEM), scanning electron microscopy (SEM-EDS), thermo-gravimetric analysis (TGA) and X-ray diffractometer (XRD). The experimental results demonstrated that the prepared Co(2+)-doped alumina-titania nanocomposites fulfill the current technological requirements for ceramic pigment applications that exhibit a high physico-chemical and thermal stabilities at high firing temperatures. Copyright © 2012 Elsevier B.V. All rights reserved.

Fundamental Parameters Line Profile Fitting in Laboratory Diffractometers

PubMed Central

Cheary, R. W.; Coelho, A. A.; Cline, J. P.

2004-01-01

The fundamental parameters approach to line profile fitting uses physically based models to generate the line profile shapes. Fundamental parameters profile fitting (FPPF) has been used to synthesize and fit data from both parallel beam and divergent beam diffractometers. The refined parameters are determined by the diffractometer configuration. In a divergent beam diffractometer these include the angular aperture of the divergence slit, the width and axial length of the receiving slit, the angular apertures of the axial Soller slits, the length and projected width of the x-ray source, the absorption coefficient and axial length of the sample. In a parallel beam system the principal parameters are the angular aperture of the equatorial analyser/Soller slits and the angular apertures of the axial Soller slits. The presence of a monochromator in the beam path is normally accommodated by modifying the wavelength spectrum and/or by changing one or more of the axial divergence parameters. Flat analyzer crystals have been incorporated into FPPF as a Lorentzian shaped angular acceptance function. One of the intrinsic benefits of the fundamental parameters approach is its adaptability any laboratory diffractometer. Good fits can normally be obtained over the whole 20 range without refinement using the known properties of the diffractometer, such as the slit sizes and diffractometer radius, and emission profile. PMID:27366594

Characterization and Selection of Polymer Materials for Binary Munitions Storage. Part 3. Branch Content Determination.

DTIC Science & Technology

1987-09-01

accuracy. The data aquisition system combines a position- sensitive X-ray detector with a 65 kilobyte microcomputer capable of operating as a...The rapid X-ray diffraction system measures intensity versus 20 patterns by placing the detector with its sensitivity axis positioned parallel to the...plane of the diffractometer (see Figure 2). As shown in Figure 2, the detector sensitivity axis z is coplanar with both the incident beam and the

Protein structural dynamics in solution unveiled via 100-ps time-resolved x-ray scattering

PubMed Central

Anfinrud, Philip

2010-01-01

We have developed a time-resolved x-ray scattering diffractometer capable of probing structural dynamics of proteins in solution with 100-ps time resolution. This diffractometer, developed on the ID14B BioCARS (Consortium for Advanced Radiation Sources) beamline at the Advanced Photon Source, records x-ray scattering snapshots over a broad range of q spanning 0.02–2.5 Å-1, thereby providing simultaneous coverage of the small-angle x-ray scattering (SAXS) and wide-angle x-ray scattering (WAXS) regions. To demonstrate its capabilities, we have tracked structural changes in myoglobin as it undergoes a photolysis-induced transition from its carbon monoxy form (MbCO) to its deoxy form (Mb). Though the differences between the MbCO and Mb crystal structures are small (rmsd < 0.2 Å), time-resolved x-ray scattering differences recorded over 8 decades of time from 100 ps to 10 ms are rich in structure, illustrating the sensitivity of this technique. A strong, negative-going feature in the SAXS region appears promptly and corresponds to a sudden > 22 Å3 volume expansion of the protein. The ensuing conformational relaxation causes the protein to contract to a volume ∼2 Å3 larger than MbCO within ∼10 ns. On the timescale for CO escape from the primary docking site, another change in the SAXS/WAXS fingerprint appears, demonstrating sensitivity to the location of the dissociated CO. Global analysis of the SAXS/WAXS patterns recovered time-independent scattering fingerprints for four intermediate states of Mb. These SAXS/WAXS fingerprints provide stringent constraints for putative models of conformational states and structural transitions between them. PMID:20406909

Protein structural dynamics in solution unveiled via 100-ps time-resolved x-ray scattering.

PubMed

Cho, Hyun Sun; Dashdorj, Naranbaatar; Schotte, Friedrich; Graber, Timothy; Henning, Robert; Anfinrud, Philip

2010-04-20

We have developed a time-resolved x-ray scattering diffractometer capable of probing structural dynamics of proteins in solution with 100-ps time resolution. This diffractometer, developed on the ID14B BioCARS (Consortium for Advanced Radiation Sources) beamline at the Advanced Photon Source, records x-ray scattering snapshots over a broad range of q spanning 0.02-2.5 A(-1), thereby providing simultaneous coverage of the small-angle x-ray scattering (SAXS) and wide-angle x-ray scattering (WAXS) regions. To demonstrate its capabilities, we have tracked structural changes in myoglobin as it undergoes a photolysis-induced transition from its carbon monoxy form (MbCO) to its deoxy form (Mb). Though the differences between the MbCO and Mb crystal structures are small (rmsd < 0.2 A), time-resolved x-ray scattering differences recorded over 8 decades of time from 100 ps to 10 ms are rich in structure, illustrating the sensitivity of this technique. A strong, negative-going feature in the SAXS region appears promptly and corresponds to a sudden > 22 A(3) volume expansion of the protein. The ensuing conformational relaxation causes the protein to contract to a volume approximately 2 A(3) larger than MbCO within approximately 10 ns. On the timescale for CO escape from the primary docking site, another change in the SAXS/WAXS fingerprint appears, demonstrating sensitivity to the location of the dissociated CO. Global analysis of the SAXS/WAXS patterns recovered time-independent scattering fingerprints for four intermediate states of Mb. These SAXS/WAXS fingerprints provide stringent constraints for putative models of conformational states and structural transitions between them.

The Optics and Alignment of the Divergent Beam Laboratory X-ray Powder Diffractometer and its Calibration Using NIST Standard Reference Materials.

PubMed

Cline, James P; Mendenhall, Marcus H; Black, David; Windover, Donald; Henins, Albert

2015-01-01

The laboratory X-ray powder diffractometer is one of the primary analytical tools in materials science. It is applicable to nearly any crystalline material, and with advanced data analysis methods, it can provide a wealth of information concerning sample character. Data from these machines, however, are beset by a complex aberration function that can be addressed through calibration with the use of NIST Standard Reference Materials (SRMs). Laboratory diffractometers can be set up in a range of optical geometries; considered herein are those of Bragg-Brentano divergent beam configuration using both incident and diffracted beam monochromators. We review the origin of the various aberrations affecting instruments of this geometry and the methods developed at NIST to align these machines in a first principles context. Data analysis methods are considered as being in two distinct categories: those that use empirical methods to parameterize the nature of the data for subsequent analysis, and those that use model functions to link the observation directly to a specific aspect of the experiment. We consider a multifaceted approach to instrument calibration using both the empirical and model based data analysis methods. The particular benefits of the fundamental parameters approach are reviewed.

Effect of Nano-TiC Dispersed Particles and Electro-Codeposition Parameters on Morphology and Structure of Hybrid Ni/TiC Nanocomposite Layers.

PubMed

Benea, Lidia; Celis, Jean-Pierre

2016-04-06

This research work describes the effect of dispersed titanium carbide (TiC) nanoparticles into nickel plating bath on Ni/TiC nanostructured composite layers obtained by electro-codeposition. The surface morphology of Ni/TiC nanostructured composite layers was characterized by scanning electron microscopy (SEM). The composition of coatings and the incorporation percentage of TiC nanoparticles into Ni matrix were studied and estimated by using energy dispersive X-ray analysis (EDX). X-ray diffractometer (XRD) has been applied in order to investigate the phase structure as well as the corresponding relative texture coefficients of the composite layers. The results show that the concentration of nano-TiC particles added in the nickel electrolyte affects the inclusion percentage of TiC into Ni/TiC nano strucured layers, as well as the corresponding morphology, relative texture coefficients and thickness indicating an increasing tendency with the increasing concentration of nano-TiC concentration. By increasing the amount of TiC nanoparticles in the electrolyte, their incorporation into nickel matrix also increases. The hybrid Ni/nano-TiC composite layers obtained revealed a higher roughness and higher hardness; therefore, these layers are promising superhydrophobic surfaces for special application and could be more resistant to wear than the pure Ni layers.

Solid State Reaction Synthesis of Si-HA as Potential Biomedical Material: An Endeavor to Enhance the Added Value of Indonesian Mineral Resources

NASA Astrophysics Data System (ADS)

Hartatiek; Yudyanto; Ratnasari, S. D.; Windari, R. Y.; Hidayat, N.

2017-05-01

In recent years, one of the most prominently investigated materials is hydroxyapatite (HA). It is because of its excellent properties for medical applications, essentially related to orthopedic. Also, the introduction of other materials to HA becomes another research focus of many leading scientists. In this present study, silicon with various concentrations was introduced, by means of solid state reaction route, to HA forming Si-HA. The crystal structure properties of the as-prepared samples were evaluated by X-ray diffractometer (XRD). Fourier Transform Infra Red (FTIR) spectroscopy data collection and analysis were done to investigate the functional groups within the samples. The microstructural characteristics as well as elemental mapping of the samples were captured by scanning electron microscopy and energy dispersive x-ray spectroscopy (SEM-EDX). Vickers hardness test was also conducted to investigate the hardness properties of the samples. Furthermore, in vitro characterization-based bio resorbability of the samples in a simulated body fluid were also described. This study revealed that Indonesian limestone can be utilized as the raw material for synthesizing HA. The silicon has been successfully incorporated into phosphate site of the HA crystal. Conclusively, the Si-HA reported in this study shows good bioresorbability characteristic.

Yttria-Stabilized Zirconia Ceramic Deposition on SS430 Ferritic Steel Grown by PLD - Pulsed Laser Deposition Method

NASA Astrophysics Data System (ADS)

Khalid Rivai, Abu; Mardiyanto; Agusutrisno; Suharyadi, Edi

2017-01-01

Development of high temperature materials are one of the key issues for the deployment of advanced nuclear reactors due to higher temperature operation. One of the candidate materials for that purpose is ceramic-coated ferritic steel that one of the functions is to be a thermal barrier coating (TBC). Thin films of YSZ (Ytrria-Stabilized Zirconia) ceramic have been deposited on a SS430 ferritic steel using Pulsed Laser Deposition (PLD) at Center For Science and Technology of Advanced Materials laboratory - National Nuclear Energy Agency of Indonesia (BATAN). The thin film was deposited with the chamber pressure range of 200-225 mTorr, the substrate temperature of 800oC, and the number of laser shots of 3×104, 6×104 and 9×104. Afterward, the samples were analyzed using Scanning Electron Microscope - Energy Dispersive X-ray Spectroscope (SEM-EDS), X-Ray Diffractometer (XRD), Atomic Force Microscope (AFM) and Vickers hardness tester. The results showed that the YSZ could homogeneously and sticky deposited on the surface of the ferritic steel. The surfaces were very smoothly formed with the surface roughness was in the range of 70 nm. Furthermore, thickness, composition of Zr4+ dan Y3+, the crystallinity, and hardness property was increased with the increasing the number of the shots.

Laser irradiation effects on the surface, structural and mechanical properties of Al-Cu alloy 2024

NASA Astrophysics Data System (ADS)

Yousaf, Daniel; Bashir, Shazia; Akram, Mahreen; kalsoom, Umm-i.-; Ali, Nisar

2014-02-01

Laser irradiation effects on surface, structural and mechanical properties of Al-Cu-Mg alloy (Al-Cu alloy 2024) have been investigated. The specimens were irradiated for various fluences ranging from 3.8 to 5.5 J/cm2 using an Excimer (KrF) laser (248 nm, 18 ns, 30 Hz) under vacuum environment. The surface and structural modifications of the irradiated targets have been investigated by scanning electron microscope (SEM) and X-ray diffractometer (XRD), respectively. SEM analysis reveals the formation of micro-sized craters along the growth of periodic surface structures (ripples) at their peripheries. The size of the craters initially increases and then decreases by increasing the laser fluence. XRD analysis shows an anomalous trend in the peak intensity and crystallite size of the specimen irradiated for various fluences. A universal tensile testing machine and Vickers microhardness tester were employed in order to investigate the mechanical properties of the irradiated targets. The changes in yield strength, ultimate tensile strength and microhardness were found to be anomalous with increasing laser fluences. The changes in the surface and structural properties of Al-Cu alloy 2024 after laser irradiation have been associated with the changes in mechanical properties.

Hidroxyapatite Coating on CoCrMo Alloy Titanium Nitride Coated Using Biomimetic Method

NASA Astrophysics Data System (ADS)

Charlena; Sukaryo, S. G.; Fajar, M.

2016-11-01

Bone implants is a way to cure broken bones which is being developed. The implants can be made of metals, ceramics and polymers. Metallic materials commonly used are titanium (Ti), stainless steel, and metal alloys. This study used Co-based alloys, i.e. CoCrMo coated with titanium nitride (TiN) which was then coated on hidroxyapatite (HAp). The HAp coating on the surface of CoCrMo alloy was done by biomimetic methods, first by soaking the metal alloys in simulated body fluid (SBF) solution for 18, 24, and 36 hours. The immersion in the SBF solution produced white coat on the surface of the metal alloy. The layers formed were analyzed by scanning electron microscope (SEM) and characterized by x-ray diffractometer (XRD). Based on the SEM results of 36 hours treatment, the morphology of apatite crystal formed fine grains. According to XRD result, there were HAp peaks at angles 2θ 31.86, 32.25, dan 39.48. However, there were also CaCO3 peaks at angles 2θ 29.46, 36.04, and 46.79. It indicated the pure HAp is not yet formed.

Bruker SMART X2S Benchtop System: A Means to Making X-Ray Crystallography More Mainstream in the Undergraduate Laboratory

ERIC Educational Resources Information Center

Guzei, Ilia A.; Hill, Nicholas J.; Zakai, Uzma I.

2010-01-01

Bruker SMART X2S is a portable benchtop diffractometer that requires only a 110 V outlet to operate. The instrument operation is intuitive and facile with an automation layer governing the workflow from behind the scenes. The user participation is minimal. At the end of an experiment, the instrument attempts to solve the structure automatically;…

Development of scanning electron and x-ray microscope

DOE Office of Scientific and Technical Information (OSTI.GOV)

Matsumura, Tomokazu, E-mail: tomokzau.matsumura@etd.hpk.co.jp; Hirano, Tomohiko, E-mail: tomohiko.hirano@etd.hpk.co.jp; Suyama, Motohiro, E-mail: suyama@etd.hpk.co.jp

We have developed a new type of microscope possessing a unique feature of observing both scanning electron and X-ray images under one unit. Unlike former X-ray microscopes using SEM [1, 2], this scanning electron and X-ray (SELX) microscope has a sample in vacuum, thus it enables one to observe a surface structure of a sample by SEM mode, to search the region of interest, and to observe an X-ray image which transmits the region. For the X-ray observation, we have been focusing on the soft X-ray region from 280 eV to 3 keV to observe some bio samples and softmore » materials. The resolutions of SEM and X-ray modes are 50 nm and 100 nm, respectively, at the electron energy of 7 keV.« less

X-ray microscopy using reflection targets based on SEM with tungsten filament

NASA Astrophysics Data System (ADS)

Liu, Junbiao; Ma, Yutian; Zhao, Weixia; Niu, Geng; Chu, Mingzhang; Yin, Bohua; Han, Li; Liu, Baodong

2016-10-01

X-ray MicroandNano imaging is developed based on the conventional x-ray tomography, it can not only provide nondestructive testing with higher resolution measurement, but also be used to examine the material or the structure with low atomic number and low density. The source with micro-focal spot size is one of the key components of x-ray MicroandNano imaging. The focused electron beam from SEM bombarding the metal target can generate x-ray with ultra-small size. It is convenient to set up x-ray microscopy based on SEM for laboratory use. This paper describes a new x-ray microscopy using reflection targets based on FEI Quanta600 SEM with tungsten filament. The flat panel detector is placed outside of the vacuum chamber with 300μm thickness Be-window to isolate vacuum from the air. A stage with 3 DOFs is added to adjust the positions of the target, the SEM's sample stage is used to move sample. And the shape of target is designed as cone with 60° half cone angle to get the maximum x-ray dosage. The attenuation coefficient of Bewindow for x-ray is about 25%. Finally, the line pair card is used to evaluate the resolution and the result shows that the resolution of the system can receive less than 750nm, when the acceleration voltage is 30keV, the beam current is 160nA, the SEM working distance is 5mm and the acquisition time of the detector is 60s.

Impurity incorporation, deposition kinetics, and microstructural evolution in sputtered Ta films

NASA Astrophysics Data System (ADS)

Whitacre, Jay Fredric

There is an increasing need to control the microstructure in thin sputtered Ta films for application as high-temperature coatings or diffusion barriers in microelectronic interconnect structures. To this end, the relationship between impurity incorporation, deposition kinetics, and microstructural evolution was examined for room-temperature low growth rate DC magnetron sputtered Ta films. Impurity levels present during deposition were controlled by pumping the chamber to various base pressures before growth. Ar pressures ranging from 2 to 20 mTorr were used to create contrasting kinetic environments in the sputter gas. This affected both the distribution of adatom kinetic energies at the substrate as well as the rate of impurity desorption from the chamber walls: at higher Ar pressures adatoms has lower kinetic energies, and there was an increase in impurity concentration. X-ray diffraction, high-resolution transmission electron microscopy (HREM), transmission electron diffraction (TED), scanning electron microscopy (SEM), secondary ion mass spectrometry (SIMS), and x-ray photoelectron. spectroscopy (XPS) were used to examine film crystallography, microstructure, and composition. A novel laboratory-based in-situ x-ray diffractometer was constructed. This new set-up allowed for the direct observation of microstructural evolution during growth. Films deposited at increasingly higher Ar pressures displayed a systematic decrease in grain size and degree of texturing, while surface morphology was found to vary from a nearly flat surface to a rough surface with several length scales of organization. In-situ x-ray results showed that the rate of texture evolution was found to be much higher in films grown using lower Ar pressures. These effects were studied in films less than 200 A thick using high resolution x-ray diffraction in conjunction with a synchrotron light source (SSRL B.L. 7-2). Films grown using higher Ar pressures (above 10 mTorr) with a pre-growth base pressure of 1 x 10--6 Torr had grains less than 10 nm in diameter and significant amorphous content Calculated radial distribution functions show a significant increase in average inter-atomic spacing in films grown using higher base pressures and Ar pressures. The amorphous content in the films was determined via comparison between ideal crystalline diffraction patterns and actual data. Thinner films grown at higher Ar pressures had relatively greater amorphous content. Real-time process control using the in-situ diffractometer was also demonstrated. The effects observed are discussed in the context of previous theories and experiments that document room-temperature sputter film growth. The changes in film microstructure observed were impurity mediated. Specifically, oxygen desorbed from the chamber walls during growth were incorporated into the film and subsequently limited grain development and texturing. A second phase consisting of amorphous Ta2O5 formed between the grain nuclei. Adatom kinetics played a role in determining surface morphology: at low Ar pressures (2 mTorr) significant adatom kinetic energies served to flattened the film surface, though impurity levels dominated grain development even in these conditions.

Crystallization behavior of polyamide-6 microcellular nanocomposites

Treesearch

Mingjun Yuan; Lih-Sheng Turng; Shaoqin Gong; Andreas Winardi

2004-09-01

The crystallization behaviors of polyamide-6 (PA-6) and its nanocomposites undergoing the microcellular injection molding process are studied using Transmission Electron Microscopy (TEM), X-ray Diffractometer (XRD), Polarized Optical Microscopy (POM), and Differential Scanning Calorimetry (DSC). The relationships among the morphology, the mechanical property of the...

Thermochemical properties of nanometer CL-20 and PETN fabricated using a mechanical milling method

NASA Astrophysics Data System (ADS)

Song, Xiaolan; Wang, Yi; An, Chongwei

2018-06-01

2,4,6,8,10,12-Hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane (CL-20) and pentaerythritol tetranitrate (PETN), with mean sizes of 73.8 nm and 267.7 nm, respectively, were fabricated on a high-energy ball-mill. Scanning electron microscope (SEM) analysis was used to image the micron-scale morphology of nano-explosives, and the particle size distribution was calculated using the statistics of individual particle sizes obtained from the SEM images. Analyses, such as X-ray diffractometer (XRD), infrared spectroscopy (IR), and X-ray photoelectron spectroscopy (XPS), were also used to confirm whether the crystal phase, molecular structure, and surface elements changed after a long-term milling process. The results were as expected. Thermal analysis was performed at different heating rates. Parameters, such as the activation energy (ES), activation enthalpy (ΔH≠), activation free energy (ΔG≠), activation entropy (ΔS≠), and critical temperature of thermal explosion (Tb), were calculated to determine the decomposition courses of the explosives. Moreover, the thermal decomposition mechanisms of nano CL-20 and nano PETN were investigated using thermal-infrared spectrometry online (DSC-IR) analysis, by which their gas products were also detected. The results indicated that nano CL-20 decomposed to CO2 and N2O and that nano PETN decayed to NO2, which implied a remarkable difference between the decomposition mechanisms of the two explosives. In addition, the mechanical sensitivities of CL-20 and PETN were tested, and the results revealed that nano-explosives were more insensitive than raw ones, and the possible mechanism for this was discussed. Thermal sensitivity was also investigated with a 5 s bursting point test, from which the 5 s bursting point (T5s) and the activation of the deflagration were obtained.

Structural, electrical and mechanical properties of selenium doped thallium based high-temperature superconductors

NASA Astrophysics Data System (ADS)

Cavdar, S.; Kol, N.; Koralay, H.; Ozturk, O.; Asikuzun, E.; Tasci, A. T.

2016-01-01

In this study, highly-refined chemical powders were synthesized by having them ready in appropriate stoichiometric proportions with conventional solid state reaction method so that they would produce the superconductor TlPb0.3Sr2Ca1-xSexCu2Oy (x = 0; 0.4; 0.6; 1.0). This study aims to understand effect of the selenium doping on the superconducting, structural and mechanical properties of the aforementioned superconducting material. The effect of the doping rates on the structural and electrical properties of the sample has been identified. Electrical characteristics of the TlPb0.3Sr2Ca1-xSexCu2Oy material were measured using standard four point probe method. Structural characteristics were examined with the powder X-ray diffractometer (XRD) and scanning electron microscope (SEM). Mechanical properties were analyzed with Vickers microhardness measurements on the sample surface. According to the results, it was observed that the reflection comes from the (00l) and parallel planes increased with Se doping. Particle size increases with increasing doping ratio. According to results of the mechanical measurements, all samples exhibit indentation size effect (ISE) behavior. Comparing the obtained results with theoretical studies, it was understood that Hays Kendall approach is the best method in determination of mechanical properties and analyzing microhardness of the materials.

Acquisition of a High-Resolution High-Intensity X-ray Diffractometer for Research and Education

DTIC Science & Technology

2015-07-20

NAME(S) AND ADDRESS (ES) U.S. Army Research Office P.O. Box 12211 Research Triangle Park, NC 27709-2211 X-ray diffraction; germanium- tin alloys...is in progress for others. Comprehensive data were acquired for pseudomorphic germanium- tin alloys grown on germanium by molecular beam epitaxy...Research  100+  2000  Federal grant  Germanium‐ tin  alloys  Tech transfer  9  180  Startup company  Metallurgy  Research  5  100  Federal grant  SAXS  Total

Dissolution Rates of Allophane, FE-Containing Allophane, and Hisingerite and Implications for Gale Crater, Mars

NASA Technical Reports Server (NTRS)

Ralston, S. J.; Hausrath, E. M.; Tschauner, O.; Rampe, E. B.; Christoffersen, R.

2018-01-01

Investigations with the CheMin Xray Diffractometer (XRD) onboard the Curiosity rover in Gale Crater demonstrate that all rock and soil samples measured to date contain approximately 15-70 weight percentage X-ray amorphous materials. The diffuse scattering hump from the X-ray amorphous materials in CheMin XRD patterns can be fit with a combination of allophane, ferrihydrite, and rhyolitic and basaltic glass. Because of the iron-rich nature of Mars' surface, Fe-rich poorly-crystalline phases, such as hisingerite, may be present in addition to allophane.

Magnetic and structural properties of CoFe 2O 4 thin films synthesized via a sol-gel process

NASA Astrophysics Data System (ADS)

dos S. Duque, J. G.; Macêdo, M. A.; Moreno, N. O.; Lopez, J. L.; Pfanes, H.-D.

2001-05-01

Using a sol-gel process having the coconut water as a precursor of organic chain, we synthesized thin films of cobalt ferrite. The films were characterized by using a SQUID magnetometer, an X-ray diffractometer, an X-ray spectrophotometer, Mössbauer spectroscopy and atomic force microscope. Co ferrite films annealed at 500°C for 2 h show grain sizes between 10 and 20 nm, grown as single-phase spinel structure and exhibit high coercivity and a moderate saturation magnetization (above 30 kOe).

The statistical kinematical theory of X-ray diffraction as applied to reciprocal-space mapping

PubMed

Nesterets; Punegov

2000-11-01

The statistical kinematical X-ray diffraction theory is developed to describe reciprocal-space maps (RSMs) from deformed crystals with defects of the structure. The general solutions for coherent and diffuse components of the scattered intensity in reciprocal space are derived. As an example, the explicit expressions for intensity distributions in the case of spherical defects and of a mosaic crystal were obtained. The theory takes into account the instrumental function of the triple-crystal diffractometer and can therefore be used for experimental data analysis.

Natural Rubber/Dendrimer Modified Montmorillonite Nanocomposites: Mechanical and Flame-Retardant Properties

PubMed Central

Zhang, Chenyang; Wang, Jincheng

2017-01-01

A series of flame-retardant nanocomposites were established based on compounding of natural rubber (NR) and dendrimer modified flame-retardant organic montmorillonite (FR-DOMt). The merits of these nanocomposites were focused on their better mechanical and flame-retardant properties. X-ray diffractometer (XRD) together with scanning electron microscopy (SEM) and transmission electron microscopy (TEM) analysis revealed that exfoliation, intercalation, or aggregation status in the NRmatrix can be achieved by addition of different amounts of FR-DOMt. The sound effects of blend ratio of FR-DOMt on mechanical, thermal stability, and flame-retardant (FR) properties of NR were studied. The NR/FR-DOMt-20 composite possessed the highest tensile strength, and this resulted from complicated interactions between layered silicates and elastomers. In addition, with loading of 20 phr of FR-DOMt, the flammability parameters of NR, such as heat release rate (HRR), smoke evolution area (SEA), and carbon monoxide (CO) concentration, were obviously reduced from cone calorimeter analysis. PMID:29283385

Synthesis of SnO2 and Ag Nanoparticles from Electronic Wastes with the Assistance of Ultrasound and Microwaves

NASA Astrophysics Data System (ADS)

Cerchier, Pietrogiovanni; Dabalà, Manuele; Brunelli, Katya

2017-09-01

In this work, SnO2 and Ag nanoparticles were produced with a raw material nitric acid solution, which came from the leaching of printed circuit boards. First, a precursor of tin oxide was precipitated from the nitric acid solution by three different techniques: (I) conventional heating, (II) microwave irradiation, and (III) ultrasound treatment. Second, this precursor was transformed into tin oxide nanoparticles by heat treatment in a furnace. Third, hydrochloric acid was added to the nitric acid solution to induce the precipitation of silver chloride. Fourth, silver chloride was reduced to metallic silver nanoparticles in an ammonia solution using glucose syrup as both the reducing agent and the capping agent. The reduction reaction was carried out through (I) conventional heating, (II) microwave irradiation, and (III) ultrasound treatment. The nanoparticles were characterized by scanning electron microscope (SEM), x-ray diffractometer (XRD), infrared (IR)-spectroscopy, transmission electron microscope (TEM), ultraviolet (UV)-spectroscopy, and laser diffraction particle size analyzer.

Phase constitution characteristics of the Fe-Al alloy layer in the HAZ of calorized steel pipe

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li Yajiang; Zou Zengda; Wei Xing

1997-09-01

Mechanical properties of the welding region and phase constitution characteristics in the iron-aluminum (Fe-Al) alloy layer of calorized steel pipes were researched by means of metallography, which included the use of scanning electron microscopy (SEM), transmission electron microscopy (TEM), electron probe microanalysis (EPMA) and an X-ray diffractometer. Experimental results indicated that the Fe-Al alloy layer of calorized steel pipe was mainly composed of an FeAl phase, an Fe{sub 3}Al phase and an {alpha}-Fe(Al) solid solution, and the microhardness in the Fe-Al coating was 600--310 HM from the surface layer to the inside. There were no higher aluminum content phases, suchmore » as brittle FeAl{sub 2}, Fe{sub 2}Al{sub 5} and FeAl{sub 3}. By controlling the aluminizing process parameters, the ability to bear deformation and weld-ability of the calorized steel pipe were remarkably improved.« less

Ca-doped LTO using waste eggshells as Ca source to improve the discharge capacity of anode material for lithium-ion battery

NASA Astrophysics Data System (ADS)

Setiawan, D.; Subhan, A.; Saptari, S. A.

2017-07-01

The necessity of high charge-discharge capacity lithium-ion battery becomes very urgent due to its applications demand. Several researches have been done to meet the demand including Ca doping on Li4Ti5O12 for anode material of lithium-ion batteries. Ca-doped Li4Ti5O12 (LTO) in the form of Li4-xCaxTi5O12 (x = 0, 0.05, 0.075, and 0.1) have been synthesized using simple solid state reaction. The materials preparation involved waste eggshells in the form of CaCO3 as Ca source. The structure and capacity of as-prepared samples were characterized using X-Ray Diffractometer and Cyclic Voltametry. X-Ray Diffractometer characterization revealed that all amount of dopant had entered the lattice structure of LTO successfully. The crystalline sizes were obtained by using Scherrer equation. No significant differences are detected in lattice parameters (˜8.35 Å) and crystalline sizes (˜27 nm) between all samples. Cyclic Voltametry characterization shows that Li4-xCaxTi5O12 (x = 0.05) has highest charge-discharge capacity of 177.14 mAh/g and 181.92 mAh/g, respectively. Redox-potentials of samples show no significant differences with the average of 1.589 V.

Effect of Nano-TiC Dispersed Particles and Electro-Codeposition Parameters on Morphology and Structure of Hybrid Ni/TiC Nanocomposite Layers

PubMed Central

Benea, Lidia; Celis, Jean-Pierre

2016-01-01

This research work describes the effect of dispersed titanium carbide (TiC) nanoparticles into nickel plating bath on Ni/TiC nanostructured composite layers obtained by electro-codeposition. The surface morphology of Ni/TiC nanostructured composite layers was characterized by scanning electron microscopy (SEM). The composition of coatings and the incorporation percentage of TiC nanoparticles into Ni matrix were studied and estimated by using energy dispersive X-ray analysis (EDX). X-ray diffractometer (XRD) has been applied in order to investigate the phase structure as well as the corresponding relative texture coefficients of the composite layers. The results show that the concentration of nano-TiC particles added in the nickel electrolyte affects the inclusion percentage of TiC into Ni/TiC nano strucured layers, as well as the corresponding morphology, relative texture coefficients and thickness indicating an increasing tendency with the increasing concentration of nano-TiC concentration. By increasing the amount of TiC nanoparticles in the electrolyte, their incorporation into nickel matrix also increases. The hybrid Ni/nano-TiC composite layers obtained revealed a higher roughness and higher hardness; therefore, these layers are promising superhydrophobic surfaces for special application and could be more resistant to wear than the pure Ni layers. PMID:28773395

Synthesis of one-dimensional gold nanostructures and the electrochemical application of the nanohybrid containing functionalized graphene oxide for cholesterol biosensing.

PubMed

Nandini, Seetharamaiah; Nalini, Seetharamaiah; Reddy, M B Madhusudana; Suresh, Gurukar Shivappa; Melo, Jose Savio; Niranjana, Pathappa; Sanetuntikul, Jakkid; Shanmugam, Sangaraju

2016-08-01

This manuscript reports a new approach for the synthesis of one dimensional gold nanostructure (AuNs) and its application in the development of cholesterol biosensor. Au nanostructures have been synthesized by exploiting β-diphenylalanine (β-FF) as an sacrificial template, whereas the Au nanoparticles (AuNPs) were synthesized by ultrasound irradiation. X-ray diffractometer (XRD), scanning electron microscope (SEM) and energy dispersive analysis of X-rays (EDAX) have been employed to characterize the morphology and composition of the prepared samples. With the aim to develop a highly sensitive cholesterol biosensor, cholesterol oxidase (ChOx) was immobilized on AuNs which were appended on the graphite (Gr) electrode via chemisorption onto thiol-functionalized graphene oxide (GO-SH). This Gr/GO-SH/AuNs/ChOx biosensor has been characterized using cyclic voltammetry (CV), electrochemical impedance spectroscopy and chronoamperometry. CV results indicated a direct electron transfer between the enzyme and the electrode surface. A new potentiostat intermitant titration technique (PITT) has been studied to determine the diffusion coefficient and maxima potential value. The proposed biosensor showed rapid response, high sensitivity, wide linear range and low detection limit. Furthermore, our AuNs modified electrode showed excellent selectivity, repeatability, reproducibility and long term stability. The proposed electrode has also been used successfully to determine cholesterol in serum samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Toward a durable superhydrophobic aluminum surface by etching and ZnO nanoparticle deposition.

PubMed

Rezayi, Toktam; Entezari, Mohammad H

2016-02-01

Fabrication of suitable roughness is a fundamental step for acquiring superhydrophobic surfaces. For this purpose, a deposition of ZnO nanoparticles on Al surface was carried out by simple immersion and ultrasound approaches. Then, surface energy reduction was performed using stearic acid (STA) ethanol solution for both methods. The results demonstrated that ultrasound would lead to more stable superhydrophobic Al surfaces (STA-ZnO-Al-U) in comparison with simple immersion method (STA-ZnO-Al-I). Besides, etching in HCl solution in another sample was carried out before ZnO deposition for acquiring more mechanically stable superhydrophobic surface. The potentiodynamic measurements demonstrate that etching in HCl solution under ultrasound leads to superhydrophobic surface (STA-ZnO-Al(E)-U). This sample shows remarkable decrease in corrosion current density (icorr) and long-term stability improvement versus immersion in NaCl solution (3.5%) in comparison with the sample prepared without etching (STA-ZnO-Al-U). Scanning electron micrograph (SEM) and energy-dispersive X-ray spectroscopy (EDX) confirmed a more condense and further particle deposition on Al substrate when ultrasound was applied in the system. The crystallite evaluation of deposited ZnO nanoparticles was carried out using X-ray diffractometer (XRD). Finally, for STA grafting verification on Al surface, Fourier transform infrared in conjunction with attenuated total reflection (FTIR-ATR) was used as a proper technique. Copyright © 2015 Elsevier Inc. All rights reserved.

Osteoinductive silk fibroin/titanium dioxide/hydroxyapatite hybrid scaffold for bone tissue engineering.

PubMed

Kim, Jung-Ho; Kim, Dong-Kyu; Lee, Ok Joo; Ju, Hyung Woo; Lee, Jung Min; Moon, Bo Mi; Park, Hyun Jung; Kim, Dong Wook; Lee, Jun Ho; Park, Chan Hum

2016-01-01

The present study demonstrated the fabrication that incorporation of titanium isopropoxide (TiO2) and hydroxyapatite (HA) nanoparticles into the silk fibroin (SF) scaffolds. In this process, we prepared TiO2 nanoparticles using sol-gel synthesis and the porous structure was developed by salt-leaching process. Homogeneous distribution of TiO2 and HA nanoparticles were confirmed by images of VP-FE-SEM and those equipped with energy dispersive X-ray spectrometer. Structural characteristics of the porous SF/TiO2/HA hybrid scaffold were also determined using FTIR analysis and X-ray diffractometer. In this study, the porous SF/TiO2/HA hybrid scaffold showed similar porosity, enhanced mechanical property, but decreased water binding abilities, compared with the porous SF scaffold. For evaluation of the osteogenic differentiation of rat bone marrow mesenchymal stem cells, alkaline phosphatase activity and osteogenic gene expression were employed. Our results revealed that the porous SF/TiO2/HA hybrid scaffold had improved osteoinductivity compared with the porous SF scaffold. These results suggest that the osteogenic property as well as mechanical property of the porous SF/TiO2/HA hybrid scaffold could be better than the porous SF scaffold. Therefore, the porous SF/TiO2/HA hybrid scaffold may be a good promising biomaterial for bone tissue engineering application. Copyright © 2015 Elsevier B.V. All rights reserved.

Cu(II), Co(II) and Ni(II) complexes of new Schiff base ligand: Synthesis, thermal and spectroscopic characterizations

NASA Astrophysics Data System (ADS)

Refat, Moamen S.; El-Sayed, Mohamed Y.; Adam, Abdel Majid A.

2013-04-01

Cu(II), Co(II), and Ni(II) complexes were synthesized from 2-[(5-o-chlorophenylazo-2-hydroxybenzylidin)amino]-phenol Schiff base (H2L). Metal ions coordinate in a tetradentate or hexadentate features with these O2N donor ligand, which are characterized by elemental analyses, magnetic moments, infrared, Raman laser, electronic, and 1H NMR spectral studies. The elemental analysis suggests the stoichiometry to be 1:1 (metal:ligand). Reactions with Cu(II), Co(II) and Ni(II), resulted [Cu(H2L)(H2O)2(Cl)]Cl, [Co(H2L)(H2O)3]Cl2ṡ3H2O and [Ni(H2L)(H2O)2]Cl2ṡ6H2O. The thermal decomposition behavior of H2L complexes has been investigated by thermogravimetric analysis (TG/DTG) at a heating rate of 10 °C min-1 under nitrogen atmosphere. The brightness side in this study is to take advantage for the preparation and characterizations of single phases of CuO, CoO and NiO nanoparticles using H2L complexes as precursors via a solid-state decomposition procedure. The crystalline structures of products using X-ray diffractometer (XRD), morphology of particles by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX) were investigated.

Enhanced Adsorption of Selenium Ions from Aqueous Solution Using Iron Oxide Impregnated Carbon Nanotubes

PubMed Central

Bakather, Omer Y.; Khraisheh, Majeda; Nasser, Mustafa S.

2017-01-01

The aim of this research was to investigate the potential of raw and iron oxide impregnated carbon nanotubes (CNTs) as adsorbents for the removal of selenium (Se) ions from wastewater. The original and modified CNTs with different loadings of Fe2O3 nanoparticles were characterized using high resolution transmission electron microscopy (HRTEM), scanning electron microscopy (SEM), X-ray diffractometer (XRD), Brunauer, Emmett, and Teller (BET) surface area analyzer, thermogravimetric analysis (TGA), zeta potential, and energy dispersive X-ray spectroscopy (EDS). The adsorption parameters of the selenium ions from water using raw CNTs and iron oxide impregnated carbon nanotubes (CNT-Fe2O3) were optimized. Total removal of 1 ppm Se ions from water was achieved when 25 mg of CNTs impregnated with 20 wt.% of iron oxide nanoparticles is used. Freundlich and Langmuir isotherm models were used to study the nature of the adsorption process. Pseudo-first and pseudo-second-order models were employed to study the kinetics of selenium ions adsorption onto the surface of iron oxide impregnated CNTs. Maximum adsorption capacity of the Fe2O3 impregnated CNTs, predicted by Langmuir isotherm model, was found to be 111 mg/g. This new finding might revolutionize the adsorption treatment process and application by introducing a new type of nanoadsorbent that has super adsorption capacity towards Se ions. PMID:28555093

Effects of phosphates on microstructure and bioactivity of micro-arc oxidized calcium phosphate coatings on Mg-Zn-Zr magnesium alloy.

PubMed

Pan, Y K; Chen, C Z; Wang, D G; Zhao, T G

2013-09-01

Calcium phosphate (CaP) coatings were prepared on Mg-Zn-Zr magnesium alloy by micro-arc oxidation (MAO) in electrolyte containing calcium acetate monohydrate (CH3COO)2Ca·H2O) and different phosphates (i.e. disodium hydrogen phosphate dodecahydrate (Na2HPO4·12H2O), sodium phosphate (Na3PO4·H2O) and sodium hexametaphosphate((NaPO3)6)). Scanning electron microscope (SEM), energy-dispersive X-ray spectrometry (EDS) and X-ray diffractometer (XRD) were employed to characterize the microstructure, elemental distribution and phase composition of the CaP coatings. Simulated body fluid (SBF) immersion test was used to evaluate the coating bioactivity and degradability. Systemic toxicity test was used to evaluate the coating biocompatibility. Fluoride ion selective electrode (ISE) was used to measure F(-) ions concentration during 30 days SBF immersion. The CaP coatings effectively reduced the corrosion rate and the surfaces of CaP coatings were covered by a new layer formed of numerous needle-like and scale-like apatites. The formation of these calcium phosphate apatites indicates that the coatings have excellent bioactivity. The coatings formed in (NaPO3)6-containging electrolyte exhibit thicker thickness, higher adhesive strength, slower degradation rate, better apatite-inducing ability and biocompatibility. Copyright © 2013 Elsevier B.V. All rights reserved.

Nondestructive method and apparatus for imaging grains in curved surfaces of polycrystalline articles

DOEpatents

Carpenter, Donald A.

1995-01-01

A nondestructive method, and associated apparatus, are provided for determining the grain flow of the grains in a convex curved, textured polycrystalline surface. The convex, curved surface of a polycrystalline article is aligned in a horizontal x-ray diffractometer and a monochromatic, converging x-ray beam is directed onto the curved surface of the polycrystalline article so that the converging x-ray beam is diffracted by crystallographic planes of the grains in the polycrystalline article. The diffracted x-ray beam is caused to pass through a set of horizontal, parallel slits to limit the height of the beam and thereafter. The linear intensity of the diffracted x-ray is measured, using a linear position sensitive proportional counter, as a function of position in a direction orthogonal to the counter so as to generate two dimensional data. An image of the grains in the curved surface of the polycrystalline article is provided based on the two-dimensional data.

Nondestructive method and apparatus for imaging grains in curved surfaces of polycrystalline articles

DOEpatents

Carpenter, D.A.

1995-05-23

A nondestructive method, and associated apparatus, are provided for determining the grain flow of the grains in a convex curved, textured polycrystalline surface. The convex, curved surface of a polycrystalline article is aligned in a horizontal x-ray diffractometer and a monochromatic, converging x-ray beam is directed onto the curved surface of the polycrystalline article so that the converging x-ray beam is diffracted by crystallographic planes of the grains in the polycrystalline article. The diffracted x-ray beam is caused to pass through a set of horizontal, parallel slits to limit the height of the beam and thereafter. The linear intensity of the diffracted x-ray is measured, using a linear position sensitive proportional counter, as a function of position in a direction orthogonal to the counter so as to generate two dimensional data. An image of the grains in the curved surface of the polycrystalline article is provided based on the two-dimensional data. 7 Figs.

Supercrystallization of KCl from solution irradiated by soft X-rays

NASA Astrophysics Data System (ADS)

Janavičius, A. J.; Rinkūnas, R.; Purlys, R.

2016-10-01

The X-rays influence on KCl crystallization in a saturated water solution has been investigated for the aim of comparing it with previously considered NaCl crystallization. The rate of crystallization has been measured in the drying drop in the solution activated by the irradiation. We have measured the influence of the irradiation time of the solution on the rates of KCl crystallization as well as the beginning of the crystallization processes on drying drops. For a longer irradiation time of the solution early crystallization in the drops occurs. A saturated water solution of KCl was irradiated with the diffractometer DRON-3M (Russian device) and this had a great influence on the two-step processes of crystallization. The ionization of the solution by soft X-rays can produce ions, metastable radicals in water, excited crystals' seeds and vacancies in growing crystals by Auger's effect. The X-rays generate a very fast crystallization in the drying drop.

New X-Ray Technique to Characterize Nanoscale Precipitates in Aged Aluminum Alloys

NASA Astrophysics Data System (ADS)

Sitdikov, V. D.; Murashkin, M. Yu.; Valiev, R. Z.

2017-10-01

This paper puts forward a new technique for measurement of x-ray patterns, which enables to solve the problem of identification and determination of precipitates (nanoscale phases) in metallic alloys of the matrix type. The minimum detection limit of precipitates in the matrix of the base material provided by this technique constitutes as little as 1%. The identification of precipitates in x-ray patterns and their analysis are implemented through a transmission mode with a larger radiation area, longer holding time and higher diffractometer resolution as compared to the conventional reflection mode. The presented technique has been successfully employed to identify and quantitatively describe precipitates formed in the Al alloy of the Al-Mg-Si system as a result of artificial aging. For the first time, the x-ray phase analysis has been used to identify and measure precipitates formed during the alloy artificial aging.

Investigation of Pb doping on electrical, structural and superconducting properties of YBa2-xPbxCu3O7-δ superconductors

NASA Astrophysics Data System (ADS)

Ezzatpour, S.; Sharifzadegan, L.; Sarvari, F.; Sedghi, H.

2018-06-01

In this study the high temperature superconductor YBa2-xPbxCu3O7-δ with doping x = ,0.05,0.1,0.15 were prepared by the standard solid-state reaction method. The effect of Pb substitution on Ba site of YBCO superconducting system, structural, electrical and superconducting properties of Y-based superconductor has been investigated. The measurements of dc resisitivity were performed on all samples with four-probe method using low frequency/lowAC current (4 mA) . The superconducting temperature, Tc, were determined from the resistivity versus temperature (R-T) curves. Results show that Pb doping reduced the cirtical temperature(Tc) and superconductivity properties of our samples. The maximum and the minimum Tc were observed for the samples with x = 0.15 and x = 0.1 respectively. The structure and phase purity of samples were examined by the X-ray powder diffraction technique (XRD) performed by means of D8 Advance Bruker diffractometer with Cu kα radiation. The grain morphology of surface of the samples was analyzed by sacanning electron microscopy (SEM). XRD patterns of polycrystalline materials of composition YBa2-xPbxCu3O7-δ revealed that all prepared samples are orthorhombic. All of the peaks of YBCO and YBa2-xPbxCu3O7-δ have been used for the estimation of volume fractions of the phases and ignored the void peaks.

Study on effect of plasma surface treatments for diamond deposition by DC arc plasmatron.

PubMed

Kang, In-Je; Joa, Sang-Beom; Lee, Heon-Ju

2013-11-01

To improve the thermal conductivity and wear resistance of ceramic materials in the field of renewable energy technologies, diamond coating by plasma processing has been carried out in recent years. This study's goal is to improve diamond deposition on Al2O3 ceramic substrates by plasma surface treatments. Before diamond deposition was carried out in a vacuum, plasma surface treatments using Ar gas were conducted to improve conditions for deposition. We also conducted plasma processing for diamond deposition on Al2O3 ceramic substrates using a DC arc Plasmatron. The Al2O3 ceramic substrates with diamond film (5 x 15 mm2), were investigated by SEM (Scanning Electron Microscopy), AFM (Atomic Force Microscopy) and XRD (X-ray Diffractometer). Then, the C-H stretching of synthetic diamond films by FTIR (Fourier Transform Infrared Spectroscopy) was studied. We identified nanocrystalline diamond films on the Al2O3 ceramic substrates. The results showed us that the deposition rate of diamond films was 2.3 microm/h after plasma surface treatments. Comparing the above result with untreated ceramic substrates, the deposition rate improved with the surface roughness of the deposited diamond films.

Development of Thin Films as Potential Structural Cathodes to Enable Multifunctional Energy-Storage Structural Composite Batteries for the U.S. Army’s Future Force

DTIC Science & Technology

2011-09-01

glancing angle X - ray diffraction (GAXRD), atomic force microscopy (AFM), scanning electron microscopy (SEM), and electrochemical...Emission SEM FWHM full width at half maximum GAXRD glancing angle X - ray diffraction H3COCH2CH2OH 2-methoxyethanol LiMn2O4 lithium manganese oxide...were characterized by scanning electron microscopy (SEM), X - ray diffraction (XRD), and atomic force microscopy (AFM). In addition,

Preparation and characterization of flame retardant n-hexadecane/silicon dioxide composites as thermal energy storage materials.

PubMed

Fang, Guiyin; Li, Hui; Chen, Zhi; Liu, Xu

2010-09-15

Flame retardant n-hexadecane/silicon dioxide (SiO(2)) composites as thermal energy storage materials were prepared using sol-gel methods. In the composites, n-hexadecane was used as the phase change material for thermal energy storage, and SiO(2) acted as the supporting material that is fire resistant. In order to further improve flame retardant property of the composites, the expanded graphite (EG) was added in the composites. Fourier transformation infrared spectroscope (FT-IR), X-ray diffractometer (XRD) and scanning electronic microscope (SEM) were used to determine chemical structure, crystalloid phase and microstructure of flame retardant n-hexadecane/SiO(2) composites, respectively. The thermal properties and thermal stability were investigated by a differential scanning calorimeter (DSC) and a thermogravimetric analysis apparatus (TGA), respectively. The SEM results showed that the n-hexadecane was well dispersed in the porous network of the SiO(2). The DSC results indicated that the melting and solidifying latent heats of the composites are 147.58 and 145.10 kJ/kg when the mass percentage of the n-hexadecane in the composites is 73.3%. The TGA results showed that the loading of the EG increased the charred residue amount of the composites at 700 degrees C, contributing to the improved thermal stability of the composites. It was observed from SEM photographs that the homogeneous and compact charred residue structure after combustion improved the flammability of the composites. Copyright 2010 Elsevier B.V. All rights reserved.

Single Crystal Diffractometry

NASA Astrophysics Data System (ADS)

Arndt, U. W.; Willis, B. T. M.

2009-06-01

Preface; Acknowledgements; Part I. Introduction; Part II. Diffraction Geometry; Part III. The Design of Diffractometers; Part IV. Detectors; Part V. Electronic Circuits; Part VI. The Production of the Primary Beam (X-rays); Part VII. The Production of the Primary Beam (Neutrons); Part VIII. The Background; Part IX. Systematic Errors in Measuring Relative Integrated Intensities; Part X. Procedure for Measuring Integrated Intensities; Part XI. Derivation and Accuracy of Structure Factors; Part XII. Computer Programs and On-line Control; Appendix; References; Index.

Characterization of calcium crystals in Abelia using x-ray diffraction and electron microscopes

USDA-ARS?s Scientific Manuscript database

Localization, chemical composition, and morphology of calcium crystals in leaves and stems of Abelia mosanensis and A. ×grandiflora were analyzed with a variable pressure scanning electron microscope (VP-SEM) equipped with an X-ray diffraction system, low temperature SEM (LT-SEM) and a transmission ...

Electronic Properties and Device Applications of III-V Compound Semiconductor Native Oxides

DTIC Science & Technology

2006-03-02

MRD X-ray diffractometer with CuKa as the radiation source. The doping level in GaAs was meassured by electrochemical voltage (ECV) using an Accent... hard to prevent the gate metal from overlapping the mesa edge thus creating a parasitic leakage path to the channel42. To reduce the gate leakage

On high-resolution reciprocal-space mapping with a triple-crystal diffractometer for high-energy X-rays.

PubMed

Liss, K D; Royer, A; Tschentscher, T; Suortti, P; Williams, A P

1998-03-01

High-energy X-rav diffraction by means of triple-crystal techniques is a powerful tool for investigating dislocations and strain in bulk materials. Radiation with an energy typically higher than 80 keV combines the advantage of low attenuation with high resolution at large momentum transfers. The triple-crystal diffractometer at the High Energy Beamline of the European Synchrotron Radiation Facility is described. It is shown how the transverse and longitudinal resolution depend on the choice of the crystal reflection, and how the orientation of a reciprocal-lattice distortion in an investigated sample towards the resolution element of the instrument can play an important role. This effect is demonstrated on a single crystal of silicon where a layer of macro pores reveals satellites around the Bragg reflection. The resulting longitudinal distortion can be investigated using the high transverse resolution of the instrument when choosing an appropriate reflection.

Symposium N: Materials and Devices for Thermal-to-Electric Energy Conversion

DTIC Science & Technology

2010-08-24

X - ray diffraction, transmission electron microscopy, scanning electron microscopy, and dynamic light scattering. Thermal conductivity measurements...SEM), X - ray diffraction (XRD) measurements as well as Raman spectroscopy. The results from these techniques indicate a clear modification...was examined by using scanning electron microscope (SEM; HITACHI S-4500 model) attached with an energy dispersive x - ray spectroscopy. The electrical

Neutron diffraction study of aqueous Laponite suspensions at the NIMROD diffractometer.

PubMed

Tudisca, V; Bruni, F; Scoppola, E; Angelini, R; Ruzicka, B; Zulian, L; Soper, A K; Ricci, M A

2014-09-01

The process of dynamical arrest, leading to formation of different arrested states such as glasses and gels, along with the closely related process of aging, is central for both basic research and technology. Here we report on a study of the time-dependent structural evolution of two aqueous Laponite clay suspensions at different weight concentrations. Neutron diffraction experiments have been performed with the near and intermediate range order diffractometer (NIMROD) that allows studies of the structure of liquids and disordered materials over a continuous length scale ranging from 1 to 300 Å, i.e., from the atomistic to the mesoscopic scales. NIMROD is presently a unique diffractometer, bridging the length scales traditionally investigated by small angle neutron scattering or small angle x-ray scattering with that accessible by traditional diffractometers for liquids. Interestingly, we have unveiled a signature of aging of both suspensions in the length scale region of NIMROD. This phenomenon, ascribed to sporadic contacts between Laponite platelets at long times, has been observed with the sample arrested as gel or as repulsive glass. Moreover, water molecules within the layers closest to Laponite platelets surface show orientational and translational order, which maps into the crystalline structure of Laponite.

Monodispersed fabrication and dielectric studies on ethylenediamine passivated α-manganese dioxide nanorods

DOE Office of Scientific and Technical Information (OSTI.GOV)

Joseph, A. Martin; Kumar, R. Thilak, E-mail: manojthilak@yahoo.com

2016-09-15

Highlights: • Monodispersed ethylenediamine (EDA) passivated α-MnO{sub 2} nanorods were fabricated by inexpensive wet chemical method. • FTIR analysis indicated that surface passivation is strongly influenced by the introduction of the organic ligand. • XRD and HR-SEM revealed the structure and morphology of the fabricated α-MnO{sub 2} nanorods with an average size of about 40 × 200 nm. • Dielectric studies pointed out that the fabricated α-MnO{sub 2} is semiconducting in nature with resistivity, ρ = 1.46 to 5.76 × 10{sup 3} Ωcm. • The optical energy gap for the fabricated α-MnO{sub 2} nanorods is found to be around 1.37more » eV. - Abstract: In this present work, pure α-MnO{sub 2} nanorods were fabricated by the reduction of 0.2 m/L of KMnO{sub 4} with 0.2 m/L of Na{sub 2}S{sub 2}O{sub 3}·5H{sub 2}O and by passivating with the organic ligand Ethylenediamine (EDA). The structural, functional, morphological and chemical composition of the nanorods were investigated by X-Ray Diffractometer (XRD), Fourier Transform Infrared Spectrometer (FTIR), High Resolution Scanning Electron Microscope (HR-SEM) and Energy Dispersive X-Ray Spectrometry (EDX). The XRD analysis indicated high crystalline nature of the product and FTIR confirmed the contribution of the organic ligand in surface passivation. HR-SEM image revealed the morphology of the α-MnO{sub 2} nanorods with an average size of about 40 × 200 nm. EDX confirmed the presence of Mn and O in the material. UV–visible spectrophotometery was used to determine the absorption behavior of the nanorods and an indirect band gap of 1.37 eV was acquired by Taucplot. Dielectric studies were carried out using Broadband Dielectric Spectrometer(BDS) and the resistivity was found to be around the semiconductor range (ρ = 1.46 to 5.76 × 10{sup 3} Ωcm).« less

Electrochemical fabrication of SrTiO3 nanowires with nanoporous alumina template.

PubMed

Kang, Jinwook; Ryu, Jaemin; Ko, Eunseong; Tak, Yongsug

2007-11-01

Strontium titanate nanowires were electrochemically synthesized with nanoporous alumina template. Both chemical and electrical variables such as electrolyte pH, temperature, and current waveform were modulated to investigate the synthesis process of SrTiO3 nanowires. Superimposed cathodic pulse and diffusion time accelerated the growth of SrTiO3 nanowires, which suggested that the concentration of H+ and Sr2+ ion inside alumina template had a strong influence on the formation of SrTiO3 nanowires. Morphology and crystallinity of SrTiO3 nanowires were investigated with scanning electron microscope, X-ray diffractometer and energy dispersive X-ray spectroscopy.

The preparation and hydrogen brittleness resistance of Pd71.5Cu12Si16.5 metallic glass ribbons

NASA Astrophysics Data System (ADS)

Du, Xiaoqing; Ye, Xiaoqiu; Ren, Qingbo

2017-12-01

Pd71.5Cu12Si16.5 metallic glass ribbons as wide as 10mm were prepared by splat quenching. Structure was identified with X-ray diffraction (XRD) spectrums from the conventional X-ray diffractometer and also short wavelength X-ray stress analyzer. The results confirm fully amorphous structure of the ribbons. Multiple H2 adsorption and desorption cycles under a pressure of 100kPa were carried out in the metallic glass ribbon and also pure palladium membrane for comparison. The former didn’t show any cracks after more than 10 cycles, and thermal desorption spectroscopy (TDS) measurement confirms that hydrogen was adsorbed abundantly in the metallic glass ribbon. Pd71.5Cu12Si16.5 metallic glass ribbons demonstrate excellent hydrogen brittleness resistance.

Investigation of microstructural and physical characteristics of nano composite tin oxide-doped Al3+ in Zn2+ based composite coating by DAECD technique

NASA Astrophysics Data System (ADS)

Anawe, P. A. L.; Fayomi, O. S. I.; Popoola, A. P. I.

In other to overcome the devastating deterioration of mild steel in service, Zn-based embedded Al/SnO2 composite coatings have been considered as reinforcing alternative replacements to the more traditional deposition for improved surface properties by using Dual Anode Electrolytic Co-deposition (DAECD) technique from chloride bath. The structural characterization of the starting materials and deposited coating are evaluated using scanning electron microscopy (SEM), equipped with energy dispersive X-ray spectroscopy (EDX) elemental analysis and atomic force microscope (AFM). The hardness behaviour, wear and intermetallic distribution was examined by diamond based microhardness tester, CETR reciprocating sliding test rig and X-ray diffractometer (XRD) respectively. The corrosion properties of the developed coating were examined in 3.5% NaCl. The microstructure of the deposited sample obtained at 7% SnO2, revealed fine-grains deposit of the Al/SnO2 on the mild steel surface. The results showed that the Al/SnO2 strengthening alloy plays a significant role in impelling the wear and corrosion behaviour of Zn-Al/SnO2 coatings in an aggressive saline environment. Interestingly Zn-30Al-7Sn-chloride showed the highest wear and improved corrosion resistance due to Al/SnO2 oxide passive film that forms during anodic polarization. This work established that co-deposition of mild steel with Al/SnO2 is auspicious in increasing the anti-wear and corrosion progression.

Preparation of Er3+:Y3Al5O12/WO3-KNbO3 composite and application in treatment of methamphetamine under ultrasonic irradiation.

PubMed

Zhang, Hongbo; Huang, Yingying; Li, Guanshu; Wang, Guowei; Fang, Dawei; Song, Youtao; Wang, Jun

2017-03-01

Er 3+ :Y 3 Al 5 O 12 /WO 3 -KNbO 3 composite powder as an effective sonocatalyst was prepared via collosol-gelling-hydrothermal and high-temperature calcination methods. The textures of materials were observed by X-ray diffractometer (XRD), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). In order to estimate the sonocatalytic activity of Er 3+ :Y 3 Al 5 O 12 /WO 3 -KNbO 3 composite powder, the sonocatalytic degradation of methamphetamine (MAPA) was performed. Furthermore, the influences of mass ratio of WO 3 and KNbO 3 , ultrasonic irradiation time, catalyst addition amount, initial methamphetamine (MAPA) concentration and used times on the sonocatalytic degradation of methamphetamine (MAPA) caused by Er 3+ :Y 3 Al 5 O 12 /WO 3 -KNbO 3 composite powder were investigated by using gas chromatography. Under optimal conditions of 1.00g/L Er 3+ :Y 3 Al 5 O 12 /WO 3 -KNbO 3 addition amount and 10.00mg/L methamphetamine (MAPA) initial concentration, 68% of methamphetamine (MAPA) could be removed after 150min ultrasonic irradiation. The experimental results showed that the Er 3+ :Y 3 Al 5 O 12 /WO 3 -KNbO 3 as sonocatalyst displayed an excellent sonocatalytic activity in degradation of methamphetamine (MAPA) under ultrasonic irradiation. Copyright © 2016 Elsevier B.V. All rights reserved.

Recovery of nickel and cobalt as MHP from limonitic ore leaching solution: Kinetics analysis and precipitate characterization

NASA Astrophysics Data System (ADS)

Safitri, Nina; Mubarok, M. Zaki; Winarko, Ronny; Tanlega, Zela

2018-05-01

In the present study, precipitation of nickel and cobalt as mixed hydroxide precipitate (MHP) from pregnant leach solution of nickel limonite ore from Soroako after iron removal stage was carried out. A series of MHP precipitation experiments was conducted by using MgO slurry as neutralizing agent and the effects of pH, temperature, duration of precipitation and the addition of MHP seed on the precipitation behavior of nickel, cobalt, as well as iron and manganese was studied. Characterization of MHP product was performed by particle size analyzer (PSA) as well as X-Ray Fluorescence (XRF), X-Ray Diffractometer (XRD) and Scanning Electron Microscope (SEM) analyses. Kinetics analysis was made by using differential-integral method for the rate of homogenous reaction. Precipitation at pH 7, temperature 50°C for 30 minute, without seed addition resulted in nickel and cobalt recoveries of 82.8% and 92%, respectively with co-precipitated iron and manganese of 70% and 24.2%, respectively. The seed addition increases nickel and cobalt precipitations significantly to 99.9% and 99.1%, respectively. However, the addition of seed into led to a significant increase of manganese co-precipitation from 24.2% without seed addition to 39.5% at the addition of 1 g seed per 200 mL of PLS. Kinetics analysis revealed that Ni precipitation to form MHP follows the second-order reaction kinetics with activation energy of 94.6 kJ/mol.

Calculation of effective penetration depth in X-ray diffraction for pharmaceutical solids.

PubMed

Liu, Jodi; Saw, Robert E; Kiang, Y-H

2010-09-01

The use of the glancing incidence X-ray diffraction configuration to depth profile surface phase transformations is of interest to pharmaceutical scientists. The Parratt equation has been used to depth profile phase changes in pharmaceutical compacts. However, it was derived to calculate 1/e penetration at glancing incident angles slightly below the critical angle of condensed matter and is, therefore, applicable to surface studies of materials such as single crystalline nanorods and metal thin films. When the depth of interest is 50-200 microm into the surface, which is typical for pharmaceutical solids, the 1/e penetration depth, or skin depth, can be directly calculated from an exponential absorption law without utilizing the Parratt equation. In this work, we developed a more relevant method to define X-ray penetration depth based on the signal detection limits of the X-ray diffractometer. Our definition of effective penetration depth was empirically verified using bilayer compacts of varying known thicknesses of mannitol and lactose.

Observation of Structure of Surfaces and Interfaces by Synchrotron X-ray Diffraction: Atomic-Scale Imaging and Time-Resolved Measurements

NASA Astrophysics Data System (ADS)

Wakabayashi, Yusuke; Shirasawa, Tetsuroh; Voegeli, Wolfgang; Takahashi, Toshio

2018-06-01

The recent developments in synchrotron optics, X-ray detectors, and data analysis algorithms have enhanced the capability of the surface X-ray diffraction technique. This technique has been used to clarify the atomic arrangement around surfaces in a non-contact and nondestructive manner. An overview of surface X-ray diffraction, from the historical development to recent topics, is presented. In the early stage of this technique, surface reconstructions of simple semiconductors or metals were studied. Currently, the surface or interface structures of complicated functional materials are examined with sub-Å resolution. As examples, the surface structure determination of organic semiconductors and of a one-dimensional structure on silicon are presented. A new frontier is time-resolved interfacial structure analysis. A recent observation of the structure and dynamics of the electric double layer of ionic liquids, and an investigation of the structural evolution in the wettability transition on a TiO2 surface that utilizes a newly designed time-resolved surface diffractometer, are presented.

Study on Plastic Deformation Characteristics of Shot Peening of Ni-Based Superalloy GH4079

NASA Astrophysics Data System (ADS)

Zhong, L. Q.; Liang, Y. L.; Hu, H.

2017-09-01

In this paper, the X-ray stress diffractometer, surface roughness tester, field emission scanning electron microscope(SEM), dynamic ultra-small microhardness tester were used to measure the surface residual stress and roughness, topography and surface hardness changes of GH4079 superalloy, which was processed by metallographic grinding, turning, metallographic grinding +shot peening and turning + shot peening. Analysized the effects of shot peening parameters on shot peening plastic deformation features; and the effects of the surface state before shot peening on shot peening plastic deformation characteristics. Results show that: the surface residual compressive stress, surface roughness and surface hardness of GH4079 superalloy were increased by shot peening, in addition, the increment of the surface residual compressive stress, surface roughness and surface hardness induced by shot peening increased with increasing shot peening intensity, shot peening time, shot peening pressure and shot hardness, but harden layer depth was not affected considerably. The more plastic deformation degree of before shot peening surface state, the less increment of the surface residual compressive stress, surface roughness and surface hardness induced by shot peening.

Preparation of anti-adhesion surfaces on aluminium substrates of rubber plastic moulds using a coupling method of liquid plasma and electrochemical machining

NASA Astrophysics Data System (ADS)

Meng, Jianbing; Dong, Xiaojuan; Wei, Xiuting; Yin, Zhanmin

2014-03-01

Hard anti-adhesion surfaces, with low roughness and wear resistance, on aluminium substrates of rubber plastic moulds were fabricated via a new coupling method of liquid plasma and electrochemical machining. With the aid of liquid plasma thermal polishing and electrochemical anodic dissolution, micro/nano-scale binary structures were prepared as the base of the anti-adhesion surfaces. The anti-adhesion behaviours of the resulting aluminium surfaces were analysed by a surface roughness measuring instrument, a scanning electron microscope (SEM), a Fourier-transform infrared spectrophotometer (FTIR), an X-ray diffractometer (XRD), an optical contact angle meter, a digital Vickers micro-hardness (Hv) tester, and electronic universal testing. The results show that, after the liquid plasma and electrochemical machining, micro/nano-scale binary structures composed of micro-scale pits and nano-scale elongated boss structures were present on the sample surfaces. As a result, the anti-adhesion surfaces fabricated by the above coupling method have good anti-adhesion properties, better wear resistance and lower roughness.

[Characteristics and mechanism of sodium removal by the synergistic action of flue gas and waste solid].

PubMed

Yi, Yuan-Rong; Han, Min-Fang

2012-07-01

The carbon dioxide (CO2) in flue gas was used to remove the sodium in the red mud (RM) , a kind of alkaline solid waste generated during alumina production. The reaction characteristics and mechanism of sodium removal by the synergistic action of CO2 and RM were studied with different medium pH, reaction time and temperature. It was demonstrated that the remove of sodium by RM was actually the result of the synergistic action of sodium-based solid waste in RM with the CO2-H2O and OH(-)-CO2 systems. The sodium removal efficiency was correlated with pH, reaction temperature and time. The characteristics of RM before and after sodium removal were analyzed using X-ray diffractometer (XRD) and scanning electron microscope (SEM), and the results showed that the alkaline materials in the red mud reacted with CO2 and the sodium content in solid phases decreased significantly after reaction. The sodium removal efficiency could reach up to 70% with scientific procedure. The results of this research will offer an efficient way for low-cost sodium removal.

Preparation of anti-adhesion surfaces on aluminium substrates of rubber plastic moulds using a coupling method of liquid plasma and electrochemical machining

DOE Office of Scientific and Technical Information (OSTI.GOV)

Meng, Jianbing, E-mail: jianbingmeng@126.com; Dong, Xiaojuan; Wei, Xiuting

Hard anti-adhesion surfaces, with low roughness and wear resistance, on aluminium substrates of rubber plastic moulds were fabricated via a new coupling method of liquid plasma and electrochemical machining. With the aid of liquid plasma thermal polishing and electrochemical anodic dissolution, micro/nano-scale binary structures were prepared as the base of the anti-adhesion surfaces. The anti-adhesion behaviours of the resulting aluminium surfaces were analysed by a surface roughness measuring instrument, a scanning electron microscope (SEM), a Fourier-transform infrared spectrophotometer (FTIR), an X-ray diffractometer (XRD), an optical contact angle meter, a digital Vickers micro-hardness (Hv) tester, and electronic universal testing. The resultsmore » show that, after the liquid plasma and electrochemical machining, micro/nano-scale binary structures composed of micro-scale pits and nano-scale elongated boss structures were present on the sample surfaces. As a result, the anti-adhesion surfaces fabricated by the above coupling method have good anti-adhesion properties, better wear resistance and lower roughness.« less

Solution-processed nanocrystalline PbS on paper substrate with pencil traced electrodes as visible photodetector

NASA Astrophysics Data System (ADS)

Vankhade, Dhaval; Chaudhuri, Tapas K.

2018-04-01

Paper-based PbS photodetector sensitive in the visible spectrum is reported. Nanocrystalline PbS-on-paper devices are fabricated by a spin coating method on white paper (300 GSM) from a methanolic precursor solution. Photodetector cells of gap 0.2 cm and length 0.5 cm are prepared by drawing contacts by monolithic cretacolor 8B pencil. X-ray diffractometer confirmed the deposition of nanocrystalline PbS films with 14 nm crystallites. The SEM illustrated the uniform coating of nanocrystalline PbS thin films on cellulose fibres of papers having an average thickness of fibres are 10 µm. The linear J-V characteristics in dark and under illumination of light using graphite trace on nanocrystalline PbS-on-paper shows good ohmic contact. The resistivity of pencil trace is 30 Ω.cm. Spectral response measurements of photodetector reveal the excellent sensitivity from 400 to 700 nm with a peak at 550 nm. The best responsivity anddetectivity are 0.7 A/W and 1.4 × 1012 Jones respectively. These paper-based low-cost photodetectors devices have fast photoresponse and recovery without baseline deviation.

FABRICATION AND PHOTOCATALYTIC PROPERTIES OF TiO2 NANOFILMS CO-DOPED WITH Fe3+ AND Bi3+ IONS

NASA Astrophysics Data System (ADS)

Gao, Qiongzhi; Liu, Xin; Liu, Wei; Liu, Fang; Fang, Yueping; Zhang, Shiying; Zhou, Wuyi

2016-12-01

In this work, the titanium dioxide (TiO2) nanofilms co-doped with Fe3+ and Bi3+ ions were successfully fabricated by the sol-gel method with dip-coating process. Methylene blue was used as the target degradation chemical to study the photocatalytic properties affected by different doping contents of Fe3+ and Bi3+ ions. The samples were characterized by X-ray diffractometer (XRD), scanning electron microscopy (SEM) and infrared (IR) spectroscopy. The results indicated that both pure TiO2 nanofilms and single-doped samples possessed the photocatalytic activity in degradation of methylene blue. However, when the nanofilms co-doped with Fe3+ and Bi3+ ions were fabricated at the molar ratio of 3:1 (Fe3+:Bi3+), they exhibited the best photocatalytic activity after the heat treatment at 500∘C for 2h. The wettability property test indicated that the TiO2 nanofilms co-doped with Fe3+ and Bi3+ ions in the molar ratio 3:1 owned an excellent hydrophilic property.

Parallel nano-assembling of a multifunctional GO/HapNP coating on ultrahigh-purity magnesium for biodegradable implants

NASA Astrophysics Data System (ADS)

Santos, C.; Piedade, C.; Uggowitzer, P. J.; Montemor, M. F.; Carmezim, M. J.

2015-08-01

This work reports the one-step fabrication of a novel coating on ultra high purity magnesium using a parallel nano assembling process. The multifunctional biodegradable surface was obtained by adding hydroxyapatite nanoparticles (HapNP) plus graphene oxide (GO). The coating was characterized by scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray diffractometer (XRD), micro-Raman spectroscopy. The thin phosphate coating (thickness of 1 μm) reveals a uniform coverage with cypress like structures. The incorporation of HapNP and GO promotes the hydrophilic behavior of the coating surface. The results revealed that the proposed coating can be used to tailor the surface properties such as wettability by adjusting the contents of HapNP and GO. The in vitro degradation rate of the coated magnesium suggests that the presence of HapNP and GO/HapNP in the phosphate coating decreased the current density compared to the single phosphate coating and uncoated magnesium. This study also reveals the HapNP/GO/phosphate coating induces apatite formation, showing suitable degradability that makes it a promising coating candidate for enhanced bone regeneration.

Precipitation behavior of σ phase in fusion zone of dissimilar stainless steel welds during multi-pass GTAW process

NASA Astrophysics Data System (ADS)

Hsieh, Chih-Chun; Chang, Tao-Chih; Lin, Dong-Yih; Chen, Ming-Che; Wu, Weite

2007-10-01

The purpose of this study is to investigate the precipitation characteristics of σ phase in the fusion zone of stainless steel welds at various welding passes during a tungsten are welding (GTAW) process. The morphology, quantity, and chemical composition of the δ-ferrite and σ phase were analyzed using optical microscopy (OM), a ferritscope (FS), a X-ray diffractometer (XRD), scanning electron microscopy (SEM), an electron probe micro-analyzer (EPMA), and a wavelength dispersive spectrometer (WDS), respectively. Massive δ-ferrite was observed in the fusion zone of the first pass welds during welding of dissimilar stainless steels. The σ phase precipitated at the inner δ-ferrite particles and decreased δ-ferrite content during the third pass welding. The σ and δ phases can be stabilized by Si element, which promoted the phase transformation of σ→ϱ+λ2 in the fusion zone of the third pass welds. It was found that the σ phase was a Fe-Cr-Si intermetallic compound found in the fusion zone of the third pass welds during multi-pass welding.

Characterization of Calcite Mineral Precipitation Process by EICP in Porous Media

NASA Astrophysics Data System (ADS)

Kim, D.; Mahabadi, N.; Hall, C.; Jang, J.; van Paassen, L. A.

2017-12-01

One of the most prevalent ground improvement techniques is injection of synthetic materials, such as cement grout or silicates into the pore space to create cementing bonds between soil particles. Besides these traditional ground improvement methods, several biological processes have been developed to improve soil properties. Enzyme induced carbonate precipitation (EICP) is a biological process in which urea hydrolyzes into ammonia and inorganic carbon, and promotes carbonate mineral precipitation. Different morphologies and patterns of calcite mineral precipitation, such as particle surface coating, pore filling, and soil particles bonding, have been observed in the previous studies. Most of the researches have detected precipitated minerals after the completion of the treatment using SEM (Scanning Electron Microscope) imaging and XRD (X-ray Diffractometer) structural analysis. In this research, an EICP reaction medium is injected into a microfluidic chip to observe the entire process of carbonate precipitation through several cycles of EICP treatment in the porous medium. Once the process of mineral precipitation is completed, water is injected into the microfluidic chip with different flow rates to evaluate the stability of carbonates during fluid flow injection.

Imaging connected porosity of crystalline rock by contrast agent-aided X-ray microtomography and scanning electron microscopy.

PubMed

Kuva, J; Sammaljärvi, J; Parkkonen, J; Siitari-Kauppi, M; Lehtonen, M; Turpeinen, T; Timonen, J; Voutilainen, M

2018-04-01

We set out to study connected porosity of crystalline rock using X-ray microtomography and scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDS) with caesium chloride as a contrast agent. Caesium is an important radionuclide regarding the final deposition of nuclear waste and also forms dense phases that can be readily distinguished by X-ray microtomography and SEM-EDS. Six samples from two sites, Olkiluoto (Finland) and Grimsel (Switzerland), where transport properties of crystalline rock are being studied in situ, were investigated using X-ray microtomography and SEM-EDS. The samples were imaged with X-ray microtomography, immersed in a saturated caesium chloride (CsCl) solution for 141, 249 and 365 days and imaged again with X-ray microtomography. CsCl inside the samples was successfully detected with X-ray microtomography and it had completely penetrated all six samples. SEM-EDS elemental mapping was used to study the location of caesium in the samples in detail with quantitative mineral information. Precipitated CsCl was found in the connected pore space in Olkiluoto veined gneiss and in lesser amounts in Grimsel granodiorite. Only a very small amount of precipitated CsCl was observed in the Grimsel granodiorite samples. In Olkiluoto veined gneiss caesium was found in pinitised areas of cordierite grains. In the pinitised areas caesium was found in notable excess compared to chloride, possibly due to the combination of small pore size and negatively charged surfaces. In addition, elevated concentrations of caesium were found in kaolinite and sphalerite phases. The findings concerning the location of CsCl were congruent with X-ray microtomography. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.

Microstructure and Properties of DCP-Derived W-ZrC Composite Using Nontoxic Sodium Alginate to Fabricate WC Preform

NASA Astrophysics Data System (ADS)

Najafzadeh Khoee, Ali Asghar; Habibolahzadeh, Ali; Qods, Fathallah; Baharvandi, Hamidreza

2015-04-01

In the present work, tungsten carbide (WC) preforms were fabricated by gel-casting process, using different nontoxic Na-alginate to tertiary calcium phosphate ratios and different loadings of WC powder in the initial slurries. The gel-cast green bodies were dried and pre-sintered at 1723 K for 4 h and then reactively infiltrated by molten Zr2Cu at 1623 K for 0.5 h, to produce W-ZrC composite via displacive compensation of porosity process. The phases, microstructures, and mechanical properties of the preforms and the W-ZrC composites were investigated by Fourier transform infrared spectroscope, x-ray diffractometer (XRD), scanning electron microscope (SEM), image analyzer, and universal mechanical testing machine. XRD results, SEM micrographs, and elemental maps indicated uniform distribution of phases (W and ZrC) and elements (W, Zr, and C). Flexural strengths and hardness of the fabricated composites were in the ranges of 429-460 MPa and 7.5-9.5 GPa, respectively. Fractography studies revealed two types of dimple rupture and cleavage fracture modes in different composite samples. The W-ZrC composite was ablated by an oxyacetylene flame for 60 s. The mean value of mass and linear ablation rates of the composite were 2.1 ± 0.1 mg/s and 3.6 ± 0.5 µm/s, respectively.

Characterization of Polycapillary Optics in a TES Microcalorimeter EDS System Installed on an SEM

NASA Astrophysics Data System (ADS)

Takano, A.; Maehata, K.; Iyomoto, N.; Yasuda, K.; Maeno, H.; Shiiyama, K.; Tanaka, K.

2016-08-01

Energy-dispersive spectroscopic measurements are performed using a superconducting transition-edge sensor (TES) microcalorimeter mounted on a scanning electron microscope (SEM) for advanced research at Kyushu University. Because the sensitive area of the TES microcalorimeter is about 0.02~mm2, polycapillary optics is used to collect the X-rays emitted by the SEM specimen on the TES microcalorimeter. The X-ray transmission efficiency of the polycapillary optics is obtained by analyzing the X-ray energy spectra measured by the TES microcalorimeter. The obtained transmission efficiency of the polycapillary optics is reproduced by the calculated results of the simulation.

Solid state parameters, structure elucidation, High Resolution X-Ray Diffraction (HRXRD), phase matching, thermal and impedance analysis on L-Proline trichloroacetate (L-PTCA) NLO single crystals.

PubMed

Kalaiselvi, P; Raj, S Alfred Cecil; Jagannathan, K; Vijayan, N; Bhagavannarayana, G; Kalainathan, S

2014-11-11

Nonlinear optical single crystal of L-Proline trichloroacetate (L-PTCA) was successfully grown by Slow Evaporation Solution Technique (SEST). The grown crystals were subjected to single crystal X-ray diffraction analysis to confirm the structure. From the single crystal XRD data, solid state parameters were determined for the grown crystal. The crystalline perfection has been evaluated using high resolution X-ray diffractometer. The frequencies of various functional groups were identified from FTIR spectral analysis. The percentage of transmittance was obtained from UV Visible spectral analysis. TGA-DSC measurements indicate the thermal stability of the crystal. The dielectric constant, dielectric loss and ac conductivity were measured by the impedance analyzer. The DC conductivity was calculated by the cole-cole plot method. Copyright © 2014 Elsevier B.V. All rights reserved.

X-ray investigations related to the shock history of the Shergotty achondrite

NASA Technical Reports Server (NTRS)

Horz, F.; Hanss, R.; Serna, C.

1986-01-01

The shock stress suffered by naturally shocked materials from the Shergotty achondrite was studied using X-ray diffraction techniques and experimentally shocked augite and enstatite as standards. The Shergotty pyroxenes revealed the formation of continuous diffraction rings, line broadening, preferred orientation of small scale diffraction domains, and other evidence of substantial lattice disorders. As disclosed by the application of Debye-Scherrer techniques, they are hybrids between single crystals and fine-grained random powders. The pyroxene lattice is very resistant to shock damage on smaller scales. While measurable lattice disaggregation and progressive fragmentation occur below 25 GPa, little additional damage is suffered from application of pressures between 30 to 60 GPa, making pressure calibration of naturally shocked pyroxenes via X-ray methods difficult. Powder diffractometer scans on pure maskelynite fractions of Shergotty revealed small amounts of still coherently diffracting plagioclase, which may contribute to the high refractive indices of the diaplectic feldspar glasses of Shergotty.

Mineralogical Changes in a Predominantly Fluviolacustrine Succession at Gale Crater, Mars

NASA Technical Reports Server (NTRS)

Rampe, E. B.; Ming, D. W.; Grotzinger. J. P.; Bristow, T. F.; Blake, D. F.; Vaniman, D. T.; Chipera, S. J.; Gellert, R.; Morris, R. V.; Morrison, S. M.

2017-01-01

The Mars Science Laboratory Curiosity rover landed in Gale crater in August 2012 to investigate the strata of lower Aeolis Mons (i.e., Mount Sharp) and characterize their depositional and diagenetic environments. Visible/short-wave infrared spectra from orbit of these strata show variations in phyllosilicate, sulfate, and Fe-oxide minerals, suggesting these units record environmental changes that occurred during the early Hesperian. Curiosity has traversed over 15 km and has climbed through Approx. 200 m of stratigraphic section, made up of predominantly fluviolacustrine (i.e., the Bradbury group and the Murray formation) and aeolian (i.e., the Stimson formation) units. Multiple geochemical and mineralogical instruments are onboard Curiosity to study these ancient rocks, including the Chemistry and Mineralogy (CheMin) instrument, which is an X-ray diffractometer (XRD) and X-ray fluorescence spectrometer, and the Alpha Particle X-ray Spectrometer (APXS).

Room Temperature Elastic Moduli and Vickers Hardness of Hot-Pressed LLZO Cubic Garnet

DTIC Science & Technology

2012-01-01

polishing compounds, Leco, St. Joseph, MI). X - ray diffraction and scanning electron microscopy (SEM) The microstructure of the hot-pressed specimens...was examined on uncoated fracture surfaces by SEM with an accelerating voltage of 1 and 3 kV. Phase purity was evaluated from X - ray diffraction data...the micro- structure appeared to be homogenous for the two hot- pressed LLZO specimens included in this study (Fig. 1). X - ray diffraction confirmed that

Laboratory and In-Flight In-Situ X-ray Imaging and Scattering Facility for Materials, Biotechnology and Life Sciences

NASA Technical Reports Server (NTRS)

2003-01-01

We propose a multifunctional X-ray facility for the Materials, Biotechnology and Life Sciences Programs to visualize formation and behavior dynamics of materials, biomaterials, and living organisms, tissues and cells. The facility will combine X-ray topography, phase micro-imaging and scattering capabilities with sample units installed on the goniometer. This should allow, for the first time, to monitor under well defined conditions, in situ, in real time: creation of imperfections during growth of semiconductors, metal, dielectric and biomacromolecular crystals and films, high-precision diffraction from crystals within a wide range of temperatures and vapor, melt, solution conditions, internal morphology and changes in living organisms, tissues and cells, diffraction on biominerals, nanotubes and particles, radiation damage, also under controlled formation/life conditions. The system will include an ultrabright X-ray source, X-ray mirror, monochromator, image-recording unit, detectors, and multipurpose diffractometer that fully accommodate and integrate furnaces and samples with other experimental environments. The easily adjustable laboratory and flight versions will allow monitoring processes under terrestrial and microgravity conditions. The flight version can be made available using a microsource combined with multilayer or capillary optics.

Standard Reference Material (SRM 1990) for Single Crystal Diffractometer Alignment

USGS Publications Warehouse

Wong-Ng, W.; Siegrist, T.; DeTitta, G.T.; Finger, L.W.; Evans, H.T.; Gabe, E.J.; Enright, G.D.; Armstrong, J.T.; Levenson, M.; Cook, L.P.; Hubbard, C.R.

2001-01-01

An international project was successfully completed which involved two major undertakings: (1) a round-robin to demonstrate the viability of the selected standard and (2) the certification of the lattice parameters of the SRM 1990, a Standard Reference Material?? for single crystal diffractometer alignment. This SRM is a set of ???3500 units of Cr-doped Al2O3, or ruby spheres [(0 420.011 mole fraction % Cr (expanded uncertainty)]. The round-robin consisted of determination of lattice parameters of a pair of crystals' the ruby sphere as a standard, and a zeolite reference to serve as an unknown. Fifty pairs of crystals were dispatched from Hauptman-Woodward Medical Research Institute to volunteers in x-ray laboratories world-wide. A total of 45 sets of data was received from 32 laboratories. The mean unit cell parameters of the ruby spheres was found to be a=4.7608 A?? ?? 0.0062 A??, and c=12.9979 A?? ?? 0.020 A?? (95 % intervals of the laboratory means). The source of errors of outlier data was identified. The SRM project involved the certification of lattice parameters using four well-aligned single crystal diffractometers at (Bell Laboratories) Lucent Technologies and at NRC of Canada (39 ruby spheres), the quantification of the Cr content using a combined microprobe and SEM/EDS technique, and the evaluation of the mosaicity of the ruby spheres using a double-crystal spectrometry method. A confirmation of the lattice parameters was also conducted using a Guinier-Ha??gg camera. Systematic corrections of thermal expansion and refraction corrections were applied. These rubies_ are rhombohedral, with space group R3c. The certified mean unit cell parameters are a=4.76080 ?? 0.00029 A??, and c=12 99568 A?? ?? 0.00087 A?? (expanded uncertainty). These certified lattice parameters fall well within the results of those obtained from the international round-robin study. The Guinier-Ha??gg transmission measurements on five samples of powdered rubies (a=4.7610 A?? ?? 0.0013 A??, and c=12.9954 A?? ?? 0.0034 A??) agreed well with the values obtained from the single crystal spheres.

Standard Reference Material (SRM 1990) For Single Crystal Diffractometer Alignment

PubMed Central

Wong-Ng, W.; Siegrist, T.; DeTitta, G. T.; Finger, L. W.; Evans, H. T.; Gabe, E. J.; Enright, G. D.; Armstrong, J. T.; Levenson, M.; Cook, L. P.; Hubbard, C. R.

2001-01-01

An international project was successfully completed which involved two major undertakings: (1) a round-robin to demonstrate the viability of the selected standard and (2) the certification of the lattice parameters of the SRM 1990, a Standard Reference Material® for single crystal diffractometer alignment. This SRM is a set of ≈3500 units of Cr-doped Al2O3, or ruby spheres [(0.420.011 mole fraction % Cr (expanded uncertainty)]. The round-robin consisted of determination of lattice parameters of a pair of crystals: the ruby sphere as a standard, and a zeolite reference to serve as an unknown. Fifty pairs of crystals were dispatched from Hauptman-Woodward Medical Research Institute to volunteers in x-ray laboratories world-wide. A total of 45 sets of data was received from 32 laboratories. The mean unit cell parameters of the ruby spheres was found to be a=4.7608 ű0.0062 Å, and c=12.9979 ű0.020 Å (95 % intervals of the laboratory means). The source of errors of outlier data was identified. The SRM project involved the certification of lattice parameters using four well-aligned single crystal diffractometers at (Bell Laboratories) Lucent Technologies and at NRC of Canada (39 ruby spheres), the quantification of the Cr content using a combined microprobe and SEM/EDS technique, and the evaluation of the mosaicity of the ruby spheres using a double-crystal spectrometry method. A confirmation of the lattice parameters was also conducted using a Guinier-Hägg camera. Systematic corrections of thermal expansion and refraction corrections were applied. These rubies– are rhombohedral, with space group R3¯c. The certified mean unit cell parameters are a=4.76080±0.00029 Å, and c=12.99568 ű0.00087 Å (expanded uncertainty). These certified lattice parameters fall well within the results of those obtained from the international round-robin study. The Guinier-Hägg transmission measurements on five samples of powdered rubies (a=4.7610 ű0.0013 Å, and c = 12.9954 ű0.0034 Å) agreed well with the values obtained from the single crystal spheres. PMID:27500067

Acquisition of an X-Ray Diffractometer with WAXS and SAXS for Materials Research

DTIC Science & Technology

2015-03-31

2. This ligand is known as a sensitizer for applications in dye -sensitized solar cells, and the presence of the amino groups could potentially...achieve different surface properties, thus making them excellent candidates for use as fillers in bio-based biodegradable composite materials...These CNCs are environmentally safe sustainable, biodegradable , carbon neutral, and have low environmental, health and safety risks. Figure 9 below

Toward in situ x-ray diffraction imaging at the nanometer scale

NASA Astrophysics Data System (ADS)

Zatsepin, Nadia A.; Dilanian, Ruben A.; Nikulin, Andrei Y.; Gable, Brian M.; Muddle, Barry C.; Sakata, Osami

2008-08-01

We present the results of preliminary investigations determining the sensitivity and applicability of a novel x-ray diffraction based nanoscale imaging technique, including simulations and experiments. The ultimate aim of this nascent technique is non-destructive, bulk-material characterization on the nanometer scale, involving three dimensional image reconstructions of embedded nanoparticles and in situ sample characterization. The approach is insensitive to x-ray coherence, making it applicable to synchrotron and laboratory hard x-ray sources, opening the possibility of unprecedented nanometer resolution with the latter. The technique is being developed with a focus on analyzing a technologically important light metal alloy, Al-xCu (where x is 2.0-5.0 %wt). The mono- and polycrystalline samples contain crystallographically oriented, weakly diffracting Al2Cu nanoprecipitates in a sparse, spatially random dispersion within the Al matrix. By employing a triple-axis diffractometer in the non-dispersive setup we collected two-dimensional reciprocal space maps of synchrotron x-rays diffracted from the Al2Cu nanoparticles. The intensity profiles of the diffraction peaks confirmed the sensitivity of the technique to the presence and orientation of the nanoparticles. This is a fundamental step towards in situ observation of such extremely sparse, weakly diffracting nanoprecipitates embedded in light metal alloys at early stages of their growth.

Experimental and theoretical investigation of the rocking curves measured for Mo K α X-ray characteristic lines in the double-crystal nondispersive scheme

NASA Astrophysics Data System (ADS)

Marchenkov, N. V.; Chukhovskii, F. N.; Blagov, A. E.

2015-03-01

The rocking curves (RCs) for Mo K α1 h Mo K α2 characteristic X-ray lines have been experimentally and theoretically studied in the nondispersive scheme of an X-ray double-crystal TPC-K diffractometer. The results of measurements and theoretical calculations of double-crystal RCs for characteristic X-rays from tubes with a molybdenum anode and different widths of slits show that a decrease in the slit width leads to an increase in the relative contribution of the Mo K α2-line RC in comparison with the intensity of the tails of the Mo K α1-line RC. It is shown that the second peak of the Mo K α2 line becomes increasingly pronounced in the tail of the Mo K α1-line RC with a decrease in the slit width. Two plane-parallel Si plates (input faces {110}, diffraction vector h <220>) were used as a monochromator crystal and a sample. The results of measuring double-crystal RCs are in good agreement with theoretical calculations.

Cryogenic coherent X-ray diffraction imaging of biological samples at SACLA: a correlative approach with cryo-electron and light microscopy.

PubMed

Takayama, Yuki; Yonekura, Koji

2016-03-01

Coherent X-ray diffraction imaging at cryogenic temperature (cryo-CXDI) allows the analysis of internal structures of unstained, non-crystalline, whole biological samples in micrometre to sub-micrometre dimensions. Targets include cells and cell organelles. This approach involves preparing frozen-hydrated samples under controlled humidity, transferring the samples to a cryo-stage inside a vacuum chamber of a diffractometer, and then exposing the samples to coherent X-rays. Since 2012, cryo-coherent diffraction imaging (CDI) experiments have been carried out with the X-ray free-electron laser (XFEL) at the SPring-8 Ångstrom Compact free-electron LAser (SACLA) facility in Japan. Complementary use of cryo-electron microscopy and/or light microscopy is highly beneficial for both pre-checking samples and studying the integrity or nature of the sample. This article reports the authors' experience in cryo-XFEL-CDI of biological cells and organelles at SACLA, and describes an attempt towards reliable and higher-resolution reconstructions, including signal enhancement with strong scatterers and Patterson-search phasing.

Size dependent structural and magnetic properties of Al substituted Co–Mg ferrites synthesized by the sol–gel auto-combustion method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ahmad, Imran, E-mail: imraan77@yahoo.com; Abbas, Tahir; Ziya, A.B.

2014-04-01

Highlights: • Well-crystalline Co{sub 0.7}Mg{sub 0.3}AlFeO{sub 4} nanoparticles with small grain size were obtained. • The approach is sol–gel auto-combustion technique for obtained nanoparticles. • The prepared Co{sub 0.7}Mg{sub 0.3}AlFeO{sub 4} ferrites are decent soft materials with low coercivity. • The minor decrease in lattice parameter with increase of temperature was observed. - Abstract: Single phased nanocrystalline Co{sub 0.7}Mg{sub 0.3}FeAlO{sub 4} ferrites having low coercivity were synthesized by the sol–gel auto-combustion route. The subsequent powder materials were sintered in a temperature range of 800–1200 °C for 2 h. The effects of sintering temperatures on the structure, morphology and magnetic propertiesmore » of the prepared soft magnetic material were studied. X-ray diffractometer (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), and magnetic property measurement system (MPMS) were used to characterize the samples. X-ray diffraction analysis confirmed a single-phase cubic spinel structure and ruled out the presence of impurities like hematite. The higher sintering temperatures have caused in enhanced mark of crystallinity and bigger average grain size of the nanocrystals. A slight decrease in lattice parameters was noticed with a rise of grain size. Magnetic measurements revealed that grain size increase led to a decrease in the coercivity and, in difference, an increase in the saturation magnetization.« less

Investigations of interatomic interaction in InAs-InAs1-xSbx heterostructures on a base of x-ray diffractometry

NASA Astrophysics Data System (ADS)

Babjuck, T. I.; Buntar, A. G.; Shevtchuk, L. S.

2001-06-01

Hetero-transitions on a base of InAs and AnSb compounds permitted to obtain cheap light diodes and detectors with the atmosphere maximal transparency region sensibility. There is assumed simultaneously, that the phon radiation in InAs-InAs1-xSbx is not large, which positively effects on receiver parameters. Changing the composition of InAs-InAs1- xSbx solution, one may obtain the structure with the width of forbidden zone of the want of 0.35 to 0,1 eV. There is developed the heterostructures crystalline lattice parameters determining method (for substrate and film) with the DRON-3M x-ray diffractometer. There was found the nonlinear dependence of the heterostructures lattice parameter on the composition. Investigations of interatomic interaction in dependence on composition and also on the forbidden zone width Eg(x) have show, that solid solutions InAs-InAs1- xSbx may be used for the obtaining of infra-red receiver.

Touch-free in situ investigation of ancient Egyptian pigments.

PubMed

Uda, M; Sassa, S; Taniguchi, K; Nomura, S; Yoshimura, S; Kondo, J; Iskander, N; Zaghloul, B

2000-06-01

Some of the pigments painted on the Funerary Stele of Amenemhat (ca. 2000 B.C.) exhibited at the Egyptian Museum, Cairo and on the walls of the Tomb of Userhat (ca. 1420 B.C.), a rock-cut tomb in Thebes, Egypt, were investigated in situ using both a convenient home-made hand-held type of X-ray diffractometer and a commercial X-ray fluorescence spectrometer in a complementary way under touch-free conditions. CaCO3.3MgCO3 (huntite) was found in the white-painted parts of these two ancient monuments. An arsenic (As)-bearing phase was detected in the yellow-painted parts of the latter monument. The occurrence of huntite in Egypt has not been reported previously.

The binary system K2SO4CaSO4

USGS Publications Warehouse

Rowe, J.J.; Morey, G.W.; Hansen, I.D.

1965-01-01

The binary system K2SO4CaSO4 was studied by means of heating-cooling curves, differential thermal analysis, high-temperature quenching technique and by means of a heating stage mounted on an X-ray diffractometer. Compositions and quench products were identified optically and by X-ray. Limited solid solution of CaSO4 in K2SO4 was found. There is a eutectic at 875??C and 34 wt. per cent CaSO4. Calcium langbeinite melts incongruently at 1011??C. The melting-point of CaSO4 (1462??C) was determined by the quenching technique using sealed platinum tubes. The only intermediate crystalline phase found in the system is K2SO4??2CaSO4 (calcium langbeinite). ?? 1965.

Unusual Thermal Stability of High-Entropy Alloy Amorphous Structure

DTIC Science & Technology

2012-06-20

incident angle X - ray diffractometer (GIAXRD, RIGAKU D/MAX2500) with Cu Kα radiation and at the incident angle of 1°. The surface morphology and...microanalyzer (EPMA, JEOL JAX-8800). The crystallographic structures of as-deposited and annealed metallic films were characterized utilizing a glancing ...field image and selected-area- diffraction (SAD) patterns of (a) 800 °C-, (b) 850 °C- and (c) 900 °C-annealed alloy thin films, respectively. Both

Hydrothermal synthesis and characterization of a novel supramolecular network compound of Co(NIA) 2(H 2O) 4 with molecular ladder hydrogen bond chains (NIA=nicotinate)

NASA Astrophysics Data System (ADS)

Jia, Hong-Bin; Yu, Jie-Hui; Xu, Ji-Qing; Ye, Ling; Ding, Hong; Jing, Wei-Jie; Wang, Tie-Gang; Xu, Jia-Ning; Li, Zeng-Chun

2002-10-01

By hydrothermal method, a novel supramolecular compound, Co(NIA) 2(H 2O) 4 was synthesized and its structure was characterized with elemental analysis, FT-IR spectrum, TGA and X-ray diffractometer, indicating that it is a novel polyporous supramolecule with molecular ladder hydrogen-bonded chains. TGA curve shows its thermal stability up to 520 °C.

A comparison of techniques for nondestructive composition measurements in CdZnTe substrates

NASA Astrophysics Data System (ADS)

Tobin, S. P.; Tower, J. P.; Norton, P. W.; Chandler-Horowitz, D.; Amirtharaj, P. M.; Lopes, V. C.; Duncan, W. M.; Syllaios, A. J.; Ard, C. K.; Giles, N. C.; Lee, Jaesun; Balasubramanian, R.; Bollong, A. B.; Steiner, T. W.; Thewalt, M. L. W.; Bowen, D. K.; Tanner, B. K.

1995-05-01

We report an overview and a comparison of nondestructive optical techniques for determining alloy composition x in Cd1-xZnxTe substrates for HgCdTe epitaxy. The methods for single-point measurements include a new x-ray diffraction technique for precision lattice parameter measurements using a standard highresolution diffractometer, room-temperature photoreflectance, and low-temperature photoluminescence. We compare measurements on the same set of samples by all three techniques. Comparisons of precision and accuracy, with a discussion of the strengths and weaknesses of different techniques, are presented. In addition, a new photoluminescence excitation technique for full-wafer imaging of composition variations is described.

Eco-friendly synthesis of core-shell structured (TiO2/Li2CO3) nanomaterials for low cost dye-sensitized solar cells.

PubMed

Karuppuchamy, S; Brundha, C

2016-12-01

Core-shell structured TiO 2 /Li 2 CO 3 electrode was successfully synthesized by eco-friendly solution growth technique. TiO 2 /Li 2 CO 3 electrodes were characterized using X-ray Diffractometer (XRD), Scanning electron microscopy (SEM) and photocurrent-voltage measurements. The synthesized core-shell electrode material was sensitized with tetrabutylammonium cis-di(thiocyanato)-N,N'-bis(4-carboxylato-4'-carboxylic acid-2,2'-bipyridine)ruthenate(II) (N-719). The performance of dye-sensitized solar cells (DSCs) based on N719 dye modified TiO 2 /Li 2 CO 3 electrodes was investigated. The effect of various shell thickness on the photovoltaic performance of the core-shell structured electrode is also investigated. We found that Li 2 CO 3 shells of all thicknesses perform as inert barriers which improve open-circuit voltage (V oc ) of the DSCs. The energy conversion efficiency was greatly dependent on the thickness of Li 2 CO 3 on TiO 2 film, and the highest efficiency of 3.7% was achieved at the optimum Li 2 CO 3 shell layer. Copyright © 2015 Elsevier Inc. All rights reserved.

Synergy effect of naphthenic acid corrosion and sulfur corrosion in crude oil distillation unit

NASA Astrophysics Data System (ADS)

Huang, B. S.; Yin, W. F.; Sang, D. H.; Jiang, Z. Y.

2012-10-01

The synergy effect of naphthenic acid corrosion and sulfur corrosion at high temperature in crude oil distillation unit was studied using Q235 carbon-manganese steel and 316 stainless steel. The corrosion of Q235 and 316 in corrosion media containing sulfur and/or naphthenic acid at 280 °C was investigated by weight loss, scanning electron microscope (SEM), EDS and X-ray diffractometer (XRD) analysis. The results showed that in corrosion media containing only sulfur, the corrosion rate of Q235 and 316 first increased and then decreased with the increase of sulfur content. In corrosion media containing naphthenic acid and sulfur, with the variations of acid value or sulfur content, the synergy effect of naphthenic acid corrosion and sulfur corrosion has a great influence on the corrosion rate of Q235 and 316. It was indicated that the sulfur accelerated naphthenic acid corrosion below a certain sulfur content but prevented naphthenic acid corrosion above that. The corrosion products on two steels after exposure to corrosion media were investigated. The stable Cr5S8 phases detected in the corrosion products film of 316 were considered as the reason why 316 has greater corrosion resistance to that of Q235.

Exploration of geo-mineral compounds in granite mining soils using XRD pattern data analysis

NASA Astrophysics Data System (ADS)

Koteswara Reddy, G.; Yarakkula, Kiran

2017-11-01

The purpose of the study was to investigate the major minerals present in granite mining waste and agricultural soils near and away from mining areas. The mineral exploration of representative sub-soil samples are identified by X-Ray Diffractometer (XRD) pattern data analysis. The morphological features and quantitative elementary analysis was performed by Scanning Electron Microscopy-Energy Dispersed Spectroscopy (SEM-EDS).The XRD pattern data revealed that the major minerals are identified as Quartz, Albite, Anorthite, K-Feldspars, Muscovite, Annite, Lepidolite, Illite, Enstatite and Ferrosilite in granite waste. However, in case of agricultural farm soils the major minerals are identified as Gypsum, Calcite, Magnetite, Hematite, Muscovite, K-Feldspars and Quartz. Moreover, the agricultural soils neighbouring mining areas, the minerals are found that, the enriched Mica group minerals (Lepidolite and Illite) the enriched Orthopyroxene group minerals (Ferrosilite and Enstatite). It is observed that the Mica and Orthopyroxene group minerals are present in agricultural farm soils neighbouring mining areas and absent in agricultural farm soils away from mining areas. The study demonstrated that the chemical migration takes place at agricultural farm lands in the vicinity of the granite mining areas.

Synthesis and characterization of nanocrystalline graphite from coconut shell with heating process

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wachid, Frischa M., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id; Perkasa, Adhi Y., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id; Prasetya, Fandi A., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id

Graphite were synthesized and characterized by heating process of coconut shell with varying temperature (400, 800 and 1000°C) and holding time (3 and 5 hours). After heating process, the samples were characterized by X-ray diffraction (XRD) and analyzed by X'pert HighScore Plus Software, Scanning Electron Microcope-Energy Dispersive X-Ray (SEM-EDX) and Transmission Electron Microscope-Energy Dispersive X-Ray (TEM-EDX). Graphite and londsdaelite phase were analyzed by XRD. According to EDX analysis, the sample was heated in 1000°C got the highest content of carbon. The amorphous carbon and nanocrystalline graphite were observed by SEM-EDX and TEM-EDX.

X-ray scattering signatures of β-thalassemia

NASA Astrophysics Data System (ADS)

Desouky, Omar S.; Elshemey, Wael M.; Selim, Nabila S.

2009-08-01

X-ray scattering from lyophilized proteins or protein-rich samples is characterized by the presence of two characteristic broad peaks at scattering angles equivalent to momentum transfer values of 0.27 and 0.6 nm -1, respectively. These peaks arise from the interference of coherently scattered photons. Once the conformation of a protein is changed, these two peaks reflect such change with considerable sensitivity. The present work examines the possibility of characterizing the most common cause of hemolytic anaemia in Egypt and many Mediterranean countries; β-thalassemia, from its X-ray scattering profile. This disease emerges from a genetic defect causing reduced rate in the synthesis of one of the globin chains that make up hemoglobin. As a result, structurally abnormal hemoglobin molecules are formed. In order to detect such molecular disorder, hemoglobin samples of β-thalassemia patients are collected, lyophilized and measured using a conventional X-ray diffractometer. Results show significant differences in the X-ray scattering profiles of most of the diseased samples compared to control. The shape of the first scattering peak at 0.27 nm -1, in addition to the relative intensity of the first to the second scattering peaks, provides the most reliable signs of abnormality in diseased samples. The results are interpreted and confirmed with the aid of Fourier Transform Infrared (FTIR) spectroscopy of normal and thalassemia samples.

Developments on a SEM-based X-ray tomography system: Stabilization scheme and performance evaluation

NASA Astrophysics Data System (ADS)

Gomes Perini, L. A.; Bleuet, P.; Filevich, J.; Parker, W.; Buijsse, B.; Kwakman, L. F. Tz.

2017-06-01

Recent improvements in a SEM-based X-ray tomography system are described. In this type of equipment, X-rays are generated through the interaction between a highly focused electron-beam and a geometrically confined anode target. Unwanted long-term drifts of the e-beam can lead to loss of X-ray flux or decrease of spatial resolution in images. To circumvent this issue, a closed-loop control using FFT-based image correlation is integrated to the acquisition routine, in order to provide an in-line drift correction. The X-ray detection system consists of a state-of-the-art scientific CMOS camera (indirect detection), featuring high quantum efficiency (˜60%) and low read-out noise (˜1.2 electrons). The system performance is evaluated in terms of resolution, detectability, and scanning times for applications covering three different scientific fields: microelectronics, technical textile, and material science.

Texture analysis at neutron diffractometer STRESS-SPEC

NASA Astrophysics Data System (ADS)

Brokmeier, H.-G.; Gan, W. M.; Randau, C.; Völler, M.; Rebelo-Kornmeier, J.; Hofmann, M.

2011-06-01

In response to the development of new materials and the application of materials and components in advanced technologies, non-destructive measurement methods of textures and residual stresses have gained worldwide significance in recent years. The materials science neutron diffractometer STRESS-SPEC at FRM II (Garching, Germany) is designed to be applied equally to texture and residual stress analyses by virtue of its very flexible configuration. Due to the high penetration capabilities of neutrons and the high neutron flux of STRESS-SPEC it allows a combined analysis of global texture, local texture, strain pole figure and FWHM pole figure in a wide variety of materials including metals, alloys, composites, ceramics and geological materials. Especially, the analysis of texture gradients in bulk materials using neutron diffraction has advantages over laboratory X-rays and EBSD for many scientific cases. Moreover, neutron diffraction is favourable for coarse-grained materials, where bulk information averaged over texture inhomogeneities is needed, and also stands out due to easy sample preparation. In future, the newly developed robot system for STRESS-SPEC will allow much more flexibility than an Eulerian cradle as on standard instruments. Five recent measurements are shown to demonstrate the wide range of possible texture applications at STRESS-SPEC diffractometer.

Microscale reconstruction of biogeochemical substrates using multimode X-ray tomography and scanning electron microscopy

NASA Astrophysics Data System (ADS)

Miller, M.; Miller, E.; Liu, J.; Lund, R. M.; McKinley, J. P.

2012-12-01

X-ray computed tomography (CT), scanning electron microscopy (SEM), electron microprobe analysis (EMP), and computational image analysis are mature technologies used in many disciplines. Cross-discipline combination of these imaging and image-analysis technologies is the focus of this research, which uses laboratory and light-source resources in an iterative approach. The objective is to produce images across length scales, taking advantage of instrumentation that is optimized for each scale, and to unify them into a single compositional reconstruction. Initially, CT images will be collected using both x-ray absorption and differential phase contrast modes. The imaged sample will then be physically sectioned and the exposed surfaces imaged and characterized via SEM/EMP. The voxel slice corresponding to the physical sample surface will be isolated computationally, and the volumetric data will be combined with two-dimensional SEM images along CT image planes. This registration step will take advantage of the similarity between the X-ray absorption (CT) and backscattered electron (SEM) coefficients (both proportional to average atomic number in the interrogated volume) as well as the images' mutual information. Elemental and solid-phase distributions on the exposed surfaces, co-registered with SEM images, will be mapped using EMP. The solid-phase distribution will be propagated into three-dimensional space using computational methods relying on the estimation of compositional distributions derived from the CT data. If necessary, solid-phase and pore-space boundaries will be resolved using X-ray differential phase contrast tomography, x-ray fluorescence tomography, and absorption-edge microtomography at a light-source facility. Computational methods will be developed to register and model images collected over varying scales and data types. Image resolution, physically and dynamically, is qualitatively different for the electron microscopy and CT methodologies. Routine CT images are resolved at 10-20 μm, while SEM images are resolved at 10-20 nm; grayscale values vary according to collection time and instrument sensitivity; and compositional sensitivities via EMP vary in interrogation volume and scale. We have so far successfully registered SEM imagery within a multimode tomographic volume and have used standard methods to isolate pore space within the volume. We are developing a three-dimensional solid-phase identification and registration method that is constrained by bulk-sample X-ray diffraction Rietveld refinements. The results of this project will prove useful in fields that require the fine-scale definition of solid-phase distributions and relationships, and could replace more inefficient methods for making these estimations.

In situ synchrotron X-ray diffraction study on epitaxial-growth dynamics of III–V semiconductors

NASA Astrophysics Data System (ADS)

Takahasi, Masamitu

2018-05-01

The application of in situ synchrotron X-ray diffraction (XRD) to the molecular-beam epitaxial (MBE) growth of III–V semiconductors is overviewed along with backgrounds of the diffraction theory and instrumentation. X-rays are sensitive not only to the surface of growing films but also to buried interfacial structures because of their large penetration depth. Moreover, a spatial coherence length up to µm order makes X-rays widely applicable to the characterization of low-dimensional structures, such as quantum dots and wires. In situ XRD studies during growth were performed using an X-ray diffractometer, which was combined with an MBE chamber. X-ray reciprocal space mapping at a speed matching a typical growth rate was achieved using intense X-rays available from a synchrotron light source and an area detector. The importance of measuring the three-dimensional distribution of XRD intensity in a reciprocal space map is demonstrated for the MBE growth of two-, one-, and zero-dimensional structures. A large amount of information about the growth process of two-dimensional InGaAs/GaAs(001) epitaxial films has been provided by three-dimensional X-ray reciprocal mappings, including the anisotropic strain relaxation, the compositional inhomogeneity, and the evolution of surface and interfacial roughness. For one-dimensional GaAs nanowires grown in a Au-catalyzed vapor-liquid–solid mode, the relationship between the diameter of the nanowires and the formation of polytypes has been suggested on the basis of in situ XRD measurements. In situ three-dimensional X-ray reciprocal space mapping is also shown to be useful for determining the lateral and vertical sizes of self-assembled InAs/GaAs(001) quantum dots as well as their internal strain distributions during growth.

A brief History of Neutron Scattering at the Oak Ridge High Flux Isotope Reactor

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nagler, Stephen E; Mook Jr, Herbert A

2008-01-01

Neutron scattering at the Oak Ridge National Laboratory dates back to 1945 when Ernest Wollan installed a modified x-ray diffractometer on a beam port of the original graphite reactor. Subsequently, Wollan and Clifford Shull pioneered neutron diffraction and laid the foundation for an active neutron scattering effort that continued through the 1950s, using the Oak Ridge Research reactor after 1958, and, starting in 1966, the High Flux Isotope Reactor, or HFIR.

Mesoporous Nitrogen Doped Carbon-Glass Ceramic Cathode for High Performance Lithium-Oxygen Battery

DTIC Science & Technology

2012-06-01

dry room with controlled moisture content. Composite 3 films on nickel foam were used as working cathodes along with lithium metal as anode and the...cathode formulation [6,7,8,9,10], efficient oxygen reduction catalysts [11,12], electrolyte compositions [13,14], effect of moisture [15], etc...specimens. Structure and purity of these materials were performed by powder X-ray diffraction (XRD) on a Rigaku D/MAX-2250 diffractometer fitted with CuKα

Scanning electron microscopy, X-ray diffraction and thermal analysis study of the TiH{sub 2} foaming agent

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mandrino, Djordje, E-mail: djordje.mandrino@imt.si; Paulin, Irena; Skapin, Sreco D.

2012-10-15

The decomposition of commercially available TiH{sub 2} was investigated while performing different thermal treatments. TiH{sub 2} powder, which is widely used as a foaming agent, was heat treated at 450 Degree-Sign C for various times, from 15 min to 120 min. Scanning electron microscopy (SEM) images of the surfaces at different magnifications were obtained and interpreted. A Bragg-Brentano X-ray diffractometer was used to measure the X-ray diffraction (XRD) spectra on all five samples. A close examination of the diffraction spectra showed that for an as-received sample and samples undergoing the longest thermal treatment (1 and 2 h) these spectra canmore » be explained as deriving from cubic TiH{sub 1.924}, while for the other two samples they can be explained as deriving from tetragonal TiH{sub 1.924}. A constant-unit-cell-volume phase transition between the cubic and tetragonal phases in TiH{sub 2-y}-type compounds had been described in the literature. The unit-cell parameters obtained from measured spectra confirm that within the measurement uncertainty the unit-cell volume is indeed constant in all five samples. Thermo-gravimetry (TG) and differential thermal analysis (DTA) measurements were performed on all the samples, showing that the intensity of the dehydrogenation depends on the previous treatment of the TiH{sub 2}. After the thermal analysis XRD of the samples was performed again and the material was found to exhibit a Ti-like unit cell, but slightly enlarged due to the unreleased hydrogen. - Highlights: Black-Right-Pointing-Pointer TiH{sub 2} samples were cubic or tetragonal TiH{sub 1.924} Black-Right-Pointing-Pointer Onset of the hydrogen release temperature increases with the pre-treatment time. Black-Right-Pointing-Pointer Thermal dehydrogenation for the as-prepared TiH{sub 2} is a three-step process. Black-Right-Pointing-Pointer After thermal analysis 2 residual hydrogen TiH{sub x} phases, close to {alpha}Ti, appeared.« less

A simple method for detection of gunshot residue particles from hands, hair, face, and clothing using scanning electron microscopy/wavelength dispersive X-ray (SEM/WDX).

PubMed

Kage, S; Kudo, K; Kaizoji, A; Ryumoto, J; Ikeda, H; Ikeda, N

2001-07-01

We devised a simple and rapid method for detection of gunshot residue (GSR) particles, using scanning electron microscopy/wavelength dispersive X-ray (SEM/WDX) analysis. Experiments were done on samples containing GSR particles obtained from hands, hair, face, and clothing, using double-sided adhesive coated aluminum stubs (tape-lift method). SEM/WDX analyses for GSR were carried out in three steps: the first step was map analysis for barium (Ba) to search for GSR particles from lead styphnate primed ammunition, or tin (Sn) to search for GSR particles from mercury fulminate primed ammunition. The second step was determination of the location of GSR particles by X-ray imaging of Ba or Sn at a magnification of x 1000-2000 in the SEM, using data of map analysis, and the third step was identification of GSR particles, using WDX spectrometers. Analysis of samples from each primer of a stub took about 3 h. Practical applications were shown for utility of this method.

Preparation of manganese doped cadmium sulfide nanoparticles in zincblende phase and their magnetic properties.

PubMed

Nakaya, Masafumi; Tanaka, Itaru; Muramatsu, Atsushi

2012-12-01

In this study, the random dope of Mn into CdS nanoparticles in zincblende phase has been carried out under the mild reaction condition. The resulting nanoparticles were characterized by energy dispersive X-ray analysis (EDX), transmission electron microscopy (TEM), X-ray diffractometer (XRD), UV-Vis spectrometer, PL spectrometer, and SQUID. EDX showed that the compositions of Mn doped CdS nanoparticles were readily controlled. TEM showed the particle sizes were not significantly affected by the compositions, retaining to be ca. 3 nm with a narrow size distribution. UV-Vis and PL spectra of the resulting nanoparticles showed the intra-Mn level may be affected by the quantum size effect. SQUID measurement showed that the resulting nanoparticles showed diamagnetism, paramagnetism and superparamagnetism dependent on Mn content.

Cementation and Aqueous Alteration of a Sandstone Unit Under Acidic Conditions in Gale Crater, Mars

NASA Technical Reports Server (NTRS)

Yen, A. S.; Blake, D. F.; Ming, D. W.; Morris, R. V.; Gellert, R.; Clark, B.; Vaniman, D. T.; Chipera, S. J.; Thompson, L. M.; Bristow, T. F.;

X-Ray diffraction on large single crystals using a powder diffractometer

DOE PAGES

Jesche, A.; Fix, M.; Kreyssig, A.; ...

2016-06-16

Information on the lattice parameter of single crystals with known crystallographic structure allows for estimations of sample quality and composition. In many cases it is sufficient to determine one lattice parameter or the lattice spacing along a certain, high- symmetry direction, e.g. in order to determine the composition in a substitution series by taking advantage of Vegard’s rule. Here we present a guide to accurate measurements of single crystals with dimensions ranging from 200 μm up to several millimeter using a standard powder diffractometer in Bragg-Brentano geometry. The correction of the error introduced by the sample height and the optimizationmore » of the alignment are discussed in detail. Finally, in particular for single crystals with a plate-like habit, the described procedure allows for measurement of the lattice spacings normal to the plates with high accuracy on a timescale of minutes.« less

Experimental and theoretical investigation of the rocking curves measured for MoK{sub α} X-ray characteristic lines in the double-crystal nondispersive scheme

DOE Office of Scientific and Technical Information (OSTI.GOV)

Marchenkov, N. V., E-mail: marchenkov@ns.crys.ras.ru; Chukhovskii, F. N.; Blagov, A. E.

2015-03-15

The rocking curves (RCs) for MoK{sub α1} and MoK{sub α2} characteristic X-ray lines have been experimentally and theoretically studied in the nondispersive scheme of an X-ray double-crystal TPC-K diffractometer. The results of measurements and theoretical calculations of double-crystal RCs for characteristic X-rays from tubes with a molybdenum anode and different widths of slits show that a decrease in the slit width leads to an increase in the relative contribution of the MoK{sub α2}-line RC in comparison with the intensity of the tails of the MoK{sub α1}-line RC. It is shown that the second peak of the MoK{sub α2} line becomesmore » increasingly pronounced in the tail of the MoK{sub α1}-line RC with a decrease in the slit width. Two plane-parallel Si plates (input faces (110), diffraction vector h 〈220〉) were used as a monochromator crystal and a sample. The results of measuring double-crystal RCs are in good agreement with theoretical calculations.« less

Micromorphology of sialoliths in submandibular salivary gland: a scanning electron microscope and X-ray diffraction analysis.

PubMed

Kasaboğlu, Oğuzcan; Er, Nuray; Tümer, Celal; Akkocaoğlu, Murat

2004-10-01

Sialoliths are common in the submandibular gland and its duct system. The exact cause of formation of a sialolith is still a matter of debate. The aim of this study was to analyze 6 sialoliths ultrastructurally to determine their development mechanism in the submandibular salivary glands. Six sialoliths retrieved from the hilus and duct of the submandibular salivary glands of 6 patients with sialadenitis were analyzed ultrastructurally by scanning electron microscope and x-ray diffractometer. Scanning electron microscope revealed mainly irregular, partly rudely hexagonal, needle-like and plate-shaped crystals. The cross-section from the surface to the inner part of the sialoliths showed no organic material. X-ray diffraction showed that the sialoliths were composed of hydroxyapatite crystals. Energy dispersive x-ray microanalysis showed that all of the samples contained high levels of Ca and P, and small amounts of Mg, Na, Cl, Si, Fe, and K. The main structures of the submandibular sialoliths were found to be hydroxyapatite crystals. No organic cores were observed in the central parts of the sialoliths. In accordance with these preliminary results, sialoliths in the submandibular salivary glands may arise secondary to sialadenitis, but not via a luminal organic nidus.

Measuring the x-ray resolving power of bent potassium acid phthalate diffraction crystals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Haugh, M. J., E-mail: haughmj@nv.doe.gov; Jacoby, K. D.; Wu, M.

2014-11-15

This report presents the results from measuring the X-ray resolving power of a curved potassium acid phthalate (KAP(001)) spectrometer crystal using two independent methods. It is part of a continuing effort to measure the fundamental diffraction properties of bent crystals that are used to study various characteristics of high temperature plasmas. Bent crystals like KAP(001) do not usually have the same diffraction properties as corresponding flat crystals. Models that do exist to calculate the effect of bending the crystal on the diffraction properties have simplifying assumptions and their accuracy limits have not been adequately determined. The type of crystals thatmore » we measured is being used in a spectrometer on the Z machine at Sandia National Laboratories in Albuquerque, New Mexico. The first technique for measuring the crystal resolving power measures the X-ray spectral line width of the characteristic lines from several metal anodes. The second method uses a diode X-ray source and a double crystal diffractometer arrangement to measure the reflectivity curve of the KAP(001) crystal. The width of that curve is inversely proportional to the crystal resolving power. The measurement results are analyzed and discussed.« less

Measuring the x-ray resolving power of bent potassium acid phthalate diffraction crystalsa)

NASA Astrophysics Data System (ADS)

Haugh, M. J.; Wu, M.; Jacoby, K. D.; Loisel, G. P.

2014-11-01

This report presents the results from measuring the X-ray resolving power of a curved potassium acid phthalate (KAP(001)) spectrometer crystal using two independent methods. It is part of a continuing effort to measure the fundamental diffraction properties of bent crystals that are used to study various characteristics of high temperature plasmas. Bent crystals like KAP(001) do not usually have the same diffraction properties as corresponding flat crystals. Models that do exist to calculate the effect of bending the crystal on the diffraction properties have simplifying assumptions and their accuracy limits have not been adequately determined. The type of crystals that we measured is being used in a spectrometer on the Z machine at Sandia National Laboratories in Albuquerque, New Mexico. The first technique for measuring the crystal resolving power measures the X-ray spectral line width of the characteristic lines from several metal anodes. The second method uses a diode X-ray source and a double crystal diffractometer arrangement to measure the reflectivity curve of the KAP(001) crystal. The width of that curve is inversely proportional to the crystal resolving power. The measurement results are analyzed and discussed.

Is scanning electron microscopy/energy dispersive X-ray spectrometry (SEM/EDS) quantitative?

PubMed

Newbury, Dale E; Ritchie, Nicholas W M

2013-01-01

Scanning electron microscopy/energy dispersive X-ray spectrometry (SEM/EDS) is a widely applied elemental microanalysis method capable of identifying and quantifying all elements in the periodic table except H, He, and Li. By following the "k-ratio" (unknown/standard) measurement protocol development for electron-excited wavelength dispersive spectrometry (WDS), SEM/EDS can achieve accuracy and precision equivalent to WDS and at substantially lower electron dose, even when severe X-ray peak overlaps occur, provided sufficient counts are recorded. Achieving this level of performance is now much more practical with the advent of the high-throughput silicon drift detector energy dispersive X-ray spectrometer (SDD-EDS). However, three measurement issues continue to diminish the impact of SEM/EDS: (1) In the qualitative analysis (i.e., element identification) that must precede quantitative analysis, at least some current and many legacy software systems are vulnerable to occasional misidentification of major constituent peaks, with the frequency of misidentifications rising significantly for minor and trace constituents. (2) The use of standardless analysis, which is subject to much broader systematic errors, leads to quantitative results that, while useful, do not have sufficient accuracy to solve critical problems, e.g. determining the formula of a compound. (3) EDS spectrometers have such a large volume of acceptance that apparently credible spectra can be obtained from specimens with complex topography that introduce uncontrolled geometric factors that modify X-ray generation and propagation, resulting in very large systematic errors, often a factor of ten or more. © Wiley Periodicals, Inc.

Effect of cobalt doping on crystallinity, stability, magnetic and optical properties of magnetic iron oxide nano-particles

NASA Astrophysics Data System (ADS)

Anjum, Safia; Tufail, Rabia; Rashid, Khalid; Zia, Rehana; Riaz, S.

2017-06-01

This paper is dedicated to investigate the effect of Co2+ ions in magnetite Fe3O4 nano-particles with stoichiometric formula CoxFe3-xO4 where (x = 0, 0.05, 0.1 and 0.15) prepared by co-precipitation method. The structural, thermal, morphological, magnetic and optical properties of magnetite and Co2+ doped magnetite nanoparticles have been carried out using X-ray Diffractometer, Fourier Transform Infrared Spectroscopy, Themogravimetric Analysis, Scanning Electron Microscopy, Vibrating Sample Magnetometer (VSM) and UV-Vis Spectrometer (UV-Vis) respectively. Structural analysis verified the formation of single phase inverse spinel cubic structure with decrease in lattice parameters due to increase in cobalt content. FTIR analysis confirms the single phase of CoxFe3-xO4 nanoparticles with the major band at 887 cm-1, which might be due to the stretching vibrations of metal-oxide bond. The DSC results corroborate the finding of an increase in the maghemite to hematite phase transition temperature with increase in Co2+ content. The decrease in enthalpy with increase in Co2+ concentration attributed to the fact that the degree of conversion from maghemite to hematite decrease which shows that the stability increases with increasing Co2+ content in B-site of Fe3O4 structure. SEM analysis demonstrated the formation of spherical shaped nanoparticles with least agglomeration. The magnetic measurements enlighten that the coercivity and anisotropy of CoxFe3-xO4 nanoparticles are significantly increased. From UV-Vis analysis it is revealed that band gap energy increases with decreasing particle size. This result has a great interest for magnetic fluid hyperthermia application (MPH).

Application of SEM and EDX in studying biomineralization in plant tissues.

PubMed

He, Honghua; Kirilak, Yaowanuj

2014-01-01

This chapter describes protocols using formalin-acetic acid-alcohol (FAA) to fix plant tissues for studying biomineralization by means of scanning electron microscopy (SEM) and qualitative energy-dispersive X-ray microanalysis (EDX). Specimen preparation protocols for SEM and EDX mainly include fixation, dehydration, critical point drying (CPD), mounting, and coating. Gold-coated specimens are used for SEM imaging, while gold- and carbon-coated specimens are prepared for qualitative X-ray microanalyses separately to obtain complementary information on the elemental compositions of biominerals. During the specimen preparation procedure for SEM, some biominerals may be dislodged or scattered, making it difficult to determine their accurate locations, and light microscopy is used to complement SEM studies. Specimen preparation protocols for light microscopy generally include fixation, dehydration, infiltration and embedding with resin, microtome sectioning, and staining. In addition, microwave processing methods are adopted here to speed up the specimen preparation process for both SEM and light microscopy.

A combination of a SEM technique and X-ray microanalysis for studying the spore germination process of Clostridium tyrobutyricum.

PubMed

Bassi, Daniela; Cappa, Fabrizio; Cocconcelli, Pier Sandro

2009-06-01

Clostridium tyrobutyricum is an anaerobic bacterium responsible for late blowing defects during cheese ripening and it is of scientific interest for biological hydrogen production. A scanning electron microscopy (SEM) coating technique and X-ray microanalysis were developed to analyze the architecture and chemical composition of spores upon germination in response to environmental changes. In addition, we investigated the effects of different compounds on this process. Agents and environmental conditions inducing germination were characterized monitoring changes in optical density (OD). Among all tested conditions, the greatest drop in OD(625) (57.4%) was obtained when spores were incubated in l-alanine/l-lactate buffer, pH 4.6. In addition, a carbon-coating SEM technique and X-ray microanalysis were used to observe the architecture of spores and to examine calcium dipicolinate release. Conditions inducing C. tyrobutyricum spore germination were identified and SEM X-ray microanalysis clearly distinguished germinating from dormant spores. We confirmed that calcium dipicolinate release is one of the first events occurring. These microscopy methods could be considered sensitive tools for evaluating morphological and chemical changes in spores of C. tyrobutyricum during the initial phase of germination. Information gathered from this work may provide new data for further research on germination.

Adsorption of Benzoic Acid in Aqueous Solution by Bagasse Fly Ash

NASA Astrophysics Data System (ADS)

Suresh, S.

2012-09-01

This paper reports the studies on the benzoic acid (BA) onto bagasse fly ash (BFA) was studied in aqueous solution in a batch system. Physico-chemical properties including surface area, surface texture of the GAC before and after BA adsorption onto BFA were analysed using X-ray diffractometer (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX). The optimum initial pH for the adsorption of BA was found to be 5.56. The adsorbent dose was 10 g/l for BFA and the equilibrium time 8 h of reaction. Pseudo first and second order models were used to find the adsorption kinetics. It was found that intraparticle diffusion played important role in the adsorption mechanisms of BA and the adsorption kinetics followed pseudo-second order kinetic model rather than the pseudo first order kinetic model. Isotherm data were generated for BA solution having initial concentrations of BA in the range of 10-200 mg/l for the BFA dosage of 10 g/l at temperatures of 288, 303, and 318 K. The adsorption of BA onto BFA was favorably influenced by an increase in temperature. Equilibrium data were well represented by the Redlich-Peterson isotherm model. Values of the change in entropy ( ΔS 0), heat of adsorption ( ΔH 0) for adsorption of BA on BFA was found to be 120.10 and 19.61 kJ/mol respectively. The adsorption of BA onto BFA was an endothermic reaction. Desorption of BA from BFA was studied by various solvents method. Acetic acid was found to be a better eluant for desorption of BA with a maximum desorption efficiency of 55.2 %. Owing to its heating value, spent BFA can be used as a co-fuel for the production of heat in boiler furnaces.

Defluoridation of water using activated alumina in presence of natural organic matter via response surface methodology.

PubMed

Samarghandi, Mohammad Reza; Khiadani, Mehdi; Foroughi, Maryam; Zolghadr Nasab, Hasan

2016-01-01

Adsorption by activated alumina is considered to be one of the most practiced methods for defluoridation of freshwater. This study was conducted, therefore, to investigate the effect of natural organic matters (NOMs) on the removal of fluoride by activated alumina using response surface methodology. To the authors' knowledge, this has not been previously investigated. Physico-chemical characterization of the alumina was determined by scanning electron microscope (SEM), Brunauer-Emmett-Teller (BET), Fourier transform infrared spectroscopy (FTIR), X-ray fluorescence (XRF), and X-ray diffractometer (XRD). Response surface methodology (RSM) was applied to evaluate the effect of single and combined parameters on the independent variables such as the initial concentration of fluoride, NOMs, and pH on the process. The results revealed that while presence of NOM and increase of pH enhance fluoride adsorption on the activated alumina, initial concentration of fluoride has an adverse effect on the efficiency. The experimental data were analyzed and found to be accurately and reliably fitted to a second-order polynomial model. Under optimum removal condition (fluoride concentration 20 mg/L, NOM concentration 20 mg/L, and pH 7) with a desirability value of 0.93 and fluoride removal efficiency of 80.6%, no significant difference was noticed with the previously reported sequence of the co-exiting ion affinity to activated alumina for fluoride removal. Moreover, aluminum residual was found to be below the recommended value by the guideline for drinking water. Also, the increase of fluoride adsorption on the activated alumina, as NOM concentrations increase, could be due to the complexation between fluoride and adsorbed NOM. Graphical abstract ᅟ.

Characterization of As-polluted soils by laboratory X-ray-based techniques coupled with sequential extractions and electron microscopy: the case of Crocette gold mine in the Monte Rosa mining district (Italy).

PubMed

Allegretta, Ignazio; Porfido, Carlo; Martin, Maria; Barberis, Elisabetta; Terzano, Roberto; Spagnuolo, Matteo

2018-06-24

Arsenic concentration and distribution were studied by combining laboratory X-ray-based techniques (wavelength dispersive X-ray fluorescence (WDXRF), micro X-ray fluorescence (μXRF), and X-ray powder diffraction (XRPD)), field emission scanning electron microscopy equipped with microanalysis (FE-SEM-EDX), and sequential extraction procedure (SEP) coupled to total reflection X-ray fluorescence (TXRF) analysis. This approach was applied to three contaminated soils and one mine tailing collected near the gold extraction plant at the Crocette gold mine (Macugnaga, VB) in the Monte Rosa mining district (Piedmont, Italy). Arsenic (As) concentration, measured with WDXRF, ranged from 145 to 40,200 mg/kg. XRPD analysis evidenced the presence of jarosite and the absence of any As-bearing mineral, suggesting a high weathering grade and strong oxidative conditions. However, small domains of Fe arsenate were identified by combining μXRF with FE-SEM-EDX. SEP results revealed that As was mainly associated to amorphous Fe oxides/hydroxides or hydroxysulfates (50-80%) and the combination of XRPD and FE-SEM-EDX suggested that this phase could be attributed to schwertmannite. On the basis of the reported results, As is scarcely mobile, even if a consistent As fraction (1-3 g As/kg of soil) is still potentially mobilizable. In general, the proposed combination of laboratory X-ray techniques could be successfully employed to unravel environmental issues related to metal(loid) pollution in soil and sediments.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bekar, Kursat B; Miller, Thomas Martin; Patton, Bruce W

The characteristic X-rays produced by the interactions of the electron beam with the sample in a scanning electron microscope (SEM) are usually captured with a variable-energy detector, a process termed energy dispersive spectrometry (EDS). The purpose of this work is to exploit inverse simulations of SEM-EDS spectra to enable rapid determination of sample properties, particularly elemental composition. This is accomplished using penORNL, a modified version of PENELOPE, and a modified version of the traditional Levenberg Marquardt nonlinear optimization algorithm, which together is referred to as MOZAIK-SEM. The overall conclusion of this work is that MOZAIK-SEM is a promising method formore » performing inverse analysis of X-ray spectra generated within a SEM. As this methodology exists now, MOZAIK-SEM has been shown to calculate the elemental composition of an unknown sample within a few percent of the actual composition.« less

Phase, compositional, and morphological changes of human dentin after Nd:YAG laser treatment.

PubMed

Lin, C P; Lee, B S; Lin, F H; Kok, S H; Lan, W H

2001-06-01

Although techniques for repairing root fracture have been proposed, the prognosis is generally poor. If the fusion of a root fracture by laser is possible, it will offer an alternative to extraction. Our group has attempted to use lasers to fuse a low melting-point bioactive glass to fractured dentin. This report is focused on the phase, compositional, and morphological changes observed by means of X-ray diffractometer, Fourier transforming infrared spectroscopy, and scanning electron microscopy-energy dispersive X-ray spectroscopy in human dentin after exposure to Nd:YAG laser. The irradiation energies were from 150 mJ/ pulse-10 pps-4 s to 150 mJ/pulse-30 pps-4 s. After exposure to Nd:YAG laser, dentin showed four peaks on the X-ray diffractometer that corresponding to a-tricalcium phosphate (TCP) and beta-TCP at 20 = 30.78 degrees/34.21 degrees and 32.47 degrees/33.05 degrees, respectively. The peaks of a-TCP and beta-TCP gradually increased in intensity with the elevation of irradiation energy. In Fourier transforming infrared analysis, two absorption bands at 2200 cm(-1) and 2015 cm(-1) could be traced on dentin treated by Nd:YAG laser with the irradiation energies beyond 150 mJ/pulse-10 pps-4 s. The energy dispersive X-ray results showed that the calcium/phosphorus ratios of the irradiated area proportionally increased with the elevation of irradiation energy. The laser energies of 150 mJ/ pulse-30 pps-4 s and 150 mJ/pulse-20 pps-4 s could result in the a-TCP formation and collagen breakdown. However, the formation of glass-like melted substances without a-TCP at the irradiated site was induced by the energy output of 150 mJ/ pulse-10 pps-4 s. Scanning electron micrographs also revealed that the laser energy of 150 mJ/ pulse-10 pps-4 s was sufficient to prompt melting and recrystallization of dentin crystals without cracking. Therefore, we suggest that the irradiation energy of Nd:YAG laser used to fuse a low melting-point bioactive glass to dentin is 150 mJ/ pulse-10 pps-4 s.

Destination Innovation: Episode 4 CheMin

NASA Image and Video Library

2012-08-02

Destination Innovation is a new series that explores the research, science and other projects underway at the NASA Ames Research Center. Episode 4 focuses on the CheMin instrument aboard the Mars Science Laboratory, NASA' s latest robotic explorer to visit Mars. CheMin, short for 'Chemistry and Mineralogy,' was developed at NASA Ames Research Center and is one of 10 instruments aboard the rover Curiosity. The instrument is an x-ray diffractometer, which will be able to identify minerals in the Martial rock and soil.

Enhancement of bioactivity of titanium carbonitride nanocomposite thin films on steels with biosynthesized hydroxyapatite

PubMed Central

Thampi, VV Anusha; Dhandapani, P; Manivasagam, Geetha; Subramanian, B

2015-01-01

Thin films of titanium carbonitride (TiCN) were fabricated by DC magnetron sputtering on medical grade steel. The biocompatibility of the coating was further enhanced by growing hydroxyapatite crystals over the TiCN-coated substrates using biologically activated ammonia from synthetic urine. The coatings were characterized using X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy (SEM)-energy dispersive spectroscopy, and Raman spectroscopy. The electrochemical behavior of the coatings was determined in simulated body fluid. In addition, hemocompatibility was assessed by monitoring the attachment of platelets on the coating using SEM. The wettability of the coatings was measured in order to correlate with biocompatibility results. Formation of a coating with granular morphology and the preferred orientation was confirmed by SEM and X-ray diffraction results. The hydroxyapatite coating led to a decrease in thrombogenicity, resulting in controlled blood clot formation, hence demonstrating the hemocompatibility of the coating. PMID:26491312

Enhancement of bioactivity of titanium carbonitride nanocomposite thin films on steels with biosynthesized hydroxyapatite.

PubMed

Thampi, V V Anusha; Dhandapani, P; Manivasagam, Geetha; Subramanian, B

2015-01-01

Thin films of titanium carbonitride (TiCN) were fabricated by DC magnetron sputtering on medical grade steel. The biocompatibility of the coating was further enhanced by growing hydroxyapatite crystals over the TiCN-coated substrates using biologically activated ammonia from synthetic urine. The coatings were characterized using X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy (SEM)-energy dispersive spectroscopy, and Raman spectroscopy. The electrochemical behavior of the coatings was determined in simulated body fluid. In addition, hemocompatibility was assessed by monitoring the attachment of platelets on the coating using SEM. The wettability of the coatings was measured in order to correlate with biocompatibility results. Formation of a coating with granular morphology and the preferred orientation was confirmed by SEM and X-ray diffraction results. The hydroxyapatite coating led to a decrease in thrombogenicity, resulting in controlled blood clot formation, hence demonstrating the hemocompatibility of the coating.

In vitro study of root fracture treated by CO2 laser and DP-bioactive glass paste.

PubMed

Wang, Yin-Lin; Lee, Bor-Shiunn; Tseng, Ching-Li; Lin, Feng-Huei; Lin, Chun-Pin

2008-01-01

An ideal material has yet to be discovered that can successfully treat vertical root fracture. Therefore, the purpose of this study was to use a continuous-wave CO2 laser of medium-energy density to fuse DP-bioactive glass paste (DPGP) to vertical root fracture. The DP-bioglass powder was based on a Na2O-CaO-SiO2-P2O5 system and it was mixed with phosphoric acid (65% concentration) with a powder/liquid ratio of 2 g/4 mL to form DPGP. The interaction of DPGP and dentin was analyzed by means of X-ray diffractometer (XRD) and differential thermal analysis/thermogravimetric analysis (DTA/TGA). Root fracture line was filled with DPGP followed by CO2 laser irradiation and the result was examined by scanning electron microscopy (SEM). The main crystal phase of DPGP was monocalcium phosphate monohydrate (Ca(H2PO4)2.H2O) and the phase transformed to dicalcium phosphate dihydrate (CaHPO4.2H2O) after mixing DPGP with dentin powder (DPG-D). Additionally, gamma-Ca2P2O7 and beta-Ca2P2O7 were identified when DPG-D was lased by CO2 laser. The reaction temperature was between 500 degrees C and 1100 degrees C. SEM results demonstrated that the fracture line was effectively sealed by DPGP. The chemical reaction of DPGP and dentin indicated that DPGP combined with CO2 laser is a potential regimen for the treatment of vertical root fracture.

U-PuO2, U-PuC, U-PuN cermet fuel for fast reactor

NASA Astrophysics Data System (ADS)

Mishra, Sudhir; Kaity, Santu; Banerjee, Joydipta; Nandi, Chiranjeet; Dey, G. K.; Khan, K. B.

2018-02-01

Cermet fuel combines beneficial properties of both ceramic and metal and attracts global interest for research as a candidate fuel for nuclear reactors. In the present study, U matrix PuC/PuN/PuO2 cermet for fast reactor have been fabricated on laboratory scale by the powder metallurgy route. Characterization of the fuel has been carried out using Dilatometer, Differential Thermal analysis (DTA), X-ray diffractometer and Optical microscope. X ray diffraction study of the fuel reveals presence of different phases. The PuN dispersed cermet was observed to have high solidus temperature as compared to PuC and PuO2 dispersed cermet. Swelling was observed in U matrix PuO2 cermet which also showed higher thermal expansion. Among the three cermets studied, U matrix PuC cermet showed maximum thermal conductivity.

The crystal structure of the new ternary antimonide Dy 3Cu 20+xSb 11-x ( x≈2)

NASA Astrophysics Data System (ADS)

Fedyna, L. O.; Bodak, O. I.; Fedorchuk, A. O.; Tokaychuk, Ya. O.

2005-06-01

New ternary antimonide Dy 3Cu 20+xSb 11-x ( x≈2) was synthesized and its crystal structure was determined by direct methods from X-ray powder diffraction data (diffractometer DRON-3M, Cu Kα-radiation, R=6.99%,R=12.27%,R=11.55%). The compound crystallizes with the own cubic structure type: space group F 4¯ 3m, Pearson code cF272, a=16.6150(2) Å,Z=8. The structure of the Dy 3Cu 20Sb 11-x ( x≈2) can be obtained from the structure type BaHg 11 by doubling of the lattice parameter and subtraction of 16 atoms. The studied structure was compared with the structures of known compounds, which crystallize in the same space group with similar cell parameters.

Laser-induced Multi-energy Processing in Diamond Growth

DTIC Science & Technology

2012-05-01

microscopy (SEM) and energy dispersive X - ray (EDX) measurements, Drs. Yi Liu and Shah Valloppilly from Nebraska Center for Materials and Nanoscience...NCMN) at UNL for help on X - Ray diffraction (XRD) measurements, and Professor Steve W. Martin and Dr. Young Sik Kim from the Department of Material...spectroscopy and X - ray diffraction ................... 62 4.4 Conclusions

Scanning electron microscopy/energy dispersive spectrometry fixedbeam or overscan x-ray microanalysis of particles can miss the real structure: x-ray spectrum image mapping reveals the true nature

NASA Astrophysics Data System (ADS)

Newbury, Dale E.; Ritchie, Nicholas W. M.

2013-05-01

The typical strategy for analysis of a microscopic particle by scanning electron microscopy/energy dispersive spectrometry x-ray microanalysis (SEM/EDS) is to use a fixed beam placed at the particle center or to continuously overscan to gather an "averaged" x-ray spectrum. While useful, such strategies inevitably concede any possibility of recognizing microstructure within the particle, and such fine scale structure is often critical for understanding the origins, behavior, and fate of particles. Elemental imaging by x-ray mapping has been a mainstay of SEM/EDS analytical practice for many years, but the time penalty associated with mapping with older EDS technology has discouraged its general use and reserved it more for detailed studies that justified the time investment. The emergence of the high throughput, high peak stability silicon drift detector (SDD-EDS) has enabled a more effective particle mapping strategy: "flash" x-ray spectrum image maps can now be recorded in seconds that capture the spatial distribution of major (concentration, C > 0.1 mass fraction) and minor (0.01 <= C <= 0.1) constituents. New SEM/SDD-EDS instrument configurations feature multiple SDDs that view the specimen from widely spaced azimuthal angles. Multiple, simultaneous measurements from different angles enable x-ray spectrometry and mapping that can minimize the strong geometric effects of particles. The NIST DTSA-II software engine is a powerful aid for quantitatively analyzing EDS spectra measured individually as well as for mapping information (available free for Java platforms at: http://www.cstl.nist.gov/div837/837.02/epq/dtsa2/index.html).

DOE Office of Scientific and Technical Information (OSTI.GOV)

Madden, Jeremy T.; Toth, Scott J.; Dettmar, Christopher M.

Nonlinear optical (NLO) instrumentation has been integrated with synchrotron X-ray diffraction (XRD) for combined single-platform analysis, initially targeting applications for automated crystal centering. Second-harmonic-generation microscopy and two-photon-excited ultraviolet fluorescence microscopy were evaluated for crystal detection and assessed by X-ray raster scanning. Two optical designs were constructed and characterized; one positioned downstream of the sample and one integrated into the upstream optical path of the diffractometer. Both instruments enabled protein crystal identification with integration times between 80 and 150 µs per pixel, representing a ~10 3–10 4-fold reduction in the per-pixel exposure time relative to X-ray raster scanning. Quantitative centering andmore » analysis of phenylalanine hydroxylase fromChromobacterium violaceumcPAH,Trichinella spiralisdeubiquitinating enzyme TsUCH37, human κ-opioid receptor complex kOR-T4L produced in lipidic cubic phase (LCP), intimin prepared in LCP, and α-cellulose samples were performed by collecting multiple NLO images. The crystalline samples were characterized by single-crystal diffraction patterns, while α-cellulose was characterized by fiber diffraction. Good agreement was observed between the sample positions identified by NLO and XRD raster measurements for all samples studied.« less

Unconventional Synthesis of γ-Fe2O3: Excellent Low-Concentration Ethanol Sensing Performance

NASA Astrophysics Data System (ADS)

Naskar, Atanu; Narjinary, Mousumi; Kundu, Susmita

2017-01-01

This study reports on a simple unconventional procedure for synthesis of γ-Fe2O3 nanopowder and its fabrication as a resistive ethanol sensor. γ-Fe2O3 powder having an average particle size of ˜15 nm was prepared by thermal decomposition of iron(III) acetylacetonate. Platinum incorporation (0.5-1.5 wt.%) was also carried out for enhancing sensing performance. The powders were characterized using an x-ray diffractometer, x-ray photoelectron spectroscopy, Brunauer-Emmett-Teller surface area, field area scanning electron microscopy, transmission electron microscopy along with energy dispersion x-ray analyses. Sensor fabricated from pure γ-Fe2O3 exhibited excellent ethanol sensing performance at concentrations down to 1 ppm, having a great demand in medical diagnosis and food-processing industries. The response observed for pure γ-Fe2O3 (˜75% for 1 ppm ethanol) was enhanced ˜10% after 1 wt.% Pt impregnation. Sensors were quite stable and selective towards ethanol vapour detection. A possible mechanism for high sensing performance has been discussed.

Crystal growth, structural, thermal and mechanical behavior of l-arginine 4-nitrophenolate 4-nitrophenol dihydrate (LAPP) single crystals.

PubMed

Mahadevan, M; Ramachandran, K; Anandan, P; Arivanandhan, M; Bhagavannarayana, G; Hayakawa, Y

2014-12-10

Single crystals of l-arginine 4-nitrophenolate 4-nitrophenol dihydrate (LAPP) have been grown successfully from the solution of l-arginine and 4-nitrophenol. Slow evaporation of solvent technique was adopted to grow the bulk single crystals. Single crystal X-ray diffraction analysis confirms the grown crystal has monoclinic crystal system with space group of P21. Powder X-ray diffraction analysis shows the good crystalline nature. The crystalline perfection of the grown single crystals was analyzed by HRXRD by employing a multicrystal X-ray diffractometer. The functional groups were identified from proton NMR spectroscopic analysis. Linear and nonlinear optical properties were determined by UV-Vis spectrophotometer and Kurtz powder technique respectively. It is found that the grown crystal has no absorption in the green wavelength region and the SHG efficiency was found to be 2.66 times that of the standard KDP. The Thermal stability of the crystal was found by obtaining TG/DTA curve. The mechanical behavior of the grown crystal has been studied by Vicker's microhardness method. Copyright © 2014 Elsevier B.V. All rights reserved.

1998 Technology Showcase. JOAP International Condition Monitoring Conference.

DTIC Science & Technology

1998-04-01

Systems using Automated SEM/ EDX and New Diagnostic Routines 276 N. W Farrant & T. Luckhurst ADVANCED DIAGNOSTIC SYSTEMS Model-Based Diagnostics of Gas...Microscopy with Energy Dispersive X-Ray (SEM/ EDX ) micro analysis packages and Energy Dispersive X-Ray Fluorescence (EDXRF) analytical equipment. Therqfore...wear particles separated by ferrogram method. a- I WEAR PARTICLE A SLAS 97 (HOME PAGE) Fig I Home Page NONFE;RROUS MATERIAL A wW~ a48 -1, rV fr , ý b

Tandem transmission/reflection mode XRD instrument including XRF for in situ measurement of Martian rocks and soils

NASA Astrophysics Data System (ADS)

Delhez, Robert; Van der Gaast, S. J.; Wielders, Arno; de Boer, J. L.; Helmholdt, R. B.; van Mechelen, J.; Reiss, C.; Woning, L.; Schenk, H.

2003-02-01

The mineralogy of the surface material of Mars is the key to disclose its present and past life and climates. Clay mineral species, carbonates, and ice (water and CO2) are and/or contain their witnesses. X-ray powder diffraction (XRPD) is the most powerful analytical method to identify and quantitatively characterize minerals in complex mixtures. This paper discusses the development of a working model of an instrument consisting of a reflection mode diffractometer and a transmission mode CCD-XRPD instrument, combined with an XRF module. The CCD-XRD/XRF instrument is analogous to the instrument for Mars missions developed by Sarrazin et al. (1998). This part of the tandem instrument enables "quick and dirty" analysis of powdered (!) matter to monitor semi-quantitatively the presence of clay minerals as a group, carbonates, and ices and yields semi-quantitative chemical information from X-ray fluorescence (XRF). The reflection mode instrument (i) enables in-situ measurements of rocks and soils and quantitative information on the compounds identified, (ii) has a high resolution and reveals large spacings for accurate identification, in particular of clay mineral species, and (iii) the shape of the line profiles observed reveals the kind and approximate amounts of lattice imperfections present. It will be shown that the information obtained with the reflection mode diffractometer is crucial for finding signs of life and changes in the climate on Mars. Obviously this instrument can also be used for other extra-terrestrial research.

Simple route to (NH4)xWO3 nanorods for near infrared absorption

NASA Astrophysics Data System (ADS)

Guo, Chongshen; Yin, Shu; Dong, Qiang; Sato, Tsugio

2012-05-01

Described here is how to synthesize one-dimensional ammonium tungsten bronze ((NH4)xWO3) by a facile solvothermal approach in which ethylene glycol and acetic acid were employed as solvents and ammonium paratungstate was used as a starting material, as well as how to develop the near infrared absorption properties of (NH4)xWO3 nanorods for application as a solar light control filter. The as-obtained product was characterized by field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), thermogravimetry (TG), atomic force microscope (AFM) and UV-Vis-NIR spectra. The SEM and TEM images clearly revealed that the obtained sample possessed rod/fiber-like morphologies with diameters around 120 nm. As determined by UV-Vis-NIR optical measurement, the thin film consisted of (NH4)xWO3 nanoparticles, which can selectively transmit most visible lights, but strongly absorb the near-infrared (NIR) lights and ultraviolet rays. These interesting optical properties make the (NH4)xWO3 nanorods suitable for the solar control windows.Described here is how to synthesize one-dimensional ammonium tungsten bronze ((NH4)xWO3) by a facile solvothermal approach in which ethylene glycol and acetic acid were employed as solvents and ammonium paratungstate was used as a starting material, as well as how to develop the near infrared absorption properties of (NH4)xWO3 nanorods for application as a solar light control filter. The as-obtained product was characterized by field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), thermogravimetry (TG), atomic force microscope (AFM) and UV-Vis-NIR spectra. The SEM and TEM images clearly revealed that the obtained sample possessed rod/fiber-like morphologies with diameters around 120 nm. As determined by UV-Vis-NIR optical measurement, the thin film consisted of (NH4)xWO3 nanoparticles, which can selectively transmit most visible lights, but strongly absorb the near-infrared (NIR) lights and ultraviolet rays. These interesting optical properties make the (NH4)xWO3 nanorods suitable for the solar control windows. Electronic supplementary information (ESI) available. See DOI: 10.1039/c2nr30612c

Phosphorus Effects of Mesoporous Bioactive Glass on Occlude Exposed Dentin

PubMed Central

Chen, Wen-Cheng; Chen, Cheng-Hwei; Kung, Jung-Chang; Hsiao, Yu-Cheng; Shih, Chi-Jen; Chien, Chi-Sheng

2013-01-01

In recent studies, sealing of exposed dentinal tubules is generally considered as one of the most effective strategies to treat dentin hypersensitivity. Mesoporous bioactive glass (MBG) is a potential material for treating dentin hypersensitivity due to its highly specific areas for dissolution and re-precipitated reaction for reduction in dentin permeability. The groups of commercial products of PerioGlas®, synthetic MBG and MBG without phosphorus (MBGNP) were compared. The MBG and MBGNP powders were prepared by the sol-gel method and mixed with different calculated ratios of phosphoric acid (PA) and then was brushed onto dentin surfaces. We used X-ray diffractometer (XRD), scanning electronic microscope (SEM), and Fourier transform infrared spectroscopy (FTIR) to investigate the physiochemistry and the occlusion ability of dentinal tubules. The results showed that MBG paste mixed with PA solution has a better ability for occluding dentinal tubules than MBGNP; it has a short reaction time and good operability. The major crystallite phase of MBG agents was monocalcium phosphate monohydrate [Ca(H2PO4)2·H2O] in the early stages of the reactions. MBG pastes that were mixed with 30% and 40% PA had the ability to create excellent penetration depth greater than 80 μm. These agents have the potential to treat dentin hypersensitivity. PMID:28788393

Microstructure and phase analyses of melt-spun Si-Ni base anode materials for Li-ion battery

NASA Astrophysics Data System (ADS)

Jeon, Sung Min; Song, Jong Jin; Kim, Sun-I.; Kwon, Hye Jin; Sohn, Keun Yong; Park, Won-Wook

2013-01-01

Si-based anode composite materials have been studied to improve the performance and the durability of Li-ion secondary batteries in this study. Si-Ni-Al, Si-Ni-Cu and Si-Ni-Cu-Al base alloys were designed and rapidly solidified at the cooling rate of about 106 °C/sec by optimizing the melt spinning. The ribbons were characterized using FE-SEM equipped with EDS, X-ray diffractometer and HR-TEM. The thin ribbons of Si-Ni-Al alloy consisted of nano-sized Si particles and amorphous matrix, which was regarded as an ideal microstructure for the anode material. At the wheel side of the ribbon, 20-30 nm of Si particles were formed (Zone A); whereas at the air side relatively large Si particles were distributed (Zone B). The Si-Ni-Cu alloy showed coarser Si particles than the Si-Ni-Al alloy, and its matrix consisted of NiSi2, Cu3Si and amorphous structures. Finally, the microstructure of the Si-Ni-Cu-Al alloy strips was composed of coarse Si particles, CuNi, Al4Cu9, NiSi2, and unknown phases, and the size of those Si particles were too large to be used for the anode materials.

Degradation phenomena of magnetic attachments used clinically in the oral environment

NASA Astrophysics Data System (ADS)

Chung, Chae-Heon; Choe, Han-Cheol; Kwak, Jong-Ha

2006-08-01

The purpose of this study was to investigate the mechanisms involved in the failure of magnetic attachments used to retain dental prostheses. Dyna magnets were retrieved from dentures that had failed after 34 months of clinical use. These magnetic attachments were prepared and sectioned so as to observe the corrosion surface and layer in order to analyze the corrosion behaviors of the attachments. The corroded surface was observed under a field emission scanning electron microscope (FE-SEM) (JSM 840A, JEOL, Japan). An X-ray diffractometer (XRD) was used to analyze the corrosion product formed due to corrosion in the oral environment. Erosion-corrosion started in the uneven portion of the stainless steel cover in the magnetic attachments composed with Nd-Fe-B alloy. Corrosion was initiated on the worn stainless steel surface, followed by spalling of magnetic material due to corrosive solution. The corrosion rate increased drastically after the corrosion product caused spalling in Nd-Fe-B alloy. Corrosion initiated in the uneven stainless steel surface as well as in the welded zone. In conclusion, the failure of magnetic attachments may occur by either welding failure or breakdown of the encapsulating material. Thus, we believe that treating the surface of magnetic attachments would resolve the corrosion problem seen in magnetic attachments to some extent.

A Nanoporous Carbon/Exfoliated Graphite Composite For Supercapacitor Electrodes

NASA Astrophysics Data System (ADS)

Rosi, Memoria; Ekaputra, Muhamad P.; Iskandar, Ferry; Abdullah, Mikrajuddin; Khairurrijal

2010-12-01

Nanoporous carbon was prepared from coconut shells using a simple heating method. The nanoporous carbon is subjected to different treatments: without activation, activation with polyethylene glycol (PEG), and activation with sodium hydroxide (NaOH)-PEG. The exfoliated graphite was synthesized from graphite powder oxidized with zinc acetate (ZnAc) and intercalated with polyvinyl alcohol (PVA) and NaOH. A composite was made by mixing the nanoporous carbon with NaOH-PEG activation, the exfoliated graphite and a binder of PVA solution, grinding the mixture, and annealing it using ultrasonic bath for 1 hour. All of as-synthesized materials were characterized by employing a scanning electron microscope (SEM), a MATLAB's image processing toolbox, and an x-ray diffractometer (XRD). It was confirmed that the composite is crystalline with (002) and (004) orientations. In addition, it was also found that the composite has a high surface area, a high distribution of pore sizes less than 40 nm, and a high porosity (67%). Noting that the pore sizes less than 20 nm are significant for ionic species storage and those in the range of 20 to 40 nm are very accessible for ionic clusters mobility across the pores, the composite is a promising material for the application as supercapacitor electrodes.

Effect of zirconia nanoparticles on the rheological properties of silica-based shear thickening fluid

NASA Astrophysics Data System (ADS)

Sun, Li; Zhu, Jie; Wei, Minghai; Zhang, Chunwei; Song, Yansheng; Qi, Peipei

2018-05-01

In this study, the rheological characteristic of shear thickening fluid (STF) with various mass ratios of zirconium dioxide (ZrO2) to silicon dioxide (SiO2) was investigated. The influence of the ZrO2 mass ratio on the sensitivity of nano-ZrO2/SiO2-STF to temperature was further discussed. Nano-ZrO2/SiO2-STF of different concentrations (9.0–20.0 wt%) were prepared via an ultrasonication and mechanical stirring technique. The presence of ZrO2 and their interaction with the SiO2 nanoparticles in the STF were analyzed using scanning electron microscope (SEM), Energy dispersive spectroscopy (EDS) and x-ray diffractometer (XRD). The rheological testing results showed that the ZrO2/SiO2-STF system produced a considerable shear thickening effect; when the nano-ZrO2 mass ratio was 12%, the critical shear rate of the system was relatively small and the peak value of apparent viscosity was relatively large. More importantly, as the nano-ZrO2 mass ratio increased, temperature exerted less influence on the viscosity of the ZrO2/SiO2-STF system diminished, but still had a significant influence on the shear thickening effect.

Microstructure and Microhardness of 17-4PH Deposited with Co-based Alloy Hardfacing Coating

NASA Astrophysics Data System (ADS)

Deng, D. W.; Zhang, C. P.; Chen, R.; Xia, H. F.

Hardfacing is widely used to improve the performance of components exposed to severe service conditions. In this paper, the surface modification was evaluated for precipitation hardening martensitic stainless steel 17-4PH deposited with Co-based alloy stellite12 by the plasma-transferred arc welding (PTAW). The microstructure and microhardness of coating and heat affected zone(HAZ) of base metal were characterized by optical microscope (OM), scanning electron scanning microscope (SEM), X-ray diffractometer and hardness tester. The results show that the interface between weld metal and base metal is favorable without pore and crack, at the same time elements diffusion is observed in the fusion area. However, as the distance from the interface increases, HAZ comprises three different microstructural zones, namely, zones of coarse overheated structures, quenching martensite and martensite, ferrite. The microhardness decreases gradually from the HAZ near interface to the base metal, except the zone of coarse overheated structures. The microhardness of the coating improves a lot and fluctuates in a definitive range, and microstructural gradient is observed including the fusion area (the planar region and the bulky dendrite in a direction perpendicular to the weld interface), the transition zone (the dendrite in a multi-direction way) and the fine grain zone near the surface in the coating (fine equiaxial structure).

High-resolution 3D analyses of the shape and internal constituents of small volcanic ash particles: The contribution of SEM micro-computed tomography (SEM micro-CT)

NASA Astrophysics Data System (ADS)

Vonlanthen, Pierre; Rausch, Juanita; Ketcham, Richard A.; Putlitz, Benita; Baumgartner, Lukas P.; Grobéty, Bernard

2015-02-01

The morphology of small volcanic ash particles is fundamental to our understanding of magma fragmentation, and in transport modeling of volcanic plumes and clouds. Until recently, the analysis of 3D features in small objects (< 250 μm) was either restricted to extrapolations from 2D approaches, partial stereo-imaging, or CT methods having limited spatial resolution and/or accessibility. In this study, an X-ray computed-tomography technique known as SEM micro-CT, also called 3D X-ray ultramicroscopy (3D XuM), was used to investigate the 3D morphology of small volcanic ash particles (125-250 μm sieve fraction), as well as their vesicle and microcrystal distribution. The samples were selected from four stratigraphically well-established tephra layers of the Meerfelder Maar (West Eifel Volcanic Field, Germany). Resolution tests performed on a Beametr v1 pattern sample along with Monte Carlo simulations of X-ray emission volumes indicated that a spatial resolution of 0.65 μm was obtained for X-ray shadow projections using a standard thermionic SEM and a bulk brass target as X-ray source. Analysis of a smaller volcanic ash particle (64-125 μm sieve fraction) showed that features with volumes > 20 μm3 (~ 3.5 μm in diameter) can be successfully reconstructed and quantified. In addition, new functionalities of the Blob3D software were developed to allow the particle shape factors frequently used as input parameters in ash transport and dispersion models to be calculated. This study indicates that SEM micro-CT is very well suited to quantify the various aspects of shape in fine volcanic ash, and potentially also to investigate the 3D morphology and internal structure of any object < 0.1 mm3.

Optimisation d'analyses de grenat almandin realisees au microscope electronique a balayage

NASA Astrophysics Data System (ADS)

Larose, Miguel

The electron microprobe (EMP) is considered as the golden standard for the collection of precise and representative chemical composition of minerals in rocks, but data of similar quality should be obtainable with a scanning electron microscope (SEM). This thesis presents an analytical protocol aimed at optimizing operational parameters of an SEM paired with an EDS Si(Li) X-ray detector (JEOL JSM-840A) for the imaging, quantitative chemical analysis and compositional X-ray maps of almandine garnet found in pelitic schists from the Canadian Cordillera. Results are then compared to those obtained for the same samples on a JEOL JXA 8900 EMP. For imaging purposes, the secondary electrons and backscattered electrons signals have been used to obtain topographic and chemical contrast of the samples, respectively. The SEM allows the acquisition of images with higher resolution than the EMP when working at high magnifications. However, for millimetric size minerals requiring very low magnifications, the EMP can usually match the imaging capabilities of an SEM. When optimizing images for both signals, the optimal operational parameters to show similar contrasts are not restricted to a unique combination of values. Optimization of operational parameters for quantitative chemical analysis resulted in analytical data with a similar precision and showing good correlation to that obtained with an EMP. Optimization of operational parameters for compositional X-ray maps aimed at maximizing the collected intensity within a pixel as well as complying with the spatial resolution criterion in order to obtain a qualitative compositional map representative of the chemical variation within the grain. Even though various corrections were needed, such as the shadow effect and the background noise removal, as well as the impossibility to meet the spatial resolution criterion because of the limited pixel density available on the SEM, the compositional X-ray maps show a good correlation with those obtained with the EMP, even for concentrations as low as 0,5%. When paired with a rigorous analytical protocol, the use of an SEM equipped with an EDS Si (Li) X-ray detector allows the collection of qualitative and quantitative results similar to those obtained with an EMP for all three of the applications considered.

Three-dimensional mapping of soil chemical characteristics at micrometric scale: Statistical prediction by combining 2D SEM-EDX data and 3D X-ray computed micro-tomographic images

NASA Astrophysics Data System (ADS)

Hapca, Simona

2015-04-01

Many soil properties and functions emerge from interactions of physical, chemical and biological processes at microscopic scales, which can be understood only by integrating techniques that traditionally are developed within separate disciplines. While recent advances in imaging techniques, such as X-ray computed tomography (X-ray CT), offer the possibility to reconstruct the 3D physical structure at fine resolutions, for the distribution of chemicals in soil, existing methods, based on scanning electron microscope (SEM) and energy dispersive X-ray detection (EDX), allow for characterization of the chemical composition only on 2D surfaces. At present, direct 3D measurement techniques are still lacking, sequential sectioning of soils, followed by 2D mapping of chemical elements and interpolation to 3D, being an alternative which is explored in this study. Specifically, we develop an integrated experimental and theoretical framework which combines 3D X-ray CT imaging technique with 2D SEM-EDX and use spatial statistics methods to map the chemical composition of soil in 3D. The procedure involves three stages 1) scanning a resin impregnated soil cube by X-ray CT, followed by precision cutting to produce parallel thin slices, the surfaces of which are scanned by SEM-EDX, 2) alignment of the 2D chemical maps within the internal 3D structure of the soil cube, and 3) development, of spatial statistics methods to predict the chemical composition of 3D soil based on the observed 2D chemical and 3D physical data. Specifically, three statistical models consisting of a regression tree, a regression tree kriging and cokriging model were used to predict the 3D spatial distribution of carbon, silicon, iron and oxygen in soil, these chemical elements showing a good spatial agreement between the X-ray grayscale intensities and the corresponding 2D SEM-EDX data. Due to the spatial correlation between the physical and chemical data, the regression-tree model showed a great potential in predicting chemical composition in particular for iron, which is generally sparsely distributed in soil. For carbon, silicon and oxygen, which are more densely distributed, the additional kriging of the regression tree residuals improved significantly the prediction, whereas prediction based on co-kriging was less consistent across replicates, underperforming regression-tree kriging. The present study shows a great potential in integrating geo-statistical methods with imaging techniques to unveil the 3D chemical structure of soil at very fine scales, the framework being suitable to be further applied to other types of imaging data such as images of biological thin sections for characterization of microbial distribution. Key words: X-ray CT, SEM-EDX, segmentation techniques, spatial correlation, 3D soil images, 2D chemical maps.

Applications of synchrotron x-ray diffraction topography to fractography

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bilello, J.C.

1983-01-01

Fractographs have been taken using a variety of probes each of which produces different types of information. Methods which have been used to examine fracture surfaces include: (a) optical microscopy, particularly interference contrast methods, (b) scanning electron microscopy (SEM), (c) SEM with electron channelling, (d) SEM with selected-area electron channelling, (e) Berg-Barrett (B-B) topography, and now (f) synchrotron x-radiation fractography (SXRF). This review concentrated on the role that x-ray methods can play in such studies. In particular, the ability to nondestructively assess the subsurface microstructure associated with the fracture to depths of the order of 5 to 10 ..mu..m becomesmore » an important attribute for observations of a large class of semi-brittle metals, semiconductors and ceramics.« less

Elucidating the Wavelength Dependence of Phonon Scattering in Nanoparticle-Matrix Composites using Phonon Spectroscopy

DTIC Science & Technology

2016-07-11

composites with x - ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), Rutherford backscattering spectroscopy...RBS), particle-induced x - ray emission (PIXE), and energy dispersive x - ray spectroscopy (EDX). This work complements earlier works on CdSe...sample shows only In2Se3 and CdIn2Se4 XRD peaks (Figure 1.4e), it is stoichiometrically   Figure 1.4. X - ray diffraction patterns of (a) γ-In2Se3

Catharanthus roseus: a natural source for the synthesis of silver nanoparticles

PubMed Central

Mukunthan, KS; Elumalai, EK; Patel, Trupti N; Murty, V Ramachandra

2011-01-01

Objective To develop a simple rapid procedure for bioreduction of silver nanoparticles (AgNPs) using aqueous leaves extracts of Catharanthus roseus (C. roseus). Methods Characterization were determined by using UV-Vis spectrophotometry, scanning electron microscopy (SEM), energy dispersive X-ray and X-ray diffraction. Results SEM showed the formation of silver nanoparticles with an average size of 67 nm to 48 nm. X-ray diffraction analysis showed that the particles were crystalline in nature with face centered cubic geometry. Conclusions C. roseus demonstrates strong potential for synthesis of silver nanoparticles by rapid reduction of silver ions (Ag+ to Ag0). This study provides evidence for developing large scale commercial production of value-added products for biomedical/nanotechnology-based industries. PMID:23569773

Effect of Doping Materials on the Low-Level NO Gas Sensing Properties of ZnO Thin Films

NASA Astrophysics Data System (ADS)

Çorlu, Tugba; Karaduman, Irmak; Yildirim, Memet Ali; Ateş, Aytunç; Acar, Selim

2017-07-01

In this study, undoped, Cu-doped, and Ni-doped ZnO thin films have been successfully prepared by successive ionic layer adsorption and reaction method. The structural, compositional, and morphological properties of the thin films are characterized by x-ray diffractometer, energy dispersive x-ray analysis (EDX), and scanning electron microscopy, respectively. Doping effects on the NO gas sensing properties of these thin films were investigated depending on gas concentration and operating temperature. Cu-doped ZnO thin film exhibited a higher gas response than undoped and Ni-doped ZnO thin film at the operating temperature range. The sensor with Cu-doped ZnO thin film gave faster responses and recovery speeds than other sensors, so that is significant for the convenient application of gas sensor. The response and recovery speeds could be associated with the effective electron transfer between the Cu-doped ZnO and the NO molecules.

Geotechnical characterization of some Indian fly ashes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Das, S.K.; Yudhbir

2005-10-01

This paper reports the findings of experimental studies with regard to some common engineering properties (e.g., grain size, specific gravity, compaction characteristics, and unconfined compression strength) of both low and high calcium fly ashes, to evaluate their suitability as embankment materials and reclamation fills. In addition, morphology, chemistry, and mineralogy of fly ashes are studied using scanning electron microscope, electron dispersive x-ray analyzer, x-ray diffractometer, and infrared absorption spectroscopy. In high calcium fly ash, mineralogical and chemical differences are observed for particles, {gt}75 {mu} m and the particles of {lt} 45 {mu} m size. The mode and duration of curingmore » significantly affect the strength and stress-strain behavior of fly ashes. The geotechnical properties of fly ash are governed by factors like lime content (CaO), iron content (Fe{sub 2}O{sub 3}) and loss on ignition. The distinct difference between self-hardening and pozzolanic reactivity has been emphasized.« less

Low orthopyroxene from a lunar deep crustal rock - A new pyroxene polymorph of space group P21ca

NASA Technical Reports Server (NTRS)

Smyth, J. R.

1974-01-01

Bronzite crystals (En86Fs11Wo3) from a slowly-cooled lunar troctolitic granulite, have space group P21ca, a postulated, but previously unreported space group. Diffractions violating the b-glide extinction conditions have been observed in long-exposure X-ray precession photographs from three of these crystals and on an automated X-ray diffractometer. P21ca is a subgroup of the common orthopyroxene space group Pbca, and its cell dimensions (a = 18.235 plus or minus 0.004 A, b = 8.831 plus or minus 0.002 A, c = 5.189 plus or minus 0.001 A) are similar to those of terrestrial bronzites. It is postulated that the lower symmetry space group has developed as a result of very slow cooling at pressures of one to two kilobars deep in the lunar crust.

The new HMI beamline MAGS: an instrument for hard X-ray diffraction at BESSY.

PubMed

Dudzik, Esther; Feyerherm, Ralf; Diete, Wolfgang; Signorato, Riccardo; Zilkens, Christopher

2006-11-01

The Hahn-Meitner-Institute Berlin is operating the new hard X-ray diffraction beamline MAGS at the Berlin synchrotron radiation source BESSY. The beamline is intended to complement the existing neutron instrumentation at the Berlin Neutron Scattering Centre. The new beamline uses a 7 T multipole wiggler to produce photon fluxes in the 10(11)-10(12) photons s(-1) (100 mA)(-1) (0.1% bandwidth)(-1) range at energies from 4 to 30 keV at the experiment. It has active bendable optics to provide flexible horizontal and vertical focusing and to compensate the large heat load from the wiggler source. The experimental end-station consists of a six-circle Huber diffractometer which can be used with an additional (polarization) analyser and different sample environments. The beamline is intended for single-crystal diffraction and resonant magnetic scattering experiments for the study of ordering phenomena, phase transitions and materials science.

Viscosity studies of water based magnetite nanofluids

DOE Office of Scientific and Technical Information (OSTI.GOV)

Anu, K.; Hemalatha, J.

2016-05-23

Magnetite nanofluids of various concentrations have been synthesized through co-precipitation method. The structural and topographical studies made with the X-Ray Diffractometer and Atomic Force Microscope are presented in this paper. The density and viscosity studies for the ferrofluids of various concentrations have been made at room temperature. The experimental viscosities are compared with theoretical values obtained from Einstein, Batchelor and Wang models. An attempt to modify the Rosensweig model is made and the modified Rosensweig equation is reported. In addition, new empirical correlation is also proposed for predicting viscosity of ferrofluid at various concentrations.

Hydrogen atoms can be located accurately and precisely by x-ray crystallography.

PubMed

Woińska, Magdalena; Grabowsky, Simon; Dominiak, Paulina M; Woźniak, Krzysztof; Jayatilaka, Dylan

2016-05-01

Precise and accurate structural information on hydrogen atoms is crucial to the study of energies of interactions important for crystal engineering, materials science, medicine, and pharmacy, and to the estimation of physical and chemical properties in solids. However, hydrogen atoms only scatter x-radiation weakly, so x-rays have not been used routinely to locate them accurately. Textbooks and teaching classes still emphasize that hydrogen atoms cannot be located with x-rays close to heavy elements; instead, neutron diffraction is needed. We show that, contrary to widespread expectation, hydrogen atoms can be located very accurately using x-ray diffraction, yielding bond lengths involving hydrogen atoms (A-H) that are in agreement with results from neutron diffraction mostly within a single standard deviation. The precision of the determination is also comparable between x-ray and neutron diffraction results. This has been achieved at resolutions as low as 0.8 Å using Hirshfeld atom refinement (HAR). We have applied HAR to 81 crystal structures of organic molecules and compared the A-H bond lengths with those from neutron measurements for A-H bonds sorted into bonds of the same class. We further show in a selection of inorganic compounds that hydrogen atoms can be located in bridging positions and close to heavy transition metals accurately and precisely. We anticipate that, in the future, conventional x-radiation sources at in-house diffractometers can be used routinely for locating hydrogen atoms in small molecules accurately instead of large-scale facilities such as spallation sources or nuclear reactors.

Hydrogen atoms can be located accurately and precisely by x-ray crystallography

PubMed Central

Woińska, Magdalena; Grabowsky, Simon; Dominiak, Paulina M.; Woźniak, Krzysztof; Jayatilaka, Dylan

2016-01-01

Precise and accurate structural information on hydrogen atoms is crucial to the study of energies of interactions important for crystal engineering, materials science, medicine, and pharmacy, and to the estimation of physical and chemical properties in solids. However, hydrogen atoms only scatter x-radiation weakly, so x-rays have not been used routinely to locate them accurately. Textbooks and teaching classes still emphasize that hydrogen atoms cannot be located with x-rays close to heavy elements; instead, neutron diffraction is needed. We show that, contrary to widespread expectation, hydrogen atoms can be located very accurately using x-ray diffraction, yielding bond lengths involving hydrogen atoms (A–H) that are in agreement with results from neutron diffraction mostly within a single standard deviation. The precision of the determination is also comparable between x-ray and neutron diffraction results. This has been achieved at resolutions as low as 0.8 Å using Hirshfeld atom refinement (HAR). We have applied HAR to 81 crystal structures of organic molecules and compared the A–H bond lengths with those from neutron measurements for A–H bonds sorted into bonds of the same class. We further show in a selection of inorganic compounds that hydrogen atoms can be located in bridging positions and close to heavy transition metals accurately and precisely. We anticipate that, in the future, conventional x-radiation sources at in-house diffractometers can be used routinely for locating hydrogen atoms in small molecules accurately instead of large-scale facilities such as spallation sources or nuclear reactors. PMID:27386545

Symposium LL: Nanowires--Synthesis Properties Assembly and Application

DTIC Science & Technology

2010-09-10

dedicated hard x - ray microscopy beamline is operated in partnership with the Advanced Photon Source to provide fluorescence, diffraction, and...characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X - ray diffraction (XRD) measurements, proving it to be...Investigation of Preferred Growth Direction of GaN Nanorods by Synchrotron X - ray Reciprocal Space Mapping. Yuri Sohn1, Sanghwa Lee1, Chinkyo Kim1 and Dong

Introducing a New Capability at SSRL: Resonant Soft X-ray Scattering

NASA Astrophysics Data System (ADS)

Lee, Jun-Sik; Jang, Hoyoung; Lu, Donghui; Kao, Chi-Chang

Stanford Synchrotron Radiation Lightsource (SSRL) at SLAC recently developed a setup for the resonant soft x-ray scattering (RSXS). In general, the RSXS technique uniquely probes not only structural information, but also chemical specific information. This is because this technique can explore the spatial periodicities of charge, orbital, spin, and lattice with spectroscopic aspect. Moreover, the soft x-ray range is particularly relevant for a study of soft materials as it covers the K-edge of C, N, F, and O, as well as the L-edges of transition metals and M-edges of rare-earth elements. Hence, the RSXS capability has been regarded as a very powerful technique for investigating the intrinsic properties of materials such as quantum- and energy-materials. The RSXS capability at the SSRL composes of in-vacuum 4-circle diffractometer. There are also the fully motorized sample-motion manipulations. Also, the sample can be cooled down to 25 K via the liquid helium. This capability has been installed at BL 13-3, where the photon source is from elliptically polarized undulator (EPU). Covering the photon energies is from 230 eV to 1400 eV. Furthermore, this EPU system offers more degree of freedoms for controlling x-ray polarizations (linear and circular). Using the advance of controlling x-ray polarization, we can also investigate a morphology effect of local domain/grain in materials. The detailed introduction of the RSXS end-station and several results will be touched in this poster presentation.

Edge-Selectively Functionalized Graphene-Like Platelets as a Co-curing Agent and a Nanoscale Additive to Epoxy Resin

DTIC Science & Technology

2012-08-12

21 For mass production , the Report Documentation Page Form ApprovedOMB No. 0704-0188 Public reporting burden for the collection of information is...analyzer. The field emission scanning electron microscope ( FE -SEM) used in this work was a NanoSem 230 (FEI, USA). High-resolution transmission...WAXD) powder patterns were recorded with a Rigaku RU-200 diffractometer using Ni-filtered Cu K radiation (40 kV, 100 mA,  = 0.15418 nm). Dynamic

An X-Ray Diffractometer for Mineralogical Analysis of Exomars Mission

NASA Astrophysics Data System (ADS)

Marinangeli, L.; Baliva, A.; Critani, F.; Stevoli, A.; Scandelli, L.; Holland, A.; Hutchinson, I.; Nelms, N.; Delhez, R.

2006-12-01

The new results of the Mars Exploration Rovers and the Mars Express mission outline the importance of a correct assessment of the variety of geological contexts to understand the evolution of a habitable environment. The need of having complex scientific payload to perform a broad range of in situ measurements is a necessary step for a successful exobiological exploration. Furthermore, the compositional analysis of the surface samples is of fundamental importance to characterize the geological environments where life could have arisen and their evolution through time. In the last years, there has been a strong interest in Europe to develop a x-ray diffractometer (XRD) for mineralogical analyses of planetary surfaces. The identification of minerals using the diffraction technique is based on the x-ray interference with the geometrical parameters of the crystal lattice allowing an unequivocal recognition of different minerals. An US XRD instrument, CHEMIN, will flight for the first time in the NASA Mars Science Laboratory in 2009. An European XRD design has also been selected for the Pasteur Payload of the ESA ExoMars mission, planned for 2011. The proposed instrument is a miniaturised concept (1 kg) configured in a reflection geometry and will allow the identification of a large spectrum of minerals including those related to the presence of water, key element for the development of life. The complete mineralogical analysis will be performed on very small quantities of powder rock samples, thought analysis of pristine (no grinded) sample can also be achieved with the reflection configuration. Information on the elemental composition of the sample can be roughly estimated by the analysis of the x-ray fluorescence spectrum simultaneously acquired by the detection system. In order to demonstrate the instrument technological readiness for the ExoMars mission, the construction of a demonstrative prototype is on going with ESA funding. Preliminary result of the scientific evaluation of the prototype will be shown to assess the capability of the proposed concept in the identification of rock mineralogy. IRSPS and and Laben are respectively the team science coordinator and the engineering responsible for the instrument development. The detector assembly for the prototype has been developed by UK and discussion for the UK involvement on the future instrument development is on going. Delft is providing scientific contribution for the prototype evaluation.

Nail Damage (Severe Onychodystrophy) Induced by Acrylate Glue: Scanning Electron Microscopy and Energy Dispersive X-Ray Investigations

PubMed Central

Pinteala, Tudor; Chiriac, Anca Eduard; Rosca, Irina; Larese Filon, Francesca; Pinteala, Mariana; Chiriac, Anca; Podoleanu, Cristian; Stolnicu, Simona; Coros, Marius Florin; Coroaba, Adina

2017-01-01

Background Scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) techniques have been used in various fields of medical research, including different pathologies of the nails; however, no studies have focused on obtaining high-resolution microscopic images and elemental analysis of disorders caused by synthetic nails and acrylic adhesives. Methods Damaged/injured fingernails caused by the use of acrylate glue and synthetic nails were investigated using SEM and EDX methods. Results SEM and EDX proved that synthetic nails, acrylic glue, and nails damaged by contact with acrylate glue have a different morphology and different composition compared to healthy human nails. Conclusions SEM and EDX analysis can give useful information about the aspects of topography (surface sample), morphology (shape and size), hardness or reflectivity, and the elemental composition of nails. PMID:28232921

Online in situ x-ray diffraction setup for structural modification studies during swift heavy ion irradiation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Grygiel, C.; Lebius, H.; Bouffard, S.

2012-01-15

The high energy density of electronic excitations due to the impact of swift heavy ions can induce structural modifications in materials. We present an x-ray diffractometer called ALIX (''Analyse en Ligne sur IRRSUD par diffraction de rayons X''), which has been set up at the low-energy beamline (IRRadiation SUD - IRRSUD) of the Grand Accelerateur National d'Ions Lourds facility, to allow the study of structural modification kinetics as a function of the ion fluence. The x-ray setup has been modified and optimized to enable irradiation by swift heavy ions simultaneously to x-ray pattern recording. We present the capability of ALIXmore » to perform simultaneous irradiation-diffraction by using energy discrimination between x-rays from diffraction and from ion-target interaction. To illustrate its potential, results of sequential or simultaneous irradiation-diffraction are presented in this article to show radiation effects on the structural properties of ceramics. Phase transition kinetics have been studied during xenon ion irradiation of polycrystalline MgO and SrTiO{sub 3}. We have observed that MgO oxide is radiation-resistant to high electronic excitations, contrary to the high sensitivity of SrTiO{sub 3}, which exhibits transition from the crystalline to the amorphous state during irradiation. By interpreting the amorphization kinetics of SrTiO{sub 3}, defect overlapping models are discussed as well as latent track characteristics. Together with a transmission electron microscopy study, we conclude that a single impact model describes the phase transition mechanism.« less

Synthesis and magnetic properties of NiFe2-xSmxO4 nanopowder

NASA Astrophysics Data System (ADS)

Hassanzadeh-Tabrizi, S. A.; Behbahanian, Shahrzad; Amighian, Jamshid

2016-07-01

NiFe2-xSmxO4 (x=0.00, 0.05, 0.10 and 0.15) nanopowders were synthesized via a sol-gel combustion route. The structural studies were carried out by X-ray diffractometer, Fourier transform infrared spectroscopy, scanning electron microscopy and transmission electron microscopy. The XRD results confirmed the formation of single-phase spinel cubic structure. The crystallite size decreased with an increase of samarium ion concentration, while lattice parameter and lattice strain increased with samarium substitution. TEM micrographs showed that agglomerated nanoparticles with particle sizes ranging from 35 to 90 nm were obtained. The magnetic studies were carried out using vibrating sample magnetometer. Magnetic measurements revealed that the saturation magnetization (Ms) of NiFe2-xSmxO4 nanoparticles decreases with increasing Sm3+substitution. The reduction of saturation magnetization is attributed to the dilution of the magnetic interaction. The coercivity (Hc) of samples increases by adding samarium.

Synthesis and statistical modelling of dry sliding wear of Al 8011/6 vol.% AlB2 in situ composite

NASA Astrophysics Data System (ADS)

Kumar, Narendra; Singh, Sandeep Kumar; Gautam, Gaurav; Padap, Aditya Kumar; Mohan, Anita; Mohan, Sunil

2017-10-01

The present study has used response surface methodology (RSM) and central composite design (CCD) for modelling, using wear parameters to predict the wear performance of an Al 8011/6.0 vol.% AlB2 composite. The effect of applied load and sliding velocity was studied at five levels for a fixed sliding distance. To understand wear behaviour, sliding wear tests were planned according to CCD and performed on a pin-on-disc apparatus at ambient temperature. An analysis of variance (ANOVA) was conducted to show the relative significance of the parameters. A second-order regression model was developed to predict the wear loss and to establish the relationships between wear parameters. Response surface and contour plots were drawn to analyse the wear results. Worn surfaces were examined under scanning electron microscope (SEM), and energy dispersive spectroscopy (EDS) was used to interpret the operative wear mechanisms. Validation tests results show good agreement between experimental and predicted data. As an initial step of this study, AlB2 particles were reinforced in Al 8011 alloy by an in situ technique to synthesise an Al 8011/6.0 vol.% AlB2 composite. During synthesis an in situ reaction takes place between molten alloy and inorganic salt KBF4 at 850 °C, which leads to the formation of AlB2 particles. The composite was analysed by x-ray diffractometer (XRD) to detect the phases present, while optical and scanning electron microscopy (OM & SEM) were carried out to ascertain morphology and particle distribution. Hardness was evaluated by a Vickers hardness testing machine.

Effects of a Ta interlayer on the phase transition of TiSi2 on Si(111)

NASA Astrophysics Data System (ADS)

Jeon, Hyeongtag; Jung, Bokhee; Kim, Young Do; Yang, Woochul; Nemanich, R. J.

2000-09-01

This study examines the effects of a thin Ta interlayer on the formation of TiSi2 on Si(111) substrate. The Ta interlayer was introduced by depositing Ta and Ti films sequentially on an atomically clean Si(111) substrate in an ultrahigh vacuum (UHV) system. Samples of 100 Å Ti with 5 and 10 Å Ta interlayers were compared to similar structures without an interlayer. After deposition, the substrates were annealed for 10 min, in situ, at temperatures between 500 and 750 °C in 50 °C increments. The TiSi2 formation with and without the Ta interlayer was analyzed with an X-ray diffractometer, Auger electron spectroscopy (AES), Scanning electron microscopy (SEM), transmission electron microscopy (TEM), and a four-point probe. The AES analysis data showed a 1:2 ratio of Ti:Si in the Ti-silicide layer and indicated that the Ta layer remained at the interface between TiSi2 and the Si(111) substrate. The C 49-C 54 TiSi2 phase transition temperature was lowered by ˜200 °C. The C 49-C 54 TiSi2 phase transition temperature was 550 °C for the samples with a Ta interlayer and was 750 °C for the samples with no Ta interlayer. The sheet resistance of the Ta interlayered Ti silicide showed lower values of resistivity at low temperatures which indicated the change in phase transition temperature. The C 54 TiSi2 displayed different crystal orientation when the Ta interlayer was employed. The SEM and TEM micrographs showed that the TiSi2 with a Ta interlayer significantly suppressed the tendency to islanding and surface agglomeration.

Phase Composition, Crystallite Size and Physical Properties of B2O3-added Forsterite Nano-ceramics

NASA Astrophysics Data System (ADS)

Pratapa, S.; Chairunnisa, A.; Nurbaiti, U.; Handoko, W. D.

2018-05-01

This study was aimed to know the effect of B2O3 addition on the phase composition, crystallite size and dielectric properties of forsterite (Mg2SiO4) nano-ceramics. It utilized a purified silica sand from Tanah Laut, South Kalimantan as the source of (amorphous) silica and a magnesium oxide (MgO) powder. They were thoroughly mixed and milled prior to calcination. The addition of 1, 2, 3, and 4 wt% B2O3 to the calcined powder was done before uniaxial pressing and then sintering at 950 °C for 4 h. The phase composition and forsterite crystallite size, the microstructure and the dielectric constant of the sintered samples were characterized using X-ray diffractometer (XRD), Scanning Electron Microscope (SEM) and Vector Network Analyzer (VNA), respectively. Results showed that all samples contained forsterite, periclase (MgO) and proto enstatite (MgSiO3) with different weight fractions and forsterite crystallite size. In general, the weight fraction and crystallite size of forsterite increased with increasing B2O3 addition. The weight fraction and crystallite size of forsterite in the 4%-added sample reached 99% wt and 164 nm. Furthermore, the SEM images showed that the average grain size became slightly larger and the ceramics also became slightly denser as more B2O3 was added. The results are in accordance with density measurements using the Archimedes method which showed that the 4% ceramic exhibited 1.845 g/cm3 apparent density, while the 1% ceramic 1.681 g/cm3. We also found that the higher the density, the higher the average dielectric constant, i.e. it was 4.6 for the 1%-added sample and 6.4 for the 4%-added sample.

ALICE—An advanced reflectometer for static and dynamic experiments in magnetism at synchrotron radiation facilities

DOE Office of Scientific and Technical Information (OSTI.GOV)

Abrudan, R.; Helmholtz-Zentrum-Berlin for Materials and Energy, 12489 Berlin; Brüssing, F.

2015-06-15

We report on significant developments of a high vacuum reflectometer (diffractometer) and spectrometer for soft x-ray synchrotron experiments which allows conducting a wide range of static and dynamic experiments. Although the chamber named ALICE was designed for the analysis of magnetic hetero- and nanostructures via resonant magnetic x-ray scattering, the instrument is not limited to this technique. The versatility of the instrument was testified by a series of pilot experiments. Static measurements involve the possibility to use scattering and spectroscopy synchrotron based techniques (photon-in photon-out, photon-in electron-out, and coherent scattering). Dynamic experiments require either laser or magnetic field pulses tomore » excite the spin system followed by x-ray probe in the time domain from nano- to femtosecond delay times. In this temporal range, the demagnetization/remagnetization dynamics and magnetization precession in a number of magnetic materials (metals, alloys, and magnetic multilayers) can be probed in an element specific manner. We demonstrate here the capabilities of the system to host a variety of experiments, featuring ALICE as one of the most versatile and demanded instruments at the Helmholtz Center in Berlin-BESSY II synchrotron center in Berlin, Germany.« less

A facile approach for the fabrication of 3D flower-like Cu2S nanostructures on brass mesh with temperature-induced wetting transition for efficient oil-water separation

NASA Astrophysics Data System (ADS)

Niu, Lei; Kang, Zhixin

2017-11-01

3D flower-like Cu2S nanostructures on brass meshes have been fabricated for the first time, with a reversible wetting transition and excellent durability. In the present work, we demonstrated a simple and environmentally-benign method to fabricate the nanostructures utilizing an electrolyte containing CuSO4·5H2O, EDTA-2Na and CH3CSNH2. The superhydrophobicity was achieved by drying thoroughly at 200 °C, instead of using low surface energy materials. After annealing at 300 °C for 6 min, the superhydrophobic surface was oxidized and became superhydrophilic. However, the superhydrophobicity can be restored by heating at 200 °C for several hours. In simpler terms, the reversible wetting transition is responded to the temperature. Scanning electron microscopy, X-ray diffractometer, energy-dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy were employed to characterize the surfaces and analyze the wetting transition mechanism. Furthermore, different kinds of oily sewages were separated by as-prepared mesh with high separation efficiency. It is believed that this method should have a promising future in expanding the applications of copper alloys.

Thermal vacancies and phase separation in bcc mixtures of helium-3 and helium-4

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fraass, Benedick Andrew

1980-01-01

Thermal vacancy concentrations in crystals of 3He- 4He mixtures have been determined. A new x-ray diffractometer-position sensitive detector system is used to make measurements of the absolute lattice parameter of the helium crystals with an accuracy of 300 ppM, and measurements of changes in lattice parameters to better than 60 ppM. The phase separation of the concentrated 3He- 4He mixtures has been studied in detail with the x-ray measurements. Vacancy concentrations in crystals with 99%, 51%, 28%, 12%, and 0% 3He have been determined. Phase separation has been studied in mixed crystals with concentrations of 51%, 28%, and 12% 3Hemore » and melting pressures between 3.0 and 6.1 MPa. The phase separation temperatures determined in this work are in general agreement with previous work. The pressure dependence of T c, the phase separation temperature for a 50% mixture, is found to be linear: dT c/dP = -34 mdeg/MPa. The x-ray measurements are used to make several comments on the low temperature phase diagram of the helium mixtures.« less

Integrated nonlinear optical imaging microscope for on-axis crystal detection and centering at a synchrotron beamline

PubMed Central

Madden, Jeremy T.; Toth, Scott J.; Dettmar, Christopher M.; Newman, Justin A.; Oglesbee, Robert A.; Hedderich, Hartmut G.; Everly, R. Michael; Becker, Michael; Ronau, Judith A.; Buchanan, Susan K.; Cherezov, Vadim; Morrow, Marie E.; Xu, Shenglan; Ferguson, Dale; Makarov, Oleg; Das, Chittaranjan; Fischetti, Robert; Simpson, Garth J.

2013-01-01

Nonlinear optical (NLO) instrumentation has been integrated with synchrotron X-ray diffraction (XRD) for combined single-platform analysis, initially targeting applications for automated crystal centering. Second-harmonic-generation microscopy and two-photon-excited ultraviolet fluorescence microscopy were evaluated for crystal detection and assessed by X-ray raster scanning. Two optical designs were constructed and characterized; one positioned downstream of the sample and one integrated into the upstream optical path of the diffractometer. Both instruments enabled protein crystal identification with integration times between 80 and 150 µs per pixel, representing a ∼103–104-fold reduction in the per-pixel exposure time relative to X-ray raster scanning. Quantitative centering and analysis of phenylalanine hydroxylase from Chromobacterium violaceum cPAH, Trichinella spiralis deubiquitinating enzyme TsUCH37, human κ-opioid receptor complex kOR-T4L produced in lipidic cubic phase (LCP), intimin prepared in LCP, and α-cellulose samples were performed by collecting multiple NLO images. The crystalline samples were characterized by single-crystal diffraction patterns, while α-cellulose was characterized by fiber diffraction. Good agreement was observed between the sample positions identified by NLO and XRD raster measurements for all samples studied. PMID:23765294

X-ray line profile analysis of BaTiO3 thin film prepared by sol-gel deposition

NASA Astrophysics Data System (ADS)

Ooi, Zeen Vee; Saif, Ala'eddin A.; Wahab, Yufridin; Jamal, Zul Azhar Zahid

2017-04-01

Barium titanate (BaTiO3) thin film was prepared using sol-gel method and spun-coated on SiO2/Si substrate. The phase and crystallinity of the synthesized film were identified using X-ray diffractometer (XRD), which scanned at the range of 20° to 60°. The phase and lattice parameters of the fabricated film were extracted from the recorded XRD patterns using lattice geometry equations. The crystallite size and lattice strain were determined using X-ray line profile analysis (XLPA) with various approaches. The Scherrer equation was applied to the perovskite peaks of the film to explore the size contribution on the peak broadening. Meanwhile, the Williamson-Hall and size-strain plot (SSP) methods were used to review two main independent contributions, i.e. crystallite sizes and lattice strain, on the X-ray line broadening. From the analysis, it is found that Scherrer method gives smallest crystallite size value by ignoring the strain-induced broadening effect. On the other hand, Williamson-Hall and SSP graphs revealed the existence of the lattice strain within the film, which contributes to the broadening in the Bragg peak. The results that analyzed via both techniques show a linear trend with all data points fitted. However, result obtained from SSP method gives better settlement due to the best fit of the data.

The synthesis of Fe3O4/MWCNT nanocomposites from local iron sands for electrochemical sensors

NASA Astrophysics Data System (ADS)

Rahmawati, Retno; Taufiq, Ahmad; Sunaryono, Yuliarto, Brian; Suyatman, Nugraha, Noviandri, Indra; Setyorini, Dian Ayu; Kurniadi, Deddy

2018-05-01

The aim of this research is producing the electrochemical sensor, especially for working electrodes based on the nanocomposites of multi-walled carbon nanotube (MWCNT) and magnetite (Fe3O4) nanoparticles from iron sands. The sonochemical method by ultrasonic horn was successfully used for the synthesis of the nanocomposites. The characterizations of the sample were conducted via X-Ray Diffractometer (XRD), Fourier Transform Infra-Red (FTIR) Spectrometer, Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), Brunauer-Emmett-Teller (BET) method for surface area, Vibrating Sample Magnetometer (VSM) and Cyclic Voltammetry (CV). The analysis of X-Ray Diffraction (XRD) pattern showed two phases of crystalline, namely MWCNT and Fe3O4, peak of MWCNT comes from (002) plan while peaks of Fe3O4 come from (2 2 0), (3 1 1), (4 0 0), (4 2 2), (5 1 1), and (4 4 0) plans. From XRD data, MWCNT has a hexagonal structure and Fe3O4 has inverse spinel cubic structure, respectively. The FTIR spectra revealed that the functionalization process of MWCNT successfully generated carboxyl and carbonyl groups to bind Fe3O4 on MWCNT surfaces. Moreover, the functional groups of Fe-O bonding that showed the existence of Fe3O4 in the nanocomposites were also detected in those spectra. Meanwhile, the SEM and TEM images showed that the nanoparticles of Fe3O4 attached on the MWCNT surface and formed agglomeration between particles due to magnetic forces. Through Brunauer-Emmett-Teller (BET) method, it is identified that the nanocomposite has a large surface area 318 m2/g that makes this material very suitable for electrochemical sensor applications. Moreover, the characterization of magnetic properties via Vibrating Sample Magnetometer (VSM) showed that the nanocomposites have superparamagnetic behavior at room temperature and the presence of the MWCNT reduced the magnetic properties of Fe3O4. Lastly, the electrochemical characterization with Cyclic Voltammetry (CV) proved that Fe3O4/MWCNT nanocomposites with iron sands as the starting materials have high sensitivity and serve as excellent electron transfer materials. Based on the results of the research, the Fe3O4/MWCNT nanocomposites from iron sands are much recommended for electrochemical sensor.

Dopant concentration dependent growth of Fe:ZnO nanostructures

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sahai, Anshuman; Goswami, Navendu, E-mail: navendugoswami@gmail.com

2016-05-23

Systematic investigations of structural properties of 1-10% Fe doped ZnO nanostructure (Fe:ZnO NS) prepared via chemical precipitation method have been reported. Structural properties were probed thoroughly employing scanning electron microscope (SEM) and transmission electron microscope (TEM), energy dispersive X-ray (EDAX) analysis and X-ray diffraction (XRD). Morphological transformation of nanostructures (NS) with Fe incorporation is evident in SEM/TEM images. Nanoparticles (NP) obtained with 1% Fe, evolve to nanorods (NR) for 3% Fe; NR transform to nanocones (NC) (for 5% and 7% Fe) and finally NC transform to nanoflakes (NF) at 10% Fe. Morover, primary phase of Zn{sub 1-x}Fe{sub x}O along withmore » secondary phases of ZnFe{sub 2}O{sub 4} and Fe{sub 2}O{sub 3} were also revealed through XRD measurements. Based on collective XRD, SEM, TEM, and EDAX interpretations, a model for morphological evolution of NS was proposed and the pivotal role of Fe dopant was deciphered.« less

A new look at lunar soil collected from the sea of tranquility during the Apollo 11 mission.

PubMed

Kiely, Carol; Greenberg, Gary; Kiely, Christopher J

2011-02-01

Complementary state-of-the-art optical, scanning electron, and X-ray microscopy techniques have been used to study the morphology of Apollo 11 lunar soil particles (10084-47). The combination of innovative lighting geometries with image processing of a through focal series of images has allowed us to obtain a unique collection of high-resolution light micrographs of these fascinating particles. Scanning electron microscopy (SEM) stereo-pair imaging has been exploited to illustrate some of the unique morphological properties of lunar regolith. In addition, for the first time, X-ray micrographs with submicron resolution have been taken of individual particles using X-ray ultramicroscopy (XuM). This SEM-based technique lends itself readily to the imaging of pores, cracks, and inclusions and allows the internal structure of an entire particle to be viewed. Rotational SEM and XuM movies have also been constructed from a series of images collected at sequential angles through 360°. These offer a new and insightful view of these complex particles providing size, shape, and spatial information on many of their internal features.

Scanning Electron Microscope-Cathodoluminescence Analysis of Rare-Earth Elements in Magnets.

PubMed

Imashuku, Susumu; Wagatsuma, Kazuaki; Kawai, Jun

2016-02-01

Scanning electron microscope-cathodoluminescence (SEM-CL) analysis was performed for neodymium-iron-boron (NdFeB) and samarium-cobalt (Sm-Co) magnets to analyze the rare-earth elements present in the magnets. We examined the advantages of SEM-CL analysis over conventional analytical methods such as SEM-energy-dispersive X-ray (EDX) spectroscopy and SEM-wavelength-dispersive X-ray (WDX) spectroscopy for elemental analysis of rare-earth elements in NdFeB magnets. Luminescence spectra of chloride compounds of elements in the magnets were measured by the SEM-CL method. Chloride compounds were obtained by the dropwise addition of hydrochloric acid on the magnets followed by drying in vacuum. Neodymium, praseodymium, terbium, and dysprosium were separately detected in the NdFeB magnets, and samarium was detected in the Sm-Co magnet by the SEM-CL method. In contrast, it was difficult to distinguish terbium and dysprosium in the NdFeB magnet with a dysprosium concentration of 1.05 wt% by conventional SEM-EDX analysis. Terbium with a concentration of 0.02 wt% in an NdFeB magnet was detected by SEM-CL analysis, but not by conventional SEM-WDX analysis. SEM-CL analysis is advantageous over conventional SEM-EDX and SEM-WDX analyses for detecting trace rare-earth elements in NdFeB magnets, particularly dysprosium and terbium.

Young's modulus and SEM analysis of leg bones exposed to simulated microgravity by hind limb suspension (HLS)

NASA Astrophysics Data System (ADS)

Patel, Niravkumar D.; Mehta, Rahul; Ali, Nawab; Soulsby, Michael; Chowdhury, Parimal

2013-04-01

The aim of this study was to determine composition of the leg bone tissue of rats that were exposed to simulated microgravity by Hind-Limb Suspension (HLS) by tail for one week. The leg bones were cross sectioned, cleaned of soft tissues, dried and sputter coated, and then placed horizontally on the stage of a Scanning Electron Microscope (SEM) for analysis. Interaction of a 17.5 keV electron beam, incident from the vertical direction on the sample, generated images using two detectors. X-rays emitted from the sample during electron bombardment were measured with an Energy Dispersive Spectroscopy (EDS) feature of SEM using a liquid-nitrogen cooled Si(Li) detector with a resolution of 144 eV at 5.9 keV (25Mn Kα x-ray). Kα- x-rays from carbon, oxygen, phosphorus and calcium formed the major peaks in the spectrum. Relative percentages of these elements were determined using a software that could also correct for ZAF factors namely Z(atomic number), A(X-ray absorption) and F(characteristic fluorescence). The x-rays from the control groups and from the experimental (HLS) groups were analyzed on well-defined parts (femur, tibia and knee) of the leg bone. The SEM analysis shows that there are definite changes in the hydroxyl or phosphate group of the main component of the bone structure, hydroxyapatite [Ca10(PO4)6(OH)2], due to hind limb suspension. In a separate experiment, entire leg bones (both from HLS and control rats) were subjected to mechanical stress by mean of a variable force. The stress vs. strain graph was fitted with linear and polynomial function, and the parameters reflecting the mechanical strength of the bone, under increasing stress, were calculated. From the slope of the linear part of the graph the Young's modulus for HLS bones were calculated and found to be 2.49 times smaller than those for control bones.

Experiments on planetary ices at UCL

NASA Astrophysics Data System (ADS)

Grindrod, P. M.; Fortes, A. D.; Wood, I. G.; Dobson, D.; Sammonds, P. R.; Stone-Drake, L.; Vocadlo, L.

2007-08-01

Using a suite of techniques and equipment, we conduct several different types of experiments on planetary ices at UCL. Samples are prepared in the Ice Physics Laboratory, which consists of a 5 chamber complex of inter-connected cold rooms, controllable from +30 to -30 deg C. Within this laboratory we have a functioning triaxial deformation cell operating at low temperature (down to -90 deg C) and high pressures (300 MPa), an Automatic Ice Fabric Analyser (AIFA) and a low-temperature microscope with CCD output. Polycrystalline samples, 40mm diameter by 100mm long, are compressed in the triaxial rig with a confining pressure; single crystal specimens are compressed in a separate uniaxial creep rig which operates at zero confining pressure for surface studies. A cold stage is also available for study of ice microstructural studies on our new Jeol JSM-6480LV SEM, which also allows tensile, compression and/or bending tests, with load ranges from less than 2N to 5000N. Finally, we also use a cold stage on a new PANalytical, X'pert PRO MPD, high resolution powder diffractometer to study the structure and phase behaviour of icy materials. Recent highlights of our work include: (1) derivation of a manufacturing process for methane clathrate at low temperatures, analysed in the X-Ray Diffraction Laboratory, for future rheological experiments, (2) analysed the growth behaviour of MS11, (3) refurbished and commenced calibration tests on the triaxial deformation cell using ice Ih, and (4) performed creep tests on gypsum and epsomite using the single crystal deformation cell. Further experiments will build on these preliminary results.

Investigation on thermo physical characteristics of ethylene glycol based Al:ZnO nanofluids

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kiruba, R., E-mail: krbranjini@gmail.com, E-mail: drkingson@karunya.edu; George, Ritty; Gopalakrishnan, M.

2015-06-24

The present work describes the experimental aspects of viscosity and thermal conductivity characteristics of nanofluids. Aluminium doped zinc oxide nanostructures were synthesized by chemical precipitation method. Ultrasonic technique is used to disperse the nanostructures in ethylene glycol. Structural and morphological properties of Al doped ZnO nanostructures are characterized using X-ray diffractometer and scanning electron microscopic technique. The effect of concentration and temperature on thermo-physical properties of Al/ZnO nanofluids is also investigated. The experimental results showed there is enhancement in thermal conductivity with rise in temperature which can be utilized for coolant application.

Synthesis of Zn1-xCdxO Nanoparticles by Co-Precipitation: Structural, Optical and Photodetection Analysis

NASA Astrophysics Data System (ADS)

Jacob, Anju Anna; Balakrishnan, L.; Meher, S. R.; Shambavi, K.; Alex, Z. C.

Zinc oxide (ZnO) is a wide bandgap semiconductor with excellent photoresponse in ultra-violet (UV) regime. Tuning the bandgap of ZnO by alloying with cadmium can shift its absorption cutoff wavelength from UV to visible (Vis) region. Our work aims at synthesis of Zn1-xCdxO nanoparticles by co-precipitation method for the fabrication of photodetector. The properties of nanoparticles were analyzed using X-ray diffractometer, UV-Vis spectrometer, scanning electron microscope and energy dispersive spectrometer. The incorporation of cadmium without altering the wurtzite structure resulted in the red shift in the absorption edge of ZnO. Further, the photoresponse characteristics of Zn1-xCdxO nanopowders were investigated by fabricating photodetectors. It has been found that with Cd alloying the photosensitivity was increased in the UVA-violet as well in the blue region.

Alloy composition effects on oxidation products of VIA, B-1900, 713C, and 738X: A high temperature diffractometer study

NASA Technical Reports Server (NTRS)

Garlick, R. G.; Lowell, C.

1973-01-01

High temperature X-ray diffraction studies were performed to investigate isothermal and cyclic oxidation at 1000 and 1100 C of the nickel-base superalloys VIA, B-1900, 713C, and 738X. Oxidation was complex. The major oxides, Al2O3, Cr2O3, and the spinels, formed in amounts consistent with alloy chemistry. The alloys VIA and B-1900 (high Al, low Cr alloys) tended to form Al2O3 and NiAl2O4; 738X (high Cr, low Al) formed Cr2O3 and NiCr2O4. A NiTa2O6 type of oxide formed in amounts approximately proportional to the refractory metal content of the alloy. One of the effects of cycling was to increase the amount of spinels formed.

Properties of WO3-x Electrochromic Thin Film Prepared by Reactive Sputtering with Various Post Annealing Temperatures

NASA Astrophysics Data System (ADS)

Kim, Min Hong; Choi, Hyung Wook; Kim, Kyung Hwan

2013-11-01

The WO3-x thin films were prepared on indium tin oxide (ITO) coated glass at 0.7 oxygen flow ratio [O2/(Ar+O2)] using the facing targets sputtering (FTS) system at room temperature. In order to obtain the annealing effect, as-deposited thin films were annealed at temperatures of 100, 200, 300, 400, and 500 °C for 1 h in open air. The structural properties of the WO3-x thin film were measured using an X-ray diffractometer. The WO3-x thin films annealed at up to 300 °C indicated amorphous properties, while those annealed above 400 °C indicated crystalline properties. The electrochemical and optical properties of WO3-x thin films were measured using cyclic voltammetry and a UV/vis spectrometer. The maximum value of coloration efficiency obtained was 34.09 cm2/C for thin film annealed at 200 °C. The WO3-x thin film annealed at 200 °C showed superior electrochromic properties.

Symposium U: Thermoelectric Power Generation. Held in Boston, Massachusetts on November 26-29, 2007

DTIC Science & Technology

2008-04-01

including X - ray /electron diffraction, TGA analysis, Raman / Fourier Transform Infrared Spectroscopy, electron microscopy, Rutherford back-scattering and...Energy dispersive X - ray analysis were performed on the treated sample. The results revealed that a surface layer (from 10 nm to up to micron in...nanoparticles into a matrix of bulk Bi2Te 3 material via a hot pressing process. These nanocomposites have been examined by SEM and X - ray powder

Low-temperature high magnetic field powder x-ray diffraction setup for field-induced structural phase transition studies from 2 to 300 K and at 0 to 8-T field

NASA Astrophysics Data System (ADS)

Shahee, Aga; Sharma, Shivani; Kumar, Dhirendra; Yadav, Poonam; Bhardwaj, Preeti; Ghodke, Nandkishor; Singh, Kiran; Lalla, N. P.; Chaddah, P.

2016-10-01

A low-temperature and high magnetic field powder x-ray diffractometer (XRD) has been developed at UGC-DAE CSR (UGC: University Grant Commission, DAE: Department of Atomic Energy, and CSR: Consortium for scientific research), Indore, India. The setup has been developed around an 18 kW rotating anode x-ray source delivering Cu-Kα x-rays coming from a vertical line source. It works in a symmetric θ-2θ parallel beam geometry. It consists of a liquid helium cryostat with an 8 T split-pair Nb-Ti superconducting magnet comprising two x-ray windows each covering an angular range of 65°. This is mounted on a non-magnetic type heavy duty goniometer equipped with all necessary motions along with data collection accessories. The incident x-ray beam has been made parallel using a parabolic multilayer mirror. The scattered x-ray is detected using a NaI detector through a 0.1° acceptance solar collimator. To control the motions of the goniometer, a computer programme has been developed. The wide-angle scattering data can be collected in a range of 2°-115° of 2θ with a resolution of ˜0.1°. The whole setup is tightly shielded for the scattered x-rays using a lead hutch. The functioning of the goniometer and the artifacts arising possibly due to the effect of stray magnetic field on the goniometer motions, on the x-ray source, and on the detector have been characterized by collecting powder XRD data of a National Institute of Standards and Technology certified standard reference material LaB6 (SRM-660b) and Si powder in zero-field and in-field conditions. Occurrence of field induced structural-phase transitions has been demonstrated on various samples like Pr0.5Sr0.5MnO3, Nd0.49Sr0.51MnO3-δ and La0.175Pr0.45Ca0.375MnO3 by collecting data in zero field cool and field cool conditions.

Preparation, Structural Characterization and Magnetic Properties of La-SUBSTITUTED co Ferrites via a Modified Citrate Precursor Route

NASA Astrophysics Data System (ADS)

Ai, Lunhong; Jiang, Jing

CoLaxFe2-xO4 (x = 0.00, 0.05 and 0.1) nanoparticles were prepared simply by a modified citrate precursor route. Effects of La-substituting level on the their magnetic properties were investigated on the basis of the structural analysis. The thermal evolution of the precursor, as well as the microstructure of as-prepared products were studied by means of a thermogravimetric analyzer (TGA), X-ray diffractometer (XRD) and Fourier transform infrared (FTIR) spectrometer. The magnetic properties of the as-prepared samples were measured using a vibrating sample magnetometer (VSM). It was found that the magnetic properties were dependent on many factors such as La-substituting level, particle size and microstructure. The observed saturation magnetization decreased with increasing La content, whereas coercivity exhibited reverse behavior.

Synthesis and luminescence properties of Sm3+ doped CaTiO3 nanophosphor for application in white LED under NUV excitation.

PubMed

Shivaram, M; Nagabhushana, H; Sharma, S C; Prashantha, S C; Daruka Prasad, B; Dhananjaya, N; Hari Krishna, R; Nagabhushana, B M; Shivakumara, C; Chakradhar, R P S

2014-07-15

CaTiO3:Sm(3+) (1-11 mol%) nanophosphors were successfully synthesized by a low temperature solution combustion method [LCS]. The structural and morphological properties of the phosphors were studied by using Powder X-ray diffractometer (PXRD), Fourier transform infrared (FTIR), X-ray photo electron spectroscopy (XPS), scanning electron microscope (SEM) and transmission electron microscopy (TEM). TEM studies indicate that the size of the phosphor is ∼20-35 nm. Photoluminescence (PL) properties of Sm(3+) (1-11 mol%) doped CaTiO3 for NUV excitation (407 nm) was studied in order to investigate the possibility of its use in White light emitting diode (WLED) applications. The emission spectra consists of intra 4f transitions of Sm(3+), such as (4)G5/2→(6)H5/2 (561 nm), (4)G5/2→(6)H7/2 (601-611 nm), (4)G5/2→(6)H9/2 (648 nm) and (4)G5/2→(6)H11/2 (703 nm) respectively. Further, the emission at 601-611 nm show strong orange-red emission and can be applied to the orange-red emission of phosphor for the application for near ultra violet (NUV) excitation. Thermoluminescence (TL) of the samples irradiated with gamma source in the dose range 100-500 Gy was recorded at a heating rate of 5°Cs(-1). Two well resolved glow peaks at 164°C and 214°C along with shouldered peak at 186°C were recorded. TL intensity increases up to 300 Gy and thereafter, it decreases with further increase of dose. The kinetic parameters namely activation energy (E), frequency factor (s) and order of kinetics were estimated and results were discussed in detail. Copyright © 2014 Elsevier B.V. All rights reserved.

Effect of mechanical alloying synthesis process on the dielectric properties of (Bi{sub 0.5}Na{sub 0.5}){sub 0.94}Ba{sub 0.06}TiO{sub 3} piezoceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ghazanfari, Mohammad Reza, E-mail: Ghazanfari.mr@gmail.com; Amini, Rasool; Shams, Seyyedeh Fatemeh

Highlights: • MA samples show higher dielectric permittivity and Curie temperature. • In MA samples, dielectric loss is almost 27% less than conventional ones. • In MA samples, sintering time and temperature are lower than conventional ones. • In MA samples, particle morphology is more homogeneous conventional ones. • In MA samples, crystallite size is smaller conventional ones. - Abstract: In present work, in order to study the effects of synthesis techniques on dielectric properties, the BNBT lead-free piezoceramics with (Bi{sub 0.5}Na{sub 0.5}){sub 0.94}Ba{sub 0.06}TiO{sub 3} stoichiometry (called as BNBT6) were synthesized by mechanical alloying (MA) and conventional mixed oxidesmore » methods. The structural, microstructural, and dielectric properties were carried out by X-ray diffractometer (XRD), scanning electron microscope (SEM), and impedance analyzer LCR meter, respectively. Based on results, the density of MA samples is considerably higher than conventional samples owning to smaller particles size and more uniformity of particle shape of MA samples. Moreover, the dielectric properties of MA samples are comparatively improved in which the dielectric loss of these samples is almost 27% less than conventional ones. Furthermore, MA samples exhibit obviously higher dielectric permittivity and Curie temperature compared to the conventional samples.« less

Estimation of Crystallinity of Nifedipine-Polyvinylpyrrolidone Solid Dispersion by Usage of Terahertz Time-Domain Spectroscopy and of X-Ray Powder Diffractometer.

PubMed

Takeuchi, Issei; Shimakura, Kemmaro; Kuroda, Hideki; Nakajima, Takehisa; Goto, Satoru; Makino, Kimiko

2015-12-01

Crystalline state of pharmaceutical materials is of great importance in preparation of pharmaceutics, because their physicochemical properties affect bioavailability, quality of products, therapeutic level and manufacturing process. In this study, we have estimated time-dependent changes of nifedipine in nifedipine-polyvinylpyrrolidone (PVP) solid dispersion by measuring terahertz time-domain spectroscopy (THz-TDS) and by X-ray powder diffractometry (XRPD), and compared their correlativity. Crystallinity of nifedipine-PVP solid dispersion was changed by storing the amorphous sample at 25°C-75°C and relative humidity of over 80% for 0.25-24.00 h. To compare the results of two types of measurements, we have used a general method of linear regression analysis. Crystallinities estimated using THz-TDS were plotted on the x-axis and that of XRPD were on the y-axis. From the result of the calculation, the correlativity of them was confirmed. THz-TDS has the capability of becoming the replacement of XRPD. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

X-ray diffraction, FTIR, UV-VIS and SEM studies on chromium (III) complexes

NASA Astrophysics Data System (ADS)

Mishra, Ashutosh; Dwivedi, Jagrati; Shukla, Kritika

2015-06-01

Five Chromium (III) complexes have been prepared using Schiff base ligands which derived from benzoin and five different amino acids (H2N-R). Samples were characterized by XRD, FTIR, UV-VIS and SEM method. X-Ray diffraction pattern analyzed that all chromium (III) complexes have hexagonal structure and crystalline, in nature, using Bruker D8 Advance instrument. Using VERTAX 70, FTIR spectroscopy reveals that Samples have (C=N), (C-O), (M-N) and (M-O) bonds in the range of 4000-400cm-1. UV-VIS spectroscopy give information that samples absorb the visible light which is in the range of 380-780nm. For this, Lambda 960 spectrometer used. SEM is designed for studying of the solid objects, using JEOL JSM 5600 instrument.

Rigorous quantitative elemental microanalysis by scanning electron microscopy/energy dispersive x-ray spectrometry (SEM/EDS) with spectrum processing by NIST DTSA-II

NASA Astrophysics Data System (ADS)

Newbury, Dale E.; Ritchie, Nicholas W. M.

2014-09-01

Quantitative electron-excited x-ray microanalysis by scanning electron microscopy/silicon drift detector energy dispersive x-ray spectrometry (SEM/SDD-EDS) is capable of achieving high accuracy and high precision equivalent to that of the high spectral resolution wavelength dispersive x-ray spectrometer even when severe peak interference occurs. The throughput of the SDD-EDS enables high count spectra to be measured that are stable in calibration and resolution (peak shape) across the full deadtime range. With this high spectral stability, multiple linear least squares peak fitting is successful for separating overlapping peaks and spectral background. Careful specimen preparation is necessary to remove topography on unknowns and standards. The standards-based matrix correction procedure embedded in the NIST DTSA-II software engine returns quantitative results supported by a complete error budget, including estimates of the uncertainties from measurement statistics and from the physical basis of the matrix corrections. NIST DTSA-II is available free for Java-platforms at: http://www.cstl.nist.gov/div837/837.02/epq/dtsa2/index.html).

Development of X-ray micro-focus computed tomography to image and quantify biofilms in central venous catheter models in vitro.

PubMed

Niehaus, Wilmari L; Howlin, Robert P; Johnston, David A; Bull, Daniel J; Jones, Gareth L; Calton, Elizabeth; Mavrogordato, Mark N; Clarke, Stuart C; Thurner, Philipp J; Faust, Saul N; Stoodley, Paul

2016-09-01

Bacterial infections of central venous catheters (CVCs) cause much morbidity and mortality, and are usually diagnosed by concordant culture of blood and catheter tip. However, studies suggest that culture often fails to detect biofilm bacteria. This study optimizes X-ray micro-focus computed tomography (X-ray µCT) for the quantification and determination of distribution and heterogeneity of biofilms in in vitro CVC model systems.Bacterial culture and scanning electron microscopy (SEM) were used to detect Staphylococcus epidermidis ATCC 35984 biofilms grown on catheters in vitro in both flow and static biofilm models. Alongside this, X-ray µCT techniques were developed in order to detect biofilms inside CVCs. Various contrast agent stains were evaluated using energy-dispersive X-ray spectroscopy (EDS) to further optimize these methods. Catheter material and biofilm were segmented using a semi-automated matlab script and quantified using the Avizo Fire software package. X-ray µCT was capable of distinguishing between the degree of biofilm formation across different segments of a CVC flow model. EDS screening of single- and dual-compound contrast stains identified 10 nm gold and silver nitrate as the optimum contrast agent for X-ray µCT. This optimized method was then demonstrated to be capable of quantifying biofilms in an in vitro static biofilm formation model, with a strong correlation between biofilm detection via SEM and culture. X-ray µCT has good potential as a direct, non-invasive, non-destructive technology to image biofilms in CVCs, as well as other in vivo medical components in which biofilms accumulate in concealed areas.

Effect Of Neodymium Substitution In Structural Characteristics Of Magnesium Ferrite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Thankachan, Smitha; Binu, P. J.; Xavier, Sheena

2011-10-20

The effect of Nd{sup 3+} substitution on the structural properties of Magnesium ferrite was studied in the series MgNd{sub x}Fe{sub 2-x}O{sub 4}, where x = 0 to 0.3 in steps of 0.05. The series was prepared by sol-gel technique which is one of the novel technique to prepare nanosized samples. Structural characterization was done using X-ray diffractometer and Fourier Transform Infrared Spectrometer. XRD analysis reveals the prepared samples are single phasic till x = 0.2. From x0 = .25, a secondary phase of iron neodymium oxide appears along with the spinel phase. Particle size calculation shows the prepared samples aremore » in the 9nm to 11 nm regime. Lattice parameter was found to increase with concentration of Nd. XRD and FTIR analysis confirmed spinel structure of the prepared samples. XRF result shows the expected composition of prepared samples. The frequency dependence of the dielectric constant in the range 100 Hz--120MHz was also studied« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Takagi, H., E-mail: takagih@post.kek.jp; Igarashi, N.; Mori, T.

BL-6A has been operational since 2011 as a small angle X-ray scattering (SAXS) beamline at the Photon Factory (PF), and beginning in 2013 its old components and systems, which were mainly inside the experimental hutch, have been extensively updated. Both the vacuum-passes located between the sample stage and the detector and the fixed surface plate have been replaced by a new semi-automatic diffractometer. These upgrades allow simultaneous SAXS/WAXS experiments and grazing-incidence small angle X-ray scattering (GISAXS) measurements to be conducted. The hybrid pixel detector PILATUS3 1M is installed for SAXS, and PILATUS 100K is available as a WAXS detector. Additionally,more » a pinhole equipped with a micro-ion chamber is available to realize a lower-background and higher-resolution of low angles. Moreover, in a simultaneous SAXS/WAXS experiment, we developed a new beam stop with an embedded photodiode. Thus, BL-6A has evolved into a multipurpose beamline capable of dealing with various types of samples and experimental techniques.« less

Study on the surface sulfidization behavior of smithsonite at high temperature

NASA Astrophysics Data System (ADS)

Lv, Jin-fang; Tong, Xiong; Zheng, Yong-xing; Xie, Xian; Wang, Cong-bing

2018-04-01

Surface sulfidization behavior of smithsonite at high temperature was investigated by X-ray powder diffractometer (XRD) along with thermodynamic calculation, X-ray photoelectron spectroscopy (XPS) and electron probe microanalysis (EPMA). The XRD and thermodynamic analyses indicated that the smithsonite was decomposed into zincite at high temperatures. After introducing a small amount of pyrite, artificial sulfides were formed at surface of the obtained zincite. The XPS analyses revealed that the sulfide species including zinc sulfide and zinc disulfide were generated at the zincite surface. The EPMA analyses demonstrated that the film of sulfides was unevenly distributed at the zincite surface. The average concentration of elemental sulfur at the sample surface increased with increasing of pyrite dosage. A suitable mole ratio of FeS2 to ZnCO3 for the surface thermal modification was determined to be about 0.3. These findings can provide theoretical support for improving the process during which the zinc recovery from refractory zinc oxide ores is achieved by xanthate flotation.

Optical, Fluorescence with quantum analysis of hydrazine (1, 3- Dinitro Phenyl) by DFT and Ab initio approach

NASA Astrophysics Data System (ADS)

Cecily Mary Glory, D.; Sambathkumar, K.; Madivanane, R.; Velmurugan, G.; Gayathri, R.; Nithiyanantham, S.; Venkatachalapathy, M.; Rajkamal, N.

2018-07-01

Experimental and computational study of molecular structure, vibrational and UV-spectral analysis of Hydrazine (1, 3- Dinitrophenyl) (HDP) derivatives. The crystal was grown by slow cooling method and the crystalline perfection of single crystals was evaluated by high resolution X-ray diffractometry (HRXRD) using a multicrystal X-ray diffractometer. Fluorescence, FT-IR and FT-Raman spectra of HDP crystal were recorded. The assignments of the vibrational spectra have been carried out with the help of normal co-ordinate analysis (NCA) followed by scaled quantum force field methodology (SQMFF). NMR studies have confirmed respectively the crystal structure and functional groups of the grown crystal. The energy and oscillator strength calculated by Time-Dependent Density Functional Theory (TD-DFT) result complements the experimental findings. The calculated MESP, UV, HOMO-LUMO energies show that charge transfer done within the molecule. And various thermodynamic parameters are studied. Fukui determines the local reactive site of electrophilic, nucleophilic, descriptor.

The influence of post-deposition annealing on the structure, morphology and luminescence properties of pulsed laser deposited La0.5Gd1.5SiO5 doped Dy3+ thin films

NASA Astrophysics Data System (ADS)

Ogugua, Simon N.; Swart, Hendrik C.; Ntwaeaborwa, Odireleng M.

2018-04-01

The influence of post-deposition annealing on the structure, particle morphology and photoluminescence properties of dysprosium (Dy3+) doped La0.5Gd1.5SiO5 thin films grown on Si(111) substrates at different substrate temperatures using pulsed laser deposition (PLD) technique were studied. The X-ray diffractometer results showed an improved crystallinity after post-annealing. The topography and morphology of the post-annealed films were studied using atomic force microscopy and field emission scanning electron microscopy respectively. The elemental composition in the surface region of the films were analyzed using energy dispersive X-ray spectroscopy. The photoluminescence studies showed an improved luminescent after post-annealing. The cathodoluminescence properties of the films are also reported. The CIE colour coordinates calculated from the photoluminescence and cathodoluminescence data suggest that the films can have potential application in white light emitting diode (LED) and field emission display (FED) applications.

Ultrastructural and elemental analysis of sialoliths and their comparison with nephroliths.

PubMed

Rakesh, Nagaraju; Bhoomareddy Kantharaj, Yashoda Devi; Agarwal, Manjushree; Agarwal, Kunal

2014-02-01

Sialoliths are common in the submandibular gland and its duct system, although their exact cause of formation is still a matter of debate. The aims of this study were to: (a) analyze sialoliths ultrastructurally, and to determine the role of foreign bodies or organic materials in the formation of sialolith nuclei; and (b) compare nephroliths with sialoliths ultrastructurally. Three sialoliths and two nephroliths were analyzed ultrastructurally by a scanning electron microscope and X-ray diffractometer. The main structures of the sialoliths were found to be hydroxyapatite crystals. No organic cores were observed in the central parts of the sialoliths. In nephroliths, calcium oxalate, calcium phosphate, and struvite crystals were found. The energy-dispersive X-ray microanalysis found that sialoliths and nephroliths were predominantly composed of elements comprising calcium, phosphorous, magnesium, sodium, chloride, silicon, iron, and potassium. Sialoliths in the submandibular salivary glands might form secondary to sialadenitis, but not via a luminal organic nidus. © 2014 Wiley Publishing Asia Pty Ltd.

Luminescence properties of Eu 3+ and Sm 3+ coactivated Gd(III) tungstate phosphor for light-emitting diodes

NASA Astrophysics Data System (ADS)

Wei, Qiong; Chen, Donghua

2009-09-01

Rare-earth ions coactivated red phosphors Gd 0.2RE 1.8(WO 4) 3 (RE=Eu 3+ and Sm 3+) were synthesized by conventional solid-state reaction using boric acid as a flux agent. The samples were characterized by X-ray diffractometer (XRD), energy-dispersive X-ray spectrometer (EDS) and luminescence spectrometer (LS). The results showed that the Eu-Sm system exhibits higher emission intensity than those of the Eu single-doped system and Sm separate-doped system under ultraviolet (UV) radiation. Samarium(III) ions are effective in broadening and strengthened absorptions around 400 nm. Furthermore, it exhibits enhanced luminescence emission. when the mole ratio of boric acid is about 0.16, the luminescence capability is optimum. Two strongest lines at ultraviolet (394 nm) and blue (465 nm) in excitation spectra of these phosphors match well with the output wavelengths of UV and blue GaN-based light-emitting diodes (LEDs) chips.

Multifunctionality of nanocrystalline lanthanum ferrite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rai, Atma, E-mail: atma@iitp.ac.in; Thakur, Awalendra K.; Centre for Energy and Environment, Indian Institute of Technology Patna 800013 India

2016-05-06

Nanocrystalline lanthanum ferrite has been synthesized by adopting modified Pechini route. No evidence of impurity or secondary phase has been detected up to the detection of error limit of X-ray diffractometer (XRD). Rietveld refinement of X-ray diffraction pattern reveals orthorhombic crystal system with space group Pnma (62).Crystallite size and lattice strain was found to be ∼42.8nm and 0.306% respectively. Optical band gap was found to be 2.109 eV, by UV-Visible diffused reflectance spectrum (DRS). Brunauer-Emmet-Teller (BET) surface area was found to be ∼3.45 m{sup 2}/g. Magnetization-hysteresis (M-H) loop was recorded at room temperature (300K) reveals weak ferromagnetism in Nanocrystalline lanthanummore » ferrite. The weak ferromagnetism in lanthanum ferrite is due to the uncompensated antiferromagnetic spin ordering. Ferroelectric loop hysteresis observed at room temperature at 100Hz depicts the presence of ferroelectric ordering in LaFeO{sub 3}.Simultanious presence of magnetic and ferroelectric ordering at room temperature makes it suitable candidate of Multiferroic family.« less

Multifunctionality of nanocrystalline lanthanum ferrite

NASA Astrophysics Data System (ADS)

Rai, Atma; Thakur, Awalendra K.

2016-05-01

Nanocrystalline lanthanum ferrite has been synthesized by adopting modified Pechini route. No evidence of impurity or secondary phase has been detected up to the detection of error limit of X-ray diffractometer (XRD). Rietveld refinement of X-ray diffraction pattern reveals orthorhombic crystal system with space group Pnma (62).Crystallite size and lattice strain was found to be ˜42.8nm and 0.306% respectively. Optical band gap was found to be 2.109 eV, by UV-Visible diffused reflectance spectrum (DRS). Brunauer-Emmet-Teller (BET) surface area was found to be ˜3.45 m2/g. Magnetization-hysteresis (M-H) loop was recorded at room temperature (300K) reveals weak ferromagnetism in Nanocrystalline lanthanum ferrite. The weak ferromagnetism in lanthanum ferrite is due to the uncompensated antiferromagnetic spin ordering. Ferroelectric loop hysteresis observed at room temperature at 100Hz depicts the presence of ferroelectric ordering in LaFeO3.Simultanious presence of magnetic and ferroelectric ordering at room temperature makes it suitable candidate of Multiferroic family.

A switch from parallel to antiparallel strand orientation in a coiled-coil X-ray structure via two core hydrophobic mutations

DOE PAGES

Malashkevich, Vladimir N.; Higgins, Chelsea D.; Almo, Steven C.; ...

2015-05-06

The coiled-coil is one of the most ubiquitous and well studied protein structural motifs. Significant effort has been devoted to dissecting subtle variations of the typical heptad repeat sequence pattern that can designate larger topological features such as relative α-helical orientation and oligomer size. Here in this paper we report the X-ray structure of a model coiled-coil peptide, HA2-Del-L2seM, which forms an unanticipated core antiparallel dimer with potential sites for discrete higher-order multimerization (trimer or tetramer). In the X-ray structure, a third, partially-ordered α-helix is weakly associated with the antiparallel dimer and analytical ultracentrifugation experiments indicate the peptide forms amore » well-defined tetramer in solution. The HA2-Del-L2seM sequence is closely related to a parent model peptide, HA2-Del, which we previously reported adopts a parallel trimer; HA2-Del-L2seM differs by only hydrophobic leucine to selenomethione mutations and thus this subtle difference is sufficient to switch both relative α-helical topology and number of α-helices participating in the coiled-coil. Comparison of the X-ray structures of HA2-Del-L2seM (reported here) with the HA2-Del parent (reported previously) reveals novel interactions involving the selenomethionine residues that promote antiparallel coiled-coil configuration and preclude parallel trimer formation. Finally, these novel atomic insights are instructive for understanding subtle features that can affect coiled-coil topology and provide additional information for design of antiparallel coiled-coils.« less

The application of scanning electron microscopy to fractography

DOE Office of Scientific and Technical Information (OSTI.GOV)

Brooks, C.R.; McGill, B.L.

1994-10-01

Many failures involve fracture, and determination of the fracture process is a key factor in understanding the failure. This is frequently accomplished by characterizing the topography of the fracture surface. Scanning electron microscopy has a prominent role in fractography due to three features of the scanning electron microscope (SEM): high resolution, great depth of field, and the ability to obtain chemical information via analysis of the X-rays generated by the electrons. A qualitative treatment is presented of the interaction of electrons with a sample and the effect of the SEM operating parameters on image formation, quality, and X-ray analysis. Fractographsmore » are presented to illustrate these features of scanning electron microscopy and to illustrate the limitations and precautions in obtaining fractographs and x-ray analyses. The review is concluded with examples of fracture surface features of metallic, ceramic, and polymeric materials.« less

Retrieving the Quantitative Chemical Information at Nanoscale from Scanning Electron Microscope Energy Dispersive X-ray Measurements by Machine Learning

NASA Astrophysics Data System (ADS)

Jany, B. R.; Janas, A.; Krok, F.

2017-11-01

The quantitative composition of metal alloy nanowires on InSb(001) semiconductor surface and gold nanostructures on germanium surface is determined by blind source separation (BSS) machine learning (ML) method using non negative matrix factorization (NMF) from energy dispersive X-ray spectroscopy (EDX) spectrum image maps measured in a scanning electron microscope (SEM). The BSS method blindly decomposes the collected EDX spectrum image into three source components, which correspond directly to the X-ray signals coming from the supported metal nanostructures, bulk semiconductor signal and carbon background. The recovered quantitative composition is validated by detailed Monte Carlo simulations and is confirmed by separate cross-sectional TEM EDX measurements of the nanostructures. This shows that SEM EDX measurements together with machine learning blind source separation processing could be successfully used for the nanostructures quantitative chemical composition determination.

A novel binary Pt 3Te x/C nanocatalyst for ethanol electro-oxidation

NASA Astrophysics Data System (ADS)

Huang, Meihua; Wang, Fei; Li, Lirong; Guo, Yonglang

The Pt 3Te x/C nanocatalyst was prepared and its catalytic performance for ethanol oxidation was investigated for the first time. The Pt 3Te/C nanoparticles were characterized by an X-ray diffractometer (XRD), transmission electron microscope (TEM) and energy dispersive X-ray spectroscopy equipped with TEM (TEM-EDX). The Pt 3Te/C catalyst has a typical fcc structure of platinum alloys with the presence of Te. Its particle size is about 2.8 nm. Among the synthesized catalysts with different atomic ratios, the Pt 3Te/C catalyst has the highest anodic peak current density. The cyclic voltammograms (CV) show that the anodic peak current density for the Pt 3Te/C, commercial PtRu/C and Pt/C catalysts reaches 1002, 832 and 533 A g -1, respectively. On the current-time curve, the anodic current on the Pt 3Te/C catalyst was higher than those for the catalysts reported. So, these findings show that the Pt 3Te/C catalyst has uniform nanoparticles and the best activity among the synthesized catalysts, and it is better than commercial PtRu/C and Pt/C catalysts for ethanol oxidation at room temperature.

Polymorphism of Alprazolam (Xanax): a review of its crystalline phases and identification, crystallographic characterization, and crystal structure of a new polymorph (form III).

PubMed

de Armas, Héctor Novoa; Peeters, Oswald M; Van den Mooter, Guy; Blaton, Norbert

2007-05-01

A new polymorphic form of Alprazolam (Xanax), 8-chloro-1-methyl-6-phenyl-4H-[1,2,4]triazolo-[4,3-alpha][1,4]benzodiazepine, C(17)H(13)ClN(4), has been investigated by means of X-ray powder diffraction (XRPD), single crystal X-ray diffraction, and differential scanning calorimetry (DSC). This polymorphic form (form III) was obtained during DSC experiments after the exothermic recrystallization of the melt of form I. The crystal unit cell dimensions for form III were determined from diffractometer methods. The monoclinic unit cell found for this polymorph using XRPD after indexing the powder diffractogram was confirmed by the cell parameters obtained from single crystal X-ray diffractometry on a crystal isolated from the DSC pans. The single crystal unit cell parameters are: a = 28.929(9), b = 13.844(8), c = 7.361(3) angstroms, beta = 92.82(3) degrees , V = 2944(2) angstroms(3), Z = 8, space group P2(1) (No.4), Dx = 1.393 Mg/m(3). The structure obtained from single crystal X-ray diffraction was used as initial model for Rietveld refinement on the powder diffraction data of form III. The temperature phase transformations of alprazolam were also studied using high temperature XRPD. A review of the different phases available in the Powder Diffraction File (PDF) database for this drug is described bringing some clarification and corrections. (c) 2007 Wiley-Liss, Inc. and the American Pharmacists Association.

Amorphous Analogs of Martian Global Soil: Pair Distribution Function Analyses and Implications for Scattering Models of Chemin X-ray Diffraction Data

NASA Technical Reports Server (NTRS)

Achilles, C. N.; Bish, D. L.; Rampe, E. B.; Morris, R. V.

2015-01-01

Soils on Mars have been analyzed by the Mars Exploration Rovers (MER) and most recently by the Mars Science Laboratory (MSL) rover. Chemical analyses from a majority of soil samples suggest that there is a relatively uniform global soil composition across much of the planet. A soil site, Rocknest, was sampled by the MSL science payload including the CheMin X-ray diffractometer and the Alpha Particle X-ray Spectrometer (APXS). Che- Min X-ray diffraction (XRD) data revealed crystalline phases and a broad, elevated background, indicating the presence of amorphous or poorly ordered materials (Fig 1). Based on the chemical composition of the bulk soil measured by APXS and the composition of crystalline phases derived from unit-cell parameters determined with CheMin data, the percentages of crystalline and amorphous phases were calculated at 51% and 49%, respectively. Attempts to model the amorphous contribution to CheMin XRD patterns were made using amorphous standards and full-pattern fitting methods and show that the broad, elevated background region can be fitted by basaltic glass, allophane, and palagonite. However, the modeling shows only that these phases have scattering patterns similar to that for the soil, not that they represent unique solutions. Here, we use pair distribution function (PDF) analysis to determine the short-range order of amorphous analogs in martian soils and better constrain the amorphous material detected by CheMin.

Bulk Crystal Growth, and High-Resolution X-ray Diffraction Results of LiZnAs Semiconductor Material

NASA Astrophysics Data System (ADS)

Montag, Benjamin W.; Reichenberger, Michael A.; Sunder, Madhana; Ugorowski, Philip B.; Nelson, Kyle A.; Henson, Luke C.; McGregor, Douglas S.

2017-08-01

LiZnAs is being explored as a candidate for solid-state neutron detectors. The compact form, solid-state device would have greater efficiency than present day gas-filled 3He and 10BF3 detectors. Devices fabricated from LiZnAs having either natural Li (nominally 7.5% 6Li) or enriched 6Li (usually 95% 6Li) as constituent atoms may provide a material for compact high efficiency neutron detectors. The 6Li( n, t)4He reaction yields a total Q-value of 4.78 MeV, an energy larger than that of the 10B reaction, which can easily be identified above background radiations. LiZnAs material was synthesized by preparing equimolar portions of Li, Zn, and As sealed under vacuum (10-6 Torr) in quartz ampoules lined with boron nitride and subsequently reacted in a compounding furnace (Montag et al. in J Cryst Growth 412:103, 2015). The raw synthesized LiZnAs was purified by a static vacuum sublimation in quartz (Montag et al. in J Cryst Growth 438:99, 2016). Bulk crystalline LiZnAs ingots were grown from the purified material with a high-temperature Bridgman-style growth process described here. One of the largest LiZnAs ingots harvested was 9.6 mm in diameter and 4.2 mm in length. Samples were harvested from the ingot and were characterized for crystallinity using a Bruker AXS Inc. D8 AXS Inc. D2 CRYSO, energy dispersive x-ray diffractometer, and a Bruker AXS Inc. D8 DISCOVER, high-resolution x-ray diffractometer equipped with molybdenum radiation, Gobel mirror, four bounce germanium monochromator and a scintillation detector. The primary beam divergence was determined to be 0.004°, using a single crystal Si standard. The x-ray based characterization revealed that the samples nucleated in the (110) direction and a high-resolution open detector rocking curve recorded on the (220) LiZnAs yielded a full width at half maximum (FWHM) of 0.235°. Sectional pole figures using off-axis reflections of the (211) LiZnAs confirmed in-plane ordering, and also indicated the presence of multiple domains. The LiZnAs bulk crystals exhibited a Primitive Cubic Bravais lattice instead of the commonly reported Face-centered Cubic Bravais lattice. The lattice constant was determined to be 5.5146 ± 0.0003 Å.

Defect structure of epitaxial layers of III nitrides as determined by analyzing the shape of X-ray diffraction peaks

NASA Astrophysics Data System (ADS)

Kyutt, R. T.

2017-04-01

The shape of X-ray diffraction epitaxial layers with high dislocation densities has been studied experimentally. Measurements with an X-ray diffractometer were performed in double- and triple-crystal setups with both Cu K α and Mo K α radiation. Epitaxial layers (GaN, AlN, AlGaN, ZnO, etc.) with different degrees of structural perfection grown by various methods on sapphire, silicon, and silicon carbide substrates have been examined. The layer thickness varied in the range of 0.5-30 μm. It has been found that the center part of peaks is well approximated by the Voigt function with different Lorentz fractions, while the wing intensity drops faster and may be represented by a power function (with the index that varies from one structure to another). A well-marked dependence on the ordering of dislocations was observed. The drop in intensity in the majority of structures with a regular system and regular threading dislocations was close to the theoretically predicted law Δθ-3; the intensity in films with a chaotic distribution decreased much faster. The dependence of the peak shape on the order of reflection, the diffraction geometry, and the epitaxial layer thickness was also examined.

Plasma-induced damage of tungsten coatings on graphite limiters

NASA Astrophysics Data System (ADS)

Fortuna, E.; Rubel, M. J.; Psoda, M.; Andrzejczuk, M.; Kurzydowski, K. J.; Miskiewicz, M.; Philipps, V.; Pospieszczyk, A.; Sergienko, G.; Spychalski, M.; Zielinski, W.

2007-03-01

Vaccum plasma sprayed tungsten coatings with an evaporated sandwich Re-W interlayer on graphite limiter blocks were studied after the experimental campaign in the TEXTOR tokamak. The coating morphology was modified by high-heat loads and co-deposition of species from the plasma. Co-deposits contained fuel species, carbon, boron and silicon. X-ray diffractometer phase analysis indicated the coexistence of metallic tungsten and its carbides (WC and W2C) and boride (W2B). In the Re-W layer the presence of carbon was detected in a several micrometres thick zone. In the overheated part of the limiter, the Re-W layer was transformed into a sigma phase.

Martensitic transformation and phase diagram in ternary Co-V-Ga Heusler alloys

NASA Astrophysics Data System (ADS)

Xu, Xiao; Nagashima, Akihide; Nagasako, Makoto; Omori, Toshihiro; Kanomata, Takeshi; Kainuma, Ryosuke

2017-03-01

We report the martensitic transformation behavior in Co-V-Ga Heusler alloys. Thermoanalysis and thermomagnetization measurements were conducted to observe the martensitic transformation. By using a transmission electron microscope and an in situ X-ray diffractometer, martensitic transformation was found to occur from the L21 Heusler parent phase to the D022 martensite phase. Phase diagrams were determined for two pseudo-binary sections where martensitic transformation was detected. Magnetic properties, including the Curie temperatures and spontaneous magnetization of the parent phase, were also investigated. The magnetic properties showing behaviors different from those of NiMn-based alloys were found.

Structural and magnetic analysis of Cu, Co substituted NiFe2O4 thin films

NASA Astrophysics Data System (ADS)

Sharma, Hakikat; Bala, Kanchan; Negi, N. S.

2016-05-01

In the present work we prepared NiFe2O4, Ni0.95Cu0.05Fe2O4 and Ni0.94Cu0.05Co0.01 Fe2O4 thin films by metallo-organic decomposition method (MOD) using spin coating technique. The thin films were analyzed by X-ray diffractometer (XRD) and Atomic force microscope (AFM) for structural studies. The XRD patterns confirmed the ferrite phase of thin films. From AFM, we analyzed surface morphology, calculated grain size (GS) and root mean square roughness (RMSR). Room temperature magnetic properties were investigated by vibrating sample magnetometer (VSM).

Electrical and magnetic properties of nano-sized magnesium ferrite

NASA Astrophysics Data System (ADS)

T, Smitha; X, Sheena; J, Binu P.; Mohammed, E. M.

2015-02-01

Nano-sized magnesium ferrite was synthesized using sol-gel techniques. Structural characterization was done using X-ray diffractometer and Fourier Transform Infrared Spectrometer. Vibration Sample Magnetometer was used to record the magnetic measurements. XRD analysis reveals the prepared sample is single phasic without any impurity. Particle size calculation shows the average crystallite size of the sample is 19nm. FTIR analysis confirmed spinel structure of the prepared samples. Magnetic measurement study shows that the sample is ferromagnetic with high degree of isotropy. Hysterisis loop was traced at temperatures 100K and 300K. DC electrical resistivity measurements show semiconducting nature of the sample.

New high- and low-temperature apparatus for synchrotron polycrystalline X-ray diffraction.

PubMed

Tang, C C; Bushnell-Wye, G; Cernik, R J

1998-05-01

A high-temperature furnace with an induction heater coil and a cryogenic system based on closed-cycle refrigeration have been assembled to enhance the non-ambient powder diffraction facilities at the Synchrotron Radiation Source, Daresbury Laboratory. The commissioning of the high- and low-temperature devices on the high-resolution powder diffractometer of Station 2.3 is described. The combined temperature range provided by the furnace/cryostat is 10-1500 K. Results from Fe and NH(4)Br powder samples are presented to demonstrate the operation of the apparatus. The developments presented in this paper are applicable to a wide range of other experiments and diffraction geometries.

Young's modulus and SEM analysis of leg bones exposed to simulated microgravity by hind limb suspension (HLS)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Patel, Niravkumar D.; Mehta, Rahul; Ali, Nawab

2013-04-19

The aim of this study was to determine composition of the leg bone tissue of rats that were exposed to simulated microgravity by Hind-Limb Suspension (HLS) by tail for one week. The leg bones were cross sectioned, cleaned of soft tissues, dried and sputter coated, and then placed horizontally on the stage of a Scanning Electron Microscope (SEM) for analysis. Interaction of a 17.5 keV electron beam, incident from the vertical direction on the sample, generated images using two detectors. X-rays emitted from the sample during electron bombardment were measured with an Energy Dispersive Spectroscopy (EDS) feature of SEM usingmore » a liquid-nitrogen cooled Si(Li) detector with a resolution of 144 eV at 5.9 keV ({sub 25}Mn K{sub {alpha}} x-ray). K{sub {alpha}}- x-rays from carbon, oxygen, phosphorus and calcium formed the major peaks in the spectrum. Relative percentages of these elements were determined using a software that could also correct for ZAF factors namely Z(atomic number), A(X-ray absorption) and F(characteristic fluorescence). The x-rays from the control groups and from the experimental (HLS) groups were analyzed on well-defined parts (femur, tibia and knee) of the leg bone. The SEM analysis shows that there are definite changes in the hydroxyl or phosphate group of the main component of the bone structure, hydroxyapatite [Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}], due to hind limb suspension. In a separate experiment, entire leg bones (both from HLS and control rats) were subjected to mechanical stress by mean of a variable force. The stress vs. strain graph was fitted with linear and polynomial function, and the parameters reflecting the mechanical strength of the bone, under increasing stress, were calculated. From the slope of the linear part of the graph the Young's modulus for HLS bones were calculated and found to be 2.49 times smaller than those for control bones.« less

GUIDELINES FOR THE APPLICATION OF SEM/EDX ANALYTICAL TECHNIQUES FOR FINE AND COARSE PM SAMPLES

EPA Science Inventory

Scanning Electron Microscopy (SEM) coupled with Energy-Dispersive X-ray analysis (EDX) is a powerful tool in the characterization and source apportionment of environmental particulate matter (PM), providing size, chemistry, and morphology of particles as small as a few tenths ...

EVALUATION OF COMPUTER-CONTROLLED SCANNING ELECTRON MICROSCOPY APPLIED TO AN AMBIENT URBAN AEROSOL SAMPLE

EPA Science Inventory

Recent interest in monitoring and speciation of particulate matter has led to increased application of scanning electron microscopy (SEM) coupled with energy-dispersive x-ray analysis (EDX) to individual particle analysis. SEM/EDX provides information on the size, shape, co...

Computer-aided screening system for cervical precancerous cells based on field emission scanning electron microscopy and energy dispersive x-ray images and spectra

NASA Astrophysics Data System (ADS)

Jusman, Yessi; Ng, Siew-Cheok; Hasikin, Khairunnisa; Kurnia, Rahmadi; Osman, Noor Azuan Bin Abu; Teoh, Kean Hooi

2016-10-01

The capability of field emission scanning electron microscopy and energy dispersive x-ray spectroscopy (FE-SEM/EDX) to scan material structures at the microlevel and characterize the material with its elemental properties has inspired this research, which has developed an FE-SEM/EDX-based cervical cancer screening system. The developed computer-aided screening system consisted of two parts, which were the automatic features of extraction and classification. For the automatic features extraction algorithm, the image and spectra of cervical cells features extraction algorithm for extracting the discriminant features of FE-SEM/EDX data was introduced. The system automatically extracted two types of features based on FE-SEM/EDX images and FE-SEM/EDX spectra. Textural features were extracted from the FE-SEM/EDX image using a gray level co-occurrence matrix technique, while the FE-SEM/EDX spectra features were calculated based on peak heights and corrected area under the peaks using an algorithm. A discriminant analysis technique was employed to predict the cervical precancerous stage into three classes: normal, low-grade intraepithelial squamous lesion (LSIL), and high-grade intraepithelial squamous lesion (HSIL). The capability of the developed screening system was tested using 700 FE-SEM/EDX spectra (300 normal, 200 LSIL, and 200 HSIL cases). The accuracy, sensitivity, and specificity performances were 98.2%, 99.0%, and 98.0%, respectively.

Comparative analysis of textile metal threads from liturgical vestments and folk costumes in Croatia

NASA Astrophysics Data System (ADS)

Šimić, Kristina; Zamboni, Ivana; Fazinić, Stjepko; Mudronja, Domagoj; Sović, Lea; Gouasmia, Sabrina; Soljačić, Ivo

2018-02-01

Textile is essential for everyday life in all societies. It is used in clothes for protection and warmth but also to indicate class and position, show wealth and social status. Threads from precious metals have also been used in combination with fibres for decoration in order to create luxury fabrics for secular and religious elites. We performed elemental analysis of 17th to 20th century metal threads from various textile articles of liturgical vestments and festive folk costumes collected in the museums of northern, southern and central Croatian regions. In order to determine elemental concentrations in threads we performed comparative X-ray Spectroscopy measurements using: (i) Scanning Electron Microscopy with Energy Dispersive X-ray Spectroscopy (SEM-EDX) at the Faculty of Textile Technology, (ii) X-ray Fluorescence Spectroscopy (XRF) at the Croatian Conservation Institute and (iii) Particle Induced X-ray Spectroscopy (PIXE) at the Ruđer Bošković Institute Tandem Accelerator Facility using ion micro beam. Rutherford Backscattering Spectroscopy (RBS) was performed as well on selected samples. SEM-EDX investigations of cross-sections along with the surfaces were also performed. In this work we report and discuss the results obtained by the three X-ray methods and RBS for major (gold, silver, copper) and minor elements on different threads like stripes, wires and "srma" (metal thread wrapped around textile yarn).

A comparative study of heterostructured CuO/CuWO4 nanowires and thin films

NASA Astrophysics Data System (ADS)

Polyakov, Boris; Kuzmin, Alexei; Vlassov, Sergei; Butanovs, Edgars; Zideluns, Janis; Butikova, Jelena; Kalendarev, Robert; Zubkins, Martins

2017-12-01

A comparative study of heterostructured CuO/CuWO4 core/shell nanowires and double-layer thin films was performed through X-ray diffraction, confocal micro-Raman spectroscopy and electron (SEM and TEM) microscopies. The heterostructures were produced using a two-step process, starting from a deposition of amorphous WO3 layer on top of CuO nanowires and thin films by reactive DC magnetron sputtering and followed by annealing at 650 °C in air. The second step induced a solid-state reaction between CuO and WO3 oxides through a thermal diffusion process, revealed by SEM-EDX analysis. Morphology evolution of core/shell nanowires and double-layer thin films upon heating was studied by electron (SEM and TEM) microscopies. A formation of CuWO4 phase was confirmed by X-ray diffraction and confocal micro-Raman spectroscopy.

An energy-dispersive X-ray analysis and SEM study of debris remaining on endodontic instruments after ultrasonic cleaning and autoclave sterilization.

PubMed

Parirokh, Masoud; Asgary, Saeed; Eghbal, Mohammad Jafar

2005-08-01

This study was carried out to investigate metallic and non-metallic debris remaining on endodontic files after ultrasonic cleaning and autoclave processing. Forty-eight unused rotary and hand endodontic files, including eight different brands, were tested. Instruments were cleaned with ultrasound, autoclaved and before and after each step were observed by scanning electron microscopy (SEM). Adherent debris was analysed by energy-dispersive X-ray analysis (EDXA). All of the instruments before ultrasound cleaning were contaminated with metallic and non-metallic debris. Although most non-metallic debris was removed by ultrasonic cleaning, most of the metallic debris remained even after the final step of sterilization.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Malashkevich, Vladimir N.; Higgins, Chelsea D.; Almo, Steven C.

The coiled-coil is one of the most ubiquitous and well studied protein structural motifs. Significant effort has been devoted to dissecting subtle variations of the typical heptad repeat sequence pattern that can designate larger topological features such as relative α-helical orientation and oligomer size. Here in this paper we report the X-ray structure of a model coiled-coil peptide, HA2-Del-L2seM, which forms an unanticipated core antiparallel dimer with potential sites for discrete higher-order multimerization (trimer or tetramer). In the X-ray structure, a third, partially-ordered α-helix is weakly associated with the antiparallel dimer and analytical ultracentrifugation experiments indicate the peptide forms amore » well-defined tetramer in solution. The HA2-Del-L2seM sequence is closely related to a parent model peptide, HA2-Del, which we previously reported adopts a parallel trimer; HA2-Del-L2seM differs by only hydrophobic leucine to selenomethione mutations and thus this subtle difference is sufficient to switch both relative α-helical topology and number of α-helices participating in the coiled-coil. Comparison of the X-ray structures of HA2-Del-L2seM (reported here) with the HA2-Del parent (reported previously) reveals novel interactions involving the selenomethionine residues that promote antiparallel coiled-coil configuration and preclude parallel trimer formation. Finally, these novel atomic insights are instructive for understanding subtle features that can affect coiled-coil topology and provide additional information for design of antiparallel coiled-coils.« less

Magnetic Properties of Rapid Cooled FeCoB Based Alloys Produced by Injection Molding

NASA Astrophysics Data System (ADS)

Nabialek, M.; Jeż, B.; Jeż, K.; Pietrusiewicz, P.; Gruszka, K.; Błoch, K.; Gondro, J.; Rzącki, J.; Abdullah, M. M. A. B.; Sandu, A. V.; Szota, M.

2018-06-01

The paper presents the results of investigations of the structure and magnetic properties of massive rapid cooled Fe50-xCo20+xB20Cu1Nb9 alloys (where x = 0, 5). Massive alloys were made using the method of injecting a liquid alloy into a copper mold. Samples were obtained in the form of 0.5 mm thick plates. The structure of the obtained samples was examined using an X-ray diffractometer equipped with a CuKα lamp. The phase composition of the alloys formed was determined using the Match program. By using Sherrer’s dependence the grain sizes of the identified crystalline phases were estimated. Using the Faraday magnetic balance, the magnetization of samples as a function of temperature in the range from room temperature to 850K was measured. Magnetization of saturation and value of the coercive field for the prepared alloys were determined on the basis of magnetic hysteresis loop measurement using the LakeShore vibration magnetometer.

Synthesis of silver nanoparticles using leaves of Catharanthus roseus Linn. G. Don and their antiplasmodial activities

PubMed Central

Ponarulselvam, S; Panneerselvam, C; Murugan, K; Aarthi, N; Kalimuthu, K; Thangamani, S

2012-01-01

Objective To develop a novel approach for the green synthesis of silver nanoparticles using aqueous leaves extracts of Catharanthus roseus (C. roseus) Linn. G. Don which has been proven active against malaria parasite Plasmodium falciparum (P. falciparum). Methods Characterizations were determined by using ultraviolet-visible (UV-Vis) spectrophotometry, scanning electron microscopy (SEM), energy dispersive X-ray and X-ray diffraction. Results SEM showed the formation of silver nanoparticles with an average size of 35–55 nm. X-ray diffraction analysis showed that the particles were crystalline in nature with face centred cubic structure of the bulk silver with the broad peaks at 32.4, 46.4 and 28.0. Conclusions It can be concluded that the leaves of C. roseus can be good source for synthesis of silver nanoparticle which shows antiplasmodial activity against P. falciparum. The important outcome of the study will be the development of value added products from medicinal plants C. roseus for biomedical and nanotechnology based industries. PMID:23569974

Structural analysis of bioceramic materials for denture application

NASA Astrophysics Data System (ADS)

Rauf, Nurlaela; Tahir, Dahlang; Arbiansyah, Muhammad

2016-03-01

Structural analysis has been performed on bioceramic materials for denture application by using X-ray diffraction (XRD), X-ray fluorescence (XRF), and Scanning Electron Microscopy (SEM). XRF is using for analysis chemical composition of raw materials. XRF shows the ratio 1 : 1 : 1 : 1 between feldspar, quartz, kaolin and eggshell, respectively, resulting composition CaO content of 56.78 %, which is similar with natural tooth. Sample preparation was carried out on temperature of 800 °C, 900 °C and 1000 °C. X-ray diffraction result showed that the structure is crystalline with trigonal crystal system for SiO2 (a=b=4.9134 Å and c=5.4051 Å) and CaH2O2 (a=b=3.5925 Å and c=4.9082 Å). Based on the Scherrer's equation showed the crystallite size of the highest peak (SiO2) increase with increasing the temperature preparation. The highest hardness value (87 kg/mm2) and match with the standards of dentin hardness. The surface structure was observed by using SEM also discussed.

Effects of annealing on the structure and magnetic properties of Fe80B20 magnetostrictive fibers.

PubMed

Zhu, Qianke; Zhang, Shuling; Geng, Guihong; Li, Qiushu; Zhang, Kewei; Zhang, Lin

2016-07-04

Fe80B20 amorphous alloys exhibit excellent soft magnetic properties, high abrasive resistance and outstanding corrosion resistance. In this work, Fe80B20 amorphous micro-fibers with HC of 3.33 Oe were firstly fabricated and the effects of annealing temperature on the structure and magnetic properties of the fibers were investigated. In this study, Fe80B20 amorphous fibers were prepared by the single roller melt-spinning method. The structures of as-spun and annealed fibers were investigated by X-ray diffractometer (XRD) (PANalytical X,Pert Power) using Cu Kα radiation. The morphology of the fibers was observed by scanning electron microscopy (SEM) (HITACHI-S4800). Differential scanning calorimetry (DSC) measurements of the fibers were performed on Mettler Toledo TGA/DSC1 device under N2 protection. Vibrating sample magnetometer (VSM, Versalab) was used to examine the magnetic properties of the fibers. The resonance behavior of the fibers was characterized by an impedance analyzer (Agilent 4294A) with a home-made copper coil. The X-ray diffusion (XRD) patterns show that the fibers remain amorphous structure until the annealing temperature reaches 500°C. The differential scanning calorimetry (DSC) results show that the crystallization temperature of the fibers is 449°C. The crystallization activation energy is calculated to be 221 kJ/mol using Kissinger formula. The scanning electron microscopy (SEM) images show that a few dendrites appear at the fiber surface after annealing. The result indicates that the coercivity HC (//) and HC (⊥) slightly increases with increasing annealing temperature until 400°C, and then dramatically increases with further increasing annealing temperature which is due to significant increase in magneto-crystalline anisotropy and magneto-elastic anisotropy. The Q value firstly increases slightly when the annealing temperature rises from room temperature (RT) to 300°C, then decreases until 400°C. Eventually, the value of Q increases to ~2000 at annealing temperature of 500°C. In this study, Fe80B20 amorphous fibers with the diameter of 60 μm were prepared by the single roller melt-spinning method and annealed at 200°C, 300°C, 400°C, and 500°C, respectively. XRD results indicate that the fiber structure remains amorphous when the annealing temperature is below 400°C. α-Fe phase and Fe3B phase appear when the annealing temperature rises to 500°C, which is above the crystallization temperature of 449°C. The recrystallization activation energy is calculated to be 221 kJ/mol. The coercivity increases with increasing annealing temperature, which attributes to the increase of total anisotropy. All the as-spun and annealed fibers exhibit good resonance behavior for magnetostrictive sensors.

The influence of temperature on a nutty-cake structural material: LiMn1-xFexPO4 composite with LiFePO4 core and carbon outer layer for lithium-ion battery

NASA Astrophysics Data System (ADS)

Huo, Zhen-Qing; Cui, Yu-Ting; Wang, Dan; Dong, Yue; Chen, Li

2014-01-01

The extremely low electronic conductivity, slow ion diffusion kinetics, and the Jahn-Teller effect of LiMnPO4 limit its electrochemical performance. In this work, a nutty-cake structural C-LiMn1-xFexPO4-LiFePO4 cathode material is synthesized by hydrothermal method and further calcined at different temperatures. The influence of calcination temperature on the electrochemical behavior is investigated by X-ray diffractometer, scanning electron microscope, field-emission high-resolution transmission electron microscope, energy-dispersive X-ray spectroscopy, electrochemical impedance spectroscopy and charge-discharge tests. And the performance of C-LiMn1-xFexPO4-LiFePO4 materials has a relationship with its crystal structure. The well-crystallized Sample-600 calcined at 600 °C shows the smallest charge transfer resistance, the largest lithium ion diffusion coefficient (DLi) and the best cycling stability. The discharge capacity of Sample-600 holds around 112 mAh g-1 after the 3rd cycle at 0.1 C rate. The performances improvement of C-LiMn1-xFexPO4-LiFePO4 material can be mainly attributed to the iron diffusion from the LiFePO4 core to the outer LiMnPO4 layer under appropriate calcination temperature.

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

PubMed

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.

Kaolinite flocculation induced by smectite addition - a transmission X-ray microscopic study.

PubMed

Zbik, Marek S; Song, Yen-Fang; Frost, Ray L

2010-09-01

The influence of smectite addition on kaolinite suspensions in water was investigated by transmission X-ray microscopy (TXM) and Scanning Electron Microscopy (SEM). Sedimentation test screening was also conducted. Micrographs were processed by the STatistic IMage Analysing (STIMAN) program and structural parameters were calculated. From the results of the sedimentation tests important influences of small smectite additions to about 3wt.% on kaolinite suspension flocculation has been found. In order to determine the reason for this smectite impact on kaolinite suspension, macroscopic behaviour micro-structural examination using Transmission X-ray Microscope (TXM) and SEM has been undertaken. TXM & SEM micrographs of freeze-dried kaolinite-smectite suspensions with up to 20% smectite showed a high degree of orientation of the fabric made of highly oriented particles and greatest density when 3wt.% of smectite was added to the 10wt.% dense kaolinite suspension. In contrast, suspensions containing pure kaolinite do not show such platelet mutual orientation but homogenous network of randomly oriented kaolinite platelets. This suggests that in kaolinite-smectite suspensions, smectite forms highly oriented basic framework into which kaolinite platelets may bond in face to face preferential contacts strengthening structure and allowing them to show plastic behaviour which is cause of platelets orientation. Copyright 2010 Elsevier Inc. All rights reserved.

Practical application of HgI2 detectors to a space-flight scanning electron microscope

NASA Technical Reports Server (NTRS)

Bradley, J. G.; Conley, J. M.; Albee, A. L.; Iwanczyk, J. S.; Dabrowski, A. J.

1989-01-01

Mercuric iodide X-ray detectors have been undergoing tests in a prototype scanning electron microscope system being developed for unmanned space flight. The detector program addresses the issues of geometric configuration in the SEM, compact packaging that includes separate thermoelectric coolers for the detector and FET, X-ray transparent hermetic encapsulation and electrical contacts, and a clean vacuum environment.

Additional of polyethylene glycol on the preparation of LaPO4:Eu3+ phosphor

NASA Astrophysics Data System (ADS)

Panatarani, Camellia; Joni, I. Made

2013-09-01

Solution phase method was used to synthesis nanocrystal LaPO4:Eu3+. Polyethylene glycol with vary molecular weight (MW) was added to allow an exothermic reaction to get a high crystalinity of LaPO4:Eu3+. The x-ray pattern of as prepared LaPO4 was obtained by using an X'pert PANalytical diffractometer with CuKα radiation (λ = 1.5406 Å) and the photoluminescent measurement spectra is obtained by using Fluorescence Spectrometer LS55, Perkin Elmer. The additional of various MW of polyethylene glycol into the precursor solution of LaPO4:Eu3+ affected the crystal structure and luminescent properties. Higher MW of PEG depressing the luminescent spectra. The emission origin from 5D0-7F4 transition vanished by additional 500,000 and 2,000,000 MW of PEG.

Adsorption of antibiotics on microplastics.

PubMed

Li, Jia; Zhang, Kaina; Zhang, Hua

2018-06-01

Microplastics and antibiotics are two classes of emerging contaminants with proposed negative impacts to aqueous ecosystems. Adsorption of antibiotics on microplastics may result in their long-range transport and may cause compound combination effects. In this study, we investigated the adsorption of 5 antibiotics [sulfadiazine (SDZ), amoxicillin (AMX), tetracycline (TC), ciprofloxacin (CIP), and trimethoprim (TMP)] on 5 types of microplastics [polyethylene (PE), polystyrene (PS), polypropylene (PP), polyamide (PA), and polyvinyl chloride (PVC)] in the freshwater and seawater systems. Scanning Electron Microscope (SEM) and X-ray diffractometer (XRD) analysis revealed that microplastics have different surface characterizes and various degrees of crystalline. Adsorption isotherms demonstrated that PA had the strongest adsorption capacity for antibiotics with distribution coefficient (K d ) values ranged from 7.36 ± 0.257 to 756 ± 48.0 L kg -1 in the freshwater system, which can be attributed to its porous structure and hydrogen bonding. Relatively low adsorption capacity was observed on other four microplastics. The adsorption amounts of 5 antibiotics on PS, PE, PP, and PVC decreased in the order of CIP > AMX > TMP > SDZ > TC with K f correlated positively with octanol-water partition coefficients (Log K ow ). Comparing to freshwater system, adsorption capacity in seawater decreased significantly and no adsorption was observed for CIP and AMX. Our results indicated that commonly observed polyamide particles can serve as a carrier of antibiotics in the aquatic environment. Copyright © 2018 Elsevier Ltd. All rights reserved.

Bioleaching combined brine leaching of heavy metals from lead-zinc mine tailings: Transformations during the leaching process.

PubMed

Ye, Maoyou; Yan, Pingfang; Sun, Shuiyu; Han, Dajian; Xiao, Xiao; Zheng, Li; Huang, Shaosong; Chen, Yun; Zhuang, Shengwei

2017-02-01

During the process of bioleaching, lead (Pb) recovery is low. This low recovery is caused by a problem with the bioleaching technique. This research investigated the bioleaching combination of bioleaching with brine leaching to remove heavy metals from lead-zinc mine tailings. The impact of different parameters were studied, including the effects of initial pH (1.5-3.0) and solid concentration (5-20%) for bioleaching, and the effects of sodium chloride (NaCl) concentration (10-200 g/L) and temperature (25 and 50 °C) for brine leaching. Complementary characterization experiments (Sequential extraction, X-ray diffractometer (XRD), scanning electronic microscope (SEM)) were also conducted to explore the transformation of tailings during the leaching process. The results showed that bioleaching efficiency was significantly influenced by initial pH and solid concentration. Approximately 85.45% of iron (Fe), 4.12% of Pb, and 97.85% of zinc (Zn) were recovered through bioleaching in optimum conditions. Increasing the brine concentration and temperature promoted lead recovery. Lead was recovered from the bioleaching residues at a rate of 94.70% at 25 °C and at a rate of 99.46% at 50 °C when the NaCl concentration was 150 g/L. The study showed that bioleaching significantly changed the speciation of heavy metals and the formation and surface morphology of tailings. The metals were mainly bound in stable fractions after bioleaching. Copyright © 2016 Elsevier Ltd. All rights reserved.

Influence of Austempering Heat Treatment on Microstructure and Mechanical Properties of Medium Carbon High Silicon Steel

NASA Astrophysics Data System (ADS)

Palaksha, P. A.; Ravishankar, K. S.

2017-08-01

In the present investigation, the influence of austempering heat treatment on the microstructure and mechanical properties of medium carbon high silicon steel was evaluated. The test specimens were machined from the as-received steel and were first austenitised at 900 °C for 45 minutes, followed by austempering heat treatment in salt bath at various temperatures 300 °C, 350 °C and 400 °C for a fixed duration of two hours, after that those specimens were air-cooled to room temperature. The characterization studies were carried out using optical microscope, scanning electron microscope (SEM) and x-ray diffractometer (XRD) and then correlated to the hardness and tensile properties. Results indicate that, the specimens austempered at lower temperature i.e. at 300 °C, which offered high hardness, tensile strength and lower ductility (1857 MPa and 13.3 %) due to the presence of acicular bainite i.e. lower bainite and also some martensite in the microstructure. At 350 °C, reduction in the tensile strength and hardness was observed, but comparatively higher ductility, which was favored by the presence of bainite laths i.e. upper bainitic structure along with higher retained austenite content. Finally at 400 °C, reduction in both ductility and tensile strength was observed, which is due to the precipitation of carbides between the banite laths, however good strain hardening response was observed at austempering temperatures of 350 °C and 400 °C.

Laser Cladding of Ti-6Al-4V Alloy with Ti-Al2O3 Coating for Biomedical Applications

NASA Astrophysics Data System (ADS)

Mthisi, A.; Popoola, A. P. I.; Adebiyi, D. I.; Popoola, O. M.

2018-05-01

The indispensable properties of Ti-6Al-4V alloy coupled with poor tribological properties and delayed bioactivity make it a subject of interest to explore in biomedical application. A quite number of numerous coatings have been employed on titanium alloys, with aim to overcome the poor properties exhibited by this alloy. In this work, the possibility of laser cladding different ad-mixed powders (Ti - 5 wt.% Al2O3 and Ti - 8wt.% Al2O3) on Ti-6Al-4V at various laser scan speed (0.6 and 0.8 m/min) were investigated. The microstructure, phase constituents and corrosion of the resultant coatings were characterized by scanning electron microscope (SEM), Optical microscope, X-Ray diffractometer (XRD) and potentiostat respectively. The electrochemical behaviour of the produced coatings was studied in a simulated body fluid (Hanks solution). The microstructural results show that a defect free coating is achieved at low scan speed and ad-mixed of Ti-5 wt. % Al2O3. Cladding of Ti - Al2O3 improved the corrosion resistance of Ti-6Al-4V alloy regardless of varying neither scan speed nor ad-mixed percentage. However, Ti-5 wt.% Al2O3 coating produced at low scan speed revealed the highest corrosion resistance among the coatings due to better quality coating layer. Henceforth, this coating may be suitable for biomedical applications.

Effect of negative bias on TiAlSiN coating deposited on nitrided Zircaloy-4

NASA Astrophysics Data System (ADS)

Jun, Zhou; Zhendong, Feng; Xiangfang, Fan; Yanhong, Liu; Huanlin, Li

2018-01-01

TiAlSiN coatings were deposited on the nitrided Zircaloy-4 by multi-arc ion plating at -100 V, -200 V and -300 V. In this study, the high temperature oxidation behavior of coatings was tested by a box-type resistance furnace in air for 3 h at 800 °C; the macro-morphology of coatings was observed and analyzed by a zoom-stereo microscope; the micro-morphology of coatings was analyzed by a scanning electron microscopy (SEM), and the chemical elements of samples were analyzed by an energy dispersive spectroscopy(EDS); the adhesion strength of the coating to the substrate was measured by an automatic scratch tester; and the phases of coatings were analyzed by an X-ray diffractometer(XRD). Results show that the coating deposited at -100 V shows better high temperature oxidation resistance behavior, at the same time, Al elements contained in the coating is of the highest amount, meanwhile, the adhesion strength of the coating to the substrate is the highest, which is 33N. As the bias increases, high temperature oxidation resistance behavior of the coating weakens first and then increases, the amount of large particles on the surface of the coating increases first and then decreases whereas the density of the coating decreases first and then increases, and adhesion strength of the coating to the substrate increases first and then weakens. The coating's quality is relatively poor when the bias is -200 V.

Fabrications and application of single crystalline GaN for high-performance deep UV photodetectors

DOE Office of Scientific and Technical Information (OSTI.GOV)

Velazquez, R.; Rivera, M.; Feng, P., E-mail: p.feng@upr.edu

2016-08-15

High-quality single crystalline Gallium Nitride (GaN) semiconductor has been synthesized using molecule beam epitaxy (MBE) technique for development of high-performance deep ultraviolet (UV) photodetectors. Thickness of the films was estimated by using surface profile meter and scanning electron microscope. Electronic states and elemental composition of the films were obtained using Raman scattering spectroscopy. The orientation, crystal structure and phase purity of the films were examined using a Siemens x-ray diffractometer radiation. The surface microstructure was studied using high resolution scanning electron microscopy (SEM). Two types of metal pairs: Al-Al, Al-Cu or Cu-Cu were used for interdigital electrodes on GaN filmmore » in order to examine the Schottky properties of the GaN based photodetector. The characterizations of the fabricated prototype include the stability, responsivity, response and recovery times. Typical time dependent photoresponsivity by switching different UV light source on and off five times for each 240 seconds at a bias of 2V, respectively, have been obtained. The detector appears to be highly sensitive to various UV wavelengths of light with very stable baseline and repeatability. The obtained photoresponsivity was up to 354 mA/W at the bias 2V. Higher photoresponsivity could be obtained if higher bias was applied but it would unavoidably result in a higher dark current. Thermal effect on the fabricated GaN based prototype was discussed.« less

The Effects of Sn Addition on the Microstructure and Surface Properties of Laser Deposited Al-Si-Sn Coatings on ASTM A29 Steel

NASA Astrophysics Data System (ADS)

Fatoba, Olawale S.; Akinlabi, Stephen A.; Akinlabi, Esther T.

2018-03-01

Aluminium and its alloys have been successful metal materials used for many applications like commodity roles, automotive and vital structural components in aircrafts. A substantial portion of Al-Fe-Si alloy is also used for manufacturing the packaging foils and sheets for common heat exchanger applications. The present research was aimed at studying the morphology and surface analyses of laser deposited Al-Sn-Si coatings on ASTM A29 steel. These Fe-intermetallic compounds influence the material properties during rapid cooling by laser alloying technique and play a crucial role for the material quality. Thus, it is of considerable technological interest to control the morphology and distribution of these phases in order to eliminate the negative effects on microstructure. A 3 kW continuous wave ytterbium laser system (YLS) attached to a KUKA robot which controls the movement of the alloying process was utilized for the fabrication of the coatings at optimum laser parameters. The fabricated coatings were investigated for its hardness and wear resistance performance. The field emission scanning electron microscope equipped with energy dispersive spectroscopy (SEM/EDS) was used to study the morphology of the fabricated coatings and X-ray diffractometer (XRD) for the identification of the phases present in the coatings. The coatings were free of cracks and pores with homogeneous and refined microstructures. The enhanced hardness and wear resistance performance were attributed to metastable intermetallic compounds formed.

Luminescent properties under X-ray excitation of Ba(1-x)PbxWO4 disordered solid solution

NASA Astrophysics Data System (ADS)

Bakiz, B.; Hallaoui, A.; Taoufyq, A.; Benlhachemi, A.; Guinneton, F.; Villain, S.; Ezahri, M.; Valmalette, J.-C.; Arab, M.; Gavarri, J.-R.

2018-02-01

A series of polycrystalline barium-lead tungstate Ba1-xPbxWO4 with 0 ≤ x ≤ 1 was synthesized using a classical solid-state method with thermal treatment at 1000 °C. These materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier Transform Raman (FT-Raman) spectroscopy. X-ray diffraction profile analyses were performed using Rietveld method. These materials crystallized in the scheelite tetragonal structure and behaved as quasi ideal solid solution. Raman spectroscopy confirmed the formation of the solid solution. Structural distortions were evidenced in X-ray diffraction profiles and in vibration Raman spectra. The scanning electron microscopy experiments showed large and rounded irregular grains. Luminescence experiments were performed under X-ray excitation. The luminescence emission profiles have been interpreted in terms of four Gaussian components, with a major contribution of blue emission. The integrated intensity of luminescence reached a maximum value in the composition range x = 0.3-0.6, in relation with distortions of crystal lattice.

Phase state of a Bi-43 wt % Sn superplastic alloy and its changes under the effect of external mechanical stresses and aging

NASA Astrophysics Data System (ADS)

Korshak, V. F.; Chushkina, R. A.; Shapovalov, Yu. A.; Mateichenko, P. V.

2011-07-01

Samples of a Bi-43 wt % Sn superplastic alloy have been studied by X-ray diffraction in the ascast state, after compression of as-cast samples to ˜70% on a hydraulic press, after aging in the as-cast and preliminarily compressed state, and using samples deformed under superplastic conditions. The X-ray diffraction studies have been carried out using a DRON-2.0 diffractometer in Cu Kα radiation. The samples aged and deformed under superplasticity conditions have been studied using electron-microprobe analysis in a JSM-820 scanning electron microscope equipped with a LINK AN/85S EDX system. It has been found that the initial structural-phase state of the alloy was amorphous-crystalline. Causes that lead to a change in this state upon deformation and aging are discussed. A conclusion is made that the superplasticity effect manifests itself against the background of processes that are stipulated by the tendency of the initially metastable alloy to phase equilibrium similarly to what is observed in the Sn-38 wt % Pb eutectic alloy studied earlier.

A new x-ray interface and surface scattering environmental cell design for in situ studies of radioactive and atmosphere-sensitive samples.

PubMed

Schmidt, M; Eng, P J; Stubbs, J E; Fenter, P; Soderholm, L

2011-07-01

We present a novel design of a purpose-built, portable sample cell for in situ x-ray scattering experiments of radioactive or atmosphere sensitive samples. The cell has a modular design that includes two independent layers of containment that are used simultaneously to isolate the sensitive samples. Both layers of containment can be flushed with an inert gas, thus serving a double purpose as containment of radiological material (either as a solid sample or as a liquid phase) and in separating reactive samples from the ambient atmosphere. A remote controlled solution flow system is integrated into the containment system that allows sorption experiments to be performed on the diffractometer. The cell's design is discussed in detail and we demonstrate the cell's performance by presenting first results of crystal truncation rod measurements. The results were obtained from muscovite mica single crystals reacted with 1 mM solutions of Th(IV) with 0.1 M NaCl background electrolyte. Data were obtained in specular as well as off-specular geometry.

Optical properties and crystallinity of silver mirrors under a 35 krad cobalt-60 radiation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chiu, Po-Kai, E-mail: pkchiu@itrc.narl.org.tw; Chiang, Donyau; Lee, Chao-Te

2015-09-15

This study addresses the effects of thin film optical design and environmental radiation on the optical properties of silver mirrors. Different experimental thin film optical designs are selected, and the film stack is built using Macleod's approach. Mirror elements are exposed to the same dose of radiation and their properties are characterized using a spectrophotometer equipped with an integration sphere and an x-ray diffractometer. Spectrophotometric analyses of mirrors exposed to about 35 krad of {sup 60}Co radiations overall show that the B270 glass substrates coated with titanium oxide (TiO{sub 2}), silicon dioxide (SiO{sub 2}), pure chrome, and pure silver effectivelymore » reduces radiation damage. The absorption spectrum of the TiO{sub 2} film in the visible region decreases after radiation and displays drifting. As thin metal films comparison, the silver thin film exhibits higher radiation resistance than the chrome thin film. The x-ray diffraction analysis on metal film layers reveals that crystallinity slightly increases when the silver thin film is irradiated.« less

Extracting the pair distribution function of liquids and liquid-vapor surfaces by grazing incidence x-ray diffraction mode.

PubMed

Vaknin, David; Bu, Wei; Travesset, Alex

2008-07-28

We show that the structure factor S(q) of water can be obtained from x-ray synchrotron experiments at grazing angle of incidence (in reflection mode) by using a liquid surface diffractometer. The corrections used to obtain S(q) self-consistently are described. Applying these corrections to scans at different incident beam angles (above the critical angle) collapses the measured intensities into a single master curve, without fitting parameters, which within a scale factor yields S(q). Performing the measurements below the critical angle for total reflectivity yields the structure factor of the top most layers of the water/vapor interface. Our results indicate water restructuring at the vapor/water interface. We also introduce a new approach to extract g(r), the pair distribution function (PDF), by expressing the PDF as a linear sum of error functions whose parameters are refined by applying a nonlinear least square fit method. This approach enables a straightforward determination of the inherent uncertainties in the PDF. Implications of our results to previously measured and theoretical predictions of the PDF are also discussed.

Diagenesis in the Murray Formation, Gale Crater, Mars

NASA Technical Reports Server (NTRS)

Rampe, E. B.; Ming, D. W.; Morris, R. V.; Blake, D. F.; Bristow, T. F.; Chipera. S. J.; Vaniman, D. T.; Yen, A. S.; Grotzinger, J. P.; Downs, R. T.;

Synchrotron radiation topography studies of the phase transition in LaGaO 3 crystals

NASA Astrophysics Data System (ADS)

Yao, G.-D.; Dudley, M.; Wang, Y.; Liu, X.; Liebermann, R. C.

1991-05-01

An investigation of the orthorhombic to rhombohedral phase transformation occurring at 145°C in lanthanum gallate has been conducted using white beam synchrotron X-ray topography (WBSXRT). The existence of the first order transition was confirmed by differential thermal analysis and X-ray diffractometer powder analysis. Subsequent to this, synchrotron white beam Laue patterns were recorded in situ as a function of temperature, during the transition. Before the transition point was reached, (112) orth type reflection twinning was found to be dominant although a small amount of (110) orth type twinning was also observed in the same crystal. Beyond the transition point, not only did the structural change become evident but also reflection twinning on the (110) rhom planes was observed. The scale of this twinning became finer as the temperature was increased beyond the transition temperature. The twinning observed in both the low and high temperature phases gives rise to deformation of the (011) rhom surface plane which creates problems for the potential use of this material as a substrate for growing high Tc superconducting epitaxial layers.

Green Synthesis of Silver Nanoparticles by using Eucalyptus Globulus Leaf Extract

NASA Astrophysics Data System (ADS)

Balamurugan, Madheswaran; Saravanan, Shanmugam

2017-12-01

A single step eco-friendly, energy efficient and economically scalable green method was employed to synthesize silver nanoparticles. In this work, the synthesis of silver nanoparticles using Eucalyptus globulus leaf extract as reducing and capping agent along with water as solvent at normal room temperature is described. Silver nanoparticles were prepared from aqueous silver nitrate solution by adding the leaf extract. The prepared nanoparticles were characterized by using UV-visible Spectrophotometer, X-ray diffractometer, High Resolution Transmission Electron Microscope (HR-TEM) and Fourier Transform Infrared Spectroscope (FTIS). X-ray diffraction studies brought to light the crystalline nature and the face centered cubic structure of the silver nanoparticles. Using HR-TEM. the nano sizes and morphology of the particles were studied. The mean sizes of the prepared silver nanoparticles ranged from 30 to 36 nm. The density of the particles was tuned by varying the molar ratio of silver nitrate. FTIS studies showed the functional group of organic molecules which were located on the surface of the silver nanoparticles. Originating from the leaf extracts, these organic molecules reduced and capped the particles.

Investigations into the Anti-Felting Properties of Sputtered Wool Using Plasma Treatment

NASA Astrophysics Data System (ADS)

M. Borghei, S.; Shahidi, S.; Ghoranneviss, M.; Abdolahi, Z.

2013-01-01

In this research the effects of mordant and plasma sputtering treatments on the crystallinity and morphological properties of wool fabrics were investigated. The felting behavior of the treated samples was also studied. We used madder as a natural dye and copper sulfate as a metal mordant. We also used copper as the electrode material in a DC magnetron plasma sputtering device. The anti-felting properties of the wool samples before and after dying was studied, and it was shown that the shrink resistance and anti-felting behavior of the wool had been significantly improved by the plasma sputtering treatment. In addition, the percentage of crystallinity and the size of the crystals were investigated using an X-ray diffractometer, and a scanning electron microscope was used for morphological analysis. The amount of copper particles on the surface of the mordanted and sputtered fabrics was studied using the energy dispersive X-ray (EDX) method, and the hydrophobic properties of the samples were examined using the water drop test. The results show that with plasma sputtering treatment, the hydrophobic properties of the surface of wool become super hydrophobic.

A high-temperature neutron diffraction study of Nb 2AlC and TiNbAlC

DOE PAGES

Bentzel, Grady W.; Lane, Nina J.; Vogel, Sven C.; ...

2014-12-16

In this paper, we report on the crystal structures of Nb 2AlC and TiNbAlC actual composition (Ti 0.45,Nb 0.55) 2AlC compounds determined from Rietveld analysis of neutron diffraction patterns in the 300-1173 K temperature range. The average linear thermal expansion coefficients of a Nb 2AlC sample in the a and c directions are, respectively, 7.9(5)x10 -6 K -1 and 7.7(5)x10 -6 K -1 on one neutron diffractometer and 7.3(3)x10 -6 K -1 and 7.0(2)x10 -6 K -1 on a second diffractometer. The respective values for the (Ti 0.45,Nb 0.55) 2AlC composition - only tested on one diffractometer - are 8.5(3)x10more » -6 K -1 and 7.5(5)x10 -6 K -1. These values are relatively low compared to other MAX phases. Like other MAX phases, however, the atomic displacement parameters show that the Al atoms vibrate with higher amplitudes than the Ti and C atoms, and 1 more along the basal planes than normal to them. In addition, when the predictions of the atomic displacement parameters obtained from density functional theory are compared to the experimental results, good quantitative agreement is found for the Al atoms. In case of the Nb and C atoms, the agreement was more qualitative.« less

3D-printing zirconia implants; a dream or a reality? An in-vitro study evaluating the dimensional accuracy, surface topography and mechanical properties of printed zirconia implant and discs.

PubMed

Osman, Reham B; van der Veen, Albert J; Huiberts, Dennis; Wismeijer, Daniel; Alharbi, Nawal

2017-11-01

The aim of this study was to evaluate the dimensional accuracy, surface topography of a custom designed, 3D-printed zirconia dental implant and the mechanical properties of printed zirconia discs. A custom designed implant was 3D-printed in zirconia using digital light processing technique (DLP). The dimensional accuracy was assessed using the digital-subtraction technique. The mechanical properties were evaluated using biaxial flexure strength test. Three different build angles were adopted to print the specimens for the mechanical test; 0°(Vertical), 45° (Oblique) and 90°(Horizontal) angles. The surface topography, crystallographic phase structure and surface roughness were evaluated using scanning electron microscopy analysis (SEM), X-ray diffractometer and confocal microscopy respectively. The printed implant was dimensionally accurate with a root mean square (RMSE) value of 0.1mm. The Weibull analysis revealed a statistically significant higher characteristic strength (1006.6MPa) of 0° printed specimens compared to the other two groups and no significant difference between 45° (892.2MPa) and 90° (866.7MPa) build angles. SEM analysis revealed cracks, micro-porosities and interconnected pores ranging in size from 196nm to 3.3µm. The mean Ra (arithmetic mean roughness) value of 1.59µm (±0.41) and Rq (root mean squared roughness) value of 1.94µm (±0.47) was found. A crystallographic phase of primarily tetragonal zirconia typical of sintered Yttria tetragonal stabilized zirconia (Y-TZP) was detected. DLP prove to be efficient for printing customized zirconia dental implants with sufficient dimensional accuracy. The mechanical properties showed flexure strength close to those of conventionally produced ceramics. Optimization of the 3D-printing process parameters is still needed to improve the microstructure of the printed objects. Copyright © 2017 Elsevier Ltd. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yashchuk, Valeriy V; Conley, Raymond; Anderson, Erik H.

We discuss the results of SEM and TEM measurements with the BPRML test samples fabricated from a BPRML (WSi2/Si with fundamental layer thickness of 3 nm) with a Dual Beam FIB (focused ion beam)/SEM technique. In particular, we demonstrate that significant information about the metrological reliability of the TEM measurements can be extracted even when the fundamental frequency of the BPRML sample is smaller than the Nyquist frequency of the measurements. The measurements demonstrate a number of problems related to the interpretation of the SEM and TEM data. Note that similar BPRML test samples can be used to characterize x-raymore » microscopes. Corresponding work with x-ray microscopes is in progress.« less

Removal of heavy metal Cu(II) in simulated aquaculture wastewater by modified palygorskite.

PubMed

Cao, Jia-Shun; Wang, Cheng; Fang, Fang; Lin, Jun-Xiong

2016-12-01

Palygorskite (PAL) is a good heavy metal adsorbent due to its high surface area, low cost, and environmentally compatibility. But the natural PAL has limited its adsorption capacity and selectivity. In this study, a cost-effective and readily-generated absorbent, l-threonine-modified palygorskite (L-PAL), was used and its performance for Cu(II) removal in simulated aquaculture wastewater was evaluated. After preparation, L-PAL was characterized by using Fourier transform infrared spectroscopy, scanning electron microscope, energy dispersive X-ray spectroscopy, X-ray diffractometer, X-ray photoelectron spectroscopy, transmission electron microscopy and thermogravimetric analysis. The impacts of pH, adsorbent dosage, contact time, and initial Cu(II) concentration on the adsorption capacity of L-PAL were examined. The Cu(II) adsorption capacity on L-PAL was enhanced almost 10 times than that of raw PAL. The adsorption isotherms of Cu(II) fit the Langmuir isotherms, and the adsorption kinetics was dominated by the pseudo-second-order model. The thermodynamic parameters at four temperatures were calculated, which indicated that the adsorption was spontaneous and endothermic. The adsorption mechanism involves complexation, chelation, electrostatic attraction, and micro-precipitation. Furthermore, L-PAL is shown to have a high regeneration capacity. These results indicate that L-PAL is a cheap and promising absorbent for Cu(II) removal and hold potential to be used for aquaculture wastewater treatment. Copyright © 2016 Elsevier Ltd. All rights reserved.

Tunable optical properties of plasmonic Au/Al2O3 nanocomposite thin films analyzed by spectroscopic ellipsometry accounting surface characteristics.

PubMed

Jaiswal, Jyoti; Mourya, Satyendra; Malik, Gaurav; Chandra, Ramesh

2018-05-01

In the present work, we have fabricated plasmonic gold/alumina nanocomposite (Au/Al 2 O 3 NC) thin films on a glass substrate at room temperature by RF magnetron co-sputtering. The influence of the film thickness (∼10-40  nm) on the optical and other physical properties of the samples was investigated and correlated with the structural and compositional properties. The X-ray diffractometer measurement revealed the formation of Au nanoparticles with average crystallite size (5-9.2 nm) embedded in an amorphous Al 2 O 3 matrix. The energy-dispersive X ray and X-ray photoelectron spectroscopy results confirmed the formation of Au/Al 2 O 3 NC quantitatively and qualitatively and it was observed that atomic% of Au increased by increasing thickness. The optical constants of the plasmonic Au/Al 2 O 3 NC thin films were examined by variable angle spectroscopic ellipsometry in the wide spectral range of 246-1688 nm, accounting the surface characteristics in the optical stack model, and the obtained results are expected to be unique. Additionally, a thickness-dependent blueshift (631-590 nm) of surface plasmon resonance peak was observed in the absorption spectra. These findings of the plasmonic Au/Al 2 O 3 NC films may allow the design and fabrication of small, compact, and efficient devices for optoelectronic and photonic applications.

Electrodeposition of Manganese-Nickel Oxide Films on a Graphite Sheet for Electrochemical Capacitor Applications.

PubMed

Lee, Hae-Min; Lee, Kangtaek; Kim, Chang-Koo

2014-01-09

Manganese-nickel (Mn-Ni) oxide films were electrodeposited on a graphite sheet in a bath consisting of manganese acetate and nickel chloride, and the structural, morphological, and electrochemical properties of these films were investigated. The electrodeposited Mn-Ni oxide films had porous structures covered with nanofibers. The X-ray diffractometer pattern revealed the presence of separate manganese oxide (g-MnO₂) and nickel oxide (NiO) in the films. The electrodeposited Mn-Ni oxide electrode exhibited a specific capacitance of 424 F/g in Na₂SO₄ electrolyte. This electrode maintained 86% of its initial specific capacitance over 2000 cycles of the charge-discharge operation, showing good cycling stability.

Study the effect of nitrogen flow rate on tribological properties of tantalum nitride based coatings

NASA Astrophysics Data System (ADS)

Chauhan, Dharmesh B.; Chauhan, Kamlesh V.; Sonera, Akshay L.; Makwana, Nishant S.; Dave, Divyeshkumar P.; Rawal, Sushant K.

2018-05-01

Tantalum Nitride (TaN) based coatings are well-known for their high temperature stability and chemical inertness. We have studied the effect of nitrogen flow rate variation on the structural and tribological properties of TaN based coating deposited by RF magnetron sputtering process. The nitrogen flow rate was varied from 5 to 30 sccm. X-ray diffractometer (XRD) and Atomic Force Microscopy (AFM) were used to determine structure and surface topography of coating. Pin on disc tribometer was used to determine tribological properties of coating. TaN coated brass and mild steel substrates shows higher wear resistance compared to uncoated substrates of brass and mild steel.

Structural and optical properties of ITO and Cu doped ITO thin films

NASA Astrophysics Data System (ADS)

Chakraborty, Deepannita; Kaleemulla, S.; Rao, N. Madhusudhana; Subbaravamma, K.; Rao, G. Venugopal

2018-04-01

(In0.95Sn0.05)2O3 and (In0.90Cu0.05Sn0.05)2O3 thin films were coated onto glass substrate by electron beam evaporation technique. The structural and optical properties of ITO and Cu doped ITO thin films have been studied by X-ray diffractometer (XRD) and UV-Vis-NIR spectrophotometer. The crystallite size obtained for ITO and Cu doped ITO thin films was in the range of 24 nm to 22 nm. The optical band gap of 4 eV for ITO thin film sample has been observed. The optical band gap decreases to 3.85 eV by doping Cu in ITO.

Electrochemical Deposition of Si-Ca/P on Nanotube Formed Beta Ti Alloy by Cyclic Voltammetry Method.

PubMed

Jeong, Yong-Hoon; Choe, Han-Cheol

2015-08-01

The purpose of this study was to investigate electrochemical deposition of Si-Ca/P on nanotube formed Ti-35Nb-10Zr alloy by cyclic voltammetry method. Electrochemical deposition of Si substituted Ca/P was performed by pulsing the applied potential on nanotube formed surface. The surface characteristics were observed by field-emission scanning electron microscopy, X-ray diffractometer, and potentiodynamic polarization test. The phase structure and surface morphologies of Si-Ca/P deposition were affected by deposition cycles. From the anodic polarization test, nanotube formed surface at 20 V showed the high corrosion resistance with lower value of Icorr, I300, and Ipass.

Synthesis of TiN/a-Si3N4 thin film by using a Mather type dense plasma focus system

NASA Astrophysics Data System (ADS)

Hussain, T.; R., Ahmad; Khalid, N.; A. Umar, Z.; Hussnain, A.

2013-05-01

A 2.3 kJ Mather type pulsed plasma focus device was used for the synthesis of a TiN/a-Si3N4 thin film at room temperature. The film was characterized using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and atomic force microscopy (AFM). The XRD pattern confirms the growth of polycrystalline TiN thin film. The XPS results indicate that the synthesized film is non-stoichiometric and contains titanium nitride, silicon nitride, and a phase of silicon oxy-nitride. The SEM and AFM results reveal that the surface of the synthesized film is quite smooth with 0.59 nm roughness (root-mean-square).

Planar techniques for fabricating X-ray diffraction gratings and zone plates

NASA Technical Reports Server (NTRS)

Smith, H. I.; Anderson, E. H.; Hawryluk, A. M.; Schattenburg, M. L.

1984-01-01

The state of current planar techniques in the fabrication of Fresnel zone plates and diffraction gratings is reviewed. Among the fabrication techniques described are multilayer resist techniques; scanning electron beam lithography; and holographic lithography. Consideration is also given to: X-ray lithography; ion beam lithography; and electroplating. SEM photographs of the undercut profiles obtained in a type AZ 135OB photoresistor by holographic lithography are provided.

Effect of shape and thickness of asbestos bundles and fibres on EDS microanalysis: A Monte Carlo simulation

NASA Astrophysics Data System (ADS)

Moro, D.; Valdre, G.

2016-02-01

Quantitative microanalysis of tiny asbestos mineral fibres by scanning electron microscopy equipped with energy-dispersive X-ray spectroscopy (SEM-EDS) still represents a complex analytical issue. This complexity arises from the variable fibre shape and small thickness (< 5 μm) compared with the penetration of the incident electron beam. Here, we present the results of Monte Carlo simulations of chrysotile, crocidolite and amosite fibres (and bundles of fibres) of circular and square section and thicknesses from 0.1 μm to 10 μm, to investigate the effect of shape and thickness on SEM-EDS microanalysis. The influence of shape and thickness on the simulated spectrum was investigated for electron beam energies of 5, 15 and 25 keV, respectively. A strong influence of the asbestos bundles and fibres shape and thickness on the detected EDS X-ray intensity was observed. The X-ray intensity trends as a function of fibre thickness showed a non-linear dependence for all the elements and minerals. In general, the X-ray intensities showed a considerable reduction for thicknesses below about 5 μm at 5 keV, 2 μm at 15 keV, and 5 μm at 25 keV. Correction parameters, k-ratios, for the asbestos fibre thickness effect, are reported.

Surface modification of tooth root canal after application of an X-ray opaque waveguide

NASA Astrophysics Data System (ADS)

Dostálová, T.; Jelínková, H.; Šulc, J.; Němec, M.; Koranda, P.; Bartoňová, M.; Radina, P.; Miyagi, M.; Shi, Y.-W.; Matsuura, Y.

The interest in endodontic use of dental laser systems has been increasing. With the development of thin and flexible delivery systems for various wavelengths, laser applications in endodontics may become even more desirable. The aim of this study is to check the X-ray opacity of a hollow waveguide and to observe the results after laser root canal treatment. The root canal systems of 10 molars were treated endodontically by laser. For the laser radiation source, an Er:YAG laser system generating a wavelength of 2940 nm and an Alexandrite laser system generating a wavelength of 375 nm were used. The hollow waveguide used was checked under X-ray . A root canal surface treated by laser radiation was analyzed by a scanning electron microscope (SEM). The special hollow glass waveguide used was visible in the root canal system under X-ray imaging. Surface modification of the root canal after laser treatment was not found. After conventional treatment the root canal was enlarged. The surface was covered with a smear layer. After application of both laser systems, the smear layer was removed. The resulting canal surface was found to be clean and smooth. Under SEM observation open dentinal tubules were visible. No cracks were present, nor were surface modifications observed.

Synthesis of Galaxite, Mn0.9Co0.1Al2O4, and its application as a novel nanocatalyst for electrochemical hydrogen evolution reaction

NASA Astrophysics Data System (ADS)

Saeidfirozeh, Homa; Shafiekhani, Azizollah; Beheshti-Marnani, Amirkhosro; Askari, Mohammad Bagher

2018-06-01

A new compound Mn0.9Co0.1Al2O4 nanowires were synthesized by thermal method. The resulting powder samples were characterized by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), and X-ray diffraction (XRD). We found that a set of phase transformation occurred during the process. Eventually, five phases including three spinal phases, the corundum (á-Al2O3) and MnO were formed at 1100 °C.As dominant morphology, the cubic galaxite nanowires were identified by X-ray analysis. Moreover, X-ray analysis showed that Mn3O4 and Co3O4 nanoparticles were formed in tetragonal and cubic symmetry respectively. The SEM image revealed that a dominate morphology of product has cubic nanowires shape with an average diameter in range 38-43 nm. Furthermore, we observed that influence of temperature was very important in the nanowire formation process. Electrochemical hydrogen evolution reaction (HER) of synthetic composite was evaluated and the over potential of HER was calculated about 110 mV with low Tafel slope equal to 42 mV dec-1, which was comparable with amounts reported transition metal dichalcogenides with satisfying durability.

Total rate imaging with x-rays (TRIX)--a simple method of forming a non-projection x-ray image in the SEM using an energy dispersive detector and its application to biological specimens.

PubMed

Ingram, P; Shelburne, J D

1980-01-01

X-ray images can be formed in a conventional scanning electron microscope equipped with a Si(Li) energy dispersive spectrometer. All the x-ray events generated in the electron beam scanning process are synchronously displayed in the same manner as for dot maps. The quasi-digital image formed using Total Rate Imaging with X-rays (TRIX) exhibits good gray scale contrast and is dependent on topography, orientation and atomic number. Although this latter dependence is complex, it has been found useful in locating several types of inclusions in lung tissue (silicosis), human alveolar macrophages and cigarette smoke condensate. This is because of the greater depth of penetration of x-rays than backscattered electrons (BSE) usually used for such localizations in a matrix, and the negligible sensitivity of the Si(Li) detector to x-rays from an organic biological matrix. The optimum procedure is to use a combination of TRIX and BSE to investigate such specimens.

Band Offset Measurements in Atomic-Layer-Deposited Al2O3/Zn0.8Al0.2O Heterojunction Studied by X-ray Photoelectron Spectroscopy.

PubMed

Yan, Baojun; Liu, Shulin; Heng, Yuekun; Yang, Yuzhen; Yu, Yang; Wen, Kaile

2017-12-01

Pure aluminum oxide (Al 2 O 3 ) and zinc aluminum oxide (Zn x Al 1-x O) thin films were deposited by atomic layer deposition (ALD). The microstructure and optical band gaps (E g ) of the Zn x Al 1-x O (0.2 ≤ x ≤ 1) films were studied by X-ray diffractometer and Tauc method. The band offsets and alignment of atomic-layer-deposited Al 2 O 3 /Zn 0.8 Al 0.2 O heterojunction were investigated in detail using charge-corrected X-ray photoelectron spectroscopy. In this work, different methodologies were adopted to recover the actual position of the core levels in insulator materials which were easily affected by differential charging phenomena. Valence band offset (ΔE V ) and conduction band offset (ΔE C ) for the interface of the Al 2 O 3 /Zn 0.8 Al 0.2 O heterojunction have been constructed. An accurate value of ΔE V  = 0.82 ± 0.12 eV was obtained from various combinations of core levels of heterojunction with varied Al 2 O 3 thickness. Given the experimental E g of 6.8 eV for Al 2 O 3 and 5.29 eV for Zn 0.8 Al 0.2 O, a type-I heterojunction with a ΔE C of 0.69 ± 0.12 eV was found. The precise determination of the band alignment of Al 2 O 3 /Zn 0.8 Al 0.2 O heterojunction is of particular importance for gaining insight to the design of various electronic devices based on such heterointerface.

Environmentally induced chemical and morphological heterogeneity of zinc oxide thin films

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jiang, Hua; Chou, Kang Wei; Petrash, Stanislas

Zinc oxide (ZnO) thin films have been reported to suffer from degradation in electrical properties, when exposed to elevated heat and humidity, often leading to failures of electronic devices containing ZnO films. This degradation appears to be linked to water and oxygen penetration into the ZnO film. However, a direct observation in the ZnO film morphological evolution detailing structural and chemical changes has been lacking. Here, we systematically investigated the chemical and morphological heterogeneities of ZnO thin films caused by elevated heat and humidity, simulating an environmental aging. X-ray fluorescence microscopy, X-ray absorption spectroscopy, grazing incidence small angle and widemore » angle X-ray scattering, scanning electron microscopy (SEM), ultra-high-resolution SEM, and optical microscopy were carried out to examine ZnO and Al-doped ZnO thin films on two different substrates—silicon wafers and flexible polyethylene terephthalate (PET) films. In the un-doped ZnO thin film, the simulated environmental aging is resulting in pin-holes. In the Al-doped ZnO thin films, significant morphological changes occurred after the treatment, with an appearance of platelet-shaped structures that are 100–200 nm wide by 1 μm long. Synchrotron x-ray characterization further confirmed the heterogeneity in the aged Al-doped ZnO, showing the formation of anisotropic structures and disordering. X-ray diffraction and X-ray absorption spectroscopy indicated the formation of a zinc hydroxide in the aged Al-doped films. Utilizing advanced characterization methods, our studies provided information with an unprecedented level of details and revealed the chemical and morphologically heterogeneous nature of the degradation in ZnO thin films.« less

Environmentally induced chemical and morphological heterogeneity of zinc oxide thin films

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jiang, Hua; Chou, Kang Wei; Petrash, Stanislas

Zinc oxide (ZnO) thin films have been reported to suffer from degradation in electrical properties, when exposed to elevated heat and humidity, often leading to failures of electronic devices containing ZnO films. This degradation appears to be linked to water and oxygen penetration into the ZnO film. However, a direct observation in the ZnO film morphological evolution detailing structural and chemical changes has been lacking. Here, we systematically investigated the chemical and morphological heterogeneities of ZnO thin films caused by elevated heat and humidity, simulating an environmental aging. X-ray fluorescence microscopy, X-ray absorption spectroscopy, grazing incidence small angle and widemore » angle X-ray scattering, scanning electron microscopy (SEM), ultra-high-resolution SEM, and optical microscopy were carried out to examine ZnO and Al-doped ZnO thin films on two different substrates—silicon wafers and flexible polyethylene terephthalate (PET) films. In the un-doped ZnO thin film, the simulated environmental aging is resulting in pin-holes. In the Al-doped ZnO thin films, significant morphological changes occurred after the treatment, with an appearance of platelet-shaped structures that are 100–200 nm wide by 1μm long. Synchrotron x-ray characterization further confirmed the heterogeneity in the aged Al-doped ZnO, showing the formation of anisotropic structures and disordering. X-ray diffraction and X-ray absorption spectroscopy indicated the formation of a zinc hydroxide in the aged Al-doped films. In conclusion, utilizing advanced characterization methods, our studies provided information with an unprecedented level of details and revealed the chemical and morphologically heterogeneous nature of the degradation in ZnO thin films.« less

Environmentally induced chemical and morphological heterogeneity of zinc oxide thin films

DOE PAGES

Jiang, Hua; Chou, Kang Wei; Petrash, Stanislas; ...

2016-09-02

Zinc oxide (ZnO) thin films have been reported to suffer from degradation in electrical properties, when exposed to elevated heat and humidity, often leading to failures of electronic devices containing ZnO films. This degradation appears to be linked to water and oxygen penetration into the ZnO film. However, a direct observation in the ZnO film morphological evolution detailing structural and chemical changes has been lacking. Here, we systematically investigated the chemical and morphological heterogeneities of ZnO thin films caused by elevated heat and humidity, simulating an environmental aging. X-ray fluorescence microscopy, X-ray absorption spectroscopy, grazing incidence small angle and widemore » angle X-ray scattering, scanning electron microscopy (SEM), ultra-high-resolution SEM, and optical microscopy were carried out to examine ZnO and Al-doped ZnO thin films on two different substrates—silicon wafers and flexible polyethylene terephthalate (PET) films. In the un-doped ZnO thin film, the simulated environmental aging is resulting in pin-holes. In the Al-doped ZnO thin films, significant morphological changes occurred after the treatment, with an appearance of platelet-shaped structures that are 100–200 nm wide by 1μm long. Synchrotron x-ray characterization further confirmed the heterogeneity in the aged Al-doped ZnO, showing the formation of anisotropic structures and disordering. X-ray diffraction and X-ray absorption spectroscopy indicated the formation of a zinc hydroxide in the aged Al-doped films. In conclusion, utilizing advanced characterization methods, our studies provided information with an unprecedented level of details and revealed the chemical and morphologically heterogeneous nature of the degradation in ZnO thin films.« less

Effect of cadmium incorporation on the properties of zinc oxide thin films

NASA Astrophysics Data System (ADS)

Bharath, S. P.; Bangera, Kasturi V.; Shivakumar, G. K.

2018-02-01

Cd x Zn1- x O (0 ≤ x ≤ 0.20) thin films are deposited on soda lime glass substrates using spray pyrolysis technique. To check the thermal stability, Cd x Zn1- x O thin films are subjected to annealing. Both the as-deposited and annealed Cd x Zn1- x O thin films are characterized using X-ray diffraction (XRD), scanning electron microscope (SEM) and energy-dispersive X-ray analysis (EDAX) to check the structural, surface morphological and compositional properties, respectively. XRD analysis reveals that the both as-deposited and annealed Cd x Zn1- x O thin films are (002) oriented with wurtzite structure. SEM studies confirm that as-deposited, as well as annealed Cd x Zn1- x O thin films are free from pinholes and cracks. Compositional analysis shows the deficiency in Cd content after annealing. Optical properties evaluated from UV-Vis spectroscopy shows red shift in the band gap for Cd x Zn1- x O thin films. Electrical property measured using two probe method shows a decrease in the resistance after Cd incorporation. The results indicate that cadmium can be successfully incorporated in zinc oxide thin films to achieve structural changes in the properties of films.

Gold nanoparticle flow sensors designed for dynamic X-ray imaging in biofluids.

PubMed

Ahn, Sungsook; Jung, Sung Yong; Lee, Jin Pyung; Kim, Hae Koo; Lee, Sang Joon

2010-07-27

X-ray-based imaging is one of the most powerful and convenient methods in terms of versatility in applicable energy and high performance in use. Different from conventional nuclear medicine imaging, contrast agents are required in X-ray imaging especially for effectively targeted and molecularly specific functions. Here, in contrast to much reported static accumulation of the contrast agents in targeted organs, dynamic visualization in a living organism is successfully accomplished by the particle-traced X-ray imaging for the first time. Flow phenomena across perforated end walls of xylem vessels in rice are monitored by a gold nanoparticle (AuNP) (approximately 20 nm in diameter) as a flow tracing sensor working in nontransparent biofluids. AuNPs are surface-modified to control the hydrodynamic properties such as hydrodynamic size (DH), zeta-potential, and surface plasmonic properties in aqueous conditions. Transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray nanoscopy (XN), and X-ray microscopy (XM) are used to correlate the interparticle interactions with X-ray absorption ability. Cluster formation and X-ray contrast ability of the AuNPs are successfully modulated by controlling the interparticle interactions evaluated as flow-tracing sensors.

Monte Carlo simulation of the effect of shape and thickness on SEM-EDS microanalysis of asbestos fibres and bundles: the case of anthophyllite, tremolite and actinolite

NASA Astrophysics Data System (ADS)

Valdrè, G.; Moro, D.; Ulian, G.

2018-01-01

Asbestos is a generic term used for six types of silicate minerals that are found in fibres or bundles of fibres, which can be easily cleaved into thinner ones. Scanning electron microscopy energy-dispersive X-ray spectrometry (SEM-EDS) quantitative microanalysis of asbestos mineral fibres still represents a complex analytical issue because of the variable fibre shape and small thickness (< 5 μm) compared with the penetration depth of the incident electron beam. Following previous work on chrysotile, crocidolite and amosite, here we present a study by means of Monte Carlo simulations of the thickness and shape effect on SEM-EDS microanalysis of anthophyllite, tremolite and actinolite asbestos. Realistic experimental conditions, such as sample geometry, SEM set-up and detector physics were taken into account. We report the results obtained on 100 μm long fibres and bundles of circular and square section and thicknesses from to 0.1 μm to 10 μm, for electron beam energies of 5, 15 and 25 keV. A strong influence of the asbestos mineral fibres and bundles shape and thickness on the detected EDS X-ray intensity was observed. In general, the X-ray intensities as a function of fibre thickness showed a considerable reduction below about 0.5 μm at 5 keV, 2 μm at 15 keV, and 5 μm at 25 keV for all the elements and minerals, with a non-linear dependence. Correction parameters, k-ratio, for the thickness effect were calculated and proposed.

The CheMin XRD on the Mars Science Laboratory Rover Curiosity: Construction, Operation, and Quantitative Mineralogical Results from the Surface of Mars

NASA Technical Reports Server (NTRS)

Blake, David F.

2015-01-01

The Mars Science Laboratory mission was launched from Cape Canaveral, Florida on Nov. 26, 2011 and landed in Gale crater, Mars on Aug. 6, 2012. MSL's mission is to identify and characterize ancient "habitable" environments on Mars. MSL's precision landing system placed the Curiosity rover within 2 km of the center of its 20 X 6 km landing ellipse, next to Gale's central mound, a 5,000 meter high pile of laminated sediment which may contain 1 billion years of Mars history. Curiosity carries with it a full suite of analytical instruments, including the CheMin X-ray diffractometer, the first XRD flown in space. CheMin is essentially a transmission X-ray pinhole camera. A fine-focus Co source and collimator transmits a 50µm beam through a powdered sample held between X-ray transparent plastic windows. The sample holder is shaken by a piezoelectric actuator such that the powder flows like a liquid, each grain passing in random orientation through the beam over time. Forward-diffracted and fluoresced X-ray photons from the sample are detected by an X-ray sensitive Charge Coupled Device (CCD) operated in single photon counting mode. When operated in this way, both the x,y position and the energy of each photon are detected. The resulting energy-selected Co Kalpha Debye-Scherrer pattern is used to determine the identities and amounts of minerals present via Rietveld refinement, and a histogram of all X-ray events constitutes an X-ray fluorescence analysis of the sample.The key role that definitive mineralogy plays in understanding the Martian surface is a consequence of the fact that minerals are thermodynamic phases, having known and specific ranges of temperature, pressure and composition within which they are stable. More than simple compositional analysis, definitive mineralogical analysis can provide information about pressure/temperature conditions of formation, past climate, water activity and the like. Definitive mineralogical analyses are necessary to establish the origin or provenance of a sample. The search for evidence of extant or extinct life on Mars will initially be a search for evidence of present or past conditions supportive of life (e.g., evidence of water), not for life itself.Results of the first 1,000 sols (Mars days) will be discussed, including the discovery of the first habitable environment on Mars.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Amusan, Akinwumi A., E-mail: akinwumi.amusan@ovgu.de; Kalkofen, Bodo; Burte, Edmund P.

Silver (Ag) layers were deposited by remote plasma enhanced atomic layer deposition (PALD) using Ag(fod)(PEt{sub 3}) (fod = 2,2-dimethyl-6,6,7,7,8,8,8-heptafluorooctane-3,5-dionato) as precursor and hydrogen plasma on silicon substrate covered with thin films of SiO{sub 2}, TiN, Ti/TiN, Co, Ni, and W at different deposition temperatures from 70  to 200 °C. The deposited silver films were analyzed by x-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), scanning electron microscopy (SEM), transmission electron microscopy (TEM) with energy dispersive x-ray spectroscopy, four point probe measurement, ellipsometric measurement, x-ray fluorescence (XRF), and x-ray diffraction (XRD). XPS revealed pure Ag with carbon and oxygen contamination close to the detectionmore » limit after 30 s argon sputtering for depositions made at 120 and 200 °C substrate temperatures. However, an oxygen contamination was detected in the Ag film deposited at 70 °C after 12 s argon sputtering. A resistivity of 5.7 × 10{sup −6} Ω cm was obtained for approximately 97 nm Ag film on SiO{sub 2}/Si substrate. The thickness was determined from the SEM cross section on the SiO{sub 2}/Si substrate and also compared with XRF measurements. Polycrystalline cubic Ag reflections were identified from XRD for PALD Ag films deposited at 120 and 200 °C. Compared to W surface, where poor adhesion of the films was found, Co, Ni, TiN, Ti/TiN and SiO{sub 2} surfaces had better adhesion for silver films as revealed by SEM, TEM, and AFM images.« less

Facile solvothermal synthesis of cube-like Ag@AgCl: a highly efficient visible light photocatalyst

NASA Astrophysics Data System (ADS)

Han, Lei; Wang, Ping; Zhu, Chengzhou; Zhai, Yueming; Dong, Shaojun

2011-07-01

In this paper, a stable and highly efficient plasmonic photocatalyst, Ag@AgCl, with cube-like morphology, has been successfully prepared via a simple hydrothermal method. Using methylene dichloride as chlorine source in the synthesis can efficiently control the morphology of Ag@AgCl, due to the low release rate of chloride ions. Scanning electron microscopy (SEM), X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and UV-vis diffuse reflectance spectra were used to characterize the obtained product. The photocatalytic activity of the obtained product was evaluated by the photodegradation of methyl orange (MO) under visible light irradiation, and it was found, interestingly, that Ag@AgCl exhibits high visible light photocatalytic activity and good stability.In this paper, a stable and highly efficient plasmonic photocatalyst, Ag@AgCl, with cube-like morphology, has been successfully prepared via a simple hydrothermal method. Using methylene dichloride as chlorine source in the synthesis can efficiently control the morphology of Ag@AgCl, due to the low release rate of chloride ions. Scanning electron microscopy (SEM), X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and UV-vis diffuse reflectance spectra were used to characterize the obtained product. The photocatalytic activity of the obtained product was evaluated by the photodegradation of methyl orange (MO) under visible light irradiation, and it was found, interestingly, that Ag@AgCl exhibits high visible light photocatalytic activity and good stability. Electronic supplementary information (ESI) available: SEM images of the AgCl samples synthesized by changing the addition amount of PVP and AgNO3. See DOI: 10.1039/c1nr10247h

Three dimensional rock microstructures: insights from FIB-SEM tomography

NASA Astrophysics Data System (ADS)

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. Quadruple point junctions between four grains cannot be investigated in 2D studies. 3D microstructural studies suggest that triple lines and quadruple points are important sites for the initiation of recrystallization, reaction and fracture.

Structural, morphological and magnetic properties of pure and Ni-doped ZnO nanoparticles synthesized by sol-gel method

NASA Astrophysics Data System (ADS)

Undre, Pallavi G.; Birajdar, Shankar D.; Kathare, R. V.; Jadhav, K. M.

2018-05-01

In this work pure and Ni-doped ZnO nanoparticles have been prepared by sol-gel method. Influence of nickel doping on structural, morphological and magnetic properties of prepared nanoparticles was investigated by X-ray diffraction technique (XRD), Scanning electron microscopy (SEM) and Pulse field magnetic hysteresis loop. X-ray diffraction pattern shows the formation of a single phase with hexagonal wurtzite structure of both pure and Ni-doped ZnO nanoparticles. The lattice parameters `an' and `c' of Ni-doped ZnO is slightly less than that of pure ZnO nanoparticles. The crystalline size of prepared nanoparticles is found to be in 29 and 31 nm range. SEM technique used to examine the surface morphology of samples, SEM image confirms the nanocrystalline nature of present samples. From the pulse field hysteresis loop technique pure and Ni-doped ZnO nanoparticles show diamagnetic and ferromagnetic behavior at room temperature respectively.

Acquisition of a High Resolution Field Emission Scanning Electron Microscope for the Analysis of Returned Samples

NASA Technical Reports Server (NTRS)

Nittler, Larry R.

2003-01-01

This grant furnished funds to purchase a state-of-the-art scanning electron microscope (SEM) to support our analytical facilities for extraterrestrial samples. After evaluating several instruments, we purchased a JEOL 6500F thermal field emission SEM with the following analytical accessories: EDAX energy-dispersive x-ray analysis system with fully automated control of instrument and sample stage; EDAX LEXS wavelength-dispersive x-ray spectrometer for high sensitivity light-element analysis; EDAX/TSL electron backscatter diffraction (EBSD) system with software for phase identification and crystal orientation mapping; Robinson backscatter electron detector; and an in situ micro-manipulator (Kleindiek). The total price was $550,000 (with $150,000 of the purchase supported by Carnegie institution matching funds). The microscope was delivered in October 2002, and most of the analytical accessories were installed by January 2003. With the exception of the wavelength spectrometer (which has been undergoing design changes) everything is working well and the SEM is in routine use in our laboratory.

Preparation, Structural and Dielectric Behaviors of CoxMn1-xMn2O4 (0 ≤ x ≤ 1) Nanoparticles

NASA Astrophysics Data System (ADS)

Taufiq, A.; Muzammil, M.; Fuad, A.; Hidayat, N.; Sunaryono, S.; Mufti, N.; Hidayat, A.; Diantoro, M.; Munasir, M.

2018-05-01

Cobalt-manganese oxide nanoparticles become remarkable metal oxides due to their physical characters, for example, their electrical properties. In this paper, we report the synthesis of Co x Mn1-x Mn2O4 (0 ≤ x ≤ 1) nanoparticles via a precipitation method. The structural and dielectric properties were investigated by means of X-ray diffractometer (XRD) and LCR-meter. From the data analysis, it was found that the Co x Mn1-x Mn2O4 particles structured spinel cubic with the particle size ranging from 22.7 to 28.6 nm. Increasing Co2+ ions led to declining lattice and crystal volume of the Co x Mn1-x Mn2O4 nanoparticles. Such phenomenon was originated from the substitution process of Co2+ ions that change the metal construction both at the octahedral and tetrahedral sites. Furthermore, the Co2+ ion substitution resulted in an increase in the dielectric properties of the Co x Mn1-x Mn2O4 nanoparticles regarding with dipole moment. Interestingly, the increase was also influenced by reducing the particle size and crystal volume of the Co x Mn1-x Mn2O4 nanoparticles.

Hydrothermal-precipitation preparation of CdS@(Er3+:Y3Al5O12/ZrO2) coated composite and sonocatalytic degradation of caffeine.

PubMed

Huang, Yingying; Wang, Guowei; Zhang, Hongbo; Li, Guanshu; Fang, Dawei; Wang, Jun; Song, Youtao

2017-07-01

Here, we reported a novel method to dispose caffeine by means of ultrasound irradiation combinated with CdS@(Er 3+ :Y 3 Al 5 O 12 /ZrO 2 ) coated composite as sonocatalyst. The CdS@(Er 3+ :Y 3 Al 5 O 12 /ZrO 2 ) was synthesized via hydrothermal-precipitation method and then characterized by X-ray diffractometer (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray analysis (EDX) and UV-vis diffuse reflectance spectra (DRS). After that, the sonocatalytic degradation of caffeine in aqueous solution was conducted adopting CdS@(Er 3+ :Y 3 Al 5 O 12 /ZrO 2 ) and CdS@ZrO 2 coated composites as sonocatalysts. In addition, some influencing factors such as CdS and ZrO 2 molar proportion, caffeine concentration, ultrasonic irradiation time, sonocatalyst dosage and addition of several inorganic oxidants on sonocatalytic degradation of caffeine were investigated by using UV-vis spectra and gas chromatograph. The experimental results showed that the presence of Er 3+ :Y 3 Al 5 O 12 could effectively improve the sonocatalytic degradation activity of CdS@ZrO 2 . To a certain extent some inorganic oxidants can also enhance sonocatalytic degradation of caffeine in the presence of CdS@(Er 3+ :Y 3 Al 5 O 12 /ZrO 2 ). The best sonocatalytic degradation ratio (94.00%) of caffeine could be obtained when the conditions of 5.00mg/L caffeine, 1.00g/L prepared CdS@(Er 3+ :Y 3 Al 5 O 12 /ZrO 2 ), 10.00mmol/LK 2 S 2 O 8 , 180min ultrasonic irradiation (40kHz frequency and 50W output power), 100mL total volume and 25-28°C temperature were adopted. It seems that the method of sonocatalytic degradation caused by CdS@(Er 3+ :Y 3 Al 5 O 12 /ZrO 2 ) displayspotentialadvantages in disposing caffeine. Copyright © 2017 Elsevier B.V. All rights reserved.

Effects of Cu and Ag as ternary and quaternary additions on some physical properties of SnSb7 bearing alloy

NASA Astrophysics Data System (ADS)

El-Bediwi, A. B.

2004-02-01

The structure, electrical resistivity, and elastic modulus of SnSb7 and SnSb7X (X = Cu , Ag, or Cu and Ag) rapidly solidified alloys have been investigated using X-ray diffractometer, double bridge, and dynamic resonance techniques. Copper and silver additions to SnSb result in the formation of a eutectic matrix containing embedded crystals (intermetallic phases) of SnCu, SnAg, and SnSb. The hard crystals SnCu, SnAg, and SnSb increase the overall hardness and wear resistance of SnSb bearing alloys. Addition of copper and silver improves internal friction, electrical conductivity, and elastic modulus values of SnSb rapidly solidified bearing alloys. The internal friction, elastic modulus, and electrical resistivity values are relatively sensitive to the composition of the intermediate phases in the matrix. The SbSb(7)Cu(2)g(2) has better properties (lowest internal friction, cost, adequate elastic modulus, and electrical resistivity) for bearing alloys as compared to cast iron and bronzes.

Seminar on "MAGNETISM"

NASA Astrophysics Data System (ADS)

Lander, Gerard H.

1998-12-01

During the course of this seminar we had 4 presentations by people who had participated in the earlier poster session. The speakers and titles were: (1) U. Gasser (PSI, Switzerland): "Dimer splitting in RxY1-xNi2B2C". High resolution inelastic work done on polycrystalline samples at the IRIS spectrometer at ISIS and determining the exchange interactions in these superconducting materials. (2) B. Roessli (PSI, Switzerland): "Enhancement of magnetic fluctuations in UPd2Al3 below Tc". High resolution work done on single crystals at the cold source IN14 triple axis spectrometer at the ILL and also involving polarisation analysis. (3) P. Wisniewski (Wroclaw, Poland): "Magnetic structures in U3X4-type uranium pnictides - neutron diffraction studies". Elastic scattering experiments done at Saclay on single crystals with both polarised and unpolarised neutrons. (4) A. Schneidewind (TU Dresden): "Investigation of magnetic structures of NdCu2 by synchrotron x-ray scattering". Work done at the ID20 diffractometer at the ESRF and involving resonant and non-resonant scattering, as well as polarisation analysis…

Temperature-Dependent Magnetic Response of Antiferromagnetic Doping in Cobalt Ferrite Nanostructures.

PubMed

Nairan, Adeela; Khan, Maaz; Khan, Usman; Iqbal, Munawar; Riaz, Saira; Naseem, Shahzad

2016-04-18

In this work Mn x Co 1- x Fe₂O₄ nanoparticles (NPs) were synthesized using a chemical co-precipitation method. Phase purity and structural analyses of synthesized NPs were performed by X-ray diffractometer (XRD). Transmission electron microscopy (TEM) reveals the presence of highly crystalline and narrowly-dispersed NPs with average diameter of 14 nm. The Fourier transform infrared (FTIR) spectrum was measured in the range of 400-4000 cm -1 which confirmed the formation of vibrational frequency bands associated with the entire spinel structure. Temperature-dependent magnetic properties in anti-ferromagnet (AFM) and ferromagnet (FM) structure were investigated with the aid of a physical property measurement system (PPMS). It was observed that magnetic interactions between the AFM (Mn) and FM (CoFe₂O₄) material arise below the Neel temperature of the dopant. Furthermore, hysteresis response was clearly pronounced for the enhancement in magnetic parameters by varying temperature towards absolute zero. It is shown that magnetic properties have been tuned as a function of temperature and an externally-applied field.

Characterization of fatigue crack growth behavior in LENS fabricated Ti-6Al-4V using high-energy synchrotron x-ray microtomography

DOE PAGES

Sandgren, Hayley R.; Zhai, Yuwei; Lados, Diana A.; ...

2016-09-28

Laser Engineered Net Shaping (LENS) is an additive manufacturing technique that belongs to the ASTM standardized directed energy deposition category. To date, very limited work has been conducted towards understanding the fatigue crack growth behavior of LENS fabricated materials, which hinders the widespread adoption of this technology for high-integrity structural applications. In this study, the propagation of a 20 μm initial crack in LENS fabricated Ti-6Al-4V was captured in-situ, using high-energy synchrotron x-ray microtomography. Fatigue crack growth (FCG) data were then determined from 2D and 3D tomography reconstructions, as well as from fracture surface striation measurements using SEM. The generatedmore » data were compared to those obtained from conventional FCG tests that used compliance and direct current potential drop (DCPD) techniques to measure long and small crack growth. In conclusion, the observed agreement demonstrates that x-ray microtomography and fractographic analysis using SEM can be successfully combined to study the propagation behavior of fatigue cracks.« less

Characterization of fatigue crack growth behavior in LENS fabricated Ti-6Al-4V using high-energy synchrotron x-ray microtomography

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sandgren, Hayley R.; Zhai, Yuwei; Lados, Diana A.

Laser Engineered Net Shaping (LENS) is an additive manufacturing technique that belongs to the ASTM standardized directed energy deposition category. To date, very limited work has been conducted towards understanding the fatigue crack growth behavior of LENS fabricated materials, which hinders the widespread adoption of this technology for high-integrity structural applications. In this study, the propagation of a 20 μm initial crack in LENS fabricated Ti-6Al-4V was captured in-situ, using high-energy synchrotron x-ray microtomography. Fatigue crack growth (FCG) data were then determined from 2D and 3D tomography reconstructions, as well as from fracture surface striation measurements using SEM. The generatedmore » data were compared to those obtained from conventional FCG tests that used compliance and direct current potential drop (DCPD) techniques to measure long and small crack growth. In conclusion, the observed agreement demonstrates that x-ray microtomography and fractographic analysis using SEM can be successfully combined to study the propagation behavior of fatigue cracks.« less

Synthesis and Characterization of Cobalt Substituted Zinc Ferrite Nanoparticles by Microwave Combustion Method.

PubMed

Sundararajan, M; Kennedy, L John; Vijaya, J Judith

2015-09-01

Pure and cobalt doped zinc ferrites were prepared by microwave combustion method using L-arginine as a fuel. The prepared samples were characterized by various instrumental techniques such as X-ray powder diffractometry, high resolution scanning electron microscopy (HR-SEM), energy dispersive X-ray analysis, Fourier transformed infrared (FT-IR) spectroscopy, photoluminescence spectroscopy and UV-Visible diffuse reflectance spectroscopy. Vibrating sample magnetometry at room temperature was recorded to study the magnetic behavior of the samples. X-ray analysis confirmed the formation of zinc ferrites normal spinel-type structure with an average crystallite sizes in the range, 25.69 nm to 35.68 nm. The lattice parameters decreased as cobalt fraction was increased. The HR-SEM images showed nanoparticles are agglomerated. The estimated band gap energy value was found to decrease with an increase in cobalt content (1.87 to 1.62 eV). Broad visible emissions are observed in the photoluminescence spectra. A gradual increase in the coercivity and saturation magnetization (M(s)) were noted at relatively higher cobalt doping fractions.

Internal iron biomineralization in Imperata cylindrica, a perennial grass: chemical composition, speciation and plant localization.

PubMed

Rodríguez, N; Menéndez, N; Tornero, J; Amils, R; de la Fuente, V

2005-03-01

* The analysis of metal distribution in Imperata cylindrica, a perennial grass isolated from the banks of Tinto River (Iberian Pyritic Belt), an extreme acidic environment with high content in metals, has shown a remarkable accumulation of iron. This property has been used to study iron speciation and its distribution among different tissues and structures of the plant. * Mossbauer (MS) and X-ray diffraction (XRD) were used to determine the iron species, scanning electron microscopy (SEM) to locate iron biominerals among plant tissue structures, and energy-dispersive X-ray microanalysis (EDAX), X-ray fluorescence (TXRF) and inductively coupled plasma emission spectroscopy (ICP-MS) to confirm their elemental composition. * The MS spectral analysis indicated that iron accumulated in this plant mainly as jarosite and ferritin. The presence of jarosite was confirmed by XRD and the distribution of both minerals in structures of different tissues was ascertained by SEM-EDAX analysis. * The convergent results obtained by complementary techniques suggest a complex iron management system in I. cylindrica, probably as a consequence of the environmental conditions of its habitat.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rauf, Nurlaela, E-mail: n-rauf@fmipa.unhas.ac.id; Tahir, Dahlang; Arbiansyah, Muhammad

Structural analysis has been performed on bioceramic materials for denture application by using X-ray diffraction (XRD), X-ray fluorescence (XRF), and Scanning Electron Microscopy (SEM). XRF is using for analysis chemical composition of raw materials. XRF shows the ratio 1 : 1 : 1 : 1 between feldspar, quartz, kaolin and eggshell, respectively, resulting composition CaO content of 56.78 %, which is similar with natural tooth. Sample preparation was carried out on temperature of 800 °C, 900 °C and 1000 °C. X-ray diffraction result showed that the structure is crystalline with trigonal crystal system for SiO{sub 2} (a=b=4.9134 Å and c=5.4051more » Å) and CaH{sub 2}O{sub 2} (a=b=3.5925 Å and c=4.9082 Å). Based on the Scherrer’s equation showed the crystallite size of the highest peak (SiO{sub 2}) increase with increasing the temperature preparation. The highest hardness value (87 kg/mm{sup 2}) and match with the standards of dentin hardness. The surface structure was observed by using SEM also discussed.« less

Synthesis of N-doped potassium tantalate perovskite material for environmental applications

NASA Astrophysics Data System (ADS)

Rao, Martha Purnachander; Nandhini, Vellangattupalayam Ponnusamy; Wu, Jerry J.; Syed, Asad; Ameen, Fuad; Anandan, Sambandam

2018-02-01

Nitrogen containing potassium tantalate perovskite material has been synthesized by the solvothermal method using urea (CH4N2O) as a nitrogen source. The as-prepared sample was characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), diffuse reflectance spectroscopy (DRS), scanning electron microscope (SEM), and energy-dispersive X-ray spectroscopy (EDX) and X-ray photoelectron spectroscopy (XPS). The particle size of nitrogen containing KTaO3 observed from SEM images was found to be 100-150 nm. Doping KTaO3 with nitrogen causes reduction of band gap from 3.5 to 2.54 eV. The incorporation of Nitrogen into the crystal lattice of KTaO3 not only extended the absorption of light from UV (ultraviolet) region to visible region and also enhanced the photocatalytic activity. As prepared nitrogen containing KTaO3 samples exhibit cubic-like morphology and noticed efficient photocatalytic activity towards methylene blue dye degradation under visible light illumination. The intermediates formed during photodegradation were identified by mass spectrometry (GC-MS) and proposed suitable degradation pathway.

Examining the ground layer of St. Anthony from Padua 19th century oil painting by Raman spectroscopy, scanning electron microscopy and X-ray diffraction

NASA Astrophysics Data System (ADS)

Vančo, Ľubomír; Kadlečíková, Magdaléna; Breza, Juraj; Čaplovič, Ľubomír; Gregor, Miloš

2013-01-01

In this paper we studied the material composition of the ground layer of a neoclassical painting. We used Raman spectroscopy (RS) as a prime method. Thereafter scanning electron microscopy combined with energy dispersive spectroscopy (SEM-EDS) and X-ray powder diffraction (XRD) were employed as complementary techniques. The painting inspected was of the side altar in King St. Stephen's Church in Galanta (Slovakia), signed and dated by Jos. Chr. Mayer 1870. Analysis was carried out on both covered and uncovered ground layers. Four principal compounds (barite, lead white, calcite, dolomite) and two minor compounds (sphalerite, quartz) were identified. This ground composition is consistent with the 19th century painting technique used in Central Europe consisting of white pigments and white fillers. Transformation of lead white occurred under laser irradiation. Subdominant Raman peaks of the components were measured. The observed results elucidate useful partnership of RS and SEM-EDS measurements supported by X-ray powder diffraction as well as possibilities and limitations of non-destructive analysis of covered lower layers by RS.

Permeable reactive barrier of coarse sand-supported zero valent iron for the removal of 2,4-dichlorophenol in groundwater.

PubMed

Gao, Weichun; Zhang, Yongxiang; Zhang, Xiaoye; Duan, Zhilong; Wang, Youhao; Qin, Can; Hu, Xiao; Wang, Hao; Chang, Shan

2015-11-01

In this study, coarse sand-supported zero valent iron (ZVI) composite was synthesized by adding sodium alginate to immobilize. Composite was detected by scanning electron microscope (SEM), X-ray diffraction (XRD), and X-ray fluorescence (XRF). SEM results showed that composite had core-shell structure and a wide porous distribution pattern. The synthesized composite was used for degradation of 2,4-dichlorophenol (2,4-DCP) contamination in groundwater. Experimental results demonstrated that degradation mechanism of 2,4-DCP using coarse sand-supported ZVI included adsorption, desorption, and dechlorination. 2,4-DCP adsorption was described as pseudo-second-order kinetic model. It was concluded that dechlorination was the key reaction pathway, ZVI and hydrogen are prime reductants in dechlorination of 2,4-DCP using ZVI.

Superdiffusion of Carbon by Vacancies Irradiated with Soft X-Rays in CZ Silicon / Superdifūzija Ar Vakancēm Iestarota Ar Mīkstajiem Rentgenstariem CZ Silīcijā

NASA Astrophysics Data System (ADS)

Janavičius, A. J.; Mekys, A.; Purlys, R.; Norgėla, Ž.; Daugėla, S.; Rinkūnas, R.

2015-10-01

The soft X-ray photons absorbed in the inner K, L, M shells of Si atoms produce photoelectrons and Auger electrons, thus generating vacancies, interstitials and metastable oxygen complexes. The samples of Czochralski silicon crystals covered with 0.1 μm thickness layer of carbon have been irradiated by X-rays using different voltages of Cu anode of the Russian diffractometer DRON-3M. The influence of X-rays on the formation of point defects and vacancy complexes, and their dynamics in Cz-Si crystals have been studied by infrared absorption. We have measured and calculated dynamics of concentration of carbon and interstitial oxygen using FTIR spectroscopy at room temperature after irradiation by soft X-rays. Using transmittance measurements and nonlinear diffusion theory we have calculated densities increasing for substitutional carbon and interstitial oxygen by reactions and very fast diffusion. The superdiffusion coefficients of carbon in silicon at room temperature generated by X-rays are about hundred thousand times greater than diffusion coefficients obtained for thermodiffusion. Rezumējums: Rentgena staru fotoni, absorbēti Si atoma iekšējos slāņos, izstaro fotoelektronus un Ožē elektronus, ģenerējot vakances, starpmezglu silīcija atomus, vakanču un skābekļa kompleksus. Čohraļska silīcija kristāli, kas pārklāti ar oglekli 0.1 μm biezuma kārtā, tika apstaroti ar rentgena stariem, izmantojot krievu difraktometru DRON-3M. Oglekļa un skābekļa difūzija un koncentrāciju izmaiņa silīcijā tika izmērīta izmantojot infrasarkano staru FTIR spektroskopiju. Rentgena staru ģenerētās ļoti ātrās oglekļa difūzijas vai superdifūzijas koeficients istabas temperatūrā silīcijā ir simtiem tūkstošu reižu lielāks nekā termodifūzijas gadījumā.

Studies of Al-Ti Alloys by SEM

NASA Astrophysics Data System (ADS)

Yildiz, K.; Atici, Y.; Keşlİ Oǧlu, K.; Yaşar, E.

2007-04-01

Al-Ti (1, 2 wt. %) alloys were investigated by Scanning Electron Microscopy (SEM). SEM observations and energy-dispersive x-ray analyses (EDX) showed that the phase structure of Al-Ti (1 %) alloy at 165 μm/s is composed of Al matrix and C, Ni, Fe and Si particles and the Al-Ti (1 %) alloys at 16 and 8 μm/s have only the Al matrix and C particles. It was also found that the Al-Ti (2 %) form the Al matrix and intermetallic TiAl.

Evaluation of enamel by scanning electron microscopy green LED associated to hydrogen peroxide 35% for dental bleaching

NASA Astrophysics Data System (ADS)

Monteiro, Juliana S. C.; de Oliveira, Susana C. P. S.; Zanin, Fátima A. A.; Santos, Gustavo M. P.; Sampaio, Fernando J. P.; Gomes Júnior, Rafael Araújo; Gesteira, Maria F. M.; Vannier-Santos, Marcos A.; Pinheiro, Antônio Luiz B.

2014-02-01

Dental bleaching is a frequently requested procedure in clinical dental practice. The literature is contradictory regarding the effects of bleaching agents on both morphology and demineralization of enamel after bleaching. The aim of this study was to analyze by SEM the effect of 35% neutral hydrogen peroxide cured by green LED. Buccal surfaces of 15 pre-molars were sectioned and marked with a central groove to allow experimental and control groups on the same specimen. For SEM, 75 electron micrographs were evaluated by tree observers at 43X, 220X and 1000X. Quantitative analysis for the determination of the surface elemental composition of the samples through X-ray microanalysis by SEM was also performed. The protocol tested neither showed significant changes in mineral composition of the samples nor to dental enamel structure when compared to controls. SEM analysis allowed inferring that there were marked morphological differences between the enamel samples highlighting the need for the use of the same tooth in comparative morphological studies. The tested protocol did not cause morphological damage the enamel surface when compared to their respective controls.

Science and Technology Text Mining: Electrochemical Power

DTIC Science & Technology

2003-07-14

X-RAY DIFFRACTION, TRANSMISSION ELECTRON MICROSCOPY, X- RAY PHOTOELECTRON SPECTROSCOPY, ELECTROCHEMICAL MEASUREMENTS, THERMOGRAVIMETRIC ANALYSIS ...0 -0 0 -0 0 -0 0 -0 -0 -0 0 0 thermogravimetric analysis -0 -0 0 -0 0 0 -0 -0 -0 0 0 0 -0 0 -0 0 -0 0 -0 -0 0 SEM 0 -0 0 0 -0 -0 -0 -0 0 -0 0 -0 -0 0...Capacitors; Energy Production; Power Production; Energy Conversion; Energy Storage; Citation Analysis ; Scientometrics; Military Requirements REPORT

Photosynthetic microorganism-mediated synthesis of akaganeite (beta-FeOOH) nanorods.

PubMed

Brayner, Roberta; Yéprémian, Claude; Djediat, Chakib; Coradin, Thibaud; Herbst, Fréderic; Livage, Jacques; Fiévet, Fernand; Couté, Alain

2009-09-01

Common Anabaena and Calothrix cyanobacteria and Klebsormidium green algae are shown to form intracellularly akaganeite beta-FeOOH nanorods of well-controlled size and unusual morphology at room temperature. X-ray diffraction (XRD), transmission electron microscopy (TEM), and scanning electron microscopy X-ray energy dispersive spectrometry (SEM-EDS) analyses are used to investigate particle structure, size, and morphology. A mechanism involving iron-siderophore complex formation is proposed and compared with iron biomineralization in magnetotactic bacteria.

Reciprocal Space Mapping of Macromolecular Crystals in the Laboratory

NASA Technical Reports Server (NTRS)

Snell, Edward H.; Boggon, T. J.; Fewster, P. F.; Siddons, D. P.; Stojanof, V.; Pusey, M. L.

1998-01-01

The technique of reciprocal space mapping applied to the physical measurement of macromolecular crystals will be described. This technique uses a triple axis diffractometer setup whereby the monochromator is the first crystal, the sample is the second and the third crystal (of the same material as the monochromator) analyzes the diffracted beam. The geometry is such that it is possible to separate mosaic volume effects from lattice strain effects. The deconvolution of the instrument parameters will also be addressed. Results from measurements at Brookhaven National Synchrotron Radiation Source carried out on microgravity and ground-grown crystals will be presented. The required beam characteristics for reciprocal space mapping are also ideal for topographic studies and the first topographs ever recorded from microgravity protein crystal samples will be shown. We are now working on a system which will enable reciprocal space mapping, mosaicity and topography studies to be carried out in the home laboratory. This system uses a rotating anode X-ray source to provide an intense beam then a Bartels double crystal, four reflection monochromator to provide the spectral and geometric beam conditioning necessary such that the instrument characteristics do not mask the measurement. This is coupled to a high precision diffractometer and sensitive detector. Commissioning data and first results from the system will be presented.

Experience with exchange and archiving of raw data: comparison of data from two diffractometers and four software packages on a series of lysozyme crystals.

PubMed

Tanley, Simon W M; Schreurs, Antoine M M; Helliwell, John R; Kroon-Batenburg, Loes M J

2013-02-01

The International Union of Crystallography has for many years been advocating archiving of raw data to accompany structural papers. Recently, it initiated the formation of the Diffraction Data Deposition Working Group with the aim of developing standards for the representation of these data. A means of studying this issue is to submit exemplar publications with associated raw data and metadata. A recent study on the effects of dimethyl sulfoxide on the binding of cisplatin and carboplatin to histidine in 11 different lysozyme crystals from two diffractometers led to an investigation of the possible effects of the equipment and X-ray diffraction data processing software on the calculated occupancies and B factors of the bound Pt compounds. 35.3 Gb of data were transferred from Manchester to Utrecht to be processed with EVAL. A systematic comparison shows that the largest differences in the occupancies and B factors of the bound Pt compounds are due to the software, but the equipment also has a noticeable effect. A detailed description of and discussion on the availability of metadata is given. By making these raw diffraction data sets available via a local depository, it is possible for the diffraction community to make their own evaluation as they may wish.

Remediation of uranium-contaminated groundwater by sorption onto hydoxyapatite derived from catfish bones

USDA-ARS?s Scientific Manuscript database

Hydroxyapatite was prepared from catfish bones, called catfish hydroxyapatite (CFHA), by mechanical and chemical treatment methods and was characterized by x-ray diffraction (X-RD) and scanning electron microscope (SEM) techniques to confirm the presence of hydroxyapatite. The ability of CFHA to rem...

The hoard of Beçin—non-destructive analysis of the silver coins

NASA Astrophysics Data System (ADS)

Rodrigues, M.; Schreiner, M.; Mäder, M.; Melcher, M.; Guerra, M.; Salomon, J.; Radtke, M.; Alram, M.; Schindel, N.

2010-05-01

We report the results of an analytical investigation on 416 silver-copper coins stemming from the Ottoman Empire (end of 16th and beginning of 17th centuries), using synchrotron micro X-ray fluorescence analysis (SRXRF). In the past, analyses had already been conducted with energy dispersive X-ray fluorescence analysis (EDXRF), scanning electron microscopy with energy dispersive X-ray spectrometry (SEM/EDX) and proton induced X-ray emission spectroscopy (PIXE). With this combination of techniques it was possible to confirm the fineness of the coinage as well as to study the provenance of the alloy used for the coins. For the interpretation of the data statistical analysis (principal component analysis—PCA) has been performed. A definite local assignment was explored and significant clustering was obtained regarding the minor and trace elements composing the coin alloys.

Remineralization of enamel subsurface lesions with casein phosphopeptide-amorphous calcium phosphate: A quantitative energy dispersive X-ray analysis using scanning electron microscopy: An in vitro study

PubMed Central

Hegde, Mithra N; Moany, Anu

2012-01-01

Aim: The objective of this study was to quantitatively evaluate the remineralization potential of casein phosphopeptide-amor-phous calcium phosphate paste on enamel subsurface lesions using scanning electron microscopy with energy dispersive X-ray analysis (SEM-EDX). Materials and Methods: Ninety enamel specimens were prepared from extracted human molars. All specimens were evaluated for mineral content (% weight) using SEM-EDX. The specimens were placed in demineralizing solution for four days to produce artificial carious lesions. The mineral content (calcium/phosphorus ratios, Ca/P ratios) was remeasured using SEM-EDX. The specimens were then randomly assigned to five study groups and one control group of 15 specimens per group. Except for the control group, all group specimens were incubated in remineralizing paste (CPP-ACP paste) for 7, 14, 21, 28, and 35 days twice daily for three minutes. The control group received no treatment with remineralizing paste. All the 90 specimens were stored in artificial saliva at 37°C. After remineralization, the mineral content (% weight) of the samples was measured using SEM-EDX. Results: All the study groups showed very highly significant differences between Ca/P ratios of the demineralized and remineralized samples. There was no significant difference seen in the control group. Conclusion: CPP-ACP paste could significantly remineralize the artificial enamel subsurface lesions in vitro: the remineralizing rates increasing with the time for which the samples were kept in the remineralizing paste. Energy dispersive X-ray analysis is an efficient way to quantitatively assess the changes in mineral content during demineralization and in vitro remineralization processes. PMID:22368338

Highly crumpled solar reduced graphene oxide electrode for supercapacitor application

NASA Astrophysics Data System (ADS)

Mohanapriya, K.; Ahirrao, Dinesh J.; Jha, Neetu

2018-04-01

Highly crumpled solar reduced graphene oxide (CSRGO) was synthesized by simple and rapid method through freezing the solar reduced graphene oxide aqueous suspension using liquid nitrogen and used as electrode material for supercapacitor application. This electrode material was characterized by transmission electron microscope (TEM), X-Ray diffractometer (XRD) and Raman Spectroscopy techniques to understand the morphology and structure. The electrochemical performance was studied by cyclic voltammetry (CV), galvanostatic charge/discharge (CD) and electrochemical impedance spectroscopy (EIS) using 6M KOH electrolyte. The CSRGO exhibit high specifc capacitance of 210.1 F g-1 at the current density of 0.5 A g-1 and shows excellent rate capability. These features make the CSRGO material as promising electrode for high-performance supercapacitors.

Growth of crystals for synchrotron radiation Mössbauer investigation

NASA Astrophysics Data System (ADS)

Kotrbova, M.; Hejduk, J.; Malnev, V. V.; Seleznev, V. N.; Yagupov, S. V.; Andronova, N. V.; Chechin, A. I.; Mikhailov, A. Yu.

1991-10-01

Iron borate crystals (FeBO 3) were flux grown at the Physical Institute (Prague) and at Simferopol State University. During the crystal growth procedure the temperature regime was held constant to 0.1°C accuracy. Crystals were investigated with the help of a double crystal X-ray diffractometer DRON-2 (SiO 2(30 overline33)FeBO 3(444), MoK α 1 radiation). The rocking curve measurements were carried out in a constant magnetic field of 1kG. Most of the crystal surface has a rocking curve 10″-15″ wide. Some parts of some crystals with the area 1 × 1 mm 2 have rocking curves of 3″-4″ width and can be considered ideal.

Dip coated TiO2 nanostructured thin film: synthesis and application

NASA Astrophysics Data System (ADS)

Vanaraja, Manoj; Muthukrishnan, Karthika; Boomadevi, Shanmugam; Karn, Rakesh Kumar; Singh, Vijay; Singh, Pramod K.; Pandiyan, Krishnamoorthy

2016-02-01

TiO2 thin film was fabricated by dip coating method using titanium IV chloride as precursor and sodium carboxymethyl cellulose as thickening as well as capping agent. Structural and morphological features of TiO2 thin film were characterized by X-ray diffractometer and field emission scanning electron microscope, respectively. Crystallinity of the film was confirmed with high-intensity peak at (101) plane, and its average crystallite size was found to be 28 nm. The ethanol-sensing properties of TiO2 thin film was studied by the chemiresistive method. Furthermore, various gases were tested in order to verify the selectivity of the sensor. Among the several gases, the fabricated TiO2 sensor showed very high selectivity towards ethanol at room temperature.

Performance of the Taiwan Contract Beamline BL12B2 at SPring-8

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tang, M.-T.; Du, C.-H.; Lee, J.-F.

2004-05-12

The recent status of the SPring-8 Taiwan Contract Beamline BL12B2 is reported. The beamline was designed to provide multiple applications for materials and biological researches. It is equipped with four end stations, including an EXAFS station, a Huber 6-circle diffractometer for X-ray scattering, a curved image plate for the studies of powder diffraction, and a station for the protein crystallography. The beamline construction was completed in 2000 and it has been in full speed operation since September 2001. To enhance the focusing capacity, the beamline optics has been modified in 2002 and a gain of factor of 10 in photonmore » flux was consequently obtained at protein crystallography station.« less

Synthesis, characterization, and photocatalytic properties of nanocrystalline NZO thin films

NASA Astrophysics Data System (ADS)

Aryanto, D.; Hastuti, E.; Husniya, N.; Sudiro, T.; Nuryadin, B. W.

2018-03-01

Nanocrystalline Ni-doped ZnO (NZO) thin films were synthesized on glass substrate using sol-gel spin coating methods. The effect of annealing on the structural and optical properties of nanocrystalline thin film was studied using X-ray diffractometer (XRD), field emission scanning electron microscopy (FESEM), UV-VIS spectrophotometry, and photoluminescence (PL). The results showed that the annealing temperature strongly influenced the physical properties of nanocrystalline NZO thin films. The photocatalytic properties of nanocrystalline NZO thin films were evaluated using an aqueous solution of Rhodamine-B. The photocatalytic activity of nanocrystalline NZO thin films increased with the increase of annealing temperature. The results indicated that the structure, morphology, and band gap energy of nanocrystalline NZO thin films played an important role in photocatalytic activity.

Morphological and spectroscopic analysis of cellulose nanocrystals extracted from oil palm empty fruit bunch fiber

NASA Astrophysics Data System (ADS)

Dasan, Y. K.; Bhat, A. H.; Faiz, A.

2015-07-01

This work evaluates the use of oil palm empty fruit bunch (OPEFB) fiber as a source of cellulose to obtain nanocrystalline cellulose (CNC) by acid hydrolysis reaction. The raw OPEFB fibers were pretreated with aqueous Sodium hydroxide at 80°C followed by bleaching treatment and further hydrolyzed with Sulphuric acid at 45°C with limited range of hydrolysis time and acid concentration. The resulting CNC's were characterized for spectroscopic, crystallographic and morphological properties using Fourier Transform Infrared Spectroscopy (FTIR), X-ray Diffractometer (XRD), Transmission Electron Microscope (TEM) and Atomic Force Microscopy (AFM). Finding of this study shows that the properties of CNC's are strongly dependent on the hydrolysis time and acid concentration.

Influence of Accumulative Roll Bonding on the Texture and Tensile Properties of an AZ31 Magnesium Alloy Sheets

PubMed Central

Džugan, Ján; Németh, Gergely; Lukáč, Pavel; Bohlen, Jan

2018-01-01

Deformation behaviour of rolled AZ31 sheets that were subjected to the accumulative roll bonding was investigated. Substantially refined microstructure of samples was achieved after the first and second pass through the rolling mill. Sheets texture was investigated using an X-ray diffractometer. Samples for tensile tests were cut either parallel or perpendicular to the rolling direction. Tensile tests were performed at temperatures ranging from room temperature up to 300 °C. Tensile plastic anisotropy, different from the anisotropy observed in AZ31 sheets by other authors, was observed. This anisotropy decreases with an increasing number of rolling passes and increasing deformation temperature. Grain refinement and texture are the crucial factors influencing the deformation behaviour. PMID:29303975

Structural and magnetic analysis of Cu, Co substituted NiFe{sub 2}O{sub 4} thin films

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sharma, Hakikat; Bala, Kanchan; Negi, N. S.

2016-05-23

In the present work we prepared NiFe{sub 2}O{sub 4}, Ni{sub 0.95}Cu{sub 0.05}Fe{sub 2}O{sub 4} and Ni{sub 0.94}Cu{sub 0.05}Co{sub 0.01} Fe{sub 2}O{sub 4} thin films by metallo-organic decomposition method (MOD) using spin coating technique. The thin films were analyzed by X-ray diffractometer (XRD) and Atomic force microscope (AFM) for structural studies. The XRD patterns confirmed the ferrite phase of thin films. From AFM, we analyzed surface morphology, calculated grain size (GS) and root mean square roughness (RMSR). Room temperature magnetic properties were investigated by vibrating sample magnetometer (VSM).

Optical Fourier diffractometry applied to degraded bone structure recognition

NASA Astrophysics Data System (ADS)

Galas, Jacek; Godwod, Krzysztof; Szawdyn, Jacek; Sawicki, Andrzej

1993-09-01

Image processing and recognition methods are useful in many fields. This paper presents the hybrid optical and digital method applied to recognition of pathological changes in bones involved by metabolic bone diseases. The trabecular bone structure, registered by x ray on the photographic film, is analyzed in the new type of computer controlled diffractometer. The set of image parameters, extracted from diffractogram, is evaluated by statistical analysis. The synthetic image descriptors in discriminant space, constructed on the base of 3 training groups of images (control, osteoporosis, and osteomalacia groups) by discriminant analysis, allow us to recognize bone samples with degraded bone structure and to recognize the disease. About 89% of the images were classified correctly. This method after optimization process will be verified in medical investigations.

The Development of the Chemin Mineralogy Instrument and Its Deployment on Mars (and Latest Results from the Mars Science Laboratory Rover Curiosity)

NASA Technical Reports Server (NTRS)

Blake, David F.

2014-01-01

The CheMin instrument (short for "Chemistry and Mineralogy") on the Mars Science Laboratory rover Curiosity is one of two "laboratory quality" instruments on board the Curiosity rover that is exploring Gale crater, Mars. CheMin is an X-ray diffractometer that has for the first time returned definitive and fully quantitative mineral identifications of Mars soil and drilled rock. I will describe CheMin's 23-year development from an idea to a spacecraft qualified instrument, and report on some of the discoveries that Curiosity has made since its entry, descent and landing on Aug. 6, 2012, including the discovery and characterization of the first habitable environment on Mars.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yakubovich, O. V., E-mail: yakubol@geol.msu.ru; Biralo, G. V.; Dimitrova, O. V.

The crystal structure of the (Al,V){sub 4}(P{sub 4}O{sub 12}){sub 3} solid solution, obtained in the single-crystal form by hydrothermal synthesis in the Al(OH){sub 3}-VO{sub 2}-NaCl-H{sub 3}PO{sub 4}-H{sub 2}O system, has been solved by X-ray diffraction analysis (Xcalibur-S-CCD diffractometer, R = 0.0257): a = 13.7477(2) Angstrom-Sign , sp. gr. I 4 bar 3d, Z = 4, and {rho}{sub calcd} = 2.736 g/cm{sup 3}. It is shown that the crystal structure of the parent cubic Al{sub 4}(P{sub 4}O{sub 12}){sub 3} modification can formally be considered an archetype for the formation of double isosymmetric tetraphosphates on its basis.

Neutron capillary optics: status and perspectives

NASA Astrophysics Data System (ADS)

Kumakhov, M. A.

2004-08-01

The article is dedicated to the current status of neutron polycapillary optics and its application. X-ray and neutron polycapillary optics was first suggested in my papers published and patented about 20 years ago. The first X-ray lens was made about 20 years ago (in 1985) in my laboratory at the Kurchatov Institute of Atomic Power. The first neutron assembled capillary lens consisting of several thousand polycapillaries was assembled and tested 2 years later at the atomic reactor of the Kurchatov Institute. A great many experiments were done at the atomic reactors in Russia, Germany, France, USA for neutron beam focusing, turning. Most successful were the experiments on turning neutron beam at the atomic reactor in Berlin, where it was possible to turn the neutron beam by the angle of 20°. Numerous experiments in Germany and France proved high efficacy of polycapillary optics in controlling thermal neutron radiation. The article gives new results obtained in creating pure beams of thermal neutrons on the basis of polycapillary optics. New polycapillary technologies developed at IRO, Moscow/Unisantis, Geneva, enable creation of neutron diffractometers, spectrometers, reflectometers, microscopes—all with a micron-size focal spot. All instruments are portable and highly efficient. Such generation of instruments has been already developed and realized for X-rays, and the same process for neutron beams has already started. So, neutron polycapillary optics makes it possible to create new instruments and raise the level of scientific research, and also enables use of neutron beam for industrial application in production environment.

Dual function of EDTA with silver nanoparticles for root canal treatment-A novel modification.

PubMed

Martinez-Andrade, Juan M; Avalos-Borja, Miguel; Vilchis-Nestor, Alfredo R; Sanchez-Vargas, Luis O; Castro-Longoria, Ernestina

2018-01-01

The chelating and antimicrobial capacity of a novel modification of 17% EDTA with silver nanoparticles (AgNPs) (EDTA-AgNPs) was evaluated in-vitro for root canal treatment (RCT). The EDTA-AgNPs solution was characterized by UV-Vis spectroscopy, ζ-potential and high-resolution transmission electron microscopy (HRTEM). Antimicrobial capacity was evaluated against Candida albicans and Staphylococcus aureus in planktonic and biofilm cells by broth macrodilution (24 h) and XTT assays, (1, 10 and 30 min) respectively. The chelating capacity of EDTA-AgNPs was assessed indirectly (smear layer removal) and directly (demineralizing effect) in bovine dentin at two silver concentrations, 16 and 512 μg/ml at 1 and 10 minutes of exposure time. Smear layer removal was evaluated by atomic force microscopy (AFM) and scanning electron microscopy (SEM). The demineralizing effect was determined by atomic absorption spectroscopy (AAS), microhardness test (MH) and X-ray diffractometer (XRD). Synthesized AgNPs were quasi-spherical in shape with an average size of 13.09 ± 8.05 nm. 17% EDTA-AgNPs was effective to inhibit C. albicans and S. aureus in planktonic and biofilm cultures. The smear layer removal and demineralizing effect were similar between 17% EDTA-AgNPs and 17% EDTA treatments. The 17% EDTA-AgNPs solution proved to be an effective antimicrobial agent, and has a similar chelating capacity to 17% EDTA alone. These in-vitro studies strongly suggest that EDTA-AgNPs could be used for effective smear layer removal, having an antimicrobial effect at the same time during RCT.

Temperature dependence of copper diffusion in different thickness amorphous tungsten/tungsten nitride layer

NASA Astrophysics Data System (ADS)

Asgary, Somayeh; Hantehzadeh, Mohammad Reza; Ghoranneviss, Mahmood

2017-11-01

The amorphous W/WN films with various thickness (10, 30 and 40 nm) and excellent thermal stability were successfully prepared on SiO2/Si substrate with evaporation and reactive evaporation method. The W/WN bilayer has technological importance because of its low resistivity, high melting point, and good diffusion barrier properties between Cu and Si. The thermal stability was evaluated by X-ray diffractometer (XRD) and Scanning Electron Microscope (SEM). In annealing process, the amorphous W/WN barrier crystallized and this phenomenon is supposed to be the start of Cu atoms diffusion through W/WN barrier into Si. With occurrence of the high-resistive Cu3Si phase, the W/WN loses its function as a diffusion barrier. The primary mode of Cu diffusion is the diffusion through grain boundaries that form during heat treatments. The amorphous structure with optimum thickness is the key factor to achieve a superior diffusion barrier characteristic. The results show that the failure temperature increased by increasing the W/WN film thickness from 10 to 30 nm but it did not change by increasing the W/WN film thickness from 30 to 40 nm. It is found that the 10 and 40 nm W/WN films are good diffusion barriers at least up to 800°C while the 30 nm W/WN film shows superior properties as a diffusion barrier, but loses its function as a diffusion barrier at about 900°C (that is 100°C higher than for 10 and 40 nm W/WN films).

Calcium phosphate/chitosan composite coating: Effect of different concentrations of Mg2+ in the m-SBF on its bioactivity

NASA Astrophysics Data System (ADS)

Zhang, Jie; Dai, Changsong; Wei, Jie; Wen, Zhaohui; Zhang, Shujuan; Lin, Lemin

2013-09-01

The purpose of this study was to investigate the effect of different concentration of Mg2+ in a modified simulated body fluid (m-SBF) on the bioactivity of calcium phosphate/chitosan composite coating. Calcium phosphate/chitosan composite coating was prepared on graphite substrate via electrophoretic deposition (EPD) followed by conversion in a phosphate buffer solution (PBS). The obtained samples were soaked in the m-SBF containing different concentration of Mg2+ for different times. And then, the composite coatings were assessed using X-ray diffractometer (XRD), Fourier-transformed infrared spectroscopy (FTIR), Raman spectra, and scanning electron microscope (SEM) with an energy dispersive spectrometer (EDS). The soaking solution was evaluated by inductively coupled plasma optical emission spectrometer (ICP-OES) test. The analytical results showed that hydroxyapatite (HA) and bone-like apatite (HCA) grew on the surface of calcium phosphate/chitosan composite coating after incubation in different m-SBF. With Mg2+ concentration in m-SBF increased from 1× Mg to 10× Mg, HA in the composite coating first presented a dissolving process and then a precipitating one slowly, while HCA presented a growing trend, continuously. The increasing of Mg2+ concentration in the m-SBF inhibited the total growing process of HA and HCA as a whole. The structure of the composite coating changed from spherical into irregular morphology with the concentration of Mg2+ increasing from 1× Mg to 10× Mg. Over all, with the Mg2+ concentration increasing, the bioactivity of calcium phosphate/chitosan composite coating tended to decrease.

Dual function of EDTA with silver nanoparticles for root canal treatment–A novel modification

PubMed Central

Martinez-Andrade, Juan M.; Avalos-Borja, Miguel; Vilchis-Nestor, Alfredo R.; Sanchez-Vargas, Luis O.

2018-01-01

The chelating and antimicrobial capacity of a novel modification of 17% EDTA with silver nanoparticles (AgNPs) (EDTA-AgNPs) was evaluated in-vitro for root canal treatment (RCT). The EDTA-AgNPs solution was characterized by UV-Vis spectroscopy, ζ-potential and high-resolution transmission electron microscopy (HRTEM). Antimicrobial capacity was evaluated against Candida albicans and Staphylococcus aureus in planktonic and biofilm cells by broth macrodilution (24 h) and XTT assays, (1, 10 and 30 min) respectively. The chelating capacity of EDTA-AgNPs was assessed indirectly (smear layer removal) and directly (demineralizing effect) in bovine dentin at two silver concentrations, 16 and 512 μg/ml at 1 and 10 minutes of exposure time. Smear layer removal was evaluated by atomic force microscopy (AFM) and scanning electron microscopy (SEM). The demineralizing effect was determined by atomic absorption spectroscopy (AAS), microhardness test (MH) and X-ray diffractometer (XRD). Synthesized AgNPs were quasi-spherical in shape with an average size of 13.09 ± 8.05 nm. 17% EDTA-AgNPs was effective to inhibit C. albicans and S. aureus in planktonic and biofilm cultures. The smear layer removal and demineralizing effect were similar between 17% EDTA-AgNPs and 17% EDTA treatments. The 17% EDTA-AgNPs solution proved to be an effective antimicrobial agent, and has a similar chelating capacity to 17% EDTA alone. These in-vitro studies strongly suggest that EDTA-AgNPs could be used for effective smear layer removal, having an antimicrobial effect at the same time during RCT. PMID:29346398

Scratch and wear behaviour of plasma sprayed nano ceramics bilayer Al2O3-13 wt%TiO2/hydroxyapatite coated on medical grade titanium substrates in SBF environment

NASA Astrophysics Data System (ADS)

Palanivelu, R.; Ruban Kumar, A.

2014-10-01

Among the various coating techniques, plasma spray coating is an efficient technique to protect the metal surface from the various surface problems like wear and corrosion. The aim of this present work is to design and produce a bilayer coating on the non- toxic commercially pure titanium (denoted as CP-Ti) implant substrate in order to improve the biocompatibility and surface properties. To achieve that, Al2O3-13 wt%TiO2 (AT13) and hydroxyapatite (HAP) were coated on CP-Ti implant substrate using plasma spray coating technique. Further, the coated substrates were subjected to various characterization techniques. The crystallite size of coated HAP and its morphological studies were carried out using X-ray diffractometer (XRD) and scanning electron microscopy (SEM) respectively. The wear test on the bilayer (AT13/HAP) coated CP-Ti implant surface was conducted using ball-on-disc tester under SBF environment at 37 °C, in order to determine the wear rate and the coefficient of friction. The adhesion strength of the bilayer coated surface was evaluated by micro scratch tester under the ramp load conditions with load range of 14-20 N. The above said studies were repeated on the single layer coated HAP and AT13 implant surfaces. The results reveal that the bilayer (AT13/HAP) coated CP-Ti surface has the improved wear rate, coefficient of friction in compared to single layer coated HAP and AT13 surfaces.

Wear and corrosion behaviour of tungsten carbide based coatings with different metallic binder

NASA Astrophysics Data System (ADS)

Kamdi, Z.; Apandi, M. N. M.; Ibrahim, M. D.

2017-12-01

Tungsten carbide based coating has been well known as wear and corrosion resistance materials. However, less study is done on comparing the coating with different binder. Thus, in this work the wear and corrosion behaviour of high velocity oxy-fuel (HVOF) coatings, namely (i) tungsten carbide cobalt and (ii) tungsten carbide nickel will be evaluated. Both coatings were characterised using X-ray Diffractometer (XRD) and Scanning Electron Microscope (SEM). The wear behaviour has been examined using the modified grinder machine by weight loss measurement. Two types of abrasive have been used that include 3 g by weight alumina and silica. While for the corrosion behaviour, it is monitored by three electrodes of electrochemical test and immersion test for 30 days in an acidic environment. The electrolyte used was 0.5 M sulphuric acids (H2SO4). It was found that the cobalt binder shows higher wear resistance compares to the nickel binder for both slurry types. The harder alumina compared to silica results in higher wear rate with removal of carbide and binder is about the same rate. For silica abrasive, due to slightly lower hardness compared to the carbide, the wear is dominated by binder removal followed by carbide detachment. For corrosion, the nickel binder shows four times higher wear resistance compared to the cobalt binder as expected due to its natural behaviour. These finding demonstrate that the selection of coating to be used in different application in this case, wear and corrosion shall be chosen carefully to maximize the usage of the coating.

Growth of surface structures correlated with structural and mechanical modifications of brass by laser-induced Si plasma ions implantation

NASA Astrophysics Data System (ADS)

Ahmad, Shahbaz; Bashir, Shazia; Rafique, M. Shahid; Yousaf, Daniel

2017-04-01

Laser-produced Si plasma is employed as an ion source for implantation on the brass substrate for its surface, structural, and mechanical modifications. Thomson parabola technique is employed for the measurement of energy and flux of Si ions using CR-39. In response to stepwise increase in number of laser pulses from 3000 to 12000, four brass substrates were implanted by laser-induced Si plasma ions of energy 290 keV at different fluxes ranging from 45 × 1012 to 75 × 1015 ions/cm2. SEM analysis reveals the formation of nano/micro-sized irregular shaped cavities and pores for the various ion fluxes for varying numbers of laser pulses from 3000 to 9000. At the maximum ion flux for 12,000 pulses, distinct and organized grains with hexagonal and irregular shaped morphology are revealed. X-ray diffractometer (XRD) analysis exhibits that a new phase of CuSi (311) is identified which confirms the implantation of Si ions in brass substrate. A significant decrease in mechanical properties of implanted brass, such as Yield Stress (YS), Ultimate Tensile Strength (UTS), and hardness, with increasing laser pulses from 3000 to 6000 is observed. However, with increasing laser pulses from 9000 to a maximum value of 12,000, an increase in mechanical properties like hardness, YS, and UTS is observed. The generation as well as annihilation of defects, recrystallization, and intermixing of Si precipitates with brass matrix is considered to be responsible for variations in surface, structural, and mechanical modifications of brass.

Dry Snow Metamorphism

DTIC Science & Technology

2012-09-19

behavior of snow during metamorphism and grain sintering using mathematical models. 2 Approach Our approach involved the collection and...examination of both types of specimens at various stages of metamorphism using the SEM and micro-CT. More specifically, the above approach involved...than 10ºC·m-1). 5. High-resolution images and X-ray spectra of snow specimens at various metamorphism stages were obtained using an SEM and EDS. 6

SILAR controlled CdSe nanoparticles sensitized ZnO nanorods photoanode for solar cell application: Electrolyte effect.

PubMed

Nikam, Pratibha R; Baviskar, Prashant K; Majumder, Sutripto; Sali, Jaydeep V; Sankapal, Babasaheb R

2018-08-15

Controlled growth of different sizes of cadmium selenide (CdSe) nanoparticles over well aligned ZnO nanorods have been performed using successive ionic layer adsorption and reaction (SILAR) technique at room temperature (27 °C) in order to form nano heterostructure solar cells. Deposition of compact layer of zinc oxide (ZnO) by SILAR technique on fluorine doped tin oxide (FTO) coated glass substrate followed by growth of vertically aligned ZnO nanorods array using chemical bath deposition (CBD) at low temperature (<100 °C). Different characterization techniques viz. X-ray diffractometer, UV-Vis spectrophotometer, field emission scanning electron microscopy, transmission electron microscopy and X-ray photoelectron spectroscopy have been used to know the structural, optical, morphological and compositional properties of synthesized nano heterostructure. The photovoltaic performance of the cells with variation in SILAR cycles for CdSe and with use of different electrolytes have been recorded as J-V characteristics and the maximum conversion efficiency of 0.63% have been attained with ferro/ferri cyanide electrolyte for 12 cycles CdSe coating over 1-D ZnO nanorods. Copyright © 2018 Elsevier Inc. All rights reserved.

Green synthesis of Copper nanoparticle using ionic liquid-based extraction from Polygonum minus and their applications.

PubMed

Ullah, Habib; Wilfred, Cecilia Devi; Shaharun, Maizatul Shima

2018-06-06

The present work reports the extraction of phenolic compounds from Polygonum minus using ionic liquid as extracting solvent. In this work, 1-Butyl-3-methylimidazolium hydrogen sulfate [BMIM][HSO 4 ] was used for the extraction of bioactive compounds. Accordingly, ionic liquids based microwave-assisted extraction treatment for separating of bioactive compounds from polygonum minus was first performed in the present study. The results obtained in this work have high extraction yield in comparison with conventional solvent. UV/Vis results showed that microwave synthesis was fast, well dispersed and nanosized copper nanoparticle (CuNPs) in comparison with conventional synthesis. CuNPs was characterized by X-Rays diffractometer (XRD), Fourier transform infrared (FTIR), dynamic light scattering (DLS), field emission scanning electron microscopy combined with energy dispersive x-rays (FESEM-EDX), and thermogravimetric analysis (TGA). All the instrumental analyses confirmed the particles were nanosized. Furthermore, the antibacterial activity of as-synthesized CuNPs showed effective inhibitory zone against three different bacteria. The photocatalytic degradation of copper nanoparticles was studied using methylene blue (MB) and methyl orange (MO) dyes under UV light and degraded 99.9% within short time 8 and 7 minutes.

Activity of plasma sprayed yttria stabilized zirconia reinforced hydroxyapatite/Ti-6Al-4V composite coatings in simulated body fluid.

PubMed

Gu, Y W; Khor, K A; Pan, D; Cheang, P

2004-07-01

Hydroxyapatite (HA)/yttria stabilized zirconia/Ti-6Al-4V bio-composite coatings deposited onto Ti-6Al-4V substrate through a plasma spray technique were immersed in simulated body fluid (SBF) to investigate their behavior in vitro. Surface morphologies and structural changes in the coatings were analyzed by scanning electron microscopy, thin-film X-ray diffractometer, and X-ray photoelectron spectroscopy. The tensile bond strength of the coatings after immersion was also conducted through the ASTM C-633 standard for thermal sprayed coatings. Results showed that carbonate-containing hydroxyapatite (CHA) layer formed on the surface of composite coatings after 4 weeks immersion in SBF solution, indicating the composite coating possessed excellent bioactivity. The mechanical properties were found to decrease with immersion duration of maximum 56 days. However, minimal variation in mechanical properties was found subsequent to achieving supersaturation of the calcium ions, which was attained with the precipitation of the calcium phosphate layers. The mechanical properties of the composite coating were found to be significantly higher than those of pure HA coatings even after immersion in the SBF solution, indicating the enhanced mechanical properties of the composite coatings.

Ternary germanides RERhGe2 (RE = Y, Gd-Ho) - New representatives of the YIrGe2 type

NASA Astrophysics Data System (ADS)

Voßwinkel, Daniel; Heletta, Lukas; Hoffmann, Rolf-Dieter; Pöttgen, Rainer

2016-11-01

The YIrGe2 type ternary germanides RERhGe2 (RE = Y, Gd-Ho) were synthesized from the elements by arc-melting and characterized by powder X-ray diffraction. The structure of DyRhGe2 was refined from single crystal X-ray diffractometer data: Immm, a = 426.49(9), b = 885.0(2), c = 1577.4(3) pm, wR2 = 0.0533, 637 F2 values, 30 variables (300 K data). The structure contains two crystallographically independent dysprosium atoms in pentagonal prismatic and hexagonal prismatic coordination. The three-dimensional [RhGe2] polyanion is stabilized through covalent Rh-Ge (243-261 pm) and Ge-Ge (245-251 pm) bonding. The close structural relationship with the slightly rhodium-poorer germanides RE5Rh4Ge10 (≡ RERh0.8Ge2) is discussed. Temperature-dependent magnetic susceptibility measurements reveal Pauli paramagnetism for YRhGe2 and Curie-Weiss paramagnetism for RERhGe2 with RE = Gd, Tb, Dy and Ho. These germanides order antiferromagnetically at TN = 7.2(5), 10.6(5), 8.1(5), and 6.4(5) K, respectively.

Facile synthesis and photocatalytic activity of ZnO/zinc titanate core-shell nanorod arrays

NASA Astrophysics Data System (ADS)

He, Ding-Chao; Fu, Qiu-Ming; Ma, Zhi-Bin; Zhao, Hong-Yang; Tu, Ya-Fang; Tian, Yu; Zhou, Di; Zheng, Guang; Lu, Hong-Bing

2018-02-01

ZnO/zinc titanate core-shell nanorod arrays (CSNRs) were successfully prepared via a simple synthesis process by combining hydrothermal synthesis and liquid phase deposition (LPD). The surface morphologies, crystalline characteristics, optical properties and surface electronic states of the ZnO/zinc titanate CSNRs were characterized by scanning electron microscope, transmission electron microscope, x-ray diffractometer, x-ray photoelectron spectroscopy, PL and ultraviolet (UV)-visible absorption spectra. By controlling the reaction time of LPD, the shell thickness could vary with the reaction time. Furthermore, the impacts of the reaction time and post-annealing temperature on the crystalline structure and chemical composition of the CSNRs were also investigated. The studies of photocatalytic activity under UV light irradiation revealed that the ZnO/zinc titanate CSNRs annealed at 700 °C with 30 min deposition exhibited the best photocatalytic activity and good stability for degradation of methylene blue. It had been found that the effective separation of photogenerated electron-hole pairs in the CSNRs led to the enhanced photocatalytic activity. Moreover, the ZnO/zinc titanate CSNRs grown on quartz glass substrate could be easily recycled for reuse with almost unchanged photocatalytic activity.

Impact of crystalline defects and size on X-ray line broadening: A phenomenological approach for tetragonal SnO{sub 2} nanocrystals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Muhammed Shafi, P.; Chandra Bose, A., E-mail: acbose@nitt.edu

2015-05-15

Nanocrystalline tin oxide (SnO{sub 2}) powders with different grain size were prepared by chemical precipitation method. The reaction was carried out by varying the period of hydrolysis and the as-prepared samples were annealed at different temperatures. The samples were characterized using X-ray powder diffractometer and transmission electron microscopy. The microstrain and crystallite size were calculated for all the samples by using Williamson-Hall (W-H) models namely, isotropic strain model (ISM), anisotropic strain model (ASM) and uniform deformation energy density model (UDEDM). The morphology and particle size were determined using TEM micrographs. The directional dependant young’s modulus was modified as an equationmore » relating elastic compliances (s{sub ij}) and Miller indices of the lattice plane (hkl) for tetragonal crystal system and also the equation for elastic compliance in terms of stiffness constants was derived. The changes in crystallite size and microstrain due to lattice defects were observed while varying the hydrolysis time and the annealing temperature. The dependence of crystallite size on lattice strain was studied. The results were correlated with the available studies on electrical properties using impedance spectroscopy.« less

Copper diffusion in Ti Si N layers formed by inductively coupled plasma implantation

NASA Astrophysics Data System (ADS)

Ee, Y. C.; Chen, Z.; Law, S. B.; Xu, S.; Yakovlev, N. L.; Lai, M. Y.

2006-11-01

Ternary Ti-Si-N refractory barrier films of 15 nm thick was prepared by low frequency, high density, inductively coupled plasma implantation of N into TixSiy substrate. This leads to the formation of Ti-N and Si-N compounds in the ternary film. Diffusion of copper in the barrier layer after annealing treatment at various temperatures was investigated using time-of-flight secondary ion mass spectrometer (ToF-SIMS) depth profiling, X-ray diffractometer (XRD), field emission scanning electron microscopy (FESEM), energy dispersive X-ray (EDX) and sheet resistance measurement. The current study found that barrier failure did not occur until 650 °C annealing for 30 min. The failure occurs by the diffusion of copper into the Ti-Si-N film to form Cu-Ti and Cu-N compounds. FESEM surface morphology and EDX show that copper compounds were formed on the ridge areas of the Ti-Si-N film. The sheet resistance verifies the diffusion of Cu into the Ti-Si-N film; there is a sudden drop in the resistance with Cu compound formation. This finding provides a simple and effective method of monitoring Cu diffusion in TiN-based diffusion barriers.

Friction and Wear Properties of CrSiCN/SiC Tribopairs in Water Lubrication

NASA Astrophysics Data System (ADS)

Wu, Zhiwei; Zhou, Fei; Wang, Qianzhi

2018-05-01

CrSiCN coatings (3.4 at.% Si) were prepared on 316L stainless steels using unbalanced magnetron sputtering. According to the analysis results of x-ray diffractometer and x-ray photoelectrons spectroscopy, silicon in CrSiCN coatings mainly presented in the amorphous forms of a-SiN, a-SiCN and a-SiC. The hardness and Young's modulus of CrSiN coatings were 19.4 ± 0.6 and 306.1 ± 5.9 GPa, respectively. In addition, the ball-on-disk sliding tests of CrSiCN/SiC tribopairs were performed in distilled water at varying velocities (0.1-0.5 m/s) and loads (2-12 N). The friction coefficient of tribopairs presented a decreasing trend with respect to velocity at low applied loads (≤ 4 N). To be specific, the low friction coefficient of 0.05-0.14 accompanied with polished wear scar was obtained at high velocities and low loads. Finally, the wear mechanism map of CrSiCN/SiC tribopairs was proposed based on a combination of friction coefficient, wear scar morphology and wear rates of tribopairs.

Corrosion Behavior and Microhardness of Ni-P-SiO2-Al2O3 Nano-composite Coatings on Magnesium Alloy

NASA Astrophysics Data System (ADS)

Sadreddini, S.; Rahemi Ardakani, S.; Rassaee, H.

2017-05-01

In the present work, nano-composites of Ni-P-SiO2-Al2O3 were coated on AZ91HP magnesium alloy. The surface morphology of the nano-composite coating was studied by field emission scanning electron microscopy (FESEM). The amount of SiO2 in the coating was determined by energy-dispersive analysis of x-ray (EDX), and the crystalline structure of the coating was examined by x-ray diffractometer (XRD). All the experiments concerning the corrosion behavior of the coating carried out in 3.5 wt.% NaCl solution and evaluated by electrochemical impedance spectroscopy (EIS) and polarization technique. The results showed that an incorporation of SiO2 and Al2O3 in Ni-P coating at the SiO2 concentration of 10 g/Land 14 g/LAl2O3 led to the lowest corrosion rate ( i corr = 1.3 µA/cm2), the most positive E corr and maximum microhardness (496 VH). Furthermore, Ni-P-SiO2-Al2O3 nano-composite coating possesses less porosity than that in Ni-P coating, resulting in improving corrosion resistance.

Influence of palmitic acid and hexadecanol on the phase transition temperature and molecular packing of dipalmitoylphosphatidyl-choline monolayers at the air-water interface

NASA Astrophysics Data System (ADS)

Lee, Ka Yee C.; Gopal, Ajaykumar; von Nahmen, Anja; Zasadzinski, Joseph A.; Majewski, Jaroslaw; Smith, Gregory S.; Howes, Paul B.; Kjaer, Kristian

2002-01-01

Palmitic acid (PA) and 1-hexadecanol (HD) strongly affect the phase transition temperature and molecular packing of dipalmitoylphosphatidylcholine (DPPC) monolayers at the air-water interface. The phase behavior and morphology of mixed DPPC/PA as well as DPPC/HD monolayers were determined by pressure-area-isotherms and fluorescence microscopy. The molecular organization was probed by synchrotron grazing incidence x-ray diffraction using a liquid surface diffractometer. Addition of PA or HD to DPPC monolayers increases the temperature of the liquid-expanded to condensed phase transition. X-ray diffraction shows that DPPC forms mixed crystals both with PA and HD over a wide range of mixing ratios. At a surface pressure (π) of 40 mN/m, increasing the amount of the single chain surfactant leads to a reduction in tilt angle of the aliphatic chains from nearly 30° for pure DPPC to almost 0° in a 1:1 molar ratio of DPPC and PA or HD. At this composition we also find closest packing of the aliphatic chains. Further increase of the amount of PA or HD does not change the lattice or the tilt.

Catalytic behavior of a palladium doped binder free paper based cobalt electrode in electroreduction of hydrogen peroxide

NASA Astrophysics Data System (ADS)

Zhang, Dongming; Ye, Ke; Cao, Dianxue; Yin, Jinling; Cheng, Kui; Wang, Bin; Xu, Yang; Wang, Guiling

2015-01-01

A piece of flexible and conductive A4 paper is prepared by coating a layer of graphite with a normal 8B pencil. Then, Co nano-plates and Pd are assembled by a simple electrodeposition and chemical-reduction methods on the surface of the electrified paper, respectively. The as-prepared paper substrate/graphite-Co film-Pd (PG-CoPd) electrode is characterized by scanning electron microscopy equipped with energy dispersive X-ray spectrometer, transmission electron microscope and X-ray diffractometer. The catalytic activity of the PG-CoPd electrode for H2O2 electroreduction is investigated by means of cyclic voltammetry and chronoamperometry. The preparation process of the PG-CoPd electrode does not use any binder and it exhibits a three dimensional (3D) nano structure, high stability and good electric conductivity. The mass of the Pd in PG-CoPd is about 0.0535 mg cm-2 and the reduction current density reaches to -4.30 A cm-2 mg-1 in 1 mol dm-3 NaOH and 1.4 mol dm-3 H2O2 at -0.5 V, which is higher than our previous reports of Au/Pd modified Co electrode.

pH-insusceptible cobalt-manganese immobilizing mesoporous siliceous MCM-41 catalyst for ozonation of dimethyl phthalate.

PubMed

Tang, Yiming; Pan, Zhaoqi; Li, Laisheng

2017-12-15

Mesoporous siliceous MCM-41 immobilized with Co and Mn metal ions (Co-Mn-MCM-41) was synthesized using a hydrothermal method. The structural regularity and the valence states of the metal species were measured by X-ray diffractometer and X-ray photoelectron spectrometer. The resultant bimetallic Co-Mn-MCM-41 catalyst was tested for the degradation of dimethyl phthalate (DMP) via a catalytic ozonation mechanism, demonstrating that the catalytic properties of Co-Mn-MCM-41 catalyst significantly accelerated the ozonation process. Total organic carbon (TOC) and DMP removal efficiency reached 94% and 99.7% at 15min under the optimal conditions. The oxidation pathways were proposed after identifying the intermediate products from ozonation using a gas chromatography-mass spectrometer. The enhanced catalytic reactivity was attributed to the highly-dispersive cobalt and manganese species in MCM-41 scaffolds, which promoted the ozone decomposition and hydroxyl radicals' generation in catalytic ozonation and accelerated the degradation of DMP. Bimetallic Co-Mn-MCM-41 catalyst remained stable in mild acidic conditions and continued to show high activity after repeated runs. Copyright © 2017 Elsevier Inc. All rights reserved.

Electrophoretic Deposition of Hydroxyapatite Film Containing Re-Doped MoS₂ Nanoparticles.

PubMed

Shalom, Hila; Feldman, Yishay; Rosentsveig, Rita; Pinkas, Iddo; Kaplan-Ashiri, Ifat; Moshkovich, Alexey; Perfilyev, Vladislav; Rapoport, Lev; Tenne, Reshef

2018-02-26

Films combining hydroxyapatite (HA) with minute amounts (ca. 1 weight %) of (rhenium doped) fullerene-like MoS₂ (IF) nanoparticles were deposited onto porous titanium substrate through electrophoretic process (EPD). The films were analyzed by scanning electron microscopy (SEM), X-ray diffraction and Raman spectroscopy. The SEM analysis showed relatively uniform coatings of the HA + IF on the titanium substrate. Chemical composition analysis using energy dispersive X-ray spectroscopy (EDS) of the coatings revealed the presence of calcium phosphate minerals like hydroxyapatite, as a majority phase. Tribological tests were undertaken showing that the IF nanoparticles endow the HA film very low friction and wear characteristics. Such films could be of interest for various medical technologies. Means for improving the adhesion of the film to the underlying substrate and its fracture toughness, without compromising its biocompatibility are discussed at the end.

Toward Quantifying the Mass-Based Hygroscopicity of Individual Submicron Atmospheric Aerosol Particles with STXM/NEXAFS and SEM/EDX

NASA Astrophysics Data System (ADS)

Yancey Piens, D.; Kelly, S. T.; OBrien, R. E.; Wang, B.; Petters, M. D.; Laskin, A.; Gilles, M. K.

2014-12-01

The hygroscopic behavior of atmospheric aerosols influences their optical and cloud-nucleation properties, and therefore affects climate. Although changes in particle size as a function of relative humidity have often been used to quantify the hygroscopic behavior of submicron aerosol particles, it has been noted that calculations of hygroscopicity based on size contain error due to particle porosity, non-ideal volume additivity and changes in surface tension. We will present a method to quantify the hygroscopic behavior of submicron aerosol particles based on changes in mass, rather than size, as a function of relative humidity. This method results from a novel experimental approach combining scanning transmission x-ray microscopy with near-edge x-ray absorption fine spectroscopy (STXM/NEXAFS), as well as scanning electron microscopy with energy dispersive x-ray spectroscopy (SEM/EDX) on the same individual particles. First, using STXM/NEXAFS, our methods are applied to aerosol particles of known composition ‒ for instance ammonium sulfate, sodium bromide and levoglucosan ‒ and validated by theory. Then, using STXM/NEXAFS and SEM/EDX, these methods are extended to mixed atmospheric aerosol particles collected in the field at the DOE Atmospheric Radiation Measurement (ARM) Climate Research Facility at the Southern Great Planes sampling site in Oklahoma, USA. We have observed and quantified a range of hygroscopic behaviors which are correlated to the composition and morphology of individual aerosol particles. These methods will have implications for parameterizing aerosol mixing state and cloud-nucleation activity in atmospheric models.

Characterization of morphology and hydration products of high-volume fly ash paste by monochromatic scanning x-ray micro-diffraction (μ-SXRD)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bae, Sungchul; Meral, Cagla; Department of Civil Engineering, Middle East Technical University, 06800 Ankara

2014-05-01

The present study focuses on identification and micro-structural characterization of the hydration products formed in high-volume fly ash (HVFA)/portland cement (PC) systems using monochromatic scanning x-ray micro-diffraction (μ-SXRD) and SEM-EDS. Pastes with up to 80% fly ash replacement were studied. Phase maps for HVFA samples using μ-SXRD patterns prove that μ-SXRD is an effective method to identify and visualize the distribution of phases in the matrix. μ-SXRD and SEM-EDS analysis shows that the C-S-H formed in HVFA system containing 50% or more of fly ash has a similar structure as C-S-H(I) with comparatively lower Ca/Si ratio than the one producedmore » in PC system. Moreover, coexistence of C-S-H(I) and strätlingite is observed in the system containing 80% of fly ash, confirming that the amount of alumina and silicate phases provided by the fly ash is a major factor for the formation of C-S-H(I) and strätlingite in HVFA system. - Highlights: • High-volume fly ash (HVFA) paste was studied by scanning x-ray micro-diffraction. • Coexistence of C-S-H(I) and strätlingite in the HVFA system is clearly shown. • The distribution of minor phases in the HVFA system is shown. • Differences between inner and outer products of fly ash are observed by SEM-EDS.« less

Room-temperature synthesis and photoluminescence of hexagonal CePO4 nanorods

NASA Astrophysics Data System (ADS)

Zhu, J.; Zhang, K.; Zhao, H. Y.

2018-01-01

Hexagonal CePO4 nanorods were synthesized via a simple chemical precipitation route at room-temperature without the presence of surfactants and then characterized by powder X-ray diffraction (XRD), energy-dispersive X-ray (EDX) spectrometry, scanning electron microscopy (SEM), transmission electron microscopy (TEM), ultraviolet-visible (UV-vis) absorption and photoluminescence (PL) spectroscopy. Hexagonal CePO4 nanorods exhibit strong ultraviolet absorption and ultraviolet luminescence, which correspond to the electronic transitions between 4f and 5d state of Ce3+ ions.

Evaluating the Performance of a Commercial Silicon Drift Detector for X-ray Microanalysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kenik, Edward A

2011-01-01

Silicon drift detectors (SDDs) are rapidly becoming the energy dispersive spectrometer (EDS) of choice, especially for scanning electron microscopy x-ray microanalysis. The complementary features of large active areas (i.e., high collection angle) and high count rate capability of these detector contribute to their popularity, as well as the absence of liquid nitrogen cooling and good energy resolution of these detectors. The performance of an EDAX Apollo 40 SDD on a JEOL 6500F SEM is discussed. The larger detector resulted in an significant increase (~3.5x) in geometric collection efficiency compared to the original 10mm2 Si(Li) detector that it replaced. The SEMmore » can provide high beam currents (up to 200nA in some conditions) at small probe diameters. The high count rate capability of the SDD and the high current capability of the SEM compliment each other and provide excellent EDS analytical capabilities for both single point and spectrum imaging applications.« less

The Microstructure and Physical Properties of Incinerated Paper-Cullet-Clay Ceramics

NASA Astrophysics Data System (ADS)

Sahar, M. R.; Hamzah, K.; Rohani, M. S.; Samah, K. A.; Razi, M. M.

A series of ceramic based on (x) incinerated recycle paper - (80-x) cullet - 20 Kaolin clay (where 10×45 wt%) has successfully been made by slip casting technique followed by sintering at 1000 °C. The actual composition of ceramic is analyzed using Energy Dispersive of X-Ray (EDAX) while the phase existence is determined using X-Ray Diffraction (XRD) technique. Their microstructural morphology is observed under Scanning Electron Microscope (SEM) and the physical properties are measured in term of their thermal shrinkage and hardness. It is found that the ceramic contain mostly of Silica and the phase is dominated by the existence of Quartz (SiO2), Wollastonite (CaSiO3) and Anorthite (Ca(Al2SiO8)). The SEM micrograph shows that the morphology is dominated by the existence of granular structure, and then become smoother as the cullet level is further increased. It is also found out that the thermal shrinkage is in the range 18% - 6.5% while the hardness is in the range of 152MPa- 1.463 GPa depending on composition.

Scanning Electron Microscopy-Energy-Dispersive X-Ray (SEM/EDX): A Rapid Diagnostic Tool to Aid the Identification of Burnt Bone and Contested Cremains.

PubMed

Ellingham, Sarah T D; Thompson, Tim J U; Islam, Meez

2018-03-01

This study investigates the use of Scanning electron microscopy-energy-dispersive X-ray (SEM-EDX) as a diagnostic tool for the determination of the osseous origin of samples subjected to different temperatures. Sheep (Ovis aries) ribs of two experimental groups (fleshed and defleshed) were burned at temperatures of between 100°C and 1100°C in 100°C increments and subsequently analyzed with the SEM-EDX to determine the atomic percentage of present elements. Three-factor ANOVA analysis showed that neither the exposure temperature, nor whether the burning occurred with or without soft tissue present had any significant influence on the bone's overall elemental makeup (p > 0.05). The Ca/P ratio remained in the osseous typical range of between 1.6 and 2.58 in all analyzed samples. This demonstrates that even faced with high temperatures, the overall gross elemental content and atomic percentage of elements in bone remain stable, creating a unique "fingerprint" for osseous material, even after exposure to extreme conditions. © 2017 American Academy of Forensic Sciences.

Intercalated chitosan/hydroxyapatite nanocomposites: Promising materials for bone tissue engineering applications.

PubMed

Nazeer, Muhammad Anwaar; Yilgör, Emel; Yilgör, Iskender

2017-11-01

Preparation and characterization of chitosan/hydroxyapatite (CS/HA) nanocomposites displaying an intercalated structure is reported. Hydroxyapatite was synthesized through sol-gel process. Formic acid was introduced as a new solvent to obtain stable dispersions of nano-sized HA particles in polymer solution. CS/HA dispersions with HA contents of 5, 10 and 20% by weight were prepared. Self-assembling of HA nanoparticles during the drying of the solvent cast films led to the formation of homogeneous CS/HA nanocomposites. Composite films were analyzed by scanning electron microscopy (SEM), atomic force microscopy (AFM), energy dispersive X-rays (EDX) analysis, Fourier transform infrared (FTIR) spectroscopy, X-rays diffraction (XRD) analysis and thermogravimetric analysis (TGA). SEM and AFM confirmed the presence of uniformly distributed HA nanoparticles on the chitosan matrix surface. XRD patterns and cross-sectional SEM images showed the formation of layered nanocomposites. Complete degradation of chitosan matrix in TGA experiments, led to the formation of nanoporous 3D scaffolds containing hydroxyapatite, β-tricalcium phosphate and calcium pyrophosphate. CS/HA composites can be considered as promising materials for bone tissue engineering applications. Copyright © 2017 Elsevier Ltd. All rights reserved.

Non-destructive determination of thickness of the dielectric layers using EDX

NASA Astrophysics Data System (ADS)

Sokolov, S. A.; Kelm, E. A.; Milovanov, R. A.; Abdullaev, D. A.; Sidorov, L. N.

2016-12-01

In this work a non-destructive method for measuring the thickness of the dielectric layers consisting of silicon dioxide and silicon nitride has been developed using a scanning electron microscope (SEM) equipped with energy dispersive X-ray spectrometer (EDS). Rising in accelerating voltage of electron beam leads to increasing in the depth of generation of the characteristic X-ray. If the ratio of the signal intensity of one of the substrate's elements to the noise equal to 3 suggests that the generation's depth of the characteristic X-ray coincides with the thickness of the overlying film. Dependence of the overlying film's thickness on the accelerating voltage can be plotted. Validation of the results was carried out by using the equation of Anderson-Hassler. The generation's volume of the characteristic X-Ray was simulated by CASINO program. The simulations results are in good agreement with experimental results for small thicknesses.

Application of biocompatible magnetite nanoparticles for the removal of arsenic and copper from water

NASA Astrophysics Data System (ADS)

Iconaru, S. L.; Beuran, M.; Turculet, C. S.; Negoi, I.; Teleanu, G.; Prodan, A. M.; Motelica-Heino, M.; Guégan, R.; Ciobanu, C. S.; Jiga, G.; Predoi, Daniela

2018-02-01

The progress of nanotechnology made possible the use of nanomaterials as adsorbents and magnetic iron oxides represents one of the first generations of nanoscale materials used in environment technologies [1]. A systematic characterization of commercial magnetite (Fe3O4) is presented in this research. The commercial (Fe3O4) magnetic adsorbents were characterized by various characterizations methods such as X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray analysis (EDX). This study was also focused on the study of adsorption isotherms and the kinetics evaluation. X-ray studies indicated that As3+ and Cu2+ removed by Fe3O4 did not seem to alter the structure of Fe3O4 but they were highlighted in the EDX analysis. In addition, the SEM studies were consistent with the XRD results. The rate of adsorption of contaminants, in contaminated solutions decreases when the amount of contaminant increases in all experiments performed. The results revealed that Fe3O4 nanoparticles are promising candidates which could be used as sorbents for the removal of arsenic from the marine environment, for site remediation and groundwater treatment.

A study of the physical, chemical and biological properties of TiO2 coatings produced by micro-arc oxidation in a Ca-P-based electrolyte.

PubMed

dos Santos, Amanda; Araujo, Joyce R; Landi, Sandra M; Kuznetsov, Alexei; Granjeiro, José M; de Sena, Lidia Ágata; Achete, Carlos Alberto

2014-07-01

In this work, a porous and homogeneous titanium dioxide layer was grown on commercially pure titanium substrate using a micro-arc oxidation (MAO) process and Ca-P-based electrolyte. The structure and morphology of the TiO2 coatings were characterized by X-ray diffraction, scanning electron microscopy (SEM), transmission electron microscopy, and profilometry. The chemical properties were studied using electron dispersive X-ray spectroscopy (SEM-EDS) and X-ray photoelectron spectroscopy. The wettability of the coating was evaluated using contact angle measurements. During the MAO process, Ca and P ions were incorporated into the oxide layer. The TiO2 coating was composed of a mixture of crystalline and amorphous structures. The crystalline part of the sample consisted of a major anatase phase and a minor rutile phase. A cross-sectional image of the coating-substrate interface reveals the presence of voids elongated along the interface. An osteoblast culture was performed to verify the cytocompatibility of the anodized surface. The results of the cytotoxicity tests show satisfactory cell viability of the titanium dioxide films produced in this study.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yashchuk, V.V.; Conley, R.; Anderson, E.H.

Verification of the reliability of metrology data from high quality X-ray optics requires that adequate methods for test and calibration of the instruments be developed. For such verification for optical surface profilometers in the spatial frequency domain, a modulation transfer function (MTF) calibration method based on binarypseudo-random (BPR) gratings and arrays has been suggested and and proven to be an effective calibration method for a number of interferometric microscopes, a phase shifting Fizeau interferometer, and a scatterometer. Here we describe the details of development of binarypseudo-random multilayer (BPRML) test samples suitable for characterization of scanning (SEM) and transmission (TEM) electronmore » microscopes. We discuss the results of TEM measurements with the BPRML test samples fabricated from a WiSi{sub 2}/Si multilayer coating with pseudo-randomly distributed layers. In particular, we demonstrate that significant information about the metrological reliability of the TEM measurements can be extracted even when the fundamental frequency of the BPRML sample is smaller than the Nyquist frequency of the measurements. The measurements demonstrate a number of problems related to the interpretation of the SEM and TEM data. Note that similar BPRML testsamples can be used to characterize X-ray microscopes. Corresponding work with X-ray microscopes is in progress.« less

Synthesis and characterization of novel 4-Tetra-4-Tolylsulfonyl ZnPc thin films for optoelectronic applications

NASA Astrophysics Data System (ADS)

Khalil, Salah; Tazarki, Helmi; Souli, Mehdi; Guasch, Cathy; Jamoussi, Bassem; Kamoun, Najoua

2017-11-01

Novel 4-Tetra-4-Tolylsulfonyl:zinc phthalocyanine and simple zinc phthalocyanine were synthesized. Our materials were grown on glass substrates by spin coating technique. Thin films were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electronic micrograph (SEM), atomic force microscopy (AFM), spectrophotometer and Hall effect measurement. X-ray spectra reveal that 4-Tetra-4-Tolylsulfonyl:zinc phthalocyanine (4T4TS:ZnPc) and zinc phthalocyanine (ZnPc) thin films have a monoclinic crystalline structure in β phase. The surface properties and chemical composition were detailed using XPS measurement. SEM were used to investigate the surface morphology for 4T4TS:ZnPc and ZnPc thin films. Atomic force microscopy images have shown a decrease in surface roughness after substitution. Optical properties were investigated by measuring transmission and reflection spectra. Electrical properties were studied and the different electrical parameters was measured and compared on glass, silicon and tin dioxide substrates by Hall Effect technique. All obtained results indicate an improvement in physical properties of 4T4TS:ZnPc which allows used it in optoelectronic applications.

Sonication-assisted synthesis of a new cationic zinc nitrate complex with a tetradentate Schiff base ligand: Crystal structure, Hirshfeld surface analysis and investigation of different parameters influence on morphological properties.

PubMed

Mousavi, S A; Montazerozohori, M; Masoudiasl, A; Mahmoudi, G; White, J M

2018-09-01

A nanostructured cationic zinc nitrate complex with a formula of [ZnLNO 3 ]NO 3 (where L = (N 2 E,N 2' E)-N 1 ,N 1' -(ethane-1,2-diyl)bis(N 2 -((E)-3-phenylallylidene)ethane-1,2-diamine)) was prepared by sonochemical process and characterized by single crystal X-ray crystallography, scanning electron microscopy (SEM), FT-IR and NMR spectroscopy and X-ray powder diffraction (XRPD). The X-ray analysis demonstrates the formation of a cationic complex that metal center is five-coordinated by four nitrogen atom from Schiff base ligand and one oxygen atom from nitrate group. The crystal packing analysis demonstrates the essential role of the nitrate groups in the organization of supramolecular structure. The morphology and size of ultrasound-assisted synthesized zinc nitrate complex have been investigated using scanning electron microscopy (SEM) by changing parameters such as the concentration of initial reactants, the sonication power and reaction temperature. In addition the calcination of zinc nitrate complex in air atmosphere led to production of zinc oxide nanoparticles. Copyright © 2018. Published by Elsevier B.V.

High temperature oxidation behavior of austenitic stainless steel AISI 304 in steam of nanofluids contain nanoparticle ZrO2

DOE Office of Scientific and Technical Information (OSTI.GOV)

Prajitno, Djoko Hadi, E-mail: djokohp@batan.go.id; Syarif, Dani Gustaman, E-mail: djokohp@batan.go.id

2014-03-24

The objective of this study is to evaluate high temperature oxidation behavior of austenitic stainless steel SS 304 in steam of nanofluids contain nanoparticle ZrO{sub 2}. The oxidation was performed at high temperatures ranging from 600 to 800°C. The oxidation time was 60 minutes. After oxidation the surface of the samples was analyzed by different methods including, optical microscope, scanning electron microscope (SEM) and X-ray diffraction (XRD). X-ray diffraction examination show that the oxide scale formed during oxidation of stainless steel AISI 304 alloys is dominated by iron oxide, Fe{sub 2}O{sub 3}. Minor element such as Cr{sub 2}O{sub 3} ismore » also appeared in the diffraction pattern. Characterization by optical microscope showed that cross section microstructure of stainless steel changed after oxidized with the oxide scale on the surface stainless steels. SEM and x-ray diffraction examination show that the oxide of ZrO{sub 2} appeared on the surface of stainless steel. Kinetic rate of oxidation of austenite stainless steel AISI 304 showed that increasing oxidation temperature and time will increase oxidation rate.« less

Optical and magnetic properties of Co-doped CuO flower/plates/particles-like nanostructures.

PubMed

Basith, N Mohamed; Vijaya, J Judith; Kennedy, L John; Bououdina, M; Hussain, Shamima

2014-03-01

In this study, pure and Co-doped CuO nanostructures (0.5, 1.0, 1.5, and 2.0 at wt% of Co) were synthesized by microwave combustion method. The prepared samples were characterized by X-ray diffraction (XRD), high resolution scanning electron microscopy (HR-SEM), energy dispersive X-ray analysis (EDX), diffuse reflectance spectroscopy (DRS), photoluminescence (PL) spectroscopy and vibrating sample magnetometry (VSM). Powder X-ray diffraction patterns refined by the Rietveld method indicated the formation of single-phase monoclinic structure. The surface morphology and elemental analysis of Co-doped CuO nanostructures were studied by using HR-SEM and EDX. Interestingly, the morphology was found to change considerably from nanoflowers to nanoplates then to nanoparticles with the variation of Co concentration. The optical band gap calculated using DRS was found to be 2.1 eV for pure CuO and increases up to 3.4 eV with increasing cobalt content. Photoluminescence measurements also confirm these results. The magnetic measurements indicated that the obtained nanostructures were ferromagnetic at room temperature with an optimum value of saturation magnetization at 1.0 wt.% of Co-doped CuO, i.e., 970 micro emu/g.

Microscopic and Metallurgical Aspects of the Space Shuttle Columbia Accident Investigation and Reconstruction

NASA Technical Reports Server (NTRS)

McDaniels, Steven J.

2004-01-01

The Space Shuttle Columbia was descending for a landing at the Kennedy Space Center (KSC) on February 1, 2003. Approximately 20 minutes prior to touchdown, the Columbia began disintegrating over the western United States; the majority of debris eventually impacted in eastern Texas and western Louisiana. A monumental effort eventually recovered approximately 84,000 pieces of debris, approximately 38% of the Orbiter's original dry weight. The debris was transported to KSC, where the items were catalogued and evaluated. Critical areas of interest, such as the left and right leading edge surfaces and the underside of the ship, were placed upon a grid to aid in the reconstruction. Items of interest included metallic structures, reinforced carbon-carbon composites, and ceramic heat insulation tiles. Many of the leading edge elements had re-solidified metallic deposits spattered on them. These deposits became known as slag and were one of the main focuses of the investigation. In order to help determine the sequence of events inside the left wing during the accident, the slag's composition, layering order, and directionality of deposition were studied. A myriad of analytical tests were performed in an attempt to ascertain the compositional and depositional characteristics of selected slag deposits, including the ordering of deposited layers within each individual slag deposit harvested. Initially, Scanning Electron Microscopy and Energy Dispersive X-Ray Spectroscopy (SEM/EDX) were performed to quickly characterize the overall composition of individual slag deposits: SEM utilizes a narrowlyfocused high-energy electron beam impinging upon a specimen. The incident beam excites and liberates lower energy secondary electrons, which are detected and analyzed, providing a visual representation of the sample's surface topography. EDX also relies on an incident electron beam, except an EDX unit measures X-ray energies generated by the impinging beam. Each element generates a unique X-ray signature; the EDX detector measures these discreet energies. EDX actually penetrates approximately 2 microns into the bulk of the sample. However, random examination of various portions of slag, coupled with the semiquantitative nature of the SEM/EDX analysis, did not yield convincingly pertinent data. Therefore, X-ray dot mapping was conducted, which provided more understandable data, both in terms of slag layering and composition. An X-ray dot map is generated by performing numerous EDX scans for individual elements, then compiling the scans in a visual representation. Eventually, specimens consisting of not only the slag, but of the adjacent RCC substrate as well were cross-sectioned. X-Ray dot mapping of the materialographicallymounted and -polished cross- sections provided a visual representation of both the layering sequence and compositional characteristics of the slag. Contemporaneously, Electron Spectroscopy for Chemical Analysis/X-Ray Photoelectron Spectroscopy (ESCA/XPS) and powdered X-Ray Diffraction (XRD) were performed to further characterize the deposits and to attempt to identify what, if any, compounds were present. The ESCA/XPS analysis allowed the analyst to "sputter" into the sample with an electron gun, aiding in the identification of the layering sequence. XPS uses photons, rather than electrons, which impinge upon the surface of the sample. XPS measures the electrons emitted from within the first 5 nm of the sample's surface. The XRD measures the scatter angles of incident X-rays; the angle and intensity of scatter depend upon the crystalline structure of the pulverized sample. XRD is considered a qualitative rather than quantitative technique. ESCA/XPS revealed that the final layer to deposit was predominantly carbonaceous. XRD was successful in identifying specific compounds, such as Al 2O3, Al and/or Al3 21SiO47, mullite (3(Al2)O3 -SiO2), and nickel-aluminides. Eventually, Electron MicroProbe Analysis (EMPA) was conducted on the marialographically-prepared cross- sections of selected slag deposits. Microprobe combines SEM and Wavelength Dispersive X-Ray Spectroscopy (WDS), and, like EDX, uses a narrowly-focused high-energy electron beam impinging upon a specimen to elicit, in the case of EPMA, characteristic X-rays with specific wavelengths. This quantitative, analytical tool proved the most useful in determining depositional layering and composition of the slag deposits. This information was utilized in verifying the location of the breach in the left leading edge of the wing of the Columbia.

Dopant concentration dependent optical and X-Ray induced photoluminescence in Eu3+ doped La2Zr2O7

NASA Astrophysics Data System (ADS)

Pokhrel, Madhab; Brik, Mikhail; Mao, Yuanbing

2015-03-01

Herein, we will be presenting the dopant (Eu) concentration dependent high density La2Zr2O7 nanoparticles for optical and X-ray scintillation applications by use of X - ray diffraction, Raman, FTIR, scanning electron microscope (SEM), transmission electron microscopy (TEM), optically and X-ray excited photoluminescence (PL). Several theoretical methods have been used in order to investigate the structural, electronic, optical, elastic, dynamic properties of Eu doped La2Zr2O7. It is observed that Eu: La2Zr2O7 shows an intense red luminescence under 258, 322, 394 and 465 nm excitation. The optical intensity of Eu: La2Zr2O7 depends on the dopant concentration of Eu3+. Following high energy excitation with X-rays, Eu: La2Zr2O7 shows an atypical Eu PL response (scintillation) with a red emission. The intense color emission of Eu obtained under 258 nm excitation, the X-ray induced luminescence property along with reportedly high density of La2Zr2O7, makes these nanomaterials attractive for optical and X-ray applications. The authors thank the support from the Defense Threat Reduction Agency (DTRA) of the U.S. Department of Defense (Award #HDTRA1-10-1-0114).

Spinel NixZn1-xFe2O4 (0.0 ≤ x ≤ 1.0) nano-photocatalysts: Synthesis, characterization and photocatalytic degradation of methylene blue dye

NASA Astrophysics Data System (ADS)

Padmapriya, G.; Manikandan, A.; Krishnasamy, V.; Jaganathan, Saravana Kumar; Antony, S. Arul

2016-09-01

Spinel NixZn1-xFe2O4 (x = 0.0 to 1.0) nanoparticles were successfully synthesized by a simple microwave combustion method (MCM) using metal nitrates as raw materials and glycine as the fuel. The structural, morphological and opto-magnetic properties of the spinel NixZn1-xFe2O4 ferrites were determined by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), high resolution scanning electron microscopy (HR-SEM), energy dispersive X-ray (EDX) spectroscopy, high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED) pattern, UV-Visible diffuse reflectance spectroscopy (DRS), photoluminescence (PL) spectroscopy and vibrating sample magnetometer (VSM). Powder XRD, and EDX analysis was confirmed the formation of pure phase of spinel ferrites. HR-SEM and HR-TEM analysis was confirmed the formation of sphere like-particle morphology of the samples with smaller agglomeration. VSM analysis clearly showed the superparamagnetic and ferromagnetic nature of the samples. The Ms value is 3.851 emu/g for undoped ZnFe2O4 sample and it increased with increase in Ni content. Photo-catalytic degradation (PCD) of methylene blue (MB) dye using the samples were carried out and observed good PCD results.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Miller, Thomas Martin; Patton, Bruce W.; Weber, Charles F.

The primary goal of this project is to evaluate x-ray spectra generated within a scanning electron microscope (SEM) to determine elemental composition of small samples. This will be accomplished by performing Monte Carlo simulations of the electron and photon interactions in the sample and in the x-ray detector. The elemental inventories will be determined by an inverse process that progressively reduces the difference between the measured and simulated x-ray spectra by iteratively adjusting composition and geometric variables in the computational model. The intended benefit of this work will be to develop a method to perform quantitative analysis on substandard samplesmore » (heterogeneous phases, rough surfaces, small sizes, etc.) without involving standard elemental samples or empirical matrix corrections (i.e., true standardless quantitative analysis).« less

Investigation on the effect of collagen and vitamins on biomimetic hydroxyapatite coating formation on titanium surfaces.

PubMed

Ciobanu, Gabriela; Ciobanu, Octavian

2013-04-01

This study uses an in vitro experimental approach to investigate the roles of collagen and vitamins in regulating the deposition of hydroxyapatite layer on the pure titanium surface. Titanium implants were coated with a hydroxyapatite layer under biomimetic conditions by using a supersaturated calcification solution (SCS), modified by adding vitamins A and D3, and collagen. The hydroxyapatite deposits on titanium were investigated by means of scanning electron microscopy (SEM) coupled with X-ray analysis (EDX), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and Fourier transformed infrared (FTIR) spectroscopy. The results obtained have shown that hydroxyapatite coatings were produced in vitro under vitamins and collagen influence. Copyright © 2012 Elsevier B.V. All rights reserved.

Comparing the detection of iron-based pottery pigment on a carbon-coated sherd by SEM-EDS and by Micro-XRF-SEM.

PubMed

Pendleton, Michael W; Washburn, Dorothy K; Ellis, E Ann; Pendleton, Bonnie B

2014-03-01

The same sherd was analyzed using a scanning electron microscope with energy dispersive spectroscopy (SEM-EDS) and a micro X-ray fluorescence tube attached to a scanning electron microscope (Micro-XRF-SEM) to compare the effectiveness of elemental detection of iron-based pigment. To enhance SEM-EDS mapping, the sherd was carbon coated. The carbon coating was not required to produce Micro-XRF-SEM maps but was applied to maintain an unbiased comparison between the systems. The Micro-XRF-SEM analysis was capable of lower limits of detection than that of the SEM-EDS system, and therefore the Micro-XRF-SEM system could produce elemental maps of elements not easily detected by SEM-EDS mapping systems. Because SEM-EDS and Micro-XRF-SEM have been used for imaging and chemical analysis of biological samples, this comparison of the detection systems should be useful to biologists, especially those involved in bone or tooth (hard tissue) analysis.

Comparing the Detection of Iron-Based Pottery Pigment on a Carbon-Coated Sherd by SEM-EDS and by Micro-XRF-SEM

PubMed Central

Pendleton, Michael W.; Washburn, Dorothy K.; Ellis, E. Ann; Pendleton, Bonnie B.

2014-01-01

The same sherd was analyzed using a scanning electron microscope with energy dispersive spectroscopy (SEM-EDS) and a micro X-ray fluorescence tube attached to a scanning electron microscope (Micro-XRF-SEM) to compare the effectiveness of elemental detection of iron-based pigment. To enhance SEM-EDS mapping, the sherd was carbon coated. The carbon coating was not required to produce Micro-XRF-SEM maps but was applied to maintain an unbiased comparison between the systems. The Micro-XRF-SEM analysis was capable of lower limits of detection than that of the SEM-EDS system, and therefore the Micro-XRF-SEM system could produce elemental maps of elements not easily detected by SEM-EDS mapping systems. Because SEM-EDS and Micro-XRF-SEM have been used for imaging and chemical analysis of biological samples, this comparison of the detection systems should be useful to biologists, especially those involved in bone or tooth (hard tissue) analysis. PMID:24600333

[Effects of dynamic high-pressure microfluidization on the structure of waxy rice starch].

PubMed

Tu, Zong-Cai; Zhu, Xiu-Mei; Chen, Gang; Wang, Hui; Zhang, Bo; Huang, Xiao-Qin; Li, Zhi

2010-03-01

The effects of dynamic ultra high-pressure microfluidization on the structure of waxy rice starch solutions (6%) were analyzed using SEM, UV-Vis spectra, polarized light microscopy, and X-ray diffraction spectra. The results showed that: SEM graphs demonstrated that the crystal structure of waxy rice starch under different pressure treatment was destroyed with different degrees and impacted into flake up to 160 MPa; from the ultraviolet-visible spectrum we know the reduction in the blue iodine value and the decrease in the amylopectin content, which illustrated that the structure of waxy rice starch was fractured; polarized microscopic images showed that the polarization crosses of starch molecules became misty with the pressure increasing, and most of starch molecules lost polarization cross when the pressure reached 160 MPa; X-ray diffraction spectra indicated that relative crystallinity began to decline at 120 MPa with pressure treatment, and the decreased amplitude was slightly lower.

Electrophoretic Deposition of Hydroxyapatite Film Containing Re-Doped MoS2 Nanoparticles

PubMed Central

Shalom, Hila; Feldman, Yishay; Rosentsveig, Rita; Pinkas, Iddo; Kaplan-Ashiri, Ifat; Moshkovich, Alexey; Perfilyev, Vladislav; Rapoport, Lev

2018-01-01

Films combining hydroxyapatite (HA) with minute amounts (ca. 1 weight %) of (rhenium doped) fullerene-like MoS2 (IF) nanoparticles were deposited onto porous titanium substrate through electrophoretic process (EPD). The films were analyzed by scanning electron microscopy (SEM), X-ray diffraction and Raman spectroscopy. The SEM analysis showed relatively uniform coatings of the HA + IF on the titanium substrate. Chemical composition analysis using energy dispersive X-ray spectroscopy (EDS) of the coatings revealed the presence of calcium phosphate minerals like hydroxyapatite, as a majority phase. Tribological tests were undertaken showing that the IF nanoparticles endow the HA film very low friction and wear characteristics. Such films could be of interest for various medical technologies. Means for improving the adhesion of the film to the underlying substrate and its fracture toughness, without compromising its biocompatibility are discussed at the end. PMID:29495394

Investigation of tin oxide nanofibers synthesized via bio-template technique

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kundu, Virender Singh, E-mail: vskundu-kuk@rediffmail.com; Dhiman, Jonny; Kumar, Suresh

In the present paper tin oxide nanofibers have been by synthesized using cotton as bio-template via sol-gel route. This is comparatively a new synthesis technique. The structure and morphology of the obtained SnO{sub 2} nanofibers were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), energy-dispersive X-ray spectroscopy (EDX). The optical properties of the same have been studied by using UV-Vis spectroscopy. The observed XRD pattern showed that peaks are very narrow and sharp which indicates crystalline nature of samples. SEM images gave an idea about the sample morphology and confirm that the obtained sample were nanofibers. The optical absorbancemore » spectrum of the sample under study was recorded in UV-visible region (200nm- 800nm). The band gap of the sample was found to be 3.95 eV which is higher than their bulk counterpart.« less

Sodium Chloride Diffusion during Muscle Salting Evidenced by Energy-Dispersive X-ray Spectroscopy Imaging.

PubMed

Filgueras, Rénata; Peyrin, Frédéric; Vénien, Annie; Hénot, Jean Marc; Astruc, Thierry

2016-01-27

To better understand the relationship between the muscle structure and NaCl transfers in meat, we used energy-dispersive X-ray spectroscopy (EDS) coupled with scanning electron microscopy (SEM) to analyze brined and dry-salted rat muscles. The muscles were freeze-dried to avoid the delocalization of soluble ions that happens in regular dehydration through a graded series of ethanol. Na and Cl maps were superimposed on SEM images to combine the muscle structure and NaCl diffusion. Brining causes rapid diffusion of NaCl through the tissue. Most brine diffuses in a linear front from the muscle surface, but a small proportion enters through the perimysium network. The muscle area penetrated by brine shows heterogeneous patterns of NaCl retention, with some connective tissue islets containing more NaCl than other parts of perimysium. NaCl penetration is considerably slower after dry salting than after brining.

Initial stages of microbiologically influenced tarnishing on titanium after 20 months of immersion in freshwater.

PubMed

Moreno, D A; Cano, E; Ibars, J R; Polo, J L; Montero, F; Bastidas, J M

2004-05-01

This paper studies the initial stages of iridescent tarnishes on titanium heat exchanger tubes in contact with running freshwater on the river Tagus in Spain for up to 20 months. Electrochemical impedance spectroscopy (EIS), scanning electron microscopy [(SEM with energy dispersive X-ray (EDX)] and X-ray photoelectron spectroscopy (XPS) in conjunction with argon-ion sputtering were the techniques used. The EIS data indicated a capacitive behavior, showing a semicircle that was better defined as the experimental time increased, indicating a decreasing tarnishing resistance of titanium. XPS and EDX results indicated that the main elements identified were calcium, phosphorus, nitrogen, and iron. The amount of these elements was higher on the tarnished titanium specimens than on the untarnished specimens. SEM analysis showed the presence of diatoms in the iridescent tarnishes on titanium tubes. Copyright 2003 Springer-Verlag

Preparation and Characterization of Silanes Films to Protect Electrogalvanized Steel

NASA Astrophysics Data System (ADS)

Seré, Pablo R.; Egli, Walter; Di Sarli, Alejandro R.; Deyá, Cecilia

2018-03-01

Silanes are an interesting alternative to chromate-based surface treatments for temporary protection of electrogalvanized steel. In this work, the protective behavior of 3-mercaptopropyltrimethoxysilane (MTMO), 3-aminopropyltriethoxysilane (AMEO), or 3-glycidoxypropyltrimethoxysilane (GLYMO) films applied on electrogalvanized automotive quality steel sheets has been studied. The silane coating morphology, composition, and porosity were characterized by scanning electron microscopy (SEM), energy-dispersive x-ray spectroscopy (EDS), x-ray fluorescence, immersion in copper sulfate, and cyclic voltammetry. The corrosion protection was evaluated by polarization curves, electrochemical noise measurements, electrochemical impedance spectrometry, and accelerated humidity chamber tests. The results showed that the silanes protect temporarily electrogalvanized steel from corrosion. MTMO forms a relatively thick and cracked film. AMEO and GLYMO films were so thin that they could not be observed by SEM but silicon was detected by EDS. MTMO provided good temporary protection, being an alternative to replace Cr(VI) as protector of electrogalvanized steel.

Enhancement in surface area and magnetization of CoFe2O4 nanoparticles for targeted drug delivery application

NASA Astrophysics Data System (ADS)

Kale, Swati B.; Somvanshi, Sandeep B.; Sarnaik, M. N.; More, S. D.; Shukla, S. J.; Jadhav, K. M.

2018-05-01

This paper reports facile synthesis, characterizations by X-ray diffraction and scanning electron microscopy and magnetic behaviour of cobalt ferrite nanoparticles. Cobalt ferrite nanoparticles were prepared by sol-gel auto combustion technique using glycine as a fuel. Phase purity and nanocrystalline nature of the prepared sample was confirmed through X-ray diffraction technique. No extra peak other than cubic spinel structure was observed in the XRD pattern. The crystallite size calculated by using Scherrer's formula is of the order of 21.6 nm indicating the nanocrystalline nature of the prepared cobalt ferrite sample. The surface morphological studies were carried out using scanning electron microscope (SEM). SEM image shows homogeneous, agglomerated particles with sponge-like form. The saturation magnetization, coercivity and remenance magnetization obtained by hysteresis curve clearly gives the evidence of excellent and enhanced magnetic behaviour.

Investigation of magnetic and structural properties of Ni-Zr co-doped M-type Sr-La hexaferrites

NASA Astrophysics Data System (ADS)

Yang, Yujie; Wang, Fanhou; Shao, Juxiang; Huang, Duohui; Tang, Jin; Rehman, Khalid Mehmood Ur

2018-02-01

In this research, Ni2+ and Zr4+ co-doped Sr-La hexaferrites Sr0.7La0.3Fe12.0-2 x (NiZr) x O19 (0.0 ≤ x ≤ 0.5) were synthesized by the standard ceramic method. The phase identification of the hexaferrites was confirmed by X-ray diffraction analysis. X-ray diffraction analysis showed that all the samples were in single phase M-type hexagonal structure and no impurity phase was observed. Lattice parameters ( c and a) increased with increasing NiZr content ( x) from 0.0 to 0.5. The morphology of the hexaferrites was analyzed by a field emission scanning electron microscopy (FE-SEM). FE-SEM micrographs showed that the grains exhibited hexagonal shape in a plate-like structure with clear grain boundaries. Magnetization properties of the hexaferrites were carried out at room temperature using a physical property measurement system-vibrating sample magnetometer. The values of saturation magnetization ( M s), remanent magnetization ( M r) and coercivity ( H c) were calculated from magnetic hysteresis ( M- H) loops. M s and H c decreased with increasing NiZr content ( x) from 0.0 to 0.5. M r and M r/ M s ratio first increased with increasing NiZr content ( x) from 0.0 to 0.1, and then decreased when NiZr content ( x) ≥ 0.1.

Morphological and spectroscopic analysis of cellulose nanocrystals extracted from oil palm empty fruit bunch fiber

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dasan, Y. K., E-mail: aamir.bhat@petronas.com.my; Bhat, A. H., E-mail: aamir.bhat@petronas.com.my; Faiz, A., E-mail: faizahmad@petronas.com.my

2015-07-22

This work evaluates the use of oil palm empty fruit bunch (OPEFB) fiber as a source of cellulose to obtain nanocrystalline cellulose (CNC) by acid hydrolysis reaction. The raw OPEFB fibers were pretreated with aqueous Sodium hydroxide at 80°C followed by bleaching treatment and further hydrolyzed with Sulphuric acid at 45°C with limited range of hydrolysis time and acid concentration. The resulting CNC’s were characterized for spectroscopic, crystallographic and morphological properties using Fourier Transform Infrared Spectroscopy (FTIR), X-ray Diffractometer (XRD), Transmission Electron Microscope (TEM) and Atomic Force Microscopy (AFM). Finding of this study shows that the properties of CNC’s aremore » strongly dependent on the hydrolysis time and acid concentration.« less

Growth and studies of cyclohexylammonium 4-methoxy benzoate single crystal for nonlinear optical applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sathya, P.; Gopalakrishnan, R., E-mail: krgkrishnan@annauniv.edu

2015-06-24

Cyclohexylammonium 4-Methoxy Benzoate (C4MB) was synthesised and the functional groups were confirmed by FTIR analysis. The purified C4MB (by repeated recrystallisation) was used for single crystal growth. Single crystal of cyclohexylammonium 4-methoxy benzoate was successfully grown by slow evaporation solution growth method at ambient temperature. Structural orientations were determined from single crystal X-ray diffractometer. Optical absorption and cut off wavelength were identified by UV-Visible spectroscopy. Thermal stability of the crystal was studied from thermogravimetric and differential thermal analyses curves. Mechanical stability of the grown crystal was analysed by Vicker’s microhardness tester. The Second Harmonic Generation (SHG) study revealed that themore » C4MB compound exhibits the SHG efficiency 3.3 times greater than KDP crystal.« less

Growth and characterization of thin Cu-phthalocyanine films on MgO(001) layer for organic light-emitting diodes

PubMed Central

2012-01-01

Surface morphology and thermal stability of Cu-phthalocyanine (CuPc) films grown on an epitaxially grown MgO(001) layer were investigated by using atomic force microscope and X-ray diffractometer. The (002) textured β phase of CuPc films were prepared at room temperature beyond the epitaxial MgO/Fe/MgO(001) buffer layer by the vacuum deposition technique. The CuPc structure remained stable even after post-annealing at 350°C for 1 h under vacuum, which is an important advantage of device fabrication. In order to improve the device performance, we investigated also current-voltage-luminescence characteristics for the new top-emitting organic light-emitting diodes with different thicknesses of CuPc layer. PMID:23181826

Growth and characterization of thin Cu-phthalocyanine films on MgO(001) layer for organic light-emitting diodes.

PubMed

Bae, Yu Jeong; Lee, Nyun Jong; Kim, Tae Hee; Cho, Hyunduck; Lee, Changhee; Fleet, Luke; Hirohata, Atsufumi

2012-11-26

Surface morphology and thermal stability of Cu-phthalocyanine (CuPc) films grown on an epitaxially grown MgO(001) layer were investigated by using atomic force microscope and X-ray diffractometer. The (002) textured β phase of CuPc films were prepared at room temperature beyond the epitaxial MgO/Fe/MgO(001) buffer layer by the vacuum deposition technique. The CuPc structure remained stable even after post-annealing at 350°C for 1 h under vacuum, which is an important advantage of device fabrication. In order to improve the device performance, we investigated also current-voltage-luminescence characteristics for the new top-emitting organic light-emitting diodes with different thicknesses of CuPc layer.

Diffractometric measurement of the temperature dependence of piezoelectric tensor in GMO monocrystal

NASA Astrophysics Data System (ADS)

Breczko, Teodor; Lempaszek, Andrzej

2007-04-01

Functional materials, of which an example is ferroelectric, ferroelastic monocrystal of molybdate (III) gadolinium (VI), are often used in the micro-motor operators (micro-servo motors) working in changeable environment conditions. Most frequently this change refers to temperature. That is why the important practical problem is the precise measurement of the value of piezoelectric tensor elements in dependence on the temperature of a particular monocrystal. In the presented article for this kind of measurements, the use of X-ray diffractometer has been shown. The advantage of the method presented is that, apart from precise dependence measurement between the temperature of a monocrystal and the value of piezoelectric tensor elements, it enables synchronous measurement of the value of thermal expansion tensor elements for a monocrystal.

Crystal structure and magnetic properties of Cr doped barium hexaferrite

NASA Astrophysics Data System (ADS)

Kumar, Sunil; Supriya, Sweety; Pandey, Rabichandra; Pradhan, Lagen Kumar; Kar, Manoranjan

2018-04-01

The Cr3+ substituted BaFe12O19 has been synthesized by modified sol-gel method to tailor the magnetic anisotropy and coercivity for technological applications. Some basic studies have revealed that this substitution leads to unusual interactions among the magnetic sublattices of the M-type hexaferrite. In order to investigate these interactions, BaFe12-xCrxO19 (x = 0.0, 0.5, 1.0, 2.0, and 4.0) M-type hexaferrites were characterized by employing XRD (X-ray Diffractometer). It is confirmed that, all the samples are in nanocrystalline and single phase, no impurity has been detected within the XRD limit. The magnetic hysteresis (m-H) loops revealed the ferromagnetic nature of nanoparticles (NPs). The coercive field were increasing with the increasing Cr3+ content, but after the percolation limit it decreases. The magnetocrystalline anisotropy is increasing with the Cr3+ concentration in samples and high values of magnetocrystalline anisotropy revealed that all samples are hard magnetic materials. Magnetic hysteresis loops were analyzed using the Law of Approach to Saturation method.

Hard X-ray irradiation of cosmic silicate analogs: structural evolution and astrophysical implications

NASA Astrophysics Data System (ADS)

Gavilan, L.; Jäger, C.; Simionovici, A.; Lemaire, J. L.; Sabri, T.; Foy, E.; Yagoubi, S.; Henning, T.; Salomon, D.; Martinez-Criado, G.

2016-03-01

Context. Protoplanetary disks, interstellar clouds, and active galactic nuclei contain X-ray-dominated regions. X-rays interact with the dust and gas present in such environments. While a few laboratory X-ray irradiation experiments have been performed on ices, X-ray irradiation experiments on bare cosmic dust analogs have been scarce up to now. Aims: Our goal is to study the effects of hard X-rays on cosmic dust analogs via in situ X-ray diffraction. By using a hard X-ray synchrotron nanobeam, we seek to simulate cumulative X-ray exposure on dust grains during their lifetime in these astrophysical environments and provide an upper limit on the effect of hard X-rays on dust grain structure. Methods: We prepared enstatite (MgSiO3) nanograins, which are analogs to cosmic silicates, via the melting-quenching technique. These amorphous grains were then annealed to obtain polycrystalline grains. These were characterized via scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM) before irradiation. Powder samples were prepared in X-ray transparent substrates and were irradiated with hard X-rays nanobeams (29.4 keV) provided by beamline ID16B of the European Synchrotron Radiation Facility (Grenoble). X-ray diffraction images were recorded in transmission mode, and the ensuing diffractograms were analyzed as a function of the total X-ray exposure time. Results: We detected the amorphization of polycrystalline silicates embedded in an organic matrix after an accumulated X-ray exposure of 6.4 × 1027 eV cm-2. Pure crystalline silicate grains (without resin) do not exhibit amorphization. None of the amorphous silicate samples (pure and embedded in resin) underwent crystallization. We analyze the evolution of the polycrystalline sample embedded in an organic matrix as a function of X-ray exposure. Conclusions: Loss of diffraction peak intensity, peak broadening, and the disappearance of discrete spots and arcs reveal the amorphization of the resin embedded (originally polycrystalline) silicate sample. We explore the astrophysical implications of this laboratory result as an upper limit to the effect of X-rays on the structure of cosmic silicates.

Crystal Structure, Magnetic and Optical Properties of Mn-Doped BiFeO₃ by Hydrothermal Synthesis.

PubMed

Zhang, Ning; Wei, Qinhua; Qin, Laishun; Chen, Da; Chen, Zhi; Niu, Feng; Wang, Jiangying; Huanag, Yuexiang

2017-01-01

In this paper, Mn doped BiFeO₃ were firstly synthesized by hydrothermal process. The influence of Mn doping on structural, optical and magnetic properties of BiFeO₃ was studied. The different amounts of Mn doping in BiFeO₃ were characterized by X-ray diffraction, Scanning Electron Microscope, Energy Dispersive X-ray Spectroscope, UV-Vis diffuse reflectance spectroscopy and magnetic measurements. The X-ray diffraction (XRD) patterns confirmed the formation of pure phase rhombohedral structure in BiFe(1−x) Mn (x) O₃ (x = 0.01, 0.03, 0.05, 0.07) samples. The morphologies and chemical compositions of as-prepared samples could be observed by Scanning Electron Microscope (SEM) and Energy Dispersive X-ray Spectroscope (EDS). A relative large saturated magnetization (Ms) of 0.53 emu/g for x = 0.07 sample was obtained at room temperature, which is considered to be Mn ions doping. UV-Vis diffuse reflectance spectroscopy showed strong absorption of light in the range of 200–1000 nm, indicating the optical band gap in the visible region for these samples. This implied that BiFe(1−x) Mn(x)O₃ may be a potential photocatalyst for utilizing solar energy.

The El Horror uranium anomaly in northeastern Sonora, Mexico: Constraints from geochemical and mineralogical approaches

NASA Astrophysics Data System (ADS)

Grijalva-Rodríguez, T.; Valencia-Moreno, M.; Calmus, T.; Del Rio-Salas, R.; Balcázar-García, M.

2017-12-01

This work reviews the characteristics of the El Horror uranium prospect in northeastern Sonora, Mexico. It was formerly detected by a radiometric anomaly after airborne gamma ray exploration carried out in the 70's by the Mexican government. As a promising site to contain important uranium resources, the El Horror was re-evaluated by CFE (Federal Electricity Commission) by in situ gamma ray surveys. The study also incorporates rock and stream sediment ICP-MS geochemistry, X-ray diffraction, X-ray fluorescence, Raman spectrometry and Scanning Electron Microscopy (SEM) to provide a better understanding of the radiometric anomaly. The results show that, instead of a single anomaly, it comprises at least five individual anomalies hosted in hydrothermally altered Laramide (80-40 Ma) andesitic volcanic rocks of the Tarahumara Formation. Concentrations for elemental uranium and uranium calculated from gamma ray surveys (i.e., equivalent uranium) are not spatially coincident within the anomaly, but, at least at some degree, they do so in specific sites. X-ray diffraction and Raman spectrometry revealed the presence of rutile/anatase, uvite, bukouvskyte and allanite as the more likely mineral phases to contain uranium. SEM studies revealed a process of iron-rich concretion formation, suggesting that uranium was initially incorporated to the system by adsorption, but was largely removed later during incorporation of Fe+3 ions. Stream sediment geochemistry reveals that the highest uranium concentrations are derived from the southern part of the Sierra La Madera batholith (∼63 Ma), and decrease toward the El Horror anomaly.

Synthesis and structural characterization of polyaniline/cobalt chloride composites

DOE Office of Scientific and Technical Information (OSTI.GOV)

Asha, E-mail: arana5752@gmail.com; Goyal, Sneh Lata; Kishore, Nawal

2016-05-23

Polyaniline (PANI) and PANI /cobalt chloride composites were synthesized by in situ chemical oxidative polymerization of aniline with CoCl{sub 2}.6H{sub 2}O using ammonium peroxidisulphate as an oxidant. These composites were characterized by X-ray diffraction (XRD) and Scanning electron microscopy (SEM). The XRD study reveals that both PANI and composites are amorphous. The XRD and SEM results confirm the presence of cobalt chloride in the composites.

Faults and foibles of quantitative scanning electron microscopy/energy dispersive x-ray spectrometry (SEM/EDS)

NASA Astrophysics Data System (ADS)

Newbury, Dale E.; Ritchie, Nicholas W. M.

2012-06-01

Scanning electron microscopy with energy dispersive x-ray spectrometry (SEM/EDS) is a powerful and flexible elemental analysis method that can identify and quantify elements with atomic numbers > 4 (Be) present as major constituents (where the concentration C > 0.1 mass fraction, or 10 weight percent), minor (0.01<= C <= 0.1) and trace (C < 0.01, with a minimum detectable limit of ~+/- 0.0005 - 0.001 under routine measurement conditions, a level which is analyte and matrix dependent ). SEM/EDS can select specimen volumes with linear dimensions from ~ 500 nm to 5 μm depending on composition (masses ranging from ~ 10 pg to 100 pg) and can provide compositional maps that depict lateral elemental distributions. Despite the maturity of SEM/EDS, which has a history of more than 40 years, and the sophistication of modern analytical software, the method is vulnerable to serious shortcomings that can lead to incorrect elemental identifications and quantification errors that significantly exceed reasonable expectations. This paper will describe shortcomings in peak identification procedures, limitations on the accuracy of quantitative analysis due to specimen topography or failures in physical models for matrix corrections, and quantitative artifacts encountered in xray elemental mapping. Effective solutions to these problems are based on understanding the causes and then establishing appropriate measurement science protocols. NIST DTSA II and Lispix are open source analytical software available free at www.nist.gov that can aid the analyst in overcoming significant limitations to SEM/EDS.

Solid-State Spun Fibers from 1 mm Long Carbon Nanotube Forests Synthesized by Water-Assisted Chemical Vapor Deposition

NASA Technical Reports Server (NTRS)

Zhang, Shanju; Zhu, Lingbo; Minus, Marilyn L.; Chae, han Gi; Jagannathan, Sudhakar; Wong, Ching-Ping; Kowalik, Janusz; Roberson, Luke B.; Kumar, Satish

2007-01-01

In this work, we report continuous carbon nanotube fibers dry-drawn directly from water-assisted CVD grown forests with millimeter scale length. As-drawn nanotube fibers exist as aerogel and can be transformed into more compact fibers through twisting or densification with a volatile liquid. Nanotube fibers are characterized by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), Raman microscopy and wide-angle X-ray diffraction (WAXD). Mechanical behavior and electrical conductivity of the post-treated nanotube fibers are investigated.

Morphology and dispersion of FeCo alloy nanoparticles dispersed in a matrix of IR pyrolized polyvinyl alcohol

NASA Astrophysics Data System (ADS)

Vasilev, A. A.; Dzidziguri, E. L.; Muratov, D. G.; Zhilyaeva, N. A.; Efimov, M. N.; Karpacheva, G. P.

2018-04-01

Metal-carbon nanocomposites consisting of FeCo alloy nanoparticles dispersed in a carbon matrix were synthesized by the thermal decomposition method of a precursor based on polyvinyl alcohol and metals salts. The synthesized powders were investigated by X-ray diffraction (XRD), X-ray fluorescent spectrometry (XRFS), transmission electron microscopy (TEM) and scanning electron microscopy (SEM). Surface characteristics of materials were measured by BET-method. The morphology and dispersity of metal nanoparticles were studied depending on the metals ratio in the composite.

Preparation of carbon nanotubes/BiOBr composites with higher visible light photocatalytic activity

NASA Astrophysics Data System (ADS)

You, Y. J.; Zhang, Y. X.; Li, R. R.; Li, C. H.

2014-12-01

A novel flower-like photocatalyst CNTs/BiOBr was successfully prepared by a facile hydrothermal method. The morphology and the physicochemical properties of the prepared samples were investigated using scanning electron microscopy (SEM), X-ray diffraction (XRD), energy dispersive X-ray spectrometry (EDX), and UV-visible diffuse reflectance spectroscopy (UV-vis DRS). The photocatalytic activity was evaluated by degradation of Rhodamin B (RhB) dye. It was demonstrated that CNTs/BiOBr photocatalyst could effectively photodegrade RhB under visible light (VL) irradiation.

Nanoscale interfacial mixing of Au/Bi layers using MeV ion beams

NASA Astrophysics Data System (ADS)

Prusty, Sudakshina; Siva, V.; Ojha, S.; Kabiraj, D.; Sahoo, P. K.

2017-05-01

We have studied nanoscale mixing of thermally deposited double bilayer films of Au/Bi after irradiating them by 1.5 MeV Au2+ ions. Post irradiation effects on the morphology and elemental identification in these films are studied by Scanning electron microscopy (SEM) and Energy dispersive X-ray spectroscopy (EDS). Glancing angle X-ray diffraction (GAXRD) of the samples indicate marginal changes in the irradiated samples due to combined effect of nuclear and electronic energy loss. The interfacial mixing is studied by Rutherford backscattering (RBS).

Synthesis and Raman scattering of GaN nanorings, nanoribbons and nanowires

NASA Astrophysics Data System (ADS)

Li, Z. J.; Chen, X. L.; Li, H. J.; Tu, Q. Y.; Yang, Z.; Xu, Y. P.; Hu, B. Q.

Low-dimensional GaN materials, including nanorings, nanoribbons and smooth nanowires have been synthesized by reacting gallium and ammonia using Ag particles as a catalyst on the substrate of MgO single crystals. They were characterized by field emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD). EDX, XRD indicated that the low-dimensional nanomaterials were wurtzite GaN. New features are found in Raman scatterings for these low-dimensional GaN materials, which are different from the previous observations of GaN materials.

DISTRIBUTION SYSTEM SOLIDS - A RESEARCH APPROACH

EPA Science Inventory

The U.S. EPA's AWBERC research facility is equipped with capabilities to analyze a variety of solids in support many Laboratory-wide research studies. Techniques available on site include X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microsco...

X-Ray study of hetero ring flexibility in norbornane, norbornene-fused 1,3-oxazin-2-thiones Structure of 5,8-methano- r-4-phenyl-c-4a, c-5,6,7, c-8, c- 8a-hexahydro-4H- 1 ,3-benzoxazin-2 (3H)-thione

NASA Astrophysics Data System (ADS)

Kálmán, A.; Argay, Gy.; Stájer, G.; Bernáth, G.

1991-08-01

The structure of S,8-methano- r-4-phenyl c4a, c5,6,7 c8 c8ahexahydro4 H 1,3 -benzoxazin- 2 (3 H)-thione (C 15H 17N0S, M r=259.37) has been established by X-ray crystallography from diffractometer data: it crystallizes in the monoclinic space group P2 1/n with a=6.150(2) Å, b=9.655(1) Å, c=22.093(4) Å,β=96.75(2)† V=1302.7(8) Å 3,4,D c=1.32gcm -3and p( Cu K) =20.4cm -. The structure has been solved by direct methods, refined to R=0.050 for 2193 observed reflections. The X-ray analysis substantiated the structure: the NMR spectra in- dicated that the 4-phenyl group assumes an exo-equatorial position. The puckering parameters of D. Cremer, J.A. Pople, J. Am. Chem. Soc., 97 (1975), 1354 (ref.1), of the distorted hetero ring (a transitional form between E 4-envelope, ( 5S 4-screw-boat) show that, depending on the positions of the hetero atoms, both the norbornane, norbornene skeletons markedly alter the characteristic transitional ( 5E/ 5H 6) shape of the 1,3-oxazine ring observed in other saturated, partly saturated l,3-benzoxazin-2-ones, analogous thiones.

Band alignment of atomic layer deposited MgO/Zn0.8Al0.2O heterointerface determined by charge corrected X-ray photoelectron spectroscopy

NASA Astrophysics Data System (ADS)

Yan, Baojun; Liu, Shulin; Yang, Yuzhen; Heng, Yuekun

2016-05-01

Pure magnesium (MgO) and zinc oxide doped with aluminum oxide (Zn0.8Al0.2O) were prepared via atomic layer deposition. We have studied the structure and band gap of bulk Zn0.8Al0.2O material by X-ray diffractometer (XRD) and Tauc method, and the band offsets and alignment of atomic layer deposited MgO/Zn0.8Al0.2O heterointerface were investigated systematically using X-ray photoelectron spectroscopy (XPS) in this study. Different methodologies, such as neutralizing electron gun, the use of C 1s peak recalibration and zero charging method, were applied to recover the actual position of the core levels in insulator materials which were easily influenced by differential charging phenomena. Schematic band alignment diagram, valence band offset (ΔEV) and conduction band offset (ΔEC) for the interface of the MgO/Zn0.8Al0.2O heterostructure have been constructed. An accurate value of ΔEV = 0.72 ± 0.11 eV was obtained from various combinations of core levels of heterojunction with varied MgO thickness. Given the experimental band gaps of 7.83 eV for MgO and 5.29 eV for Zn0.8Al0.2O, a type-II heterojunction with a ΔEC of 3.26 ± 0.11 eV was found. Band offsets and alignment studies of these heterojunctions are important for gaining deep consideration to the design of various optoelectronic devices based on such heterointerface.

Koster van Groos, A F

NASA Astrophysics Data System (ADS)

Guggenheim, S.

2008-12-01

The deep-ocean environment, including the ocean floor and crust, represents one of the last scientific frontiers on earth. The surprising lack of information on the mineralogy, the geochemical processes, or the biota of the ocean floor is the result of the inability to simulate ocean-floor conditions and to study geochemical systems at these conditions. A proto-type high-pressure environmental chamber (HPEC) has been constructed for use on a transmission- mode X-ray diffractometer to study geochemical processes at the deep-ocean sediment cover and crust. The HPEC has a designed pressure range to 1000 bars and temperature range from -20 oC to 200 oC. In this chamber, a liquid (e.g., sea water) plus sample in suspension can be pressurized either by gas or liquid. A cell-pump system continuously agitates the liquid to keep particles in suspension, thereby allowing the examination of mineral phases, including clays minerals. A major feature of the HPEC is that the mineral component moves freely and can react with its environment while being illuminated by the X-ray beam. The cell-pump also allows applied gas, such as CH4 or CO2, or O2, to interact efficiently with the aqueous liquid so that the system may rapidly reach equilibrium. In addition, mixing these gases with inert gases, e.g. He or Ar, allows control of the fugacity of these gas components. The design components and how data are manipulated to remove X-ray dispersion effects caused by the liquid will be discussed, along with examples showing the effects of temperature, pressure, and salt content on smectite clay.

Optical and Structural Characterization of ZnO/TiO2 Bilayer Thin Films Grown by Sol-Gel Spin Coating

NASA Astrophysics Data System (ADS)

Gareso, P. L.; Musfitasari; Juarlin, Eko

2018-03-01

Structural and optical properties of ZnO/TiO2 bilayers thin films have been investigated using x-ray diffraction (X-RD), scanning electron microscopy (SEM), and optical transmittance UV-Vis measurements. ZnO thin films were prepared by dissolving zinc acetate dehydrated into a solvent of ethanol and then added triethanolamin. In the case of TiO2 layers, tetraisoproxide was dissolved into ethanol and then added an acetate acid. The layer of ZnO was deposited first followed by TiO2 layer on a glass substrate using a spin coating technique. The ZnO/TiO2 bilayers were annealed at various temperatures from 300°C until 600°C for 60 minutes. The X-ray diffraction results show that there was an enhancement of the x-ray spectra as annealed temperature increased to 600°C in comparison to the samples that were annealed at 300°C. Based on the optical measurement of UV-Vis, the band gap energy of ZnO/TiO2 bilayer is around 3.2 eV at temperature of 300°C. This value is similar to the band gap energy of ZnO. SEM results show that there is no cluster in the surface of ZnO/TiO2 bilayer.

Sintering mechanism of the CaF2 on hydroxyapatite by a 10.6-l microm CO2 laser.

PubMed

Wu, Cheng-Chei; Roan, Rong-Tai; Chen, Jeng-Huey

2002-01-01

Laser has been reported as a heat source for melting and re-crystallization. Occurring at about 1100 degrees C, the melting of surface dental enamel along with re-crystallization might have an assistant role in the therapy of hypersensitive tooth, apical sealing of endodontic surgery in dentistry, preventive dentistry for pit and fissure sealing, and fluoridation. For laser to be accepted in clinical applications, it is desired that, studies must show the incorporation of CaF(2) into hydroxyapatite could reduce the sintering temperature for the sake of safety. In this study, the Sharplan 20XJ CO(2) laser with 10.6- microm wavelength was set under the following parameters: power, 5 W; repetitive mode, 0.1 second; beam, focused. Fluorite was added to hydroxyapatite as a synthetic compound to lower the sintering temperature. Human dental enamel without caries was used for in vitro sintering test. Scanning electron microscopy (SEM), X-ray diffractometer (XRD), Fourier transforming infrared spectroscopy (FTIR), and differential thermal analysis/thermogravimetric analysis (DAT/TGA) were used for the investigation of sintering mechanism of CaF(2). Fusion between hexagonal shape crystals and cubic shape crystals (CaF(2)) were observed under SEM study. Hexagonal shape crystals indicated the formation of fluorapatite under XRD analysis. Under FTIR study, we examined reductions of water (3445 cm(-1)) and hydroxyl bands (3567 and 627 cm(-1)) in irradiated compounds. From the DTA pattern of synthetic compound, it showed the endothermic reaction reaching its peak point around 1180 +/- 20 degrees C. It was attributed to the phase transformation and/or initial melting. In this study, we proposed the interrelationship of the eutectics between initiator (CaF(2)) and the reaction product (calcium hydroxide) that reduced the sintering temperature. It appeared that the co-eutectics interacted to reduce the sintering temperature of hydroxyapatite below 800 degrees C and that the key eutectic was calcium hydroxide. The clinical feasibility of the melting and re-crystallization of hydroxyapatite under 10.6-microm CO(2) laser would be therefore enhanced. Copyright 2002 Wiley-Liss, Inc.

Determination of anisotropy and multimorphology in fly ash based geopolymers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Khan, M. Irfan, E-mail: mirfanwazir@gmail.com; Azizli, Khairun, E-mail: khairun-azizli@petronas.com.my; Sufian, Suriati, E-mail: suriati@petronas.com.my

2015-07-22

In this study, Malaysian coal fly ash-based geopolymers were investigated for its morphology and chemical composition using scanning electron microscopy coupled with energy dispersive X-rays (SEM-EDX). Geopolymer was synthesized using sodium hydroxide as activator. SEM studies revealed multiphasous structure of the material, composed of geopolymeric gel, partially reacted fly ashparticles and selectively leached particles. EDX analysis confirmed the chemical composition of different regions. Infra red spectroscopic studies supported the SEM-EDX analysis by confirming presence of unreacted quartzite and mullite in geopolymers. It is concluded that geopolymers possese a non uniform chemistry through out the structure.

Determination of anisotropy and multimorphology in fly ash based geopolymers

NASA Astrophysics Data System (ADS)

Khan, M. Irfan; Azizli, Khairun; Sufian, Suriati; Man, Zakaria; Siyal, Ahmer Ali; Ullah, Hafeez

2015-07-01

In this study, Malaysian coal fly ash-based geopolymers were investigated for its morphology and chemical composition using scanning electron microscopy coupled with energy dispersive X-rays (SEM-EDX). Geopolymer was synthesized using sodium hydroxide as activator. SEM studies revealed multiphasous structure of the material, composed of geopolymeric gel, partially reacted fly ashparticles and selectively leached particles. EDX analysis confirmed the chemical composition of different regions. Infra red spectroscopic studies supported the SEM-EDX analysis by confirming presence of unreacted quartzite and mullite in geopolymers. It is concluded that geopolymers possese a non uniform chemistry through out the structure.

Structural and mechanical properties of hydroxyapatite coatings formed by ion-beam assisted deposition

NASA Astrophysics Data System (ADS)

Zykova, A.; Safonov, V.; Dudin, S.; Yakovin, S.; Donkov, N.; Ghaemi, M. H.; Szkodo, M.; Antoszkiewicz, M.; Szyfelbain, M.; Czaban, A.

2018-03-01

The ion-beam assisted deposition (IBAD) is an advanced method capable of producing crystalline coatings at low temperatures. We determined the characteristics of hydroxyapatite Ca10(PO4)6(OH)2 target and coatings formed by IBAD using X-ray photoemission spectroscopy (XPS), X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and energy dispersive X-ray (EDX). The composition of the coatings’ cross-section and surface was close to those of the target. The XPS spectra showed that the binding energy values of Ca (2p1/2, 2p3/2), P (2p3/2), and O 1s levels are related to the hydroxyapatite phase. The coatings demonstrate an optimal H/E ratio, and a good resistance to scratch tests.

High-compactness coating grown by plasma electrolytic oxidation on AZ31 magnesium alloy in the solution of silicate-borax

NASA Astrophysics Data System (ADS)

Shen, M. J.; Wang, X. J.; Zhang, M. F.

2012-10-01

A ceramic coating was formed on the surface of AZ31 magnesium alloy by plasma electrolytic oxidation (PEO) in the silicate solution with and without borax doped. The composition, morphology, elements and roughness as well as mechanical property of the coating were investigated by X-ray diffraction (XRD), scanning electron microscope (SEM), energy dispersive X-ray spectrometry (EDS), X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM) and reciprocal-sliding tribometer. The results show that the PEO coating is mainly composed of magnesia. When using borax dope, boron element is permeating into the coating and the boron containing phase exist in the form of amorphous. In addition, the microhardness and compactness of the PEO coating are improved significantly due to doped borax.

Incorporation of Tin on copper clad laminate to increase the interface adhesion for signal loss reduction of high-frequency PCB lamination

NASA Astrophysics Data System (ADS)

Wang, Chong; Wen, Na; Zhou, Guoyun; Wang, Shouxu; He, Wei; Su, Xinhong; Hu, Yongsuan

2017-11-01

A novel method of improving the adhesion between copper and prepreg in high frequency PCB was proposed and studied in this work. This process which aimed to decrease the IEP (isoelectric point) of the copper to obtain higher adhesion, was achieved by depositing a thin tin layer with lower IEP on copper. It was characterized by scanning electron microscopy (SEM), 3D microscope, peel strength test, X-Ray thickness test, grazing incidence X-ray diffraction (GXRD), X-ray photoelectron spectroscopy (XPS), Agilent vector network analyzer (VNA), which confirmed its excellent adhesion performance and outstanding electrical properties in high-frequency signal transmission compared with traditional brown oxide method. Moreover, the mechanism of achieving high adhesion for this method was also investigated.

Unimpeded permeation of water through biocidal graphene oxide sheets anchored on to 3D porous polyolefinic membranes

NASA Astrophysics Data System (ADS)

Mural, Prasanna Kumar S.; Jain, Shubham; Kumar, Sachin; Madras, Giridhar; Bose, Suryasarathi

2016-04-01

3D porous membranes were developed by etching one of the phases (here PEO, polyethylene oxide) from melt-mixed PE/PEO binary blends. Herein, we have systematically discussed the development of these membranes using X-ray micro-computed tomography. The 3D tomograms of the extruded strands and hot-pressed samples revealed a clear picture as to how the morphology develops and coarsens over a function of time during post-processing operations like compression molding. The coarsening of PE/PEO blends was traced using X-ray micro-computed tomography and scanning electron microscopy (SEM) of annealed blends at different times. It is now understood from X-ray micro-computed tomography that by the addition of a compatibilizer (here lightly maleated PE), a stable morphology can be visualized in 3D. In order to anchor biocidal graphene oxide sheets onto these 3D porous membranes, the PE membranes were chemically modified with acid/ethylene diamine treatment to anchor the GO sheets which were further confirmed by Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS) and surface Raman mapping. The transport properties through the membrane clearly reveal unimpeded permeation of water which suggests that anchoring GO on to the membranes does not clog the pores. Antibacterial studies through the direct contact of bacteria with GO anchored PE membranes resulted in 99% of bacterial inactivation. The possible bacterial inactivation through physical disruption of the bacterial cell wall and/or reactive oxygen species (ROS) is discussed herein. Thus this study opens new avenues in designing polyolefin based antibacterial 3D porous membranes for water purification.3D porous membranes were developed by etching one of the phases (here PEO, polyethylene oxide) from melt-mixed PE/PEO binary blends. Herein, we have systematically discussed the development of these membranes using X-ray micro-computed tomography. The 3D tomograms of the extruded strands and hot-pressed samples revealed a clear picture as to how the morphology develops and coarsens over a function of time during post-processing operations like compression molding. The coarsening of PE/PEO blends was traced using X-ray micro-computed tomography and scanning electron microscopy (SEM) of annealed blends at different times. It is now understood from X-ray micro-computed tomography that by the addition of a compatibilizer (here lightly maleated PE), a stable morphology can be visualized in 3D. In order to anchor biocidal graphene oxide sheets onto these 3D porous membranes, the PE membranes were chemically modified with acid/ethylene diamine treatment to anchor the GO sheets which were further confirmed by Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS) and surface Raman mapping. The transport properties through the membrane clearly reveal unimpeded permeation of water which suggests that anchoring GO on to the membranes does not clog the pores. Antibacterial studies through the direct contact of bacteria with GO anchored PE membranes resulted in 99% of bacterial inactivation. The possible bacterial inactivation through physical disruption of the bacterial cell wall and/or reactive oxygen species (ROS) is discussed herein. Thus this study opens new avenues in designing polyolefin based antibacterial 3D porous membranes for water purification. Electronic supplementary information (ESI) available: SEM micrographs of porous PE with and without maleated PE, X-ray micro-computed tomogram of porous extruded PE, FTIR spectra of GO, XPS wide spectra of untreated and GO immobilized PE and Raman spectra of PE and GO. See DOI: 10.1039/c6nr01356b

DOE Office of Scientific and Technical Information (OSTI.GOV)

Singh, Paviter; Kaur, Manpreet; Singh, Bikramjeet

Boron-carbon core shell structures have been synthesized by solvo-thermal synthesis route. The synthesized material is highly pure. X-ray diffraction analysis confirms the reduction of reactants in to boron and carbon. Scanning Electron Microscopy (SEM) analysis showed that the shell is uniform with average thickness of 340 nm. Photo luminescence studies showed that the material is blue light emitting with CIE color coordinates: x=0.16085, y=0.07554.

Zr doping dependence of structural and magnetic properties of cobalt ferrite synthesized by sol-gel based Pechini method

NASA Astrophysics Data System (ADS)

Motavallian, Pourya; Abasht, Behzad; Abdollah-Pour, Hassan

2018-04-01

Nanocrystalline CoZrxFe2-xO4 (0 ≤ x ≤ 0.3 in a step of 0.05) powders were synthesized by Pechini sol-gel method. The dry gel was grinded and calcined at 700 °C in a static air atmosphere for 1 h. Some tests such as thermo gravimetric analysis (TGA) combined with differential analysis (DTA), fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and vibrating sample magnetometer (VSM) were carried out to investigate the thermal behaviour, structural bonds identification, crystallographic properties, morphology and magnetic properties of the obtained powders. X-ray diffraction revealed a single-phase cubic spinel structure for all samples, where the crystallite size decreases; the lattice parameter simultaneously increases with substitution of Zr. The results of FE-SEM showed that the particle size is in the 20-70 nm range. The magnetic properties such as saturation magnetization (Ms), remanent magnetization (Mr) and coercivity (Hc) were measured from the hysteresis loops. The greatest amount of saturation magnetization for CoZr0.05Fe1.95O4 sample was 67.9 emu·g-1.

X-ray diffraction and SEM study of kidney stones in Israel: quantitative analysis, crystallite size determination, and statistical characterization.

PubMed

Uvarov, Vladimir; Popov, Inna; Shapur, Nandakishore; Abdin, Tamer; Gofrit, Ofer N; Pode, Dov; Duvdevani, Mordechai

2011-12-01

Urinary calculi have been recognized as one of the most painful medical disorders. Tenable knowledge of the phase composition of the stones is very important to elucidate an underlying etiology of the stone disease. We report here the results of quantitative X-ray diffraction phase analysis performed on 278 kidney stones from the 275 patients treated at the Department of Urology of Hadassah Hebrew University Hospital (Jerusalem, Israel). Quantification of biominerals in multicomponent samples was performed using the normalized reference intensity ratio method. According to the observed phase compositions, all the tested stones were classified into five chemical groups: oxalates (43.2%), phosphates (7.7%), urates (10.3%), cystines (2.9%), and stones composed of a mixture of different minerals (35.9%). A detailed analysis of each allocated chemical group is presented along with the crystallite size calculations for all the observed crystalline phases. The obtained results have been compared with the published data originated from different geographical regions. Morphology and spatial distribution of the phases identified in the kidney stones were studied with scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS). This type of detailed study of phase composition and structural characteristics of the kidney stones was performed in Israel for the first time.

DOE Office of Scientific and Technical Information (OSTI.GOV)

V Yashchuk; R Conley; E Anderson

Verification of the reliability of metrology data from high quality X-ray optics requires that adequate methods for test and calibration of the instruments be developed. For such verification for optical surface profilometers in the spatial frequency domain, a modulation transfer function (MTF) calibration method based on binary pseudo-random (BPR) gratings and arrays has been suggested [1] and [2] and proven to be an effective calibration method for a number of interferometric microscopes, a phase shifting Fizeau interferometer, and a scatterometer [5]. Here we describe the details of development of binary pseudo-random multilayer (BPRML) test samples suitable for characterization of scanningmore » (SEM) and transmission (TEM) electron microscopes. We discuss the results of TEM measurements with the BPRML test samples fabricated from a WiSi2/Si multilayer coating with pseudo-randomly distributed layers. In particular, we demonstrate that significant information about the metrological reliability of the TEM measurements can be extracted even when the fundamental frequency of the BPRML sample is smaller than the Nyquist frequency of the measurements. The measurements demonstrate a number of problems related to the interpretation of the SEM and TEM data. Note that similar BPRML test samples can be used to characterize X-ray microscopes. Corresponding work with X-ray microscopes is in progress.« less

Small angle X-ray scattering analysis of the effect of cold compaction of Al/MoO3 thermite composites.

PubMed

Hammons, Joshua A; Wang, Wei; Ilavsky, Jan; Pantoya, Michelle L; Weeks, Brandon L; Vaughn, Mark W

2008-01-07

Nanothermites composed of aluminum and molybdenum trioxide (MoO(3)) have a high energy density and are attractive energetic materials. To enhance the surface contact between the spherical Al nanoparticles and the sheet-like MoO(3) particles, the mixture can be cold-pressed into a pelleted composite. However, it was found that the burn rate of the pellets decreased as the density of the pellets increased, contrary to expectation. Ultra-small angle X-ray scattering (USAXS) data and scanning electron microscopy (SEM) were used to elucidate the internal structure of the Al nanoparticles, and nanoparticle aggregate in the composite. Results from both SEM imaging and USAXS analysis indicate that as the density of the pellet increased, a fraction of the Al nanoparticles are compressed into sintered aggregates. The sintered Al nanoparticles lost contrast after forming the larger aggregates and no longer scattered X-rays as individual particles. The sintered aggregates hinder the burn rate, since the Al nanoparticles that make them up can no longer diffuse freely as individual particles during combustion. Results suggest a qualitative relationship for the probability that nanoparticles will sinter, based on the particle sizes and the initial structure of their respective agglomerates, as characterized by the mass fractal dimension.

Microstructural characterization of Ti-6Al-4V alloy subjected to the duplex SMAT/plasma nitriding.

PubMed

Pi, Y; Faure, J; Agoda-Tandjawa, G; Andreazza, C; Potiron, S; Levesque, A; Demangel, C; Retraint, D; Benhayoune, H

2013-09-01

In this study, microstructural characterization of Ti-6Al-4V alloy, subjected to the duplex surface mechanical attrition treatment (SMAT)/nitriding treatment, leading to improve its mechanical properties, was carried out through novel and original samples preparation methods. Instead of acid etching which is limited for morphological characterization by scanning electron microscopy (SEM), an original ion polishing method was developed. Moreover, for structural characterization by transmission electron microscopy (TEM), an ion milling method based with the use of two ions guns was also carried out for cross-section preparation. To demonstrate the efficiency of the two developed methods, morphological investigations were done by traditional SEM and field emission gun SEM. This was followed by structural investigations through selected area electron diffraction (SAED) coupled with TEM and X-ray diffraction techniques. The results demonstrated that ionic polishing allowed to reveal a variation of the microstructure according to the surface treatment that could not be observed by acid etching preparation. TEM associated to SAED and X-ray diffraction provided information regarding the nanostructure compositional changes induced by the duplex SMAT/nitriding process. Copyright © 2013 Wiley Periodicals, Inc.

Scanning electron microscopy-energy dispersive X-ray spectrometry (SEM-EDX) and aerosol time-of-flight mass spectrometry (ATOFMS) single particle analysis of metallurgy plant emissions.

PubMed

Arndt, J; Deboudt, K; Anderson, A; Blondel, A; Eliet, S; Flament, P; Fourmentin, M; Healy, R M; Savary, V; Setyan, A; Wenger, J C

2016-03-01

The chemical composition of single particles deposited on industrial filters located in three different chimneys of an iron-manganese (Fe-Mn) alloy manufacturing plant have been compared using aerosol time-of-flight mass spectrometry (ATOFMS) and scanning electron microscopy-energy dispersive X-ray spectrometry (SEM-EDX). Very similar types of particles were observed using both analytical techniques. Calcium-containing particles dominated in the firing area of the sintering unit, Mn and/or Al-bearing particles were observed at the cooling area of the sintering unit, while Mn-containing particles were dominant at the smelting unit. SEM-EDX analysis of particles collected downstream of the industrial filters showed that the composition of the particles emitted from the chimneys is very similar to those collected on the filters. ATOFMS analysis of ore samples was also performed to identify particulate emissions that could be generated by wind erosion and manual activities. Specific particle types have been identified for each emission source (chimneys and ore piles) and can be used as tracers for source apportionment of ambient PM measured in the vicinity of the industrial site. Copyright © 2015 Elsevier Ltd. All rights reserved.

Reduced graphene oxide-induced recrystallization of NiS nanorods to nanosheets and the improved Na-storage properties.

PubMed

Pan, Qin; Xie, Jian; Zhu, Tiejun; Cao, Gaoshao; Zhao, Xinbing; Zhang, Shichao

2014-04-07

Preparation of two-dimensional (2D) graphene-like materials is currently an emerging field in materials science since the discovery of single-atom-thick graphene prepared by mechanical cleavage. In this work, we proposed a new method to prepare 2D NiS, where reduced graphene oxide (rGO) was found to induce the recrystallization of NiS from nanorods to nanosheets in a hydrothermal process. The process and mechanism of recrystallization have been clarified by various characterization techniques, including scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS) mapping, and X-ray photoelectron spectroscopy (XPS). The characterization of ex situ NiS/rGO products by SEM and EDS mapping indicates that the recrystallization of NiS from nanorods to nanosheets is realized actually through an exfoliation process, while the characterization of in situ NiS/rGO products by SEM, TEM, and EDS mapping reveals the exfoliation process. The XPS result demonstrates that hydrothermally assisted chemical bonding occurs between NiS and rGO, which induces the exfoliation of NiS nanorods into nanosheets. The obtained NiS/rGO composite shows promising Na-storage properties.

Structural and dielectric properties of Zn1-xAlxO nanoparticles

NASA Astrophysics Data System (ADS)

Giri, N.; Mondal, A.; Sarkar, S.; Ray, R.

2018-05-01

Aluminium doped ZnO (AZO) nano-crystalline sample has been synthesized using chemical precipitation method with different doping concentrations. Detailed structural and morphological investigations of Zn1-xAlxO have been carried out using X-ray diffraction (XRD) and FE-SEM, respectively. Dependence of grain size of AZO with dopant concentration has been studied. Ac conductivity, dielectric constant and dielectric loss of Zn1-xAlxO (0 ≤ x ≤ 0.1) are investigated as a function of frequency (ω) and doping concentration (x) at room temperature.

Synthesis and characterization of spinel type high-power cathode materials Li MxMn2-x O4 (M=Ni, Co, Cr)

NASA Astrophysics Data System (ADS)

Yoon, Y. K.; Park, C. W.; Ahn, H. Y.; Kim, D. H.; Lee, Y. S.; Kim, J.

2007-05-01

The transition metal-doped spinel cathode materials, LiM0.5Mn1.5O4 (M=Ni. Co, Cr) were prepared by solid-state reaction. The structure and morphology of the samples were investigated by X-ray diffraction, Rietveld refinement and scanning electron microscopy (SEM). The diffraction peaks of all the samples corresponded to a single phase of cubic spinel structure with a space group Fd3m. Field-emission SEM shows octahedron like shapes and the primary particles size was between 500 nm and 2 μm. Oxidation states of Ni, Co and Cr were found to be 2+, 2+ and 3+ as revealed by X-ray photoelectron spectroscopy. During discharging, LiNi0.5Mn1.5O4 and LiCo0.5Mn1.5O4 sample shows more than 130 mAh/g between 3.5 and 5.2 V at a current density of 0.65 mA/cm2 and well developed plateau around 5 V, respectively.

Stress-induced microcrack density evolution in β-eucryptite ceramics: Experimental observations and possible route to strain hardening

DOE PAGES

Müller, B. R.; Cooper, R. C.; Lange, A.; ...

2017-11-01

In order to investigate their microcracking behaviour, the microstructures of several β-eucryptite ceramics, obtained from glass precursor and cerammed to yield different grain sizes and microcrack densities, were characterized by laboratory and synchrotron x-ray refraction and tomography. Here, results were compared with those obtained from scanning electron microscopy (SEM). In SEM images, the characterized materials appeared fully dense but computed tomography showed the presence of pore clusters. Uniaxial tensile testing was performed on specimens while strain maps were recorded and analyzed by Digital Image Correlation (DIC). X-ray refraction techniques were applied on specimens before and after tensile testing to measuremore » the amount of the internal specific surface (i.e., area per unit volume). X-ray refraction revealed that (a) the small grain size (SGS) material contained a large specific surface, originating from the grain boundaries and the interfaces of TiO 2 precipitates; (b) the medium (MGS) and large grain size (LGS) materials possessed higher amounts of specific surface compared to SGS material due to microcracks, which decreased after tensile loading; (c) the precursor glass had negligible internal surface. The unexpected decrease in the internal surface of MGS and LGS after tensile testing is explained by the presence of compressive regions in the DIC strain maps and further by theoretical arguments. It is suggested that while some microcracks merge via propagation, more close mechanically, thereby explaining the observed X-ray refraction results. Lastly, the mechanisms proposed would allow the development of a strain hardening route in ceramics.« less

Structural, magnetic and electronic structure properties of Co doped ZnO nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Shalendra, E-mail: shailuphy@gmail.com; School of Materials Science and Engineering, Changwon National University, Changwon, Gyeongnam 641-773; Song, T.K., E-mail: tksong@changwon.ac.kr

Highlights: • XRD and HR-TEM results show the single phase nature of Co doped ZnO nanoparticles. • XMCD and dc magnetization results indicate the RT-FM in Co doped ZnO nanoparticles. • Co L{sub 3,2} NEXAFS spectra infer that Co ions are in 2+ valence state. • O K edge NEXAFS spectra show that O vacancy increases with Co doping in ZnO. - Abstract: We reported structural, magnetic and electronic structure studies of Co doped ZnO nanoparticles. Doping of Co ions in ZnO host matrix has been studied and confirmed using various methods; such as X-ray diffraction (XRD), field emission scanningmore » electron microscopy (FE-SEM), energy dispersed X-ray (EDX), high resolution transmission electron microscopy (HR-TEM), Fourier transform infrared spectroscopy (FT-IR), near edge X-ray absorption fine structure (NEXAFS) spectroscopy, magnetic hysteresis loop measurements and X-ray magnetic circular dichroism (XMCD). From the XRD and HR-TEM results, it is observed that Co doped ZnO nanoparticles have single phase nature with wurtzite structure and exclude the possibility of secondary phase formation. FE-SEM and TEM micrographs show that pure and Co doped nanoparticles are nearly spherical in shape. O K edge NEXAFS spectra indicate that O vacancies increase with Co doping. The Co L{sub 3,2} edge NEXAFS spectra revealed that Co ions are in 2+ valence state. DC magnetization hysteresis loops and XMCD results clearly showed the intrinsic origin of temperature ferromagnetism in Co doped ZnO nanoparticles.« less

Stress-induced microcrack density evolution in β-eucryptite ceramics: Experimental observations and possible route to strain hardening

DOE Office of Scientific and Technical Information (OSTI.GOV)

Müller, B. R.; Cooper, R. C.; Lange, A.

In order to investigate their microcracking behaviour, the microstructures of several β-eucryptite ceramics, obtained from glass precursor and cerammed to yield different grain sizes and microcrack densities, were characterized by laboratory and synchrotron x-ray refraction and tomography. Here, results were compared with those obtained from scanning electron microscopy (SEM). In SEM images, the characterized materials appeared fully dense but computed tomography showed the presence of pore clusters. Uniaxial tensile testing was performed on specimens while strain maps were recorded and analyzed by Digital Image Correlation (DIC). X-ray refraction techniques were applied on specimens before and after tensile testing to measuremore » the amount of the internal specific surface (i.e., area per unit volume). X-ray refraction revealed that (a) the small grain size (SGS) material contained a large specific surface, originating from the grain boundaries and the interfaces of TiO 2 precipitates; (b) the medium (MGS) and large grain size (LGS) materials possessed higher amounts of specific surface compared to SGS material due to microcracks, which decreased after tensile loading; (c) the precursor glass had negligible internal surface. The unexpected decrease in the internal surface of MGS and LGS after tensile testing is explained by the presence of compressive regions in the DIC strain maps and further by theoretical arguments. It is suggested that while some microcracks merge via propagation, more close mechanically, thereby explaining the observed X-ray refraction results. Lastly, the mechanisms proposed would allow the development of a strain hardening route in ceramics.« less

Covalently Bonded Three-Dimensional Carbon Nanotube Solids via Boron Induced Nanojunctions

DTIC Science & Technology

2012-04-13

Novel Carbon Morphologies: From Covalent Y-Junctions to Sea - Urchin -Like Structures. Adv. Func. Mater. 19, 1193–1199 (2009). 15. Sumpter, B. G. et al...amorphous carbon as depicted from SEM (Fig. 1c). The X-ray powder diffraction pattern shows that as-produced CBXMWNT sponges are indeed crystalline and...material as-produced; (b) shows photograph of the flexibility and mechanical stablility upon bending the sample (a) by hand; (c) SEM image after ion

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vilches, J.; Lopez, A.; Martinez, M.C.

This paper discusses the value of scanning electron microscopy (SEM) and x-ray microanalysis in the classification of craniopharyngiomas. This neoplasm shows epithelial nest, cords of cuboid cells, foci of squamous metaplasia, and microcystic degeneration. SEM reveals that the epithelial cysts are lined with elongated cells that possess numerous microvilli and blebs and that some cysts are lined with polyhedral cells. The microvilli are interpreted as characteristic of the fast growing craniopharyngiomas. A microanalytical study of the calcified areas reveals the presence of magnesium, phosphorus, and calcium.

Mineralogical Characterization of Hispano-Moresque Glazes: A µ-Raman and Scanning Electron Microscopy with X-Ray Energy Dispersive Spectrometry (SEM-EDS) Study.

PubMed

Coentro, Susana; da Silva, Rui C; Relvas, Cátia; Ferreira, Teresa; Mirão, José; Pleguezuelo, Alfonso; Trindade, Rui; Muralha, Vânia S F

2018-06-05

This work explores the combination of µ-Raman spectroscopy and scanning electron microscopy with X-ray energy dispersive spectrometry (SEM-EDS) for the study of the glazes in 15th-16th century Hispano-Moresque architectural tiles. These are high lead glazes that can be tin-opacified or transparent, and present five colors: tin-white, cobalt-blue, copper-green, iron-amber, and manganese-brown. They are generally homogenous and mineral inclusions are mostly concentrated in the glaze-ceramic interface. Through SEM-EDS, these inclusions were observed and chemically analyzed, whereas µ-Raman allowed their identification on a molecular level. K-feldspars, wollastonite and diopside were the most common compounds, as well as cassiterite agglomerates that render the glaze opaque. Malayaite was identified in green glazes, and andradite and magnesioferrite in amber glazes. Co-Ni-ferrites were identified in blue glazes, as well as Ni-Fe-olivines. Manganese-brown is the color where most compounds were identified: bustamite, jacobsite, hausmannite, braunite, and kentrolite. Through the µ-Raman analysis of different areas in large inclusions previously observed by SEM, it was possible to identify intermediate phases that illustrate the reaction process that occurs between the color-conferring compounds and the surrounding lead glaze. Furthermore, the obtained results allowed inference of the raw materials and firing temperatures used on the manufacture of these tiles.

SEM (Symmetry Equivalent Molecules): a web-based GUI to generate and visualize the macromolecules

PubMed Central

Hussain, A. S. Z.; Kumar, Ch. Kiran; Rajesh, C. K.; Sheik, S. S.; Sekar, K.

2003-01-01

SEM, Symmetry Equivalent Molecules, is a web-based graphical user interface to generate and visualize the symmetry equivalent molecules (proteins and nucleic acids). In addition, the program allows the users to save the three-dimensional atomic coordinates of the symmetry equivalent molecules in the local machine. The widely recognized graphics program RasMol has been deployed to visualize the reference (input atomic coordinates) and the symmetry equivalent molecules. This program is written using CGI/Perl scripts and has been interfaced with all the three-dimensional structures (solved using X-ray crystallography) available in the Protein Data Bank. The program, SEM, can be accessed over the World Wide Web interface at http://dicsoft2.physics.iisc.ernet.in/sem/ or http://144.16.71.11/sem/. PMID:12824326

Hot corrosion behavior of YSZ, Gd2Zr2O7 and YSZ/Gd2Zr2O7 thermal barrier coatings exposed to molten sulfate and vanadate salt

NASA Astrophysics Data System (ADS)

Ozgurluk, Yasin; Doleker, Kadir Mert; Karaoglanli, Abdullah Cahit

2018-04-01

Thermal barrier coatings (TBCs) are mostly used in critical components of aircraft gas turbine engines. Hot corrosion is among the main deteriorating factors in TBCs which results from the effect of molten salt on the coating-gas interface. This type of corrosion is observed as a result of contamination accumulated during combustion processes. Fuels used in aviation industry generally contain impurities such as vanadium oxide (V2O5) and sodium sulfate (Na2SO4). These impurities damage turbines' inlet at elevated temperatures because of chemical reaction. Yttria stabilized zirconia (YSZ) is a conventional top coating material for TBCs while Gd2Zr2O7 is a new promising top coating material for TBCs. In this study, CoNiCrAlY metallic bond coat was deposited on Inconel 718 nickel based superalloy substrate material with a thickness about 100 μm using cold gas dynamic spray (CGDS) method. Production of TBCs were done with deposition of YSZ, Gd2Zr2O7, YSZ/Gd2Zr2O7 ceramic top coating materials using EB-PVD method, having a total thickness of 300 μm. Hot corrosion behavior of YSZ, Gd2Zr2O7, YSZ/Gd2Zr2O7 TBC systems were exposed to 45 wt.% Na2SO4 and 55 wt.% V2O5 molten salt mixtures at 1000 °C temperature. TBC samples were investigated and compared using scanning electron microscope (SEM), energy dispersive spectroscopy (EDS) analysis and X-ray diffractometer (XRD). The hot corrosion failure mechanisms of YSZ, Gd2Zr2O7 and YSZ/Gd2Zr2O7 TBCs in the molten salts were evaluated.

Optical properties of MgF2 nano-composite films dispersed with noble metal nanoparticles synthesized by sol-gel method

NASA Astrophysics Data System (ADS)

Wakaki, Moriaki; Soujima, Nobuaki; Shibuya, Takehisa

2015-03-01

Porous MgF2 films synthesized by a sol-gel method exhibit the lowest refractive index among the dielectric optical materials and are the most useful materials for the anti-reflection coatings. On the other hand, surface plasmon resonance (SPR) absorptions of noble metal nanoparticles in various solid matrices have been extensively studied. New functional materials like a SERS (Surface Enhanced Raman Spectroscopy) tips are expected by synthesizing composite materials between porous MgF2 films featured by the network of MgF2 nanoparticles and noble metal nanoparticles introduced within the network. In this study, fundamental physical properties including morphology and optical properties are characterized for these materials to make clear the potential of the composite system. Composite materials of MgF2 films dispersed with noble metal (Ag, Au) nanoparticles were prepared using the sol-gel technique with various annealing temperatures and densities of noble metal nanoparticles. The structural morphology was analyzed by an X-ray diffractometer (XRD) and a scanning electron microscope (SEM). The size and shape distributions of the metal nanoparticles were observed using a transmission electron microscope (TEM). The optical properties of fabricated composite films were characterized by UV-Vis-NIR and FT-IR spectrophotometers. The absorption spectra due to the surface plasmon resonance (SPR) of the metal nanoparticles were analyzed using the dielectric function considering the effective medium approximation, typically Maxwell-Garnett model. The Raman scattering spectra were also studied to check the enhancement effect of specimen dropped on the MgF2: Ag nano-composite films deposited on Si substrate. Enhancement of the Raman intensity of pyridine solution specimen was observed.

Effect of calcium hydroxide on mechanical strength and biological properties of bioactive glass.

PubMed

Shah, Asma Tufail; Batool, Madeeha; Chaudhry, Aqif Anwar; Iqbal, Farasat; Javaid, Ayesha; Zahid, Saba; Ilyas, Kanwal; Bin Qasim, Saad; Khan, Ather Farooq; Khan, Abdul Samad; Ur Rehman, Ihtesham

2016-08-01

In this manuscript for the first time calcium hydroxide (Ca(OH)2) has been used for preparation of bioactive glass (BG-2) by co-precipitation method and compared with glass prepared using calcium nitrate tetrahydrate Ca(NO3)2·4H2O (BG-1), which is a conventional source of calcium. The new source positively affected physical, biological and mechanical properties of BG-2. The glasses were characterized by Fourier transform infrared (FTIR), X-Ray Diffractometer (XRD), Scanning Electron Microscopy (SEM), Thermogravimetric Analysis/Differential Scanning Calorimetry (TGA-DSC), BET surface area analysis and Knoop hardness. The results showed that BG-2 possessed relatively larger surface properties (100m(2)g(-1) surface area) as compared to BG-1 (78m(2)g(-1)), spherical morphology and crystalline phases (wollastonite and apatite) after sintering at lower than conventional temperature. These properties contribute critical role in both mechanical and biological properties of glasses. The Knoop hardness measurements revealed that BG-2 possessed much better hardness (0.43±0.06GPa at 680°C and 2.16±0.46GPa at 980°C) than BG-1 (0.24±0.01 at 680°C and 0.57±0.07GPA at 980°C) under same conditions. Alamar blue Assay and confocal microscopy revealed that BG-2 exhibited better attachment and proliferation of MG63 cells. Based on the improved biological properties of BG-2 as a consequent of novel calcium source selection, BG-2 is proposed as a bioactive ceramic for hard tissue repair and regeneration applications. Copyright © 2016 Elsevier Ltd. All rights reserved.

A novel sol-gel-derived calcium silicate cement with short setting time for application in endodontic repair of perforations

PubMed Central

Lee, Bor-Shiunn; Lin, Hong-Ping; Chan, Jerry Chun-Chung; Wang, Wei-Chuan; Hung, Ping-Hsuan; Tsai, Yu-Hsin; Lee, Yuan-Ling

2018-01-01

Mineral trioxide aggregate (MTA) is the most frequently used repair material in endodontics, but the long setting time and reduced mechanical strength in acidic environments are major shortcomings. In this study, a novel sol-gel-derived calcium silicate cement (sCSC) was developed using an initial Ca/Si molar ratio of 3, with the most effective mixing orders of reactants and optimal HNO3 catalyst volumes. A Fourier transform infrared spectrometer, scanning electron microscope with energy-dispersive X-ray spectroscopy, and X-ray powder diffractometer were used for material characterization. The setting time, compressive strength, and microhardness of sCSC after hydration in neutral and pH 5 environments were compared with that of MTA. Results showed that sCSC demonstrated porous microstructures with a setting time of ~30 min, and the major components of sCSC were tricalcium silicate, dicalcium silicate, and calcium oxide. The optimal formula of sCSC was sn200, which exhibited significantly higher compressive strength and microhardness than MTA, irrespective of neutral or pH 5 environments. In addition, both sn200 and MTA demonstrated good biocompatibility because cell viability was similar to that of the control. These findings suggest that sn200 merits further clinical study for potential application in endodontic repair of perforations. PMID:29386894

A novel sol-gel-derived calcium silicate cement with short setting time for application in endodontic repair of perforations.

PubMed

Lee, Bor-Shiunn; Lin, Hong-Ping; Chan, Jerry Chun-Chung; Wang, Wei-Chuan; Hung, Ping-Hsuan; Tsai, Yu-Hsin; Lee, Yuan-Ling

2018-01-01

Mineral trioxide aggregate (MTA) is the most frequently used repair material in endodontics, but the long setting time and reduced mechanical strength in acidic environments are major shortcomings. In this study, a novel sol-gel-derived calcium silicate cement (sCSC) was developed using an initial Ca/Si molar ratio of 3, with the most effective mixing orders of reactants and optimal HNO 3 catalyst volumes. A Fourier transform infrared spectrometer, scanning electron microscope with energy-dispersive X-ray spectroscopy, and X-ray powder diffractometer were used for material characterization. The setting time, compressive strength, and microhardness of sCSC after hydration in neutral and pH 5 environments were compared with that of MTA. Results showed that sCSC demonstrated porous microstructures with a setting time of ~30 min, and the major components of sCSC were tricalcium silicate, dicalcium silicate, and calcium oxide. The optimal formula of sCSC was sn200, which exhibited significantly higher compressive strength and microhardness than MTA, irrespective of neutral or pH 5 environments. In addition, both sn200 and MTA demonstrated good biocompatibility because cell viability was similar to that of the control. These findings suggest that sn200 merits further clinical study for potential application in endodontic repair of perforations.

Grain Refinement by Authigenic Inoculation Inherited from the Medium-Range Order Structure of Ni-Cr-W Superalloy

NASA Astrophysics Data System (ADS)

Gao, Zhongtang; Hu, Rui; Guo, Wei; Zhang, Chuanwei

2018-04-01

The combination of liquidus casting and thermal control solidification furnace was applied to obtain a fine-grained ingot. A rapid quenching method and x-ray diffraction measurement were used to investigate the effect of authigenic inoculation on grain refinement. The structure factor S(Q) of liquid Ni-Cr-W superalloy at 1400 °C (Liquidus temperature) and bright-field image of the microstructures quenched from 1400 °C have been measured by the high-temperature x-ray diffractometer and the transmission electron microscopy (TEM), respectively. The results show that a pre-peak exists on a S(Q) curve at the liquidus temperature. The clusters of atom in rapidly quenched microstructures obtained by isothermal heat treatment at 1400 °C were studied using TEM. Meanwhile, the effect of isothermal different temperatures on rapidly quenched microstructures was studied. The results also show that there are only the globular, equiaxed grains distributed in the solidification structure. These particles are inherited from the medium-range order structure, which is beneficial for grain refinement. The normalized work-hardening rate-strain curve indicates the work-hardening rate of fine grain is higher than that of conventional grain at the same temperature and the same deformation.

Grain Refinement by Authigenic Inoculation Inherited from the Medium-Range Order Structure of Ni-Cr-W Superalloy

NASA Astrophysics Data System (ADS)

Gao, Zhongtang; Hu, Rui; Guo, Wei; Zhang, Chuanwei

2018-05-01

The combination of liquidus casting and thermal control solidification furnace was applied to obtain a fine-grained ingot. A rapid quenching method and x-ray diffraction measurement were used to investigate the effect of authigenic inoculation on grain refinement. The structure factor S( Q) of liquid Ni -Cr-W superalloy at 1400 °C (Liquidus temperature) and bright-field image of the microstructures quenched from 1400 °C have been measured by the high-temperature x-ray diffractometer and the transmission electron microscopy (TEM), respectively. The results show that a pre-peak exists on a S( Q) curve at the liquidus temperature. The clusters of atom in rapidly quenched microstructures obtained by isothermal heat treatment at 1400 °C were studied using TEM. Meanwhile, the effect of isothermal different temperatures on rapidly quenched microstructures was studied. The results also show that there are only the globular, equiaxed grains distributed in the solidification structure. These particles are inherited from the medium-range order structure, which is beneficial for grain refinement. The normalized work-hardening rate-strain curve indicates the work-hardening rate of fine grain is higher than that of conventional grain at the same temperature and the same deformation.

Properties of CoO doped in Glasses Prepared from Rice Hush Fly Ash in Thailand

NASA Astrophysics Data System (ADS)

Ruangtaweep, Y.; Kaewkhao, J.; Kirdsiri, K.; Kedkaew, C.; Limsuwan, P.

2011-10-01

In this work, properties of glass from local rice husk ash (RHA) in Thailand have been investigated. RHA was sintered in different temperature. Compositions and phases of RHA were analyzed by energy dispersive x-ray fluorescence spectrometer (EDXRF) and X-ray diffractometer (XRD). The glasses were melt from RHA in formula 20 Na2O : 1.0 Al2O3 : 13 B2O3 : 6.3 CaO : 0.2 Sb2O3 : 4.5 BaO : 55SiO2 (using RHA as a SiO2 source) The density values of all RHA glasses are comparable and larger than glass from pure SiO2 under same glass formula and preparing condition. These results are corresponding with refractive index values. The RHA glasses showing colorless with absorption edge in ultraviolet region were obtained. The dark blue color glasses were melted from RHA with different CoO concentration. From this part, not found to be the relation of density and refractive index of glass with CoO concentration in glass matrix. From absorption spectra, the absorption peak were appeared around 600 nm, and peak intensity are increased, with increase CoO, correspond to 4A2(4F) → 4T1(4P) state of Co2+ in tetrahedral symmetry.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Voßwinkel, Daniel; Heletta, Lukas; Hoffmann, Rolf-Dieter

The YIrGe{sub 2} type ternary germanides RERhGe{sub 2} (RE = Y, Gd-Ho) were synthesized from the elements by arc-melting and characterized by powder X-ray diffraction. The structure of DyRhGe{sub 2} was refined from single crystal X-ray diffractometer data: Immm, a = 426.49(9), b = 885.0(2), c = 1577.4(3) pm, wR2 = 0.0533, 637 F{sup 2} values, 30 variables (300 K data). The structure contains two crystallographically independent dysprosium atoms in pentagonal prismatic and hexagonal prismatic coordination. The three-dimensional [RhGe{sub 2}] polyanion is stabilized through covalent Rh–Ge (243–261 pm) and Ge–Ge (245–251 pm) bonding. The close structural relationship with the slightlymore » rhodium-poorer germanides RE{sub 5}Rh{sub 4}Ge{sub 10} (≡ RERh{sub 0.8}Ge{sub 2}) is discussed. Temperature-dependent magnetic susceptibility measurements reveal Pauli paramagnetism for YRhGe{sub 2} and Curie-Weiss paramagnetism for RERhGe{sub 2} with RE = Gd, Tb, Dy and Ho. These germanides order antiferromagnetically at T{sub N} = 7.2(5), 10.6(5), 8.1(5), and 6.4(5) K, respectively. - Graphical abstract: The germanides RERhGe{sub 2} (RE = Y, Gd-Ho) are new representatives of the YIrGe{sub 2} type.« less

Growth and characterization of novel organic 3-Hydroxy Benzaldehyde-N-methyl 4 Stilbazolium Tosylate crystals for NLO applications.

PubMed

Jagannathan, K; Umarani, P; Ratchagar, V; Ramesh, V; Kalainathan, S

2016-01-15

The 3-Hydroxy Benzaldehyde-N-methyl 4-Stilbazolium Tosylate (3- HBST) is a new organic NLO crystal and it is a new derivative in stilbazolium tosylate family. In this work we have synthesized 3-HBST and the single crystal was grown by conventional slow cooling method. The structure and lattice parameters of the grown crystal were determined by the single crystal X-ray diffraction (XRD) technique and it is exhibiting good crystalline nature which is observed from the powder XRD. In order to check the crystalline quality the rocking curve was recorded using multi crystal X-ray diffractometer. The functional groups were identified from both FTIR and NMR spectral analyses. The π-π* and n-π* optical transition energy levels were estimated from the absorption peaks. The NLO property was confirmed by measuring relative SHG efficiency by Kurtz powder test; it shows 24 times higher SHG efficiency than that of urea. In order to test the mechanical stability the Vickers and Knoop micro hardness measurement were carried out and found that the micro hardness number decreases with increasing load. The melting point was determined from Differential Scanning Colorimetry (DSC). Copyright © 2015 Elsevier B.V. All rights reserved.

Stereostructure of a norbornane diexo-condensed 1,3-oxazine[2,3-a]isoindolone An X-ray study

NASA Astrophysics Data System (ADS)

Argay, Gy.; Kálmán, A.; Stájer, G.; Bernáth, G.

1994-12-01

The structure of 3,6-methano-12b-p-tolyl-2a,3,4,5,6,6a,7,12b-octahydro-2H-3,1-benzoxazino[2,3-a]isoindol-8-one (C23H23NO2, Mr = 345.42), prepared from 2-p-toluoylbenzoic acid and diexo-3-hydroxymethylbicyclo[2.2.1]heptyl-2-amine, has been established by X-ray crystallography from diffractometer data: it crystallizes in the triclinic space group Poverline1 with a = 8.186(2) Å, b = 8.683(2) Å, c = 13.324(5) Å, α = 83.46(4)°, β = 75.48(6)°, γ = 77.60(4)°, V = 893.6(4) Å3, Z = 2, Dc = 1.284 g cm-3 and μ(Cu Kα) = 0.641 mm-1. The structure was solved by direct methods and refined to R = 0.061 for 3685 observed reflections. The molecule exhibits diexo-annelation between the 1,3-oxazine ring and the norbornane moiety. The p-tolyl group and norbonane annelation hydrogens are trans and the 1,3-oxazine ring is fused to an almost planar γ-lactam ring. Consequently, the six-membered hetero ring assumes an irregular conformation among the canonical forms 1S6, 1T3 and B3,6.

Berberine and zinc oxide-based nanoparticles for the chemo-photothermal therapy of lung adenocarcinoma.

PubMed

Kim, Sungyun; Lee, Song Yi; Cho, Hyun-Jong

2018-05-16

Organic/inorganic hydrid nanoparticles (NPs) composed of berberine (BER) and zinc oxide (ZnO) were developed for the therapy of lung cancers. Without the use of pharmaceutical excipients, NPs were fabricated with only dual anticancer agents (BER and ZnO) by facile blending method. The mean weight ratio between BER and ZnO in BER-ZnO NPs was 39:61 in this study. BER-ZnO NPs dispersed in water exhibited 200-300 nm hydrodynamic size under 5 mg/mL concentration. The exposure of both BER and ZnO in the outer layers of BER-ZnO NPs was identified by X-ray photoelectron spectroscopy analysis. The amorphization of BER and the maintenance of ZnO structure were observed in the results of X-ray powder diffractometer analysis. Improved antiproliferation efficacy, based on the chemo-photothermal therapeutic efficacy, of BER-ZnO NPs in A549 (human lung adenocarcinoma) cells was presented. According to the blood tests in rats after intravenous administration, BER-ZnO NPs did not induce severe hepatotoxicity, renal toxicity, and hemotoxicity. Developed BER-ZnO NPs can be used efficiently and safely for the chemo-photothermal therapy of lung cancers. Copyright © 2018 Elsevier Inc. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Broadbridge, Christine C.

DOE grant used for partial fulfillment of necessary laboratory equipment for course enrichment and new graduate programs in nanotechnology at the four institutions of the Connecticut State University System (CSUS). Equipment in this initial phase included variable pressure scanning electron microscope with energy dispersive x-ray spectroscopy elemental analysis capability [at Southern Connecticut State University]; power x-ray diffractometer [at Central Connecticut State University]; a spectrophotometer and spectrofluorimeter [at Eastern Connecticut State University; and a Raman Spectrometer [at Western Connecticut State University]. DOE's funding was allocated for purchase and installation of this scientific equipment and instrumentation. Subsequently, DOE funding was allocated tomore » fund the curriculum, faculty development and travel necessary to continue development and implementation of the System's Graduate Certificate in Nanotechnology (GCNT) program and the ConnSCU Nanotechnology Center (ConnSCU-NC) at Southern Connecticut State University. All of the established outcomes have been successfully achieved. The courses and structure of the GCNT program have been determined and the program will be completely implemented in the fall of 2013. The instrumentation has been purchased, installed and has been utilized at each campus for the implementation of the nanotechnology courses, CSUS GCNT and the ConnSCU-NC. Additional outcomes for this grant include curriculum development for non-majors as well as faculty and student research.« less

Crystal growth and properties of Ag 7_ xTaSe 6_ xI x (0 x 1)

NASA Astrophysics Data System (ADS)

Wada, H.; Sato, A.

1993-03-01

National Institute for Research in Inorganic Materials, Namiki 1-1, Tsukuba, Ibaraki 305, Japan A series of argyrodite compounds with the formula Ag7 xTaSe6 xIx (0 x 1) have been prepared for the first time by a sealed silica tube method. Single crystals have been obtained by heating at 800°C for 2 weeks. Their morphology and crystal structure have been studied by reflected-light microscopy, SEM, EDAX and X-ray diffraction. The silver ionic conductivities of the samples have been also measured.

Phosphate Remediation and Recovery using Iron Oxide-based Adsorbents

EPA Science Inventory

E33-modified sorbents for the removal of phosphate from lake water was investigated in this study. E33-modified sorbents were synthesized by coating with manganese and nanoparticles. Characterization was done by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-...

WEATHERING DEGRADATION OF A POLYURETHANE COATING. (R828081E01)

EPA Science Inventory

The degradation of polyurethane topcoat over a chromate pigmented epoxy primer was examined by atomic force microscopy (AFM), scanning electronic microscopy (SEM), X-ray photo-electron spectroscopy (XPS) and Fourier transform infra-red spectroscopy (FTIR) after the coated pane...

Synthesis of BaTiO3 and Ba(ZrxTi1-X)O3 by using the soft combustion method

NASA Astrophysics Data System (ADS)

Ahmad, Atiqah; Razak, Khairunisak Abdul

2017-07-01

In this work, barium titanate, BaTiO3 (BT) and Zr doped BT, BaZrxTi1-xO3 (BZT) with powders were successfully produced using the soft combustion method. Barium nitrate and titanium (IV) isopropoxide were used as the starting materials while zirconium (IV) oxynitrate hydrate as the doping precursors, and glycine as the combustion agent. The produced powders were pressed into 12 mm diameter pellets by using 150 MPa cold press. The effect of Zr dopant in BT was studied with molar ratio of x = 0.00, 0.03, 0.05, 0.08 and 0.10. The phase presence was identified using X-ray diffractometer. Morphology of powders and sintered pellets was observed using a scanning electron microscope. Density of the sintered pellets was measured by using Archimedes' principle, while dielectric properties were analysed by using an LCR meter. Pure perovskite BT and BZT structure were obtained after sintering at 1400 °C for 5 h. BZT with x = 0.03 has grain size of 3.9 µm and shows the highest dielectric constant of 525, compared to undoped BT that has the average grain size of 4.2 µm with dielectric constant 223. The results is in agreement with microstructure observation and density of the sample.

Effect of annealing temperature on physical properties of solution processed nickel oxide thin films

NASA Astrophysics Data System (ADS)

Sahoo, Pooja; Thangavel, R.

2018-05-01

In this report, NiO thin films were prepared at different annealing temperatures from nickel acetate precursor by sol-gel spin coating method. These films were characterized by different analytical techniques to obtain their structural, optical morphological and electrical properties using X-ray diffractometer (XRD), Field emission scanning electron microscopy (FESEM), UV-Vis NIR double beam spectrophotometer and Keithley 2450 source meter respectively. FESEM images clearly indicates the formation of a homogenous and porous films. Due to their porosity, they can be used in sensing applications. The optical absorption spectra elucidated that the films are highly transparent and have a suitable band gap which are in similar agreement with earlier reports. The current enhancement under illumination shows the suitability of nanostructured NiO thin films in its application in photovoltaics.

Study on GaN nanostructures: Growth and the suppression of the yellow emission

NASA Astrophysics Data System (ADS)

Wang, Ting; Chen, Fei; Ji, Xiaohong; Zhang, Qinyuan

2018-07-01

GaN nanostructures were synthesized via a simple chemical vapor deposition using Ga2O3 and NH3 as precursors. Structural and morphological properties were systematically characterized by field emission scanning electron microscopy, X-ray diffractometer, transmission electron microscopy, and Raman spectroscopy. The configuration of GaN nanostructures was found to be strongly dependent on the growth temperature and the NH3 flow rate. Photoluminescence analysis revealed that all the fabricated GaN NSs exhibited a strong ultra-violet emission (∼364 nm), and the yellow emission of GaN nanorods can be suppressed at appropriate III/V ratio. The suppression of the yellow emission was attributed to the low density of surface or the VGa defect. The work demonstrates that the GaN nanostructures have potential applications in the optoelectronic and nanoelectronic devices.

Feasibility study of ferromagnetic/ferroelectric films for enhanced microwave devices

NASA Technical Reports Server (NTRS)

Ijiri, Yumi

2005-01-01

This report summarizes exploratory work conducted to assess the feasibility of ferromagnetic/ferroelectric films for next-generation microwave devices. From literature review, it is established that while an increasing number of ferroelectric/ferromagnetic composites are being investigated, a number have transition temperatures that are too low and structures that are not robust enough for low cost, room temperature antenna arrays. On the other hand, several promising systems are identified, including the multiferroic BiFeO3 and a composite system of Ba/SrTiO3 and a related perovskite manganite. It is suggested that when the NASA pulsed laser deposition chamber is fully operational, thin films of these systems be investigated. In preparation for such work, we have reconfirmed several structural features of an existing Ba/SrTiO3 film using the x-ray diffractometer at Oberlin College.

Sensitive and Specific Guest Recognition through Pyridinium-Modification in Spindle-Like Coordination Containers.

PubMed

Bhuvaneswari, Nagarajan; Dai, Feng-Rong; Chen, Zhong-Ning

2018-05-02

An elaborately designed pyridinium-functionalized octanuclear zinc(II) coordination container 1-Zn was prepared through the self-assembly of Zn 2+ , p-tert-butylsulfonylcalix[4]arene, and pyridinium-functionalized angular flexible dicarboxylate linker (H 2 BrL1). The structure was determined by a single-crystal X-ray diffractometer. 1-Zn displays highly sensitive and specific recognition to 2-picolylamine as revealed by drastic blueshifts of the absorption and emission spectra, ascribed to the decrease of intramolecular charge transfer (ICT) character of the container and the occurrence of intermolecular charge transfer between the host and guest molecules. The intramolecular charge transfer plays a key role in the modulation of the electronic properties and is tunable through endo-encapsulation of specific guest molecules. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis, Characterization and Comparative Luminescence Studies of Rare-Earth-Doped Gd2O3 Nanoparticles

NASA Astrophysics Data System (ADS)

Pyngrope, D.; Singh, L. R.; Prasad, A. I.; Bora, A.

2018-04-01

A facile direct precipitation method was used for the synthesis of luminescence nanomaterial. Gd2O3 doped with rare earth element Eu3+ is synthesized by polyol route. The synthesized nanoparticles show their characteristic red emission. The nanoparticles are characterized by x-ray diffractometer (XRD), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM) and photoluminescence (PL) study. The synthesized nanoparticles are spherical particles with 30 nm size. The photoluminescence studies show the characteristic Eu3+ red emission. The PL study shows the intensity of the magnetic dipole transition ( 5 D0 \\to 7 F1 ) at 592 nm compared to that of the electronic dipole transition ( 5 D0 \\to 7 F2 ) at 615 nm. The nanomaterials can show significant application in various display devices and biomedical applications for tracking.

Thermal etching rate of GaN during MOCVD growth interruption in hydrogen and ammonia ambient determined by AlGaN/GaN superlattice structures

NASA Astrophysics Data System (ADS)

Zhang, Feng; Ikeda, Masao; Zhang, Shuming; Liu, Jianping; Tian, Aiqin; Wen, Pengyan; Cheng, Yang; Yang, Hui

2017-10-01

Thermal etching effect of GaN during growth interruption in the metalorganic chemical vapor deposition reactor was investigated in this paper. The thermal etching rate was determined by growing a series of AlGaN/GaN superlattice structures with fixed GaN growth temperature at 735 °C and various AlGaN growth temperature changing from 900 °C to 1007 °C. It was observed that the GaN layer was etched off during the growth interruption when the growth temperature ramped up to AlGaN growth temperature. The etching thickness was determined by high resolution X-ray diffractometer and the etching rate was deduced accordingly. An activation energy of 2.53 eV was obtained for the thermal etching process.

Synthesis of Flexible Graphene/Polymer Composites for Supercapacitor Applications

NASA Astrophysics Data System (ADS)

Pal, Himangshu; Bhubna, Shuvam; Kumar, Praduman; Mahapatra, Rajat; Chatterjee, Somenath

2018-01-01

In this paper, the graphene was synthesized using biocompatible cellulosic component from onions. Onion epidermal cells were chosen as raw material. During heating at high temperature, the bonding among atoms in material was rearranged and forms two-dimensional hexagonal carbon layer (graphene). The characterization of synthesized graphene was done by x-ray diffractometer, Raman spectrometer and field emission scanning electron microscopy, respectively. An attempt has been taken to form the capacitors with two different current collector electrodes, anticipating the performance of the supercapacitors. The observed capacitance values as-obtained for Al and Au current collector were 1.3 μF and 6.08 μF, respectively. However, when thermally exfoliated graphene was used as an electrode on Al and Au current collector, the capacitance value was drastically increased and found to be 1.6 and 41.25 μF, respectively.

Study on the light-color mixing of rare earth luminescent materials for anti-counterfeiting application

NASA Astrophysics Data System (ADS)

Zhang, Jishu; Zhang, Yingzi; Tao, Jin; Zhu, Yanan

2018-04-01

In order to find out the light color mixing mechanism of rare earth luminescent materials used in anti-counterfeiting fibers, we prepared three kinds of rare earth luminescent materials according to RGB tri-primary color, and mixed it together to form different mixtures in certain proportion. The phase structures of the luminescent material monomers were measured by x-ray diffractometer. The photochromic properties of the luminescent materials were tested and analyzed by fluorescence spectrophotometer. The results show that the light color mixing was consistent with the blending principle of additive color, but not the same because of the photochromic properties of rare earth luminescent materials, and we explored the reasons in the light wavelength and intensity. It was found that the enhancement of the luminescence intensity of the mixture on account of the superimposing of luminescence.

Characterization of Micro-arc Oxidation Coatings on 6N01 Aluminum Alloy Under Different Electrolyte Temperature Control Modes

NASA Astrophysics Data System (ADS)

Wang, Xuefei; Zhu, Zongtao; Li, Yuanxing; Chen, Hui

2018-03-01

The micro-arc oxidation coatings of 6N01 aluminum alloy produced under different control modes of the electrolyte temperature are discussed in detail. Compared to those coated by a thermostatically controlled treatment, the coatings had different surface characterizations when they were coated without controlling the electrolyte temperature, particularly after treatment involving boiling electrolytes. Scanning electron microscopy and confocal laser scanning microscopy were used to observe the morphology of the coatings. Energy-dispersive spectrometry and x-ray diffractometer were used to characterize their elemental and crystalline phase compositions. The results indicate that the treatment without a controlled electrolyte temperature ultimately led to a thicker and rougher film with a respectably thick inner barrier film, a lower content of γ-Al2O3 and better corrosion resistance.

Significant enhancement in volumetric and gravimetric capacitance of Cu-TiO2/PPY composite for supercapacitor application

NASA Astrophysics Data System (ADS)

Purty, B.; Choudhary, R. B.

2018-04-01

Copper doped titanium dioxide-polypyrrole (Cu-TiO2/PPY) composite was successfully synthesized via chemical oxidative in-situ polymerization process. The structural and morphological properties of Cu-TiO2/PPY composite were investigated using X-ray diffractometer (XRD), field emission electron microscopy (FESEM) and transmission electron microscopy(TEM) techniques. The electrochemical properties of as-synthesized composite were studied using cyclic voltammetry (CV), galvanostatic charge discharge (GCD) and electrochemical impedance spectroscopic (EIS) techniques. The novel Cu-TiO2/PPY composite showed enhanced volumetric capacitance ˜714 F cm-1 and gravimetric capacitance ˜674 F g-1 at 1 A g-1. In addition an excellent coulombic efficiency and comparabley low charge transfer resistance than pure PPY suggests improved supercapacitive performance of Cu-TiO2/PPY composite as an electrode material.

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

PubMed

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.

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

PubMed

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.

Analytical investigation of Mudéjar polychrome on the carpentry in the Casa de Pilatos palace in Seville using non-destructive XRF and complementary techniques

NASA Astrophysics Data System (ADS)

Garrote, M. A.; Robador, M. D.; Perez-Rodriguez, J. L.

2017-02-01

The pigments, execution technique and repainting used on the polychrome wood ceilings and doors in the Casa de Pilatos (Seville, Spain) were studied using portable X-ray fluorescence equipment. Cross-sections of small samples were also analysed by optical microscopy, SEM with EDX analysis, micro-Raman and micro-infrared spectroscopy and X-ray diffraction. These carpentry works are magnificent examples of the Mudéjar art made in Spain in the early 16th century. Portable X-ray fluorescence gave good information on the different components of the polychrome. The SEM-EDX study of the surfaces of small samples gave information on their components and also characterized the compounds that had been deposited or formed by environmental contamination or by the alteration of some pigments. The SEM-EDX study of cross-sections facilitated the characterization of all layers and pigments from the support to the most external layer. The following pigments were characterized: red (cinnabar/vermillion, lead oxide, iron oxides and orpiment/realgar), black (carbon black), white (white lead and titanium barium white), yellow-orange-red-brown (orpiment/realgar and iron oxides), green (chromium oxide), blue (indigo blue and ultramarine blue), and gilding (gold leaf on bole). False gold, bronze and brass were also found. The pigments were applied with the oil painting technique over a support layer that had been primed with animal glue. This support layer was gypsum in some cases and white lead in others. This study is essential to the polychrome conservation of the studied artwork, and it will help clarify uncertainties in the history and painting of Mudéjar art.

Analytical investigation of Mudéjar polychrome on the carpentry in the Casa de Pilatos palace in Seville using non-destructive XRF and complementary techniques.

PubMed

Garrote, M A; Robador, M D; Perez-Rodriguez, J L

2017-02-15

The pigments, execution technique and repainting used on the polychrome wood ceilings and doors in the Casa de Pilatos (Seville, Spain) were studied using portable X-ray fluorescence equipment. Cross-sections of small samples were also analysed by optical microscopy, SEM with EDX analysis, micro-Raman and micro-infrared spectroscopy and X-ray diffraction. These carpentry works are magnificent examples of the Mudéjar art made in Spain in the early 16th century. Portable X-ray fluorescence gave good information on the different components of the polychrome. The SEM-EDX study of the surfaces of small samples gave information on their components and also characterized the compounds that had been deposited or formed by environmental contamination or by the alteration of some pigments. The SEM-EDX study of cross-sections facilitated the characterization of all layers and pigments from the support to the most external layer. The following pigments were characterized: red (cinnabar/vermillion, lead oxide, iron oxides and orpiment/realgar), black (carbon black), white (white lead and titanium barium white), yellow-orange-red-brown (orpiment/realgar and iron oxides), green (chromium oxide), blue (indigo blue and ultramarine blue), and gilding (gold leaf on bole). False gold, bronze and brass were also found. The pigments were applied with the oil painting technique over a support layer that had been primed with animal glue. This support layer was gypsum in some cases and white lead in others. This study is essential to the polychrome conservation of the studied artwork, and it will help clarify uncertainties in the history and painting of Mudéjar art. Copyright © 2016 Elsevier B.V. All rights reserved.

Boehmite nanostructures preparation by hydrothermal method from anodic aluminium oxide membrane.

PubMed

Yang, X; Wang, J Y; Pan, H Y

2009-02-01

Boehmite nanostructures were successfully synthesized from porous anodic aluminium oxide (AAO) membrane by a simple and efficient hydro-thermal method. The experiment used high purity alumina as raw material, and the whole reaction process avoided superfluous impurities to be introduced. Thus, the purity of Boehmite products was ensured. The examinations of the morphology and structure were carried out by atomic force microscope (AFM), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Composition of the specimens was analyzed using energy dispersive X-ray spectroscope (EDX) and X-ray diffraction (XRD). Based on these observations the growth process was analyzed.

Relative impact of H 2 O and O 2 in the oxidation of UO 2 powders from 50 to 300 °C

DOE Office of Scientific and Technical Information (OSTI.GOV)

Donald, Scott B.; Davisson, M. Lee; Dai, Zurong

Here, we studied the reaction of water and molecular oxygen with stoichiometric uranium dioxide (i.e. UO 2) powder at elevated temperature by high-resolution x-ray photoelectron spectroscopy (XPS), infrared (IR) spectroscopy, powder x-ray diffraction (XRD), and scanning electron microscopy (SEM). We observed and quatified oxidation resulting from the dissociative chemisorption of the adsorbing molecules and subsequent incorporation into the oxide lattice. Molecular oxygen was found to be a stronger oxidation agent than water at elevated temperatures but not at ambient.

Sonochemical fabrication of 8-hydroxyquinoline aluminum (Alq3) nanoflowers with high electrogenerated chemiluminescence.

PubMed

Mao, Chang-Jie; Wang, Dan-Chen; Pan, Hong-Cheng; Zhu, Jun-Jie

2011-03-01

Well-defined Alq(3) nanoflowers were fabricated via a facile and fast sonochemical route. X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field-emission scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to characterize the structure and shape of the as-prepared product. The results showed that the resulting Alq(3) was composed of nanobelts with thickness about 50 nm, average widths of 200 nm, and length up to 10 μm. The Alq(3) nanoflowers exhibited good electrogenerated chemiluminescence behavior. Copyright © 2010 Elsevier B.V. All rights reserved.

Composition, speciation and distribution of iron minerals in Imperata cylindrica.

PubMed

Amils, Ricardo; de la Fuente, Vicenta; Rodríguez, Nuria; Zuluaga, Javier; Menéndez, Nieves; Tornero, Jesús

2007-05-01

A comparative study of the roots, rhizomes and leaves of an iron hyperaccumulator plant, Imperata cylindrica, isolated from the banks of an extreme acidic environment, using complementary techniques: Mösbauer spectroscopy (MS), X-ray diffraction (XRD), scanning electron microscopy (SEM) coupled to energy-dispersive X-ray microanalysis (EDAX) and transmission electron microscopy (TEM), has shown that two main biominerals, jarosite and ferrihydrate-ferritin, accumulate in the different tissues. Jarosite accumulates mainly in roots and rhizomes, while ferritin has been detected in all the structures. A model of iron management in I. cylindrica is presented.

Relative impact of H2O and O2 in the oxidation of UO2 powders from 50 to 300 °C

NASA Astrophysics Data System (ADS)

Donald, Scott B.; Davisson, M. Lee; Dai, Zurong; Roberts, Sarah K.; Nelson, Art J.

2017-12-01

The reaction of water and molecular oxygen with stoichiometric uranium dioxide (i.e. UO2) powder at elevated temperature was studied by high-resolution x-ray photoelectron spectroscopy (XPS), infrared (IR) spectroscopy, powder x-ray diffraction (XRD), and scanning electron microscopy (SEM). Oxidation resulting from the dissociative chemisorption of the adsorbing molecules and subsequent incorporation into the oxide lattice was observed and quantified. Molecular oxygen was found to be a stronger oxidation agent than water at elevated temperatures but not at ambient.

Relative impact of H 2 O and O 2 in the oxidation of UO 2 powders from 50 to 300 °C

DOE PAGES

Donald, Scott B.; Davisson, M. Lee; Dai, Zurong; ...

2017-10-04

Here, we studied the reaction of water and molecular oxygen with stoichiometric uranium dioxide (i.e. UO 2) powder at elevated temperature by high-resolution x-ray photoelectron spectroscopy (XPS), infrared (IR) spectroscopy, powder x-ray diffraction (XRD), and scanning electron microscopy (SEM). We observed and quatified oxidation resulting from the dissociative chemisorption of the adsorbing molecules and subsequent incorporation into the oxide lattice. Molecular oxygen was found to be a stronger oxidation agent than water at elevated temperatures but not at ambient.

Novel Electrochemical Process for Treatment of Perchlorate in Waste Water

DTIC Science & Technology

2011-03-06

Prepared in Different Processes: (b) in 0.1 M Pyrrole Solution with 0.1 M NaCl at 0.8 V for 20 min; (c) at 0.5 V for 400 s in 0.1 M ClO4- Solution and...polypyrrole Py pyrrole SEM scanning electron microscopy SON statement of need XPS X-ray photoelectron spectroscopy v Acknowledgments This work is...shows the scanning electron microscopy (SEM) images of carbon fiber paper and a CNT array grown on carbon fiber paper. Pyrrole (Py) deposition

Gallium oxide thin films from the AACVD of [Ga(NMe2)3]2 and donor functionalised alcohols.

PubMed

Basharat, Siama; Carmalt, Claire J; Binions, Russell; Palgrave, Robert; Parkin, Ivan P

2008-02-07

Thin films of Ga(2)O(3) have been produced from [Ga(NMe(2))(3)](2) and ROH (R = CH(2)CH(2)NMe(2), CH(CH(2)NMe(2))(2), CH(CH(3))CH(2)NMe(2), CH(2)CH(2)OMe and C(CH(3))(2)CH(2)OMe) by aerosol assisted chemical vapour deposition on glass. Transparent, unreflective films were obtained at a deposition temperature of 550 degrees C using toluene as solvent. The gallium oxide films were analyzed by Scanning electron microscopy (SEM), Raman spectroscopy, wavelength dispersive analysis of X-rays (WDX) and X-ray photoelectron spectroscopy (XPS). The gallium oxide films obtained were X-ray amorphous. Gas-sensing experiments indicated that the films showed an n-type response to ethanol at a variety of temperatures.

Sonochemical fabrication of fluorinated mesoporous titanium dioxide microspheres

NASA Astrophysics Data System (ADS)

Yu, Changlin; Yu, Jimmy C.; Chan, Mui

2009-05-01

A sonochemical-hydrothermal method for preparing fluorinated mesoporous TiO 2 microspheres was developed. Formation of mesoporous TiO 2 and doping of fluorine was achieved by sonication and then hydrothermal treatment of a solution containing titanium isopropoxide, template, and sodium fluoride. The as-synthesized TiO 2 microspheres were characterized by X-ray diffraction (XRD), Fourier translation infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray (EDX) spectroscopy, photoluminescence spectroscopy (PL), and BET surface areas. The P123 template was removed completely during the hydrothermal and washing steps, which was different from the conventional calcination treatment. The as- synthesized TiO 2 microspheres had good crystallinity and high stability. Results from the photocatalytic degradation of methylene blue (MB) showed that fluorination could remarkably improve the photocatalytic activity of titanium dioxide.

Leaching behavior and ESEM characterization of water-sensitive mudstone in southwestern Taiwan.

PubMed

Chen, Hung-Ta; Lin, Tzong-Tzeng; Chang, Juu-En

2003-05-01

This investigation attempts to understand the critical soluble salts in natural mudstone and the leaching, microstructural, and microchemical characteristics in soaked mudstone using scanning electron microscopy (SEM)/energy-dispersive X-ray analysis (EDAX), X-ray fluorescence spectrometry (XRF), X-ray diffractometry (XRD), conductivity measurement, ion chromatography (IC), and environmental scanning electron microscopy (ESEM)/EDAX techniques. Natural mudstone probably includes soluble salts such as Na2SO4, NaCl, NaCO3, and CaCO3. The dissolution of Na2SO4 controls water-sensitive mudstone very susceptible to slaking and dispersion. ESEM micrographs clearly show evidence of mudstone-slaking during soaking since the visible pores are filled with small aggregative masses. A calcium-bearing precipitate from the soaked mudstone is speculated to be attributable to the decomposition of the hydrated product of the fresh mudstone.