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

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

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.

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

Synthesis of nanocrystalline CdS thin film by SILAR and their characterization

NASA Astrophysics Data System (ADS)

Mukherjee, A.; Satpati, B.; Bhattacharyya, S. R.; Ghosh, R.; Mitra, P.

2015-01-01

Cadmium sulphide (CdS) thin film was prepared by successive ion layer adsorption and reaction (SILAR) technique using ammonium sulphide as anionic precursor. Characterization techniques of XRD, SEM, TEM, FTIR and EDX were utilized to study the microstructure of the films. Structural characterization by x-ray diffraction reveals the polycrystalline nature of the films. Cubic structure is revealed from X-ray diffraction and selected area diffraction (SAD) patterns. The particle size estimated using X-ray line broadening method is approximately 7 nm. Instrumental broadening was taken into account while particle size estimation. TEM shows CdS nanoparticles in the range 5-15 nm. Elemental mapping using EFTEM reveals good stoichiometric composition of CdS. Characteristic stretching vibration mode of CdS was observed in the absorption band of FTIR spectrum. Optical absorption study exhibits a distinct blue shift in band gap energy value of about 2.56 eV which confirms the size quantization.

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.

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

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

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...

[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.

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.

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...

Room temperature chemical synthesis of lead selenide thin films with preferred orientation

NASA Astrophysics Data System (ADS)

Kale, R. B.; Sartale, S. D.; Ganesan, V.; Lokhande, C. D.; Lin, Yi-Feng; Lu, Shih-Yuan

2006-11-01

Room temperature chemical synthesis of PbSe thin films was carried out from aqueous ammoniacal solution using Pb(CH3COO)2 as Pb2+ and Na2SeSO3 as Se2- ion sources. The films were characterized by a various techniques including, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED), Fast Fourier transform (FFT) and UV-vis-NIR techniques. The study revealed that the PbSe thin film consists of preferentially oriented nanocubes with energy band gap of 0.5 eV.

Carbonate formation in non-aqueous environments by solid-gas carbonation of silicates

NASA Astrophysics Data System (ADS)

Day, S. J.; Thompson, S. P.; Evans, A.; Parker, J. E.

2012-02-01

We have produced synthetic analogues of cosmic silicates using the Sol Gel method, producing amorphous silicates of composition Mg(x)Ca(1-x)SiO3. Using synchrotron X-ray powder diffraction on Beamline I11 at the Diamond Light Source, together with a newly-commissioned gas cell, real-time powder diffraction scans have been taken of a range of silicates exposed to CO2 under non-ambient conditions. The SXPD is complemented by other techniques including Raman and Infrared Spectroscopy and SEM imaging.

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.

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.

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

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-...

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.

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.

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.

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.

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

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.

Hexagonal OsB 2: Sintering, microstructure and mechanical properties

DOE PAGES

Xie, Zhilin; Lugovy, Mykola; Orlovskaya, Nina; ...

2015-02-07

In this study, the metastable high pressure ReB 2-type hexagonal OsB 2 bulk ceramics was produced by spark plasma sintering. The phase composition, microstructure, and mechanical behavior of the sintered OsB 2 were studied by X-ray diffraction, optical microscopy, TEM, SEM, EDS, and nanoindentation. The produced ceramics was rather porous and contained a mixture of hexagonal (~80 wt.%) and orthorhombic (~20 wt.%) phases as identified by X-ray diffraction and EBSD analysis. Two boron-rich phases, which do not contain Os, were also identified by TEM and SEM/EDS analysis. Nanoindentation measurements yielded a hardness of 31 ± 9 GPa and Young’s modulusmore » of 574 ± 112 GPa, indicating that the material is rather hard and very stiff; but, it is very prone to crack formation and propagation, which is indicative of a very brittle nature of this material. Improvements in the sintering regime are required in order to produce dense, homogeneous and single phase hexagonal OsB 2 bulk ceramics.« less

Formulation of glutaraldehyde disinfectant for alginate impressions.

PubMed

Unemori, M; Matsuya, Y; Matsuya, S; Akashi, A; Mizuno, K; Akamine, A

1999-12-01

The effect of buffer agents incorporated in glutaraldehyde disinfectants on the surface quality of dental models was examined by the measurement of surface roughness, X-ray diffraction analysis and SEM observation. Seven experimental glutaraldehyde disinfectants were prepared using two buffer agents, potassium acetate alone or potassium acetate and sodium hydrogen carbonate in combination. Four kinds of sulfate--zinc, calcium, potassium and magnesium sulfate--were added to these disinfectants in order to accelerate the hydration of calcium sulfate hemihydrate. The impressions treated with the experimental disinfectants for 1 h produced stone surfaces which had significantly lower surface roughness values than those treated with the commercial disinfectants (p < 0.05). The X-ray diffraction analysis and SEM observation showed that these superior surfaces were produced as a result of significant reductions in the amount of residual calcium sulfate hemihydrate. Replacement of buffer agents in commercial glutaraldehyde disinfectants with chemicals such as those studied in the present study will improve the surface quality of dental stone.

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.

Cd-doped ZnO nano crystalline thin films prepared at 723K by spray pyrolysis

NASA Astrophysics Data System (ADS)

Joishy, Sumanth; Rajendra B., V.

2018-04-01

Ternary Zn1-xCdxO(x=0.10, 0.40, 0.70 at.%) thin films of 0.025M precursor concentration have been successfully deposited on preheated (723K) glass substrates using spray pyrolysis route. The structure, morphology and optical properties of deposited films have been characterized by X-ray diffraction, Scanning Electron Microscopy (SEM) and UV-Visible spectrophotometry. X-ray diffraction study shows that the prepared films are polycrystalline in nature. 10% Cd doped ZnO film belongs to the hexagonal wurtzite system and 70% Cd doped ZnO film belongs to the cubic system, although mixed phases were formed for 40% Cd doped ZnO film. The optical transmittance spectra has shown red shift with increasing cadmium content. Optical energy band gap has been reduced with cadmium dopant.

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.

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).

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.

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.

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.

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.

Green synthesis of BiVO4 nanorods via aqueous extracts of Callistemon viminalis

NASA Astrophysics Data System (ADS)

Mohamed, H. E. A.; Sone, B. T.; Fuku, X. G.; Dhlamini, M. S.; Maaza, M.

2018-05-01

Nowadays, the development of efficient green chemistry methods for synthesis of metal oxides nanoparticles has become a major focus of researchers. These methods are being investigated in order to find an eco-friendly technique for production of well-characterized nanoparticles. In this contribution we report for the first time, the synthesis and structural characterization of n-type Bismuth vanadate (BiVO4) nanoparticles using aqueous extracts of Callistemon viminalis as a chelating agent. To ascertain the formation of BiVO4, X-Ray diffraction analysis (XRD), Scanning Electron Microscopy (SEM), High Resolution Transmission Electron Microscopy (TEM), Selected Area Electron Diffraction (SAED), Electron Dispersion X-ray Spectroscopy (EDS), Fourier Transform Infra-red Spectroscopy (FTIR), and Photoluminescence spectroscopy (PL) were carried out.

A hydrous Ca-bearing magnesium carbonate from playa lake sediments, Salines Lake, Spain

USGS Publications Warehouse

Queralt, I.; Julia, R.; Plana, F.; Bischoff, J.L.

1997-01-01

Sediments of playa Lake Salines, SE, Spain, contain a carbonate mineral characterized by X-ray diffraction peaks very similar to, but systematically shifted from those of pure magnesite. Analyses (SEM, IR and Raman spectroscopy, DTA, TGA, and ICP) indicate the mineral is a hydrous Ca-bearing magnesium carbonate with the chemical formula (Mg0.92,Ca0.08)CO3??3H2O. Thermal characteristics of the mineral are similar to those of other known hydrated magnesium carbonates. X-ray and electron diffraction data suggests a monoclinic system (P21/n space group) with unit-cell parameters of a = 6.063(6), b = 10.668(5), and c = 6.014(4) A?? and ?? = 107.28??.

Structural and photoluminescence properties of Ni doped CdS nanoparticles synthesis by sol gel method

NASA Astrophysics Data System (ADS)

Mahdi, Hadeel Salih; Parveen, Azra; Azam, Ameer

2018-05-01

Ni doped CdS nanoparticles have been successfully synthesized by sol-gel method. Nickel nitrate, cadmium nitrate, sodium sulfide has been used as precursors for the preparation of these Ni-doped CdS nanoparticles. The structural properties were studied by X-ray diffraction analysis. Surface morphology and the composition of the samples were studied by scanning electron microscope (SEM). The X-ray diffraction results revealed that the Ni-doped CdS nanoparticles were in hexagonal structure. The crystallite size was determined from Debye-Scherer equation and showed that the particle size increases with the doping of Ni. Optical absorption spectra of Ni doped CdS also was studied by Photoluminescence spectroscopy in the range of 200-600 nm.

Structural and magnetic properties of FeCoC system obtained by mechanical alloying

NASA Astrophysics Data System (ADS)

Rincón Soler, A. I.; Rodríguez Jacobo, R. R.; Medina Barreto, M. H.; Cruz-Muñoz, B.

2017-11-01

Fe96-XCoXC4 (x = 0, 10, 20, 30, 40 at. %) alloys were obtained by mechanical alloying of Fe, C and Co powders using high-energy milling. The structural and magnetic properties of the alloy system were analyzed by X-ray diffraction, Scanning Electron Microscopy (SEM), Vibrating Sample Magnetometer (VSM) and Mössbauer Spectrometry at room temperature. The X-ray diffraction patterns showed a BCC-FeCoC structure phase for all samples, as well as a lattice parameter that slightly decreases with Co content. The saturation magnetization and coercive field were analyzed as a function of Co content. The Mössbauer spectra were fitted with a hyperfine magnetic field distribution showing the ferromagnetic behavior and the disordered character of the samples. The mean hyperfine magnetic field remained nearly constant (358 T) with Co content.

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

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.

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.

Dislocation, crystallite size distribution and lattice strain of magnesium oxide nanoparticles

NASA Astrophysics Data System (ADS)

Sutapa, I. W.; Wahid Wahab, Abdul; Taba, P.; Nafie, N. L.

2018-03-01

The oxide of magnesium nanoparticles synthesized using sol-gel method and analysis of the structural properties was conducted. The functional groups of nanoparticles has been analysed by Fourier Transform Infrared Spectroscopy (FT-IR). Dislocations, average size of crystal, strain, stress, the energy density of crystal, crystallite size distribution and morphologies of the crystals were determined based on X-ray diffraction profile analysis. The morphological of the crystal was analysed based on the image resulted from SEM analysis. The crystallite size distribution was calculated with the contention that the particle size has a normal logarithmic form. The most orientations of crystal were determined based on the textural crystal from diffraction data of X-ray diffraction profile analysis. FT-IR results showed the stretching vibration mode of the Mg-O-Mg in the range of 400.11-525 cm-1 as a broad band. The average size crystal of nanoparticles resulted is 9.21 mm with dislocation value of crystal is 0.012 nm-2. The strains, stress, the energy density of crystal are 1.5 x 10-4 37.31 MPa; 0.72 MPa respectively. The highest texture coefficient value of the crystal is 0.98. This result is supported by morphological analysis using SEM which shows most of the regular cubic-shaped crystals. The synthesis method is suitable for simple and cost-effective synthesis model of MgO nanoparticles.

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.

High spin state driven magnetism and thermoelectricity in Mn doped topological insulator Bi2Se3

NASA Astrophysics Data System (ADS)

Maurya, V. K.; Dong, C. L.; Chen, C. L.; Asokan, K.; Patnaik, S.

2018-06-01

We report on the synthesis, and structural - magnetic characterizations of Mn doped Bi2Se3 towards achieving a magnetically doped topological insulator. High quality single crystals of MnxBi2-xSe3 (x = 0, 0.03, 0.05, 0.1) are grown and analysed by X-ray diffraction (XRD), Low Energy Electron Diffraction (LEED), Scanning electron microscopy (SEM), and X-ray absorption near-edge structure spectroscopy (XANES). Magnetic properties of these samples under ZFC-FC protocol and isothermal magnetization confirm ferromagnetic correlation above x = 0.03 value. XANES measurements confirm that the dopant Mn is in Mn2+ state. This is further reconfirmed to be in high spin state by fitting magnetic data with Brillouin function for J = 5/2. Both Hall and Seebeck measurements indicate a sign change of charge carriers above x = 0.03 value of Mn doping. We propose Mn doped Bi2Se3 to be a potential candidate for electromagnetic and thermoelectric device applications involving topological surface states.

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.

Studies on rock characteristics and timing of creep at selected landslide sites in Taiwan

Treesearch

Cheng-Yi Lee

2000-01-01

A study was conducted to investigate the causes of and rock characteristics at three landslide sites in the Tesngwen Reservoir watershed of southern Taiwan. Research methods used included the petrographic microscope, X-ray diffraction (XRD), scanning electron microscope (SEM), inductively coupled plasma spectroscope (ICP), constant head permeameter in triaxial...

Crystallographic Study of Itokawa Particle, RA-QD02-0127 by Using Energy-Scanning X-Ray Diffraction Method with Synchrotron Radiation

NASA Technical Reports Server (NTRS)

Hagiya, K.; Ohsumi, K.; Komatsu, M.; Mikouchi, T.; Zolensky, M. E.; Hirata, A.; Yamaguchi, S.; Kurokawa, A.

2016-01-01

The petrographic study of Itokawa particle, RA-QD02-0127 has been performed by SEM-EDS and optical microscope observations. The purpose of this study is to understand better the metamorphic and impact shock history of asteroid Itokawa, and other S-class asteroids.

Structural and Spectral Characterization of Co2+- and Ni2+-DOPED CdO Powder Prepared From Solution at Room Temperature

NASA Astrophysics Data System (ADS)

Reddy, C. V.; Rao, L. V. Krishna; Satish, D. V.; Shim, J.; Ravikumar, R. V. S. S. N.

2015-11-01

The mild and simple solution method was used for the synthesis of Co2+- and Ni2+-doped CdO powders at room temperature. The prepared powders were characterized using powder X-ray diffraction, scanning electron microscopy (SEM) with energy dispersive spectroscopy (EDS), optical absorption, and Fourier transform infrared spectroscopy (FTIR). From the powder X-ray diffraction patterns, it has been observed that the prepared Co2+ and Ni2+ ion-doped CdO powders belong to the cubic phase, and the evaluated average crystalline sizes of the powders are 20 and 14 nm, respectively. The SEM images and the EDS spectra show that the prepared powders are distributed over different sizes in the grain boundaries. Optical absorption studies allow determination of site symmetry of the metal ion with its ligands. The crystal field (Dq) and inter-electronic repulsion (B and C) parameters have been evaluated from the optical absorption spectra. The FTIR spectra show the characteristic fundamental vibrations of the metal oxide and CdO.

Electroless Nickel Deposition for Front Side Metallization of Silicon Solar Cells

PubMed Central

Hsieh, Shu Huei; Hsieh, Jhong Min; Chen, Wen Jauh; Chuang, Chia Chih

2017-01-01

In this work, nickel thin films were deposited on texture silicon by electroless plated deposition. The electroless-deposited Ni layers were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive x-ray spectroscopy (EDS), X-ray diffraction analysis (XRD), and sheet resistance measurement. The results indicate that the dominant phase was Ni2Si and NiSi in samples annealed at 300–800 °C. Sheet resistance values were found to correlate well with the surface morphology obtained by SEM and the results of XRD diffraction. The Cu/Ni contact system was used to fabricate solar cells by using two different activating baths. The open circuit voltage (Voc) of the Cu/Ni samples, before and after annealing, was measured under air mass (AM) 1.5 conditions to determine solar cell properties. The results show that open circuit voltage of a solar cell can be enhanced when the activation solution incorporated hydrofluoric acid (HF). This is mainly attributed to the native silicon oxide layer that can be decreased and/or removed by HF with the corresponding reduction of series resistance. PMID:28805724

Synthesis of TiO2 Nanoparticle and its phase Transition

NASA Astrophysics Data System (ADS)

Mangrola, M. H.; Joshi, V. G.; Parmar, B. H.

2011-12-01

Here we report the synthesis of titanium dioxide (TiO2) nanoparticles and study of its phase transition from anataze to rutile. Titanium dioxide (TiO2) nanoparticles have been prepared by hydrolysis of Titanium isopropoxide an aqueous solution with constant value of pH 2 and peptizing the resultant suspension gel(white-Blue) and calcinate gel at different temperature. Structures of synthetic samples of TiO2 have been examined by X-ray diffraction (XRD) and scanning electron microscope (SEM). The anatase-rutile transition has been a popular topic due to its interest to scientific and engineering fields. . Here we have seen that the 100 °C calcinate powder consist of anatase fine crystalline phase with a particle size 14 to 15 nm. The prepared TiO2 nanoparticles have uniform size and morphology, and the phase transformation kinetics of obtained material was studied by interpretation of the X-ray diffraction patterns peaks. The phase transform occurred from anatase to rutile at calcinate temperature up to 600 °C. A very fine network texture made from uniform nanoparticles was revealed by scanning electron microscopy (SEM) analyses.

Optical, Magnetic and Photocatalytic Activity Studies of Li, Mg and Sr Doped and Undoped Zinc Oxide Nanoparticles.

PubMed

Shanthi, S I; Poovaragan, S; Arularasu, M V; Nithya, S; Sundaram, R; Magdalane, C Maria; Kaviyarasu, K; Maaza, M

2018-08-01

Nanoparticles of Li, Mg and Sr doped and undoped zinc oxide was prepared by simple precipitation method. The structural, optical, and magnetic properties of the samples were investigated by the Powder X-ray Diffraction (XRD), Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM), Fourier Transform Infrared (FTIR) spectroscopy, Ultra-violet Visible spectroscopy (UV-vis) spectra, Photoluminescence (PL) and Vibrational Sample Magnetometer (VSM). The Powder X-ray diffraction data confirm the formation of hexagonal wurtzite structure of all doped and undoped ZnO. The SEM photograph reveals that the pores availability and particles size in the range of 10 nm-50 nm. FTIR and UV-Visible spectra results confirm the incorporation of the dopant into the ZnO lattice nanostructure. The UV-Visible spectra indicate that the shift of blue region (lower wavelength) due to bandgap widening. Photoluminescence intensity varies with doping due to the increase of oxygen vacancies in prepared ZnO. The pure ZnO exist paramagnetic while doped (Li, Mg and Sr) ZnO exist ferromagnetic property. The photocatalytic activity of the prepared sample also carried out in detail.

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

Wang, Hongfen, E-mail: wanghongfen11@163.com; Wang, Zhiqi; Chen, Shougang

Molybdenum carbides with surfactants as carbon sources were prepared using the carbothermal reduction of the appropriate precursors (molybdenum oxides deposited on surfactant micelles) at 1023 K under hydrogen gas. The carburized products were characterized using scanning electron microscopy (SEM), X-ray diffraction and BET surface area measurements. From the SEM images, hollow microspherical and rod-like molybdenum carbides were observed. X-ray diffraction patterns showed that the annealing time of carburization had a large effect on the conversion of molybdenum oxides to molybdenum carbides. And BET surface area measurements indicated that the difference of carbon sources brought a big difference in specific surfacemore » areas of molybdenum carbides. - Graphical abstract: Molybdenum carbides having hollow microspherical and hollow rod-like morphologies that are different from the conventional monodipersed platelet-like morphologies. Highlights: Black-Right-Pointing-Pointer Molybdenum carbides were prepared using surfactants as carbon sources. Black-Right-Pointing-Pointer The kinds of surfactants affected the morphologies of molybdenum carbides. Black-Right-Pointing-Pointer The time of heat preservation at 1023 K affected the carburization process. Black-Right-Pointing-Pointer Molybdenum carbides with hollow structures had larger specific surface areas.« less

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.

Glancing-incidence X-ray diffraction of Ag nanoparticles in gold lustre decoration of Italian Renaissance pottery

NASA Astrophysics Data System (ADS)

Bontempi, E.; Colombi, P.; Depero, L. E.; Cartechini, L.; Presciutti, F.; Brunetti, B. G.; Sgamellotti, A.

2006-06-01

Lustre is known as one of the most significant decorative techniques of Medieval and Renaissance pottery in the Mediterranean basin, characterized by brilliant gold and red metallic reflections and iridescence effects. Previous studies by various techniques (SEM-EDS and TEM, UV-VIS, XRF, RBS and EXAFS) demonstrated that lustre consists of a heterogeneous metal-glass composite film, formed by Cu and Ag nanoparticles dispersed within the outer layer of a tin-opacified lead glaze. In the present work the investigation of an original gold lustre sample from Deruta has been carried out by means of glancing-incidence X-ray diffraction techniques (GIXRD). The study was aimed at providing information on structure and depth distribution of Ag nanoparticles. Exploiting the capability of controlling X-ray penetration in the glaze by changing the incidence angle, we used GIXRD measurements to estimate non-destructively thickness and depth of silver particles present in the first layers of the glaze.

Nanobelt formation of magnesium hydroxide sulfate hydrate via a soft chemistry process.

PubMed

Zhou, Zhengzhi; Sun, Qunhui; Hu, Zeshan; Deng, Yulin

2006-07-13

The nanobelt formation of magnesium hydroxide sulfate hydrate (MHSH) via a soft chemistry approach using carbonate salt and magnesium sulfate as reactants was successfully demonstrated. X-ray diffraction (XRD), energy dispersion X-ray spectra (EDS), selected area electron diffraction (SAED), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) analysis revealed that the MHSH nanobelts possessed a thin belt structure (approximately 50 nm in thickness) and a rectangular cross profile (approximately 200 nm in width). The MHSH nanobelts suffered decomposition under electron beam irradiation during TEM observation and formed MgO with the pristine nanobelt morphology preserved. The formation process of the MHSH nanobelts was studied by tracking the morphology of the MHSH nanobelts during the reaction. A possible chemical reaction mechanism is proposed.

Uranium oxidation kinetics monitored by in-situ X-ray diffraction

NASA Astrophysics Data System (ADS)

Zalkind, S.; Rafailov, G.; Halevy, I.; Livneh, T.; Rubin, A.; Maimon, H.; Schweke, D.

2017-03-01

The oxidation kinetics of U-0.1 wt%Cr at oxygen pressures of 150 Torr and the temperature range of 90-150 °C was studied by means of in-situ X-ray diffraction (XRD). A "breakaway" in the oxidation kinetics is found at ∼0.25 μm, turning from a parabolic to a linear rate law. At the initial stage of oxidation the growth plane of UO2(111) is the prominent one. As the oxide thickens, the growth rate of UO2(220) plane increases and both planes grow concurrently. The activation energies obtained for the oxide growth are Qparabolic = 17.5 kcal/mol and Qlinear = 19 kcal/mol. Enhanced oxidation around uranium carbide (UC) inclusions is clearly observed by scanning electron microscopy (SEM).

Synthesis and dc electrical conductivity of Cr-doped CeO2 nanoparticles by solution combustion method

NASA Astrophysics Data System (ADS)

Harish, B. M.; Avinash, B. S.; Chaturmukha, V. S.; Jayanna, H. S.; Suresh, S.; Naveen, C. S.; Lamani, Ashok R.

2018-04-01

NPs of Ce1-xCrxO2 (x=0, 0.04, 0.08, 0.12) have been synthesized by solution combustion method using glycine as fuel. The effect of chromium on structural and dc electrical conductivity of cerium oxide nanoparticles were investigated. The obtained powder is characterized by UV-visible spectrometer, X-ray diffractometer (XRD), Scanning electron microscope (SEM) and Energy dispersive X-Ray analysis (EDS). X-ray diffraction analysis carried out on calcined samples reveals that successful incorporation of Cr2+ in CeO2 lattice where as SEM studies confirms the porous morphological structure of the prepared sample. The Keithley source meter is used to measure the dc conductivity of samples in the temperature range from 303K to 623K. The conductivity was found to be increases with increase of temperature as well as the Cr concentration due to semiconducting behavior of material and change in the charge carrier concentration. The activation energy decreases with increasing chromium concentration. The present work deals with the effect of chromium additive on structural and the D.C electrical properties Ce1-xCrxO2 NPs.

X-ray diffraction and infrared spectroscopy studies of Ba(Fe1/2Nb1/2)O3-(Na1/2Bi1/2)TiO3 ceramics

NASA Astrophysics Data System (ADS)

Chandra, K. P.; Yadav, Anjana; Prasad, K.

2018-05-01

Ceramics (1-x)Ba(Fe1/2Nb1/2)O3-x(Na1/2Bi1/2)TiO3; 0≤x≤1.0 were prepared by conventional ceramic synthesis technique. Rietveld refinements of X-ray diffraction data of these ceramics were carried out using FullProf software and determined their crystal symmetry, space group and unit cell dimensions. Rietveld refinement revealed that Ba(Fe1/2Nb1/2)O3 has cubic structure with space group Pm 3 ¯ m and Na1/2Bi1/2)TiO3 has rhombohedral structure with space group R3c. Addition of (Na1/2Bi1/2)TiO3 to Ba(Fe1/2Nb1/2)O3 resulted in the change of unit cell structure from cubic to tetragonal (P4/mmm) for x = 0.75 and the X-Ray diffraction peaks slightly shift towards higher Bragg's angle, suggesting slight decrease in unit cell volume. SEM studies were carried out in order to access the quality of the prepared ceramics which showed a change in grain shapes with the increase of (Na1/2Bi1/2)TiO3 content. FTIR spectra confirmed the formation of perovskite type solid solutions.

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.

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.

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.

Ag/CuO nanoparticles prepared from a novel trinuclear compound [Cu(Imdz)4(Ag(CN)2)2] (Imdz = imidazole) by a pyrolysis display excellent antimicrobial activity

NASA Astrophysics Data System (ADS)

Adhikary, Jaydeep; Das, Balaram; Chatterjee, Sourav; Dash, Sandeep Kumar; Chattopadhyay, Sourav; Roy, Somenath; Chen, Jeng-Wei; Chattopadhyay, Tanmay

2016-06-01

One copper and two silver containing one hetero tri-nuclear precursor compound [Cu(Imdz)4(Ag(CN)2)2] (1) (Imdz = Imidazole) has been synthesized and characterized by single crystal X-ray diffraction. Simple pyrolysis of the complex at 550 °C for 4 h afforded Ag/CuO nanoparticles (NPs). The synthesized nanoparticles were characterized by ultraviolet-visible (UV-Vis), Fourier transform infrared (FT-IR), X-ray powder diffraction (XRPD), dynamic light scattering (DLS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray (EDX) and X-ray photo electron spectroscopy (XPS). Staphylococcus aureus (S. aureus) and Escherichia coli (E. coli) have been employed as model microbial species to study the anti-microbial activity of the synthesized NPs. The NPs showed potent anti-microbial activity evidenced from the Minimum Inhibitory Concentration (MIC) and Minimum Bactericidal Concentration (MBC) values. Very high level of cell uptake and then generation of reactive oxygen species (ROS) are the origin of such strong antimicrobial activity for the NPs. However, the cytotoxicity level of the NPs towards normal human cell is very low.

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.

Synthesis, crystal structure and characterization of a new organic-inorganic hybrid material 4-(ammonium methyl) pipyridinium hexachloro stanate (II) trihydrate

NASA Astrophysics Data System (ADS)

Lassoued, Mohamed Saber; Abdelbaky, Mohammed S. M.; Lassoued, Abdelmajid; Ammar, Salah; Gadri, Abdellatif; Ben Salah, Abdelhamid; García-Granda, Santiago

2018-03-01

The present paper undertakes the study of (C6H16N2) SnCl6·3H2O which is a new hybrid compound. It was prepared and characterized by single crystal X-ray diffraction, X-ray powder, Hirshfeld surface, Spectroscopy measurement, thermal study and photoluminescence properties. The single crystal X-ray diffraction studies revealed that the compound crystallizes in monoclinic Cc space group with cell parameters a = 8.3309(9) Å, b = 22.956(2) Å, c = 9.8381(9) Å, β = 101.334(9) ° and Z = 4. The atomic arrangement shows an alternation of organic and inorganic entities. The cohesion between these entities is performed via Nsbnd H⋯Cl, Nsbnd H⋯O, Osbnd H⋯Cl and Osbnd H⋯O hydrogen bonding to form a three-dimensional network. Hirshfeld surface analysis was used to investigate intermolecular interactions, as well 2D finger plots were conducted to reveal the contribution of these interactions in the crystal structure quantitatively. The X-ray powder is in agreement with the X-ray structure. Scanning electron microscope (SEM) was carried out. Furthermore, the room temperature infrared (IR) spectrum of the title compound was recorded and analyzed on the basis of data found in the literature. Solid state 13C NMR spectrum shows four signals, confirming the solid state structure determined by X-ray diffraction. Besides, the thermal analysis studies were performed, but no phase transition was found in the temperature range between 30 and 450 °C. The optical and PL properties of the compound were investigated in the solid state at room temperature and exhibited three bands at 348 and 401 cm-1 and a strong fluorescence at 480 nm.

Tropical sea snail shells: Possible exotic sources for ceramic biomaterial synthesis

NASA Astrophysics Data System (ADS)

Oktar, F. N.; Kiyici, I. A.; Gökçe, H.; Aǧaogulları, D.; Kayali, E. S.

2013-12-01

In this study, chemical and structural properties of sea snail shell based bioceramic materials (i.e. hydroxyapatite, whitlockite and other phases) are produced by using mechano-chemical (ultrasonic) conversion method. For this purpose, differential thermal and gravimetric analysis (DTA/TG), X-ray diffraction, infra-red (IR) and scanning electron microscope (SEM) studies are performed.

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.

Growth and properties of wide bandgap (MgSe)n(ZnxCd1-xSe)m short-period superlattices

NASA Astrophysics Data System (ADS)

Garcia, Thor A.; Tamargo, Maria C.

2017-12-01

We report the molecular beam epitaxy (MBE) growth and properties of (MgSe)n(ZnxCd1-x Se)m short-period superlattices(SPSLs) for potential application in II-VI devices grown on InP substrates. SPSL structures up to 1 μm thick with effective bandgaps ranging from 2.6 eV to above 3.42 eV are grown and characterized, extending the typical range possible for the ZnxCdyMg1-x-ySe random alloy beyond 3.2 eV. Additionally, ZnxCd1-xSe single and multiple quantum well structures using the SPSL barriers are also grown and investigated. The structures are characterized utilizing reflection high-energy electron diffraction, X-ray reflectance, X-ray diffraction and photoluminescence. We observed layer-by-layer growth and smoother interfaces in the QWs grown with SPSL when compared to the ZnxCdyMg1-x-ySe random alloy. The results indicate that this materials platform is a good candidate to replace the random alloy in wide bandgap device applications.

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.

Structural and optical properties of WTe2 single crystals synthesized by DVT technique

NASA Astrophysics Data System (ADS)

Dixit, Vijay; Vyas, Chirag; Pathak, V. M.; Soalanki, G. K.; Patel, K. D.

2018-05-01

Layered transition metal di-chalcogenide (LTMDCs) crystals have attracted much attention due to their potential in optoelectronic device applications recently due to realization of their monolayer based structures. In the present investigation we report growth of WTe2 single crystals by direct vapor transport (DVT) technique. These crystals are then characterized by energy dispersive analysis of x-rays (EDAX) to study stoichiometric composition after growth. The structural properties are studied by x-ray diffraction (XRD) and selected area electron diffraction (SAED) is used to confirm orthorhombic structure of grown WTe2 crystal. Surface morphological properties of the crystals are also studied by scanning electron microscope (SEM). The optical properties of the grown crystals are studied by UV-Visible spectroscopy which gives direct band gap of 1.44 eV for grown WTe2 single crystals.

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.

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.

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.

Graphene nanoplate-MnO2 composites for supercapacitors: a controllable oxidation approach

NASA Astrophysics Data System (ADS)

Huang, Huajie; Wang, Xin

2011-08-01

Graphene nanoplate-MnO2 composites have been synthesized by oxidising part of the carbon atoms in the framework of graphene nanoplates at ambient temperature. The composites were characterized by means of X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV). It was found that the oxidation extent of the carbon atoms in the graphene framework in these composites was dependent on the reaction time, which also influenced their microstructure, morphology and electrochemical properties. Compared with MnO2 nanolamellas, the nanocomposite prepared with a reaction time of 3 h reveals better electrochemical properties as a supercapacitor electrode material.Graphene nanoplate-MnO2 composites have been synthesized by oxidising part of the carbon atoms in the framework of graphene nanoplates at ambient temperature. The composites were characterized by means of X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV). It was found that the oxidation extent of the carbon atoms in the graphene framework in these composites was dependent on the reaction time, which also influenced their microstructure, morphology and electrochemical properties. Compared with MnO2 nanolamellas, the nanocomposite prepared with a reaction time of 3 h reveals better electrochemical properties as a supercapacitor electrode material. Electronic supplementary information (ESI) available: Fig. S1, AFM image (5 μm × 5 μm) of graphene nanoplate-MnO2 composite obtained at 3 h; Fig. S2, nitrogen adsorption/desorption isotherm of graphene nanoplate-MnO2 composite obtained at 3 h. See DOI: 10.1039/c1nr10229j

Preparation and Characterization of Cellulose Microcrystalline (MCC) from Fiber of Empty Fruit Bunch Palm Oil

NASA Astrophysics Data System (ADS)

Nasution, H.; Yurnaliza; Veronicha; Irmadani; Sitompul, S.

2017-03-01

Alpha cellulose which was isolated from cellulose of fiber empty fruit bunch palm oil was hidrolized with hydrochloric acid (2,5N) at 80°C to produce microcrystalline cellulose (MCC). Microcrystalline cellulose is an important additional ingredient in the pharmaceutical, food, cosmetics, and structural composites. In this study, MCC, alpha cellulose, and cellulose were characterized and thereafter were compared. Characterizations were made using some equipment such as x-ray diffraction (XRD), Fourier transform infrared (FTIR), scanning electron microscopy (SEM) and thermogravimetry analyzer (TGA). X-ray diffraction and infrared spectroscopy were studied to determine crystallinity and molecular structure of MCC, where scanning electron microscopy images were conducted for information about morfology of MCC. Meanwhile, thermal resistance of MCC was determined using thermogravimetry analyzer (TGA). From XRD and FTIR, the obtained results showed that the crystalline part was traced on MCC, where the -OH and C-O groups tended to reduced as alpha cellulose has changed to MCC. From SEM the image showed the reduction of particle size of MCC, while the thermal resistance of MCC was found lower as compared with cellulose and alpha cellulose as well, which was attributed to the lower molecular weight of MCC.

Microwave synthesis and electrochemical characterization of Mn/Ni mixed oxide for supercapacitor application

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

Prasankumar, T.; Jose, Sujin P., E-mail: sujamystica@yahoo.com; Ilangovan, R.

Nanostructured Mn/Ni mixed metal oxide was synthesized at ambient temperature by facile microwave irradiation technique. The crystal structure and surface morphology were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. X-ray diffraction analysis confirmed the formation of Mn/Ni mixed oxide in rhombohedral phase and the grain size calculated was found to be 87 nm. The irregular spherical morphology of the prepared sample was exhibited by the SEM images. The characteristic peaks of FTIR at about 630 cm{sup −1} and 749 cm{sup −1} were attributed to the Mn-O and Ni-O stretching vibrations respectively. The presence of both Mn and Ni inmore » the prepared sample was validated by the EDS spectra which in turn confirmed the formation of mixed oxide. Cyclic voltammetry and galvanostatic chargedischarge measurements were employed to investigate the electrochemical performance of the mixed oxide. The cyclic voltammetry curves demonstrated good capacitive performance of the sample in the potential window −0.2V to 0.9V. The charge discharge study revealed the suitability of the prepared mixed oxide for the fabrication of supercapacitor electrode.« less

Synthesis and characterization of magnesium aluminate (MgAl2O4) spinel (MAS) thin films

NASA Astrophysics Data System (ADS)

Ahmad, Syed Muhammad; Hussain, Tousif; Ahmad, Riaz; Siddiqui, Jamil; Ali, Dilawar

2018-01-01

In a quest to identify more economic routes for synthesis of magnesium aluminate (MgAl2O4) spinel (MAS) thin films, dense plasma focus device was used with multiple plasma focus shots. Structural, bonding between composite films, surface morphological, compositional and hardness properties of MAS thin films were investigated by using x-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), energy dispersive x-rays (EDX) analysis and Vickers micro hardness test respectively. In XRD graph, the presence of MgAl2O4 diffraction peaks in crystallographic orientations (222), (400) and (622) pointed out the successful formation of polycrystalline thin films of MgAl2O4 with face centered cubic structure. The FTIR spectrums showed a major common transmittance band at 697.95 cm-1 which belongs to MgAl2O4. SEM micrographs illustrated a mesh type, granular and multi layers microstructures with significant melting effects. EDX spectrum confirmed the existence of magnesium, oxygen and aluminum in MAS films. A common increasing behavior in micro-hardness of composite MgAl2O4 films by increasing number of plasma focus shots was found.

Diffraction leveraged modulation of X-ray pulses using MEMS-based X-ray optics

DOEpatents

Lopez, Daniel; Shenoy, Gopal; Wang, Jin; Walko, Donald A.; Jung, Il-Woong; Mukhopadhyay, Deepkishore

2016-08-09

A method and apparatus are provided for implementing Bragg-diffraction leveraged modulation of X-ray pulses using MicroElectroMechanical systems (MEMS) based diffractive optics. An oscillating crystalline MEMS device generates a controllable time-window for diffraction of the incident X-ray radiation. The Bragg-diffraction leveraged modulation of X-ray pulses includes isolating a particular pulse, spatially separating individual pulses, and spreading a single pulse from an X-ray pulse-train.

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.

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.

Synthesis and characterization of Ce, Cu co-doped ZnS nanoparticles

NASA Astrophysics Data System (ADS)

Harish, G. S.; Sreedhara Reddy, P.

2015-09-01

Ce, Cu co-doped ZnS nanoparticles were prepared at room temperature using a chemical co-precipitation method. The prepared nanoparticles were characterized by X- ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive analysis of X-rays (EDAX), diffuse reflectance spectroscopy (DRS), photoluminescence (PL) and high resolution Raman spectroscopic techniques. Transmission electron microscopy (TEM) and X-ray diffraction studies showed that the diameter of the particles was around 2-3 nm. Broadened XRD peaks revealed the formation of nanoparticles with a face centered cubic (fcc) structure. DRS studies confirmed that the band gap increased with an increase in the dopant concentration. The Raman spectra of undoped and Ce, Cu ions co-doped ZnS nanoparticles showed longitudinal optical mode and transverse optical mode. Compared with the Raman modes (276 and 351 cm-1) of undoped ZnS nanoparticles, the Raman modes of Ce, Cu co- doped ZnS nanoparticles were slightly shifted towards lower frequency. PL spectra of the samples showed remarkable enhancement in the intensity upon doping.

Interaction of atomic oxygen with thin film and bulk copper: An XPS, AES, XRD, and profilometer study

NASA Technical Reports Server (NTRS)

Raikar, Genesh N.; Gregory, John C.; Christl, Ligia C.; Peters, Palmer N.

1992-01-01

The University of Alabama in Huntsville (UAH) experiment A-0114 was designed primarily to study degradation of material surfaces due to low earth orbital (LEO) atmospheric oxygen. The experiment contained 128 one inch circular samples: metals, polymers, carbons, and semiconductors. Among metal samples, copper has shown some interesting new results. Two types of copper samples, a film sputter coated on fused silica and a bulk piece of OFHC copper, were characterized employing a variety of techniques such as X-ray and Auger electron spectroscopies, X-ray diffraction, and high resolution profilometry. Cu 2p core level spectra were used to characterize the presence of Cu2O and CuO in addition to Cu Auger LMM lines. These results are supported by our recent X-ray diffraction studies which clearly establish the presence of Cu oxides which we were unable to prove in our earlier work. Profilometry showed an increase in thickness of the film sample where exposed to 106.7 +/- 0.5 nm from an initial thickness of 74.2 +/- 1.1 nm. Further studies with SEM and ellipsometry are underway.

Na0.44MnO2 nanorods as a cathode material for Na-ion batteries

NASA Astrophysics Data System (ADS)

Avci, Sevda; Oz, Erdinc; Demirel, Serkan; Altin, Emine; Altin, Serdar; Bayri, Ali; Yakinci, Eyyuphan

2014-03-01

Lithium-ion batteries have dominated the rechargeable battery market because of their high energy and power capability. On the other hand, sodium is one of the more abundant elements on Earth unlike Li. Moreover, Na has similar chemical properties to Li, indicating that Na-ion batteries can be an alternative to Li counterparts. With that respect, we have synthesized Na0.44MnO2 nanorods as cathode materials for Na-ion batteries. We have investigated the effects of structural, electrical, and magnetic properties on battery performance. We report the synthesis conditions and growth mechanism of the nanorods. The structure and the morphology of the materials were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX), and atomic force microscopy (AFM) techniques. Temperature dependent structural changes were determined via in situ X-ray diffraction and TG-DTA measurements showing structural changes above room temperature. This work is funded by The Scientific and Technological Research Council of Turkey with Grant No:112M487.

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

Effect of annealing temperature on the stress and structural properties of Ge core fibre

NASA Astrophysics Data System (ADS)

Zhao, Ziwen; Cheng, Xueli; Xue, Fei; He, Ting; Wang, Tingyun

2017-09-01

Effect of annealing temperature on the stress and structural properties of a Ge core fibre via the molten core drawing (MCD) method is investigated using Raman spectroscopy, Scanning electronic microscopy (SEM), and X-ray diffraction. The experimental results showed that the Raman peak position of the Ge fibre shifted from 297.6 cm-1 to 300.5 cm-1, and the FWHM value decreased from 4.53 cm-1 to 4.31 cm-1, when the annealing is carried out at 700 °C, 800 °C, and 900 °C, respectively. For the Ge core annealed at 900 °C, an apparent crystal grain can be seen in the SEM image, and the diffraction peaks of the (3 3 1) plane are generated in the X-ray diffraction spectra. These results show that optimising the annealing temperature allows the release of the residual stress in the Ge core. When the Ge core fibre is annealed at 900 °C, it exhibits the lowest residual stress and the highest crystal quality, and the quality improvement relative to that of the sample annealed at 800 °C is significant. Hence, annealing at around 900 °C can greatly improve the quality of a Ge core fibre. Further performance improvement of the Ge core fibre by annealing techniques can be anticipated.

Effect of Annealing Temperature on Structural and Optical Properties of Sol-Gel-Derived ZnO Thin Films

NASA Astrophysics Data System (ADS)

Arif, Mohd.; Sanger, Amit; Vilarinho, Paula M.; Singh, Arun

2018-04-01

Nanocrystalline ZnO thin films were deposited on glass substrate via sol-gel dip-coating technique then annealed at 300°C, 400°C, and 500°C for 1 h. Their optical, structural, and morphological properties were studied using ultraviolet-visible (UV-Vis) spectrophotometry, x-ray diffraction (XRD) analysis, and scanning electron microscopy (SEM). XRD diffraction revealed that the crystalline nature of the thin films increased with increasing annealing temperature. The c-axis orientation improved, and the grain size increased, as indicated by increased intensity of the (002) plane peak at 2θ = 34.42° corresponding to hexagonal ZnO crystal. The average crystallite size of the thin films ranged from 13 nm to 23 nm. Increasing the annealing temperature resulted in larger crystallite size and higher crystallinity with increased surface roughness. The grain size according to SEM analysis was in good agreement with the x-ray diffraction data. The optical bandgap of the thin films narrowed with increasing annealing temperature, lying in the range of 3.14 eV to 3.02 eV. The transmission of the thin films was as high as 94% within the visible region. The thickness of the thin films was 400 nm, as measured by ellipsometry, after annealing at the different temperatures of 300°C, 400°C, and 500°C.

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.

Thermoluminescence (TL) properties and x-ray diffraction (XRD) analysis of high purity CaSO4:Dy TL material

NASA Astrophysics Data System (ADS)

Kamarudin, Nadira; Abdullah, Wan Saffiey Wan; Hamid, Muhammad Azmi Abdul; Dollah, Mohd Taufik

2014-09-01

This paper presents the characterization and TL properties of dysprosium (Dy) doped calcium sulfate (CaSO4) TL material produced by co-precipitation technique with 0.5mol% concentration of dopant. The morphology of the produced TL material was studied using scanning electron microscope (SEM) and the micrograph shows that rectangular parallelepiped shaped crystal with the average of 150 μm in length were produced. The crystallinity of the produced powder was studied using x-ray powder diffraction (XRD). The XRD spectra show that the TL material produced is high purity anhydrite CaSO4 with average crystallite size of 74 nm with orthorhombic crystal system. The TL behavior of produced CaSO4:Dy was studied using a TLD reader after exposure to gamma ray by Co60 source with the doses of 1,5 and 10 Gy. The glow curve shows linear response with glow peak around 230°C which is desired development in the field of radiation dosimetry.

Preparation of K-doped TiO2 nanostructures by wet corrosion and their sunlight-driven photocatalytic performance

NASA Astrophysics Data System (ADS)

Shin, Eunhye; Jin, Saera; Kim, Jiyoon; Chang, Sung-Jin; Jun, Byung-Hyuk; Park, Kwang-Won; Hong, Jongin

2016-08-01

K-doped TiO2 nanowire networks were prepared by the corrosion reaction of Ti nanoparticles in an alkaline (potassium hydroxide: KOH) solution. The prepared nanostructures were characterized by scanning electron microscopy (SEM), Brunauer-Emmett-Teller (BET) analysis, X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, X-ray diffraction (XRD) and photoluminescence (PL) spectra. Their sunlight-driven photocatalytic activity was also investigated with differently charged dye molecules, such as methylene blue, rhodamine B and methyl orange. The adsorption of the dye molecules on the photocatalyst surface would play a critical role in their selective photodegradation under sunlight illumination.

Characteristics of Volcanic Soils in Landslide during the 2016 Kumamoto Earthquake, Japan

NASA Astrophysics Data System (ADS)

Hazarika, H.; Fukuoka, H.; Kokusho, T.; Sumartini, O.; Bhoopendra, D.

2017-12-01

There were many seismic subsidence, debris flows, landslides and slope failures, which occurred in Aso area due to the 2016 Kumamoto earthquake, Japan. This research aims to determine the failure mechanism of many mild slopes, and elucidate the strength characteristics of volcanic soils collected from the sites. A series of undrained static and cyclic triaxial tests, ring shear tests and direct shear tests were performed. Also, for further understanding of volcanic soils' material strength, X-ray powder diffraction analysis (XRD), X-ray fluorescence analysis (XRF), and Scanning electron microscope analysis (SEM) were performed. In this paper, preliminary results of the experimental testing program are discussed.

Preparation and Optoelectrical Properties of p-CuO/n-Si Heterojunction by a Simple Sol-Gel Method

NASA Astrophysics Data System (ADS)

He, Bo; Xu, Jing; Ning, Huanpo; Zhao, Lei; Xing, Huaizhong; Chang, Chien-Cheng; Qin, Yuming; Zhang, Lei

The Cuprous oxide (CuO) thin film was prepared on texturized Si wafer by a simple sol-gel method to fabricate p-CuO/n-Si heterojunction photoelectric device. The novel sol-gel method is very cheap and convenient. The structural, optical and electrical properties of the CuO film were studied by X-ray diffraction (XRD), Scanning Electron Microscope (SEM), X-ray photoelectron spectroscopy (XPS), UV-Vis spectrophotometer and Hall effect measurement. A good nonlinear rectifying behavior is obtained for the p-CuO/n-Si heterojunction. Under reverse bias, good photoelectric behavior is obtained.

Influence of sodium bis(2-ethylhexyl) sulfosuccinate (AOT) on zinc electrodeposition

NASA Astrophysics Data System (ADS)

Lehr, I. L.; Saidman, S. B.

2012-03-01

This work is a study of the electrodeposition of zinc onto SAE 4140 steel electrodes using solutions containing zinc sulfate and bis(2-ethylhexyl) sodium sulfosuccinate (AOT). The influence of different parameters such as electrolyte concentration, electrodeposition time and temperature on the morphology of the electrodeposits was analyzed. The deposits were characterized by scanning electron microscopy (SEM), energy dispersive X-ray (EDX) and X-ray diffraction. The variation of open circuit potential over time in chloride solutions was also evaluated. The nucleation-growth process and consequently the morphology of the electrodeposits are modified in the presence of AOT. The surfactant induces the formation of a porous deposit.

Synthesis, characterizations and catalytic activities of CoFe2O4 nanoparticles

NASA Astrophysics Data System (ADS)

Verma, Divya; Sharma, Vikash; Parmar, Sarita; Okram, Gunadhor Singh; Jain, Shubha

2018-05-01

We report the synthesis of CoFe2O4 nanoparticles (NPs) through a novel one-step coprecipitation method. These NPs were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDAX), Fourier transform infrared (FTIR), and Raman spectroscopy. These nano ferrites were successfully used for the synthesis of 3, 4-dihydropyrimidin-2(1H)-ones and thiones. They can be easily recovered by simple filtration and their catalytic activity remains nearly unaltered even after 4 consecutive cycles, making them ecofriendly and widely applicable due to their efficiency, ease of handling, and cost effectiveness.

Structural and physical property study of sol-gel synthesized CoFe2-xHoxO4 nano ferrites

NASA Astrophysics Data System (ADS)

Patankar, K. K.; Ghone, D. M.; Mathe, V. L.; Kaushik, S. D.

2018-05-01

CoFe2-xHoxO4 (x = 0.00, 0.05, 0.10, 0.15, 0.20) ferrites were prepared by the suitably modified Sol-Gel technique. X-ray diffraction (XRD) analysis revealed that the substituted samples show phase pure formation till 10% substitution, which is far higher phase pure than the earlier reports. Upon further substitution an inevitable secondary phase of HoFeO3 along with the spinel phase despite regulating synthesis parameters in the sol-gel reaction route. These results are further corroborated more convincingly by room temperature neutron diffraction. Morphological features of the ferrites were studied by Scanning Electron Microscopy (SEM). The magnetic parameters viz. the saturation magnetization (Ms), coercivity (Hc) and remanence (Mr) were determined from room temperature isothermal magnetization. These parameters were found to decrease with increase in Ho substitution. The decrease in magnetization is analyzed in the light of exchange interactions between rare earth and transition metal ions. Magnetostriction measurements revealed interesting results and the presence of a secondary phase was found to be responsible for decreased measu-red magnetostriction values. The solubility limit of Ho in CoFe2O4 lattice is also reflected from the X-ray and neutron diffraction analysis and magnetostriction studies.

New frontiers in water purification: highly stable amphopolycarboxyglycinate-stabilized Ag-AgCl nanocomposite and its newly discovered potential

NASA Astrophysics Data System (ADS)

Krutyakov, Yurii A.; Zherebin, Pavel M.; Kudrinskiy, Alexey A.; Zubavichus, Yan V.; Presniakov, Mikhail Yu; Yapryntsev, Alexey D.; Karabtseva, Anastasia V.; Mikhaylov, Dmitry M.; Lisichkin, Georgii V.

2016-09-01

A simple synthetic procedure for high-stable dispersions of porous composite Ag/AgCl nanoparticles stabilized with amphoteric surfactant sodium tallow amphopolycarboxyglycinate has been proposed for the first time. The prepared samples were characterized by UV-vis spectroscopy, x-ray powder diffraction (XRD), x-ray photoelectron spectroscopy, small area electron diffraction (SAED), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and electron probe micro-analysis. In addition, measurements (carried out at the Kurchatov synchrotron radiation source stations) of the Ag K-edge extended x-ray absorption fine structure (EXAFS) and x-ray absorption near edge structure (XANES) spectra and XRD of the prepared nanoparticles have been performed. The obtained results suggest that small-sized Ag clusters are homogeneously distributed in the mass of the AgCl nanoparticle (~80 nm) formed during the synthesis. The Ag/AgCl dispersion demonstrates photocatalytic activity (with respect to methyl orange) and high bactericidal activity against E. coli. This activity is superior to the activity of both Ag and AgCl nanoparticles stabilized by the same surfactant. Thus, porous composite Ag/AgCl nanoparticles can be used as a multifunctional agent that is able to remove both pollutants and bacterium from water.

Structural and magnetic properties of nanocrystalline NiFe2O4 thin film prepared by spray pyrolysis technique

NASA Astrophysics Data System (ADS)

Chavan, Apparao R.; Chilwar, R. R.; Shisode, M. V.; Hivrekar, Mahesh M.; Mande, V. K.; Jadhav, K. M.

2018-05-01

The nanocrystalline NiFe2O4 thin film has been prepared using a spray pyrolysis technique on glass substrate. The prepared thin film was characterized by using X-ray diffraction (XRD), Fourier transform Infrared spectroscopy (FTIR), and Field Emission-Scanning Electron Microscopy (FE-SEM) characterization techniques for the structural and microstructural analysis. The magnetic property was measured using vibrating sample magnetometer (VSM) at room temperature. X-ray diffraction studies show the formation of single phase spinel structure of the thin film. The octahedral and tetrahedral vibration in the sample was studied by Fourier transform infrared (FT-IR) spectra. Magnetic hysteresis loop was recorded for thin film at room temperature. At 15 kOe, saturation magnetization (Ms) was found to increase while coercivity (Hc) decreases with thickness of the NiFe2O4 thin film.

Influence of BN fiber coatings on the interfacial structure of sapphire fiber reinforced NiAl composites

NASA Astrophysics Data System (ADS)

Reichert, K.; Wen, K.; Cremer, R.; Hu, W.; Neuschütz, D.; Gottstein, G.

2001-07-01

A new concept for a tailored fiber-matrix interface for sapphire fiber reinforced NiAl matrix composites is proposed, consisting of an initial hexagonal boron nitride (hBN) fiber coating. For this, single crystal Al 2O 3 fibers were coated with hBN by chemical vapor deposition (CVD). Following a comprehensive characterization of the CVD coating as to composition and structure by means of X-ray photoelectron spectroscopy (XPS) and grazing incidence X-ray diffraction (GIXRD), the fiber reinforced NiAl matrix composites were fabricated by diffusion bonding at 1400°C. The interfaces NiAl/BN and BN/Al 2O 3 were analyzed by scanning electron microscopy (SEM), analytical transmission electron microscopy (TEM), and selected area diffraction (SAD). An interfacial reaction between NiAl and hBN to form AlN was revealed using these analytical techniques.

Algan/Gan Hemt By Magnetron Sputtering System

NASA Astrophysics Data System (ADS)

Garcia Perez, Roman

In this thesis, the growth of the semiconductor materials AlGaN and GaN is achieved by magnetron sputtering for the fabrication of High Electron Mobility Transistors (HEMTs). The study of the deposited nitrides is conducted by spectroscopy, diffraction, and submicron scale microscope methods. The preparation of the materials is performed using different parameters in terms of power, pressure, temperature, gas, and time. Silicon (Si) and Sapphire (Al2O3) wafers are used as substrates. The chemical composition and surface topography of the samples are analyzed to calculate the materials atomic percentages and to observe the devices surface. The instruments used for the semiconductors characterization are X-ray Photoelectron Spectroscopy (XPS), X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), and Atomic Force Microscope (AFM). The project focused its attention on the reduction of impurities during the deposition, the controlled thicknesses of the thin-films, the atomic configuration of the alloy AlxGa1-xN, and the uniformity of the surfaces.

Thin single-crystalline Bi2(Te1-xSex)3 ternary nanosheets synthesized by a solvothermal technique

NASA Astrophysics Data System (ADS)

Guo, Jing; Jian, Jikang; Zhang, Zhihua; Wu, Rong; Li, Jin; Sun, Yanfei

2016-01-01

Bi2(Te1-xSex)3 ternary nanosheets have been successfully synthesized through a facile solvothermal technique using diethylenetriamine as solvent, where x can vary from 0 to 1. X-ray diffraction (XRD) and Scanning electron microscopy (SEM) indicate that the as-synthesized Bi2(Te1-xSex)3 samples are nanosheets with rhombohedral structure, and the thickness of the nanosheets can be as thin as several nanometers. High resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED) reveal that the nanosheets are single crystalline with a rhombohedral structure. Energy disperse spectroscopy (EDS) and XRD analysis by Vegard's law confirm that the ternary Bi2(Te1-xSex)3 nanosheets have been obtained here. The growth of the nanosheets is discussed based on an amine-based molecular template mechanism that has been employed to synthesize some other metal chalcogenides.

Mayenite Synthesized Using the Citrate Sol-Gel Method

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

Ude, Sabina N; Rawn, Claudia J; Meisner, Roberta A

2014-01-01

A citrate sol-gel method has been used to synthesize mayenite (Ca12Al14O33). X-ray powder diffraction data show that the samples synthesized using the citrate sol-gel method contained CaAl2O4 and CaCO3 along with mayenite when fired ex-situ in air at 800 C but were single phase when fired at 900 C and above. Using high temperature x-ray diffraction, data collected in-situ in air at temperatures of 600 C and below showed only amorphous content; however, data collected at higher temperatures indicated the first phase to crystallize is CaCO3. High temperature x-ray diffraction data collected in 4% H2/96% N2 does not show themore » presence of CaCO3, and Ca12Al14O33 starts to form around 850 C. In comparison, x-ray powder diffraction data collected ex-situ on samples synthesized using traditional solid-state synthesis shows that single phase was not reached until samples were fired at 1350 C. DTA/TGA data collected either in a nitrogen environment or air on samples synthesized using the citrate gel method suggest the complete decomposition of metastable phases and the formation of mayenite at 900 C, although the phase evolution is very different depending on the environment. Brunauer-Emmett-Teller (BET) measurements showed a slightly higher surface area of 7.4 0.1 m2/g in the citrate gel synthesized samples compared to solid-state synthesized sample with a surface area of 1.61 0.02 m2/g. SEM images show a larger particle size for samples synthesized using the solid-state method compared to those synthesized using the citrate gel method.« 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.

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.

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.

Preparation and characterization of Fe50Co50 nanostructured alloy

NASA Astrophysics Data System (ADS)

Yepes, N.; Orozco, J.; Caamaño, Z.; Mass, J.; Pérez, G.

2014-04-01

Nanostructured Fe50Co50 alloy was prepared by mechanical alloying of Fe and Co powders in a planetary high energy ball milling. The microstructure and structural evolution of the alloy have been investigated as a function of milling time (0 h, 8 h, 20 h and 35 h) by scanning electron microscopy (SEM) and X-Ray diffraction (XRD) characterization techniques. SEM micrographs showed different powder particles morphologies during the mechanical alloying stages. By XRD analysis it could be identified the structural phases of the alloy and the crystallite size was calculated as a function of the milling time.

Synthesis and Characterization of Nd(3+)-Doped CaF2 Nanoparticles.

PubMed

Yuan, Dan; Li, Weiwei; Mei, Bingchu; Song, Jinghong

2015-12-01

The Ca(1-x)F(2+x):Nd(x) nanoparticles were synthesized by chemical direct precipitation method. X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Image analyzer, absorption spectrum and transmittance were taken to characterization the phases, morphologies, sizes, size distribution and optical properties of the samples. The results indicate that the Ca(1-x)F(2+x):Nd(x) samples can be rationally modified in size and morphology by altering the Nd3+ ions doping concentration. With increasing concentration of Nd3+ ions, the particle size decreased from 24 to 14 nm, the intensity of the diffraction peaks decreased, the Ca(1-x)F(2+x):Nd(x) particles aggregated ion of the formed clusters which should have an effect on both speed and orientation of the particles growth. The transmittance of ceramics with a thickness of 2 mm showed that the transmittance can reach 90% when the doping concentration was 5%, which should be profitable for LD pumping.

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.

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.

Micro X-ray diffraction analysis of thin films using grazing-exit conditions.

PubMed

Noma, T; Iida, A

1998-05-01

An X-ray diffraction technique using a hard X-ray microbeam for thin-film analysis has been developed. To optimize the spatial resolution and the surface sensitivity, the X-ray microbeam strikes the sample surface at a large glancing angle while the diffracted X-ray signal is detected with a small (grazing) exit angle. Kirkpatrick-Baez optics developed at the Photon Factory were used, in combination with a multilayer monochromator, for focusing X-rays. The focused beam size was about 10 x 10 micro m. X-ray diffraction patterns of Pd, Pt and their layered structure were measured. Using a small exit angle, the signal-to-background ratio was improved due to a shallow escape depth. Under the grazing-exit condition, the refraction effect of diffracted X-rays was observed, indicating the possibility of surface sensitivity.

Structural and magnetic properties of ytterbium substituted spinel ferrites

NASA Astrophysics Data System (ADS)

Alonizan, Norah H.; Qindeel, Rabia

2018-06-01

Chemical co-precipitation route adopted to synthesize the magnetic materials. In the present work, iron is replaced by ytterbium ion in manganese-based spinel ferrites. The yield chemically represented by MnYb x Fe2- x O4 ( x = 0.00, 0.025, 0.05, 0.075, 0.10) and its structural, magnetic and electrical properties were observed. The cubic structure of spinel ferrites was confirmed by X-ray diffraction analysis. Spherically shaped grains were perceived in SEM pictures and size lessened with the growth of ytterbium concentration. SEM profile also shows little irregularity in spherical particles. The substitution of ytterbium (Yb) results in the enhancement of electrical resistivity. The resistivity was reduced with the gradual increase in temperature from 303 to 693 K. The trend of activation energy was found to be similar to that of room temperature resistivity. The coercivity of samples was raised with Yb-ion substitution while saturation magnetization and remanence reduced.

Investigations on the in vitro bioactivity of swift heavy oxygen ion irradiated hydroxyapatite.

PubMed

Suganthi, R V; Prakash Parthiban, S; Elayaraja, K; Girija, E K; Kulariya, P; Katharria, Y S; Singh, F; Asokan, K; Kanjilal, D; Narayana Kalkura, S

2009-12-01

The effect of swift heavy oxygen ion irradiation of hydroxyapatite on its in vitro bioactivity was studied. The irradiation experiment was performed using oxygen ions at energy of 100 MeV with 1 x 10(12) and 1 x 10(13) ions/cm2 fluence range. The irradiated samples were characterized by glancing angle X-ray diffraction (GXRD), photoluminescence spectroscopy (PL) and scanning electron microscopy (SEM). GXRD showed that irradiated samples exhibited better crystallinity. The irradiated samples revealed an increase in PL intensity. In addition, the irradiated hydroxyapatite was found to have enhanced bioactivity.

Stable tetragonal phase and magnetic properties of Fe-doped HfO2 nanoparticles

NASA Astrophysics Data System (ADS)

Sales, T. S. N.; Cavalcante, F. H. M.; Bosch-Santos, B.; Pereira, L. F. D.; Cabrera-Pasca, G. A.; Freitas, R. S.; Saxena, R. N.; Carbonari, A. W.

2017-05-01

In this paper, the effect in structural and magnetic properties of iron doping with concentration of 20% in hafnium dioxide (HfO2) nanoparticles is investigated. HfO2 is a wide band gap oxide with great potential to be used as high-permittivity gate dielectrics, which can be improved by doping. Nanoparticle samples were prepared by sol-gel chemical method and had their structure, morphology, and magnetic properties, respectively, investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM) with electron back scattering diffraction (EBSD), and magnetization measurements. TEM and SEM results show size distribution of particles in the range from 30 nm to 40 nm with small dispersion. Magnetization measurements show the blocking temperature at around 90 K with a strong paramagnetic contribution. XRD results show a major tetragonal phase (94%).

Synthesis & characterization of Bi7.38Ce0.62O12.3 and its optical and electrocatalytic property

NASA Astrophysics Data System (ADS)

Padmanaban, A.; Dhanasekaran, T.; Kumar, S. Praveen; Gnanamoorthy, G.; Stephen, A.; Narayanan, V.

2017-05-01

Bismuth cerium oxide was synthesized by thermal decomposition method. The material was characterized by X-ray diffraction technique, DRS UV-Vis, Raman spectral methods and FE-SEM. The electrocatalytic sensing activity of bismuth cerium oxide modified GCE toward 4-nitrophenol exhibits better activity than the bare GCE. The modified electrode shows higher anodic current response with lower potential.

Green synthesis of gold nanoparticles using Stevia rebaudiana leaf extracts: Characterization and their stability.

PubMed

Sadeghi, Babak; Mohammadzadeh, M; Babakhani, B

2015-07-01

Various methods invented and developed for the synthesis of gold nanoparticles that increases daily consumed. According to this method, including potential environmental pollution problems and the complexity of the synthesis, in this study, the feasibility of using the leaves extract of Stevia rebaudiana (SR) for the reduction of gold ions to nanoparticles form have been studied. Stevia leaves were used to prepare the aqueous extract for this study. Gold nanoparticles were characterized with different techniques such as UV-vis spectroscopy, FT-IR spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Transmission electron microscopy experiments showed that these nanoparticles are spherical and uniformly distributed and its size is from 5 to 20 nm. FT-IR spectroscopy revealed that gold nanoparticles were functionalized with biomolecules that have primary amine group (NH2), carbonyl group, OH groups and other stabilizing functional groups. X-ray diffraction pattern showed high purity and face centered cubic structure of gold nanoparticles with size of 17 nm. The scanning electron microscopy (SEM) implies the right of forming gold nanoparticles. The results, confirm that gold nanoparticles have synthesized by the leaves extract of S. rebaudiana (SR). Copyright © 2015 Elsevier B.V. All rights reserved.

The effects of fuel type in synthesis of NiFe2O4 nanoparticles by microwave assisted combustion method

NASA Astrophysics Data System (ADS)

Karcıoğlu Karakaş, Zeynep; Boncukçuoğlu, Recep; Karakaş, İbrahim H.

2016-04-01

In this study, it was investigated the effects of the used fuels on structural, morphological and magnetic properties of nanoparticles in nanoparticle synthesis with microwave assisted combustion method with an important method in quick, simple and low cost at synthesis of the nanoparticles. In this aim, glycine, urea and citric acid were used as fuel, respectively. The synthesised nanoparticles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Brunauer-Emmet-Teller surface area (BET), and vibrating sample magnetometry (VSM) techniques. We observed that fuel type is quite effective on magnetic properties and surface properties of the nanoparticles. X-ray difractograms of the obtained nanoparticles were compared with standard powder diffraction cards of NiFe2O4 (JCPDS Card Number 54-0964). The results demonstrated that difractograms are fully compatible with standard reflection peaks. According to the results of the XRD analysis, the highest crystallinity was observed at nanoparticles synthesized with glycine. The results demonstrated that the nanoparticles prepared with urea has the highest surface area. The micrographs of SEM showed that all of the nanoparticles have nano-crystalline behaviour and particles indication cubic shape. VSM analysis demonstrated that the type of fuel used for synthesis is highly effective a parameter on magnetic properties of nanoparticles.

Phase transformation from cubic ZnS to hexagonal ZnO by thermal annealing

NASA Astrophysics Data System (ADS)

Mahmood, K.; Asghar, M.; Amin, N.; Ali, Adnan

2015-03-01

We have investigated the mechanism of phase transformation from ZnS to hexagonal ZnO by high-temperature thermal annealing. The ZnS thin films were grown on Si (001) substrate by thermal evaporation system using ZnS powder as source material. The grown films were annealed at different temperatures and characterized by X-ray diffraction (XRD), photoluminescence (PL), four-point probe, scanning electron microscope (SEM) and energy dispersive X-ray diffraction (EDX). The results demonstrated that as-deposited ZnS film has mixed phases but high-temperature annealing leads to transition from ZnS to ZnO. The observed result can be explained as a two-step process: (1) high-energy O atoms replaced S atoms in lattice during annealing process, and (2) S atoms diffused into substrate and/or diffused out of the sample. The dissociation energy of ZnS calculated from the Arrhenius plot of 1000/T versus log (resistivity) was found to be 3.1 eV. PL spectra of as-grown sample exhibits a characteristic green emission at 2.4 eV of ZnS but annealed samples consist of band-to-band and defect emission of ZnO at 3.29 eV and 2.5 eV respectively. SEM and EDX measurements were additionally performed to strengthen the argument.

In search of the elusive IrB{sub 2}: Can mechanochemistry help?

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

Xie, Zhilin; Blair, Richard G.; Department of Physics, University of Central Florida, Orlando, FL 32816

The previously unknown hexagonal ReB{sub 2}-type IrB{sub 2} diboride and orthorhombic IrB monoboride phases were produced by mechanochemical syntheses. High energy ball milling of elemental Ir and B powder for 30 h, followed by annealing of the powder at 1050 °C for 48 h, resulted in the formation of the desired phases. Both traditional laboratory and high resolution synchrotron X-ray diffraction (XRD) analyses were used for phase identification of the synthesized powder. In addition to XRD, scanning electron microscopy and transmission electron microscopy were employed to further characterize the microstructure of the phases produced. - Graphical abstract: ReB{sub 2}-type IrB{submore » 2} and a new IrB have been successfully synthesized for the first time using mechanochemical method. Crystal structures of IrB{sub 2} and IrB were studied by synchrotron X-ray diffraction. Microstructures of the new phases were characterized by SEM and TEM. - Highlights: • ReB{sub 2}-type IrB{sub 2} and a new IrB have been synthesized by mechanochemical method. • Crystal structures of IrB{sub 2} and IrB were studied by synchrotron XRD. • Microstructures of the new phases were characterized by SEM and TEM.« less

Evolution processes of the corrosion behavior and structural characteristics of plasma electrolytic oxidation coatings on AZ31 magnesium alloy

NASA Astrophysics Data System (ADS)

Chen, Dong; Wang, Ruiqiang; Huang, Zhiquan; Wu, Yekang; Zhang, Yi; Wu, Guorui; Li, Dalong; Guo, Changhong; Jiang, Guirong; Yu, Shengxue; Shen, Dejiu; Nash, Philip

2018-03-01

Evolution processes of the corrosion behavior and structural characteristics of the plasma electrolytic oxidation (PEO) coated AZ31 magnesium alloy were investigated by using scanning electron microscope (SEM) equipped with energy dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), potentio-dynamic polarization curves and electrochemical impedance spectroscopy (EIS) measurements. Detached coating samples were fabricated by an electrochemical method and more details of the internal micro-structure of coatings were clearly observed on the fractured cross-section morphologies of the samples compared to general polished cross-section morphologies. Evolution mechanisms of the coating corrosion behavior in relation to the evolution of micro-structural characteristics were discussed in detail.

SnS thin films deposited by chemical bath deposition, dip coating and SILAR techniques

NASA Astrophysics Data System (ADS)

Chaki, Sunil H.; Chaudhary, Mahesh D.; Deshpande, M. P.

2016-05-01

The SnS thin films were synthesized by chemical bath deposition (CBD), dip coating and successive ionic layer adsorption and reaction (SILAR) techniques. In them, the CBD thin films were deposited at two temperatures: ambient and 70 °C. The energy dispersive analysis of X-rays (EDAX), X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM) and optical spectroscopy techniques were used to characterize the thin films. The electrical transport properties studies on the as-deposited thin films were done by measuring the I-V characteristics, DC electrical resistivity variation with temperature and the room temperature Hall effect. The obtained results are deliberated in this paper.

Preparation and characterisation of titania/hydroxyapatite composite coatings obtained by sol-gel process.

PubMed

Milella, E; Cosentino, F; Licciulli, A; Massaro, C

2001-06-01

In the present work a titania network encapsulating a hydroxyapatite particulate phase is proposed as a bioceramic composite coating. The coating on a titanium substrate was produced starting from a sol containing a mixture of titania colloidal particles and hydroxyapatite submicron particles using the dip-coating technique. The microstructure, the morphology and the surface chemical composition of the coating were characterised using X-ray diffraction (XRD), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS), respectively. Adhesion tests were also performed. These analyses showed that the obtained coating was chemically clean, homogeneous, rough, porous, with a low thickness and well-defined phase composition as well as a good adhesion to the substrate.

Growth of GaN@InGaN Core-Shell and Au-GaN Hybrid Nanostructures for Energy Applications

DOE PAGES

Kuykendall, Tevye; Aloni, Shaul; Jen-La Plante, Ilan; ...

2009-01-01

We demonstrated a method to control the bandgap energy of GaN nanowires by forming GaN@InGaN core-shell hybrid structures using metal organic chemical vapor deposition (MOCVD). Furthermore, we show the growth of Au nanoparticles on the surface of GaN nanowires in solution at room temperature. The work shown here is a first step toward engineering properties that are crucial for the rational design and synthesis of a new class of photocatalytic materials. The hybrid structures were characterized by various techniques, including photoluminescence (PL), energy dispersive x-ray spectroscopy (EDS), transmission and scanning electron microscopy (TEM and SEM), and x-ray diffraction (XRD).

ZnO:Gd nanocrystals for fluorescent applications

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

Divya, N. K., E-mail: divyank90@gmail.com; Pradyumnan, P. P.

2016-05-23

Gadolinium doped ZnO crystals within the solubility limit of gadolinium in ZnO matrix were prepared by solid state reaction technique. The method is relatively less expense and enables the production in large scale. The samples were characterised by X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS), scanning electron microscopy (SEM), UV/Vis diffuse reflectance spectroscopy and photoluminescence techniques. Fluorescent property studies of gadolinium doped ZnO at room temperature show enhanced visible light emission due to the defects and oxygen vacancies produced via doping. This work reports the impact of gadolinium doping in the structural, optical and luminescent properties of ZnO inmore » detail.« less

Hydrothermal Synthesis of Nanoclusters of ZnS Comprised on Nanowires

PubMed Central

Ibupoto, Zafar Hussain; Khun, Kimleang; Liu, Xianjie; Willander, Magnus

2013-01-01

Cetyltrimethyl ammonium bromide cationic (CTAB) surfactant was used as template for the synthesis of nanoclusters of ZnS composed of nanowires, by hydrothermal method. The structural and morphological studies were performed by using X-ray diffraction (XRD), scanning electron microscopy (SEM) and high resolution transmission electron microscopy (HRTEM) techniques. The synthesized ZnS nanoclusters are composed of nanowires and high yield on the substrate was observed. The ZnS nanocrystalline consists of hexagonal phase and polycrystalline in nature. The chemical composition of ZnS nanoclusters composed of nanowires was studied by X-ray photo electron microscopy (XPS). This investigation has shown that the ZnS nanoclusters are composed of Zn and S atoms. PMID:28348350

Hydrothermal Synthesis of Nanoclusters of ZnS Comprised on Nanowires.

PubMed

Ibupoto, Zafar Hussain; Khun, Kimleang; Liu, Xianjie; Willander, Magnus

2013-09-09

Cetyltrimethyl ammonium bromide cationic (CTAB) surfactant was used as template for the synthesis of nanoclusters of ZnS composed of nanowires, by hydrothermal method. The structural and morphological studies were performed by using X-ray diffraction (XRD), scanning electron microscopy (SEM) and high resolution transmission electron microscopy (HRTEM) techniques. The synthesized ZnS nanoclusters are composed of nanowires and high yield on the substrate was observed. The ZnS nanocrystalline consists of hexagonal phase and polycrystalline in nature. The chemical composition of ZnS nanoclusters composed of nanowires was studied by X-ray photo electron microscopy (XPS). This investigation has shown that the ZnS nanoclusters are composed of Zn and S atoms.

Structural, Morphological, Differential Scanning Calorimetric and Thermogravimetric Studies of Ball Milled Fe Doped Nanoscale La0.67Sr0.33MnO3 Manganite

NASA Astrophysics Data System (ADS)

Astik, Nidhi; Jha, Prafulla K.; Pratap, Arun

2018-03-01

The ball milling route has been used to produce the La0.67Sr0.33Mn0.85Fe0.15O3 (LSMFO) nanocrystalline sample from oxide precursors. The sample was characterized using x-ray diffraction (XRD), a scanning electron microscope (SEM), energy dispersive x-ray spectroscopy (EDAX), differential scanning calorimetry (DSC) and thermogravimetric (TGA) measurements. The x-ray diffraction confirms the phase purity of sample and shows that the sample crystallizes in the rhombohedral perovskite structure with a R-3c space group. The scanning electron micrograph shows the presence of well-faceted crystallites of LSMFO. The EDAX spectrum demonstrates the molar ratio of different elements of nanocrystalline LSMFO. Furthermore, the crystallite size using the Debye-Scherrer formula and William-Hall analysis has been found as 24 nm and 29 nm, respectively. Our results support the idea that a good quality nanocrystalline LSMFO sample can be obtained using the ball milling route. We also discuss the DSC and TGA curves and analyse the results in terms of phase transition, calcination temperature and activation barrier energies.

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

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).

Simultaneous phase and morphology controllable synthesis of copper selenide films by microwave-assisted nonaqueous approach

NASA Astrophysics Data System (ADS)

Li, Jing; Fa, Wenjun; Li, Yasi; Zhao, Hongxiao; Gao, Yuanhao; Zheng, Zhi

2013-02-01

Copper selenide films with different phase and morphology were synthesized on copper substrate through controlling reaction solvent by microwave-assisted nonaqueous approach. The films were characterized by X-ray diffraction (XRD) and scanning electron microscope (SEM). The result showed that the pure films could be obtained using cyclohexyl alcohol or benzyl alcohol as solvent. The cubic Cu2-xSe dendrites were synthesized in cyclohexyl alcohol reaction system and hexagonal CuSe flaky crystals were obtained with benzyl alcohol as solvent.

X-ray diffraction from shock-loaded polycrystals.

PubMed

Swift, Damian C

2008-01-01

X-ray diffraction was demonstrated from shock-compressed polycrystalline metals on nanosecond time scales. Laser ablation was used to induce shock waves in polycrystalline foils of Be, 25-125 microm thick. A second laser pulse was used to generate a plasma x-ray source by irradiation of a Ti foil. The x-ray source was collimated to produce a beam of controllable diameter, which was directed at the Be sample. X-rays were diffracted from the sample, and detected using films and x-ray streak cameras. The diffraction angle was observed to change with shock pressure. The diffraction angles were consistent with the uniaxial (elastic) and isotropic (plastic) compressions expected for the loading conditions used. Polycrystalline diffraction will be used to measure the response of the crystal lattice to high shock pressures and through phase changes.

Preparation and physical properties of polycrystalline (Bi1-xPbx)2Sr2Ca2Cu3Oy high T c superconductors

NASA Astrophysics Data System (ADS)

Awan, M. S.; Maqsood, M.; Mirza, S. A.; Yousaf, M.; Maqsood, A.

1995-02-01

(Bi1-xPbx:)2Sr2Ca2Cu3Oy ( x = 0.3) high critical transition temperature ( T c) superconductors are synthesized by the solid-state reaction method in polycrystalline form. X-ray diffraction (XRD) studies, direct current (dc) electrical resistivity measurements, scanning electron microscopic (SEM) studies, critical current density measurements, and zero-field alternating current (ac) susceptibility measurements are performed to investigate the physical changes, structural changes, and magnetic behavior of the superconducting samples. X-ray diffraction studies show that a high T c phase exists with orthorhombic symmetry in the specimen. According to the XRD data, the lattice parameters of the high T c phase were determined as a = 0.537(1) nm, b = 0.539(1) nm, and c = 3.70(1) nm. The compound exhibits a superconducting transition at 106 ±1 K for zero resistance. The ac susceptibility measurements in zero field confirm the dc electrical resistivity results; hence both support the XRD results. The particle size and structural changes as a function of the cold-pressing and aging effect are also reported.

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

Non-Noble Metal Oxide Catalysts for Methane Catalytic Combustion: Sonochemical Synthesis and Characterisation

PubMed Central

Jędrzejczyk, Roman J.; Dziedzicka, Anna; Kuterasiński, Łukasz; Sitarz, Maciej

2017-01-01

The aim of this study was to obtain nanocrystalline mixed metal-oxide–ZrO2 catalysts via a sonochemically-induced preparation method. The effect of a stabiliser’s addition on the catalyst parameters was investigated by several characterisation methods including X-ray Diffraction (XRD), nitrogen adsorption, X-ray fluorescence (XRF), scanning electron microscopy (SEM) equipped with energy dispersive X-ray spectrometer (EDS), transmission electron microscopy (TEM) and µRaman. The sonochemical preparation method allowed us to manufacture the catalysts with uniformly dispersed metal-oxide nanoparticles at the support surface. The catalytic activity was tested in a methane combustion reaction. The activity of the catalysts prepared by the sonochemical method was higher than that of the reference catalysts prepared by the incipient wetness method without ultrasonic irradiation. The cobalt and chromium mixed zirconia catalysts revealed their high activities, which are comparable with those presented in the literature. PMID:28686190

Synthesis and characterization of CdS-based ternary composite for enhanced visible light-driven photocatalysis

NASA Astrophysics Data System (ADS)

Singh, Arvind; Sinha, A. S. K.

2018-09-01

Active ternary graphite and alumina-supported cadmium sulphide (CdS) composite was synthesized by impregnation method followed by high-temperature solid-gas reaction and characterized by X-ray diffraction (XRD), photoluminescence spectroscopy (PL), diffuse reflectance spectroscopy (DRS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDX) and X-ray photoelectron spectroscopy (XPS) techniques. The ternary CdS-graphite-alumina composite exhibited superior catalytic activity compared with the binary CdS-alumina composite due to its better visible-light absorption and higher charge separation. The ternary composite has a bed-type structure. It permits a greater interaction at the interface due to intimate contact between CdS and graphite in the ternary composite. This composite has a highly efficient visible light-driven photocatalytic activity for sustainable hydrogen production. It is also capable of degrading organic dyes in wastewater.

Corrosion product layers on magnesium alloys AZ31 and AZ61: Surface chemistry and protective ability

NASA Astrophysics Data System (ADS)

Feliu, S.; Llorente, I.

2015-08-01

This paper studies the chemical composition of the corrosion product layers formed on magnesium alloys AZ31 and AZ61 following immersion in 0.6 M NaCl, with a view to better understanding their protective action. Relative differences in the chemical nature of the layers were quantified by X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), energy dispersive analysis of X-ray (EDX) and low-angle X-ray diffraction (XRD). Corrosion behavior was investigated by Electrochemical Impedance Spectroscopy (EIS) and hydrogen evolution measurement. An inhibitive effect from the corrosion product layers was observed from EIS, principally in the case of AZ31, as confirmed by hydrogen evolution tests. A link was found between carbonate enrichment observed by XPS in the surface of the corrosion product layer, concomitant with the increase in the protective properties observed by EIS.

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

Garcia-Mateo, Carlos, E-mail: cgm@cenim.csic.es

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

Synthesis and characterization of NiO nanopowder by sol-gel process

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

Ningsih, Sherly Kasuma Warda

2015-09-30

Preparation of nickel oxide (NiO) nanopowder by sol-gel process has been studied. NiO nanopowders were obtained by sol-gel method by using nickel nitrate hexahydrate and sodium hydroxide and aquadest were used as precursor, agent precipitator and solvent, respectively. The powders were formed by drying at 110°C and followed by heating in the furnace at 400°C for 1.5 hours. The product was obtained black powder. The product was characterized by Energy Dispesive X-ray Fluorescence (ED-XRF), X-ray diffraction (XRD) and Scanning Electron Microscopy (SEM). The ED-XRF pattern shows the composition of NiO produced was 97.1%. The XRD pattern showed NiO forms weremore » produced generally in monoclinic stucture. The crystalline size of NiO was obtained in the range 40-85 nm. SEM micrograph clearly showed that powder had a spherical with uniform distribution size is 0.1-1.0 µm approximately.« less

Hydrogen Gas Sensing Characteristics of Nanostructured NiO Thin Films Synthesized by SILAR Method

NASA Astrophysics Data System (ADS)

Karaduman, Irmak; Çorlu, Tugba; Yıldırım, M. Ali; Ateş, Aytunç; Acar, Selim

2017-07-01

Nanostructured NiO thin films have been synthesized by a facile, low-cost successive ionic layer adsorption and reaction (SILAR) method, and the effects of the film thickness on their hydrogen gas sensing properties investigated. The samples were characterized by scanning electron microscopy (SEM), x-ray diffraction (XRD) analysis, and energy-dispersive x-ray analysis. The XRD results revealed that the crystallinity improved with increasing thickness, exhibiting polycrystalline structure. SEM studies showed that all the films covered the glass substrate well. According to optical absorption measurements, the optical bandgap decreased with increasing film thickness. The gas sensing properties of the nanostructured NiO thin films were studied as a function of operating temperature and gas concentration. The samples showed good sensing performance of H2 gas with high response. The maximum response was 75% at operating temperature of 200°C for hydrogen gas concentration of 40 ppm. These results demonstrate that nanostructured NiO thin films synthesized by the SILAR method have potential for application in hydrogen detection.

One-dimensional nanoferroic rods; synthesis and characterization

NASA Astrophysics Data System (ADS)

Ahmed, M. A.; Seddik, U.; Okasha, N.; Imam, N. G.

2015-11-01

One-dimensional nanoferroic rods of BaTiO3 were synthesized by improved citrate auto-combustion technology using tetrabutyl titanate. X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX), transmission electron microscopy (TEM), atomic force microscopy (AFM) and Fourier transform infrared spectroscopy (FTIR) have been used to characterize the prepared sample. The results indicated that the crystal structure of BaTiO3 is tetragonal phase with an average crystallite size of 47 nm. SEM image gives a cauliflower-like morphology of the agglomerated nanorods. The stoichiometry of the chemical composition of the BaTiO3 ceramic was confirmed by EDX. TEM micrograph exhibited that BaTiO3 nanoparticles have rod-like shape with an average length of 120 nm and width of 43 nm. AFM was used to investigate the surface topography and its roughness. The topography image in 3D showed that the BaTiO3 particles have a rod shape with an average particle size of 116 nm which in agreement with 3D TEM result.

Sonochemical synthesis and photocatalytic property of zinc oxide nanoparticles doped with magnesium(II)

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

Lu, Xianyong, E-mail: xylu@buaa.edu.cn; Liu, Zhaoyue; Zhu, Ying

2011-10-15

Highlights: {yields} Mg-doped ZnO nanoparticles were synthesized by sonochemical strategy. {yields} Mg-doped ZnO nanoparticles present good photocatalytic properties. {yields} The change of band gap contributes to their high efficiency in photocatalyst. -- Abstract: Mg-doped ZnO nanoparticles were successfully synthesized by sonochemical method. The products were characterized by scan electron microscopy (SEM) and X-ray powder diffraction (XRD). SEM images revealed that ZnO doped with Mg(II) nanoparticles and ZnO nanoparticles synthesized by the same strategy all had spherical topography. XRD patterns showed that the doped nanoparticles had the same crystals structures as the pure ZnO nanoparticles. The Mg-doped ZnO nanoparticles had largermore » lattice volume than the un-doped nanoparticles. X-ray photoelectron spectroscopy (XPS) not only demonstrated the moral ratio of Mg and Zn element on the surface of nanoparticles, but their valence in nanoparticles as well. The Mg-doped ZnO nanoparticles presented good properties in photocatalyst compared with pure ZnO nanoparticles.« less

Synthesis and characterization of bovine femur bone hydroxyapatite containing silver nanoparticles for the biomedical applications

NASA Astrophysics Data System (ADS)

Nirmala, R.; Sheikh, Faheem A.; Kanjwal, Muzafar A.; Lee, John Hwa; Park, Soo-Jin; Navamathavan, R.; Kim, Hak Yong

2011-05-01

Bovine femur bone hydroxyapatite (HA) containing silver (Ag) nanoparticles was synthesized by thermal decomposition method and subsequent reduction of silver nitrate with N, N-dimethylformamide (DMF) in the presence of poly(vinylacetate) (PVAc). The structural, morphological, and chemical properties of the HA-Ag nanoparticles were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS). TEM images showed that the Ag nanoparticles with size ranging from 8 to 20 nm and were arranged at the periphery of HA crystals. Bactericidal activity of HA-Ag with different concentration of Ag nanoparticles immobilized on the surface of HA was investigated against gram-positive Staphylococcus aureus ( S. aureus, non-MRSA), Methicillin resistant S. aureus (MRSA) and gram-negative Escherichia coli ( E. coli) by the disc diffusion susceptibility test. The HA-Ag nanoparticles showed that broad spectrum activity against non-MRSA, MRSA, and E. coli bacterial strains.

Metal copper films deposited on cenosphere particles by magnetron sputtering method

NASA Astrophysics Data System (ADS)

Yu, Xiaozheng; Xu, Zheng; Shen, Zhigang

2007-05-01

Metal copper films with thicknesses from several nanometres to several micrometres were deposited on the surface of cenosphere particles by the magnetron sputtering method under different working conditions. An ultrasonic vibrating generator equipped with a conventional magnetron sputtering apparatus was used to prevent the cenosphere substrates from accumulating during film growth. The surface morphology, the chemical composition, the average grain size and the crystallization of cenosphere particles were characterized by field emission scanning electron microscopy (FE-SEM), inductively coupled plasma-atom emission spectrometer, x-ray photoelectron spectroscopy and x-ray diffraction (XRD) analysis, respectively, before and after the plating process. The results indicate that the copper films were successfully deposited on cenosphere particles. It was found from the FE-SEM results that the films were well compacted and highly uniform in thickness. The XRD results show that the copper film coated on cenospheres has a face centred cubic structure and the crystallization of the film sample increases with increasing sputtering power.

Progress toward Synthesis and Characterization of Rare-Earth Nanoparticles

NASA Astrophysics Data System (ADS)

Romero, Dulce G.; Ho, Pei-Chun; Attar, Saeed; Margosan, Dennis

2010-03-01

Magnetic nanoparticles exhibit interesting phenomena, such as enhanced magnetization and reduced magnetic ordering temperature (i.e. superparamagnetism), which has technical applications in industry, including magnetic storage, magnetic imaging, and magnetic refrigeration. We used the inverse micelle technique to synthesize Gd and Nd nanoparticles given its potential to control the cluster size, amount of aggregation, and prevent oxidation of the rare-earth elements. Gd and Nd were reduced by NaBH4 from the chloride salt. The produced clusters were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDX). The results from the XRD show that the majority of the peaks match those of the surfactant, DDAB. No peaks of Gd were observed due to excess surfactant or amorphous clusters. However, the results from the SEM and EDX indicate the presence of Gd and Nd in our clusters microscopically, and current synthesized samples contain impurities. We are using liquid-liquid extraction method to purify the sample, and the results will be discussed.

Spectroscopic, microchemical and petrographic analyses of plasters from ancient buildings in Lamezia Terme (Calabria, Southern Italy)

NASA Astrophysics Data System (ADS)

De Luca, Raffaella; Gigliotti, Valentina; Panarello, Mario; Bloise, Andrea; Crisci, Gino M.; Miriello, Domenico

2016-01-01

This work shows the results of the spectroscopic, microchemical and petrographic study carried out on six plasters coming from three important residential buildings of the 18th century, located in Lamezia Terme (Catanzaro, Southern Italy). To study the provenance of the raw materials used to make the plasters, one sample of limestone and two samples of sand were also collected from the quarries near Lamezia Terme and compared with the historical plasters. Samples were studied by polarized optical microscopy (OM), X-ray powder diffraction (XRPD), scanning electron microscopy (SEM) with energy dispersive X-ray spectroscopy (EDS) and Raman spectroscopy. The results of these analyses allowed to determine the mineralogical, petrographical and chemical characteristics of the plasters, identify the pigments used for their coloration and provide useful information about the building techniques, the raw materials employed and the production technology of plasters during the 18th century in Lamezia Terme. SEM-EDS microanalysis also revealed the presence of gold and silver on the surface of two samples.

Template-Free Synthesis and Enhanced Photocatalytic Performance of Uniform BiOCI Flower-Like Microspheres.

PubMed

Chang, Fei; Xie, Yunchao; Chen, Juan; Luo, Jieru; Li, Chenlu; Hu, Xuefeng; Xu, Bin

2015-02-01

Preparation of uniform BiOCI flower-like microspheres was facilely accomplished through a sim- ple protocol involving regulation of pH value in aqueous with sodium hydroxide in the presence of n-propanol. The as-prepared samples were characterized by a collection of techniques, such as X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDX), UV-vis diffuse reflectance spectroscopy (UV-vis DRS), and nitrogen adsorption-desorption isotherms. Based upon the SEM analyses, uniform microspheres could be formed with coexistence of some fragments of BiOCI nanosheets without n-propanol. The addition of appropriate amount of n-propanol was beneficial to provide BiOCI samples containing only flower-like microspheres, which were further subjected to the photocatalytic measurements towards Rhodamine B in aqueous under visible light irradiation and exhibited the best catalytic performance among all samples tested. In addition, the photocatalytic process was confirmed to undergo through a photosensitization pathway, in which superoxide radicals (.O-) played critical roles.

Eco-friendly and green synthesis of BiVO4 nanoparticle using microwave irradiation as photocatalayst for the degradation of Alizarin Red S

NASA Astrophysics Data System (ADS)

Abraham, S. Daniel; David, S. Theodore; Bennie, R. Biju; Joel, C.; Kumar, D. Sanjay

2016-06-01

Bismuth vanadate (BiVO4) nanocrystals have been successfully synthesised using microwave-assisted combustion synthesis (MCS), and characterised using Fourier transform infrared (FT-IR) and Raman spectra, surface area analysis (BET), X-ray diffraction (XRD), scanning electron microscopy (SEM), Energy Dispersive X-ray analysis (EDX), diffused reflectance spectroscopy (DRS) and Photoluminescence (PL) spectroscopy. The XRD results confirmed the formation of monoclinic bismuth vanadate. The formations of BiO & VO43-vibrations were ascertained from FT-IR data. The morphology of hallow internal structural micro entities were confirmed by SEM. The optical properties were determined by DRS and PL spectra. Hence, the influence of the preparation methods on the structure, morphology and optical activities of bismuth vanadate was investigated systematically. Photocatalytic degradation (PCD) of Alizarin Red S (ARS), an effective disrupting chemical in aqueous medium was investigated using BiVO4 nanoparticles. The kinetics of PCD was found to follow pseudo first-order.

Hydrothermal synthesis of β-Ni(OH)2 and its supercapacitor properties

NASA Astrophysics Data System (ADS)

Waghmare, Suraj S.; Patil, Prashant B.; Baruva, Shiva K.; Rajput, Madhuri S.; Deokate, Ramesh J.; Mujawar, Sarfraj H.

2018-04-01

In present manuscript, we synthesized the Nickel hydroxide as an electrode material or supercapacitor application, using hydrothermal method with nickel nitrate as nickel source and hexamethylenetetramine as a directing agent. The reaction was carried out at 160°C temperature for 18 hrs. The structural, morphological and electrochemical characterizations were studied by X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Cyclic Voltammetry (CV) and Galvanostatic Charge Discharge (GCD) respectively. Phase purity and crystalline nature of as prepared nickel hydroxide β-Ni(OH)2 was reveled from X-ray study. Using Debye Scherer's formula crystallite size of ˜15 nm was estimated for Nickel hydroxide. SEM reveals β-platelets like morphology of Ni(OH)2 average of platelets length of the order of 1 µm. Electrochemical studies (CV and GCD) were carried out in 2M KOH electrolyte solution. The maximum capacitance of 225 Fg-1 was observed for scan rate 5 mV within the potential window of 0.1 to 0.4 V.

Single-pulse x-ray diffraction using polycapillary optics for in situ dynamic diffraction

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

Maddox, B. R., E-mail: maddox3@llnl.gov; Akin, M. C., E-mail: akin1@llnl.gov; Teruya, A.

2016-08-15

Diagnostic use of single-pulse x-ray diffraction (XRD) at pulsed power facilities can be challenging due to factors such as the high flux and brightness requirements for diffraction and the geometric constraints of experimental platforms. By necessity, the x-ray source is usually positioned very close, within a few inches of the sample. On dynamic compression platforms, this puts the x-ray source in the debris field. We coupled x-ray polycapillary optics to a single-shot needle-and-washer x-ray diode source using a laser-based alignment scheme to obtain high-quality x-ray diffraction using a single 16 ns x-ray pulse with the source >1 m from themore » sample. The system was tested on a Mo sample in reflection geometry using 17 keV x-rays from a Mo anode. We also identified an anode conditioning effect that increased the x-ray intensity by 180%. Quantitative measurements of the x-ray focal spot produced by the polycapillary yielded a total x-ray flux on the sample of 3.3 ± 0.5 × 10{sup 7} molybdenum Kα photons.« less

Thermoluminescence (TL) properties and x-ray diffraction (XRD) analysis of high purity CaSO{sub 4}:Dy TL material

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

Kamarudin, Nadira; Abdullah, Wan Saffiey Wan; Dollah, Mohd Taufik

2014-09-03

This paper presents the characterization and TL properties of dysprosium (Dy) doped calcium sulfate (CaSO{sub 4}) TL material produced by co-precipitation technique with 0.5mol% concentration of dopant. The morphology of the produced TL material was studied using scanning electron microscope (SEM) and the micrograph shows that rectangular parallelepiped shaped crystal with the average of 150 μm in length were produced. The crystallinity of the produced powder was studied using x-ray powder diffraction (XRD). The XRD spectra show that the TL material produced is high purity anhydrite CaSO{sub 4} with average crystallite size of 74 nm with orthorhombic crystal system. Themore » TL behavior of produced CaSO{sub 4}:Dy was studied using a TLD reader after exposure to gamma ray by Co{sup 60} source with the doses of 1,5 and 10 Gy. The glow curve shows linear response with glow peak around 230°C which is desired development in the field of radiation dosimetry.« less

Study of the Decomposition and Phase Transition of Uranium Nitride under UHV Conditions via TDS, XRD, SEM, and XPS.

PubMed

Wang, Xiaofang; Long, Zhong; Bin, Ren; Yang, Ruilong; Pan, Qifa; Li, Fangfang; Luo, Lizhu; Hu, Yin; Liu, Kezhao

2016-11-07

Uranium nitrides are among the most promising fuels for Generation IV nuclear reactors, but until now, very little has been known about their thermal stability properties under nonequilibrium conditions. In this work, thermal decomposition of nitrogen-rich uranium nitride (denoted as UN 2-x ) under ultrahigh-vacuum (UHV) conditions was investigated by thermal desorption spectroscopy (TDS). It has been shown that the nitrogen TDS spectrum consists of two peaks at about 723 and 1038 K. The X-ray diffraction, scanning electron microscopy, and X-ray photoelectron microscopy results indicate that UN 2-x (UN 2 phase) decomposed into the α-U 2 N 3 phase in the first step and the α-U 2 N 3 phase decomposed into the UN phase in the second step.

Synthesis and photocatalytic properties of TiO{sub 2} nanostructures

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

Xia, X.H.; Liang, Y.; Wang, Z.

2008-08-04

TiO{sub 2} particles, rods, flowers and sheets were prepared by hydrothermal method via adjusting the temperature, the pressure and the concentration of TiCl{sub 4}. The as-prepared TiO{sub 2} powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectra and N{sub 2} adsorption-desorption measurements. It was found that pressure is the most important factor influencing the morphology of TiO{sub 2}. The photocatalytic activity of the products was evaluated by the photodegradation of aqueous brilliant red X-3B solution under UV light. Among the as-prepared nanostructures, the flower-like TiO{sub 2}more » exhibited the highest photocatalytic activity.« less

Low temperature nucleation of Griffiths Phase in Co doped LaMnO3 nanostructures

NASA Astrophysics Data System (ADS)

Adeela, N.; Khan, U.; Naz, S.; Iqbal, M.; Irfan, M.; Cheng, Y.

2017-11-01

We have reported magnetic properties of La1-xCoxMnO3 nanostructures synthesized by hydrothermal route. The crystal structure has been characterized by X-ray diffraction (XRD) technique, which shows rhombohedral perovskite structure at room temperature. Scanning electron microscope (SEM) and energy dispersive X-ray spectroscopy (EDS) have been used to analyse morphology and chemical composition of prepared nanoparticles. Magnetic hysteresis loops of all the samples exhibit ferromagnetic behaviour at 10 K. Inverse susceptibility graphs as a function of temperature represent deviation from Curie Weiss law. The indication for short range ferromagnetic clusters well above Curie temperature is observed due to the Griffiths Phase (GP). It is proposed that the presence of GP arises from induced size effects of La and Co ions.

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 Diffraction Apparatus

NASA Technical Reports Server (NTRS)

Blake, David F. (Inventor); Bryson, Charles (Inventor); Freund, Friedmann (Inventor)

1996-01-01

An x-ray diffraction apparatus for use in analyzing the x-ray diffraction pattern of a sample is introduced. The apparatus includes a beam source for generating a collimated x-ray beam having one or more discrete x-ray energies, a holder for holding the sample to be analyzed in the path of the beam, and a charge-coupled device having an array of pixels for detecting, in one or more selected photon energy ranges, x-ray diffraction photons produced by irradiating such a sample with said beam. The CCD is coupled to an output unit which receives input information relating to the energies of photons striking each pixel in the CCD, and constructs the diffraction pattern of photons within a selected energy range striking the CCD.

Fabrication, characterization and gas sensing studies of PPy/MWCNT/SLS nanocomposite

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

Tiwari, D. C., E-mail: dctiwari2001@yahoo.com; Atri, Priyanka, E-mail: dctiwari2001@yahoo.com; Sharma, R.

2014-04-24

Multiwall carbon nanotubes (MWCNT) coated with polypyrrole nanocomposite was prepared by in-situ chemical oxidative polymerization method in the presence of surfactant (SLS). The scanning electron microscope (SEM) pictures indicate the core shell structure of PPy/MWCNT/SLS nanocomposite. Nature of the prepared material was investigated by X-ray diffraction spectroscopy. This nanocomposite shows the excellent gas sensing behaviour for ammonia gas at 150 ppm and 300 ppm levels.

Structural and dielectric studies on Ag doped nano ZnSnO3

NASA Astrophysics Data System (ADS)

Deepa, K.; Angel, S. Lilly; Rajamanickam, N.; Jayakumar, K.; Ramachandran, K.

2018-04-01

Undoped and Ag-doped nano Zinc Stannate (ZSO) ternary oxide were prepared by co-precipitation method. The crystallographic, morphological and optical properties of the synthesized nanoparticles were studied using X-ray diffraction (XRD) and UV-Visible spectroscopy (UV-Vis) and Scanning electron microscopy (SEM). The electrical properties of the synthesized samples were studied by dielectric measurements. Higher concentration Ag doped ZSO nanoparticles exhibit higher dielectric constant at low frequency.

Removal of Micrometer Size Morphological Defects and Enhancement of Ultraviolet Emission by Thermal Treatment of Ga-Doped ZnO Nanostructures

PubMed Central

Manzoor, Umair; Kim, Do K.; Islam, Mohammad; Bhatti, Arshad S.

2014-01-01

Mixed morphologies of Ga-doped Zinc Oxide (ZnO) nanostructures are synthesized by vapor transport method. Systematic scanning electron microscope (SEM) studies of different morphologies, after periodic heat treatments, gives direct evidence of sublimation. SEM micrographs give direct evidence that morphological defects of nanostructures can be removed by annealing. Ultra Violet (UV) and visible emission depends strongly on the annealing temperatures and luminescent efficiency of UV emission is enhanced significantly with each subsequent heat treatment. X-Ray diffraction (XRD) results suggest that crystal quality improved by annealing and phase separation may occur at high temperatures. PMID:24489725

Removal of micrometer size morphological defects and enhancement of ultraviolet emission by thermal treatment of Ga-doped ZnO nanostructures.

PubMed

Manzoor, Umair; Kim, Do K; Islam, Mohammad; Bhatti, Arshad S

2014-01-01

Mixed morphologies of Ga-doped Zinc Oxide (ZnO) nanostructures are synthesized by vapor transport method. Systematic scanning electron microscope (SEM) studies of different morphologies, after periodic heat treatments, gives direct evidence of sublimation. SEM micrographs give direct evidence that morphological defects of nanostructures can be removed by annealing. Ultra Violet (UV) and visible emission depends strongly on the annealing temperatures and luminescent efficiency of UV emission is enhanced significantly with each subsequent heat treatment. X-Ray diffraction (XRD) results suggest that crystal quality improved by annealing and phase separation may occur at high temperatures.

Ba0.06(Na,Bi)0.94Ti1-x(Ni1/3Nb2/3)xO3 ceramics: X-ray diffraction and infrared spectroscopy studies

NASA Astrophysics Data System (ADS)

Mishra, R. K.; Prasad, Ashutosh; Chandra, K. P.; Prasad, K.

2018-05-01

Non-lead ceramic samples of Ba0.06(Na0.5Bi0.5)0.94Ti1-x(Ni1/3Nb2/3)xO3; 0 ≤ x ≤ 1.0 were prepared by standard high temperature ceramic synthesis method. Rietveld refinements of X-ray diffraction data of these ceramics were carried out using FullProf software and determined their crystal symmetry, space group and unit cell dimensions. Rietveld refinement revealed that Ba0.06(Na0.5Bi0.5)0.94TiO3 has a monoclinic structure with space group P4/m while B0.06(Na0.5Bi0.5)0.94(Ni1/3Nb2/3)O3 has tetragonal (pseudo-cubic) structure with space group P4/mmm. Partial replacement of Ti4+ ion by pseudo-cation (Ni1/33 +Nb2/3 5 +) 4 + resulted in the change of unit cell structure from monoclinic to tetragonal. SEM studies were carried out in order to access the quality of the prepared ceramics which showed a change in grain sizes with the increase of (Ni1/33 +Nb2/3 5 +) 4 + content. FTIR spectra confirmed the formation of perovskite type solid solutions.

Real-time X-ray Diffraction: Applications to Materials Characterization

NASA Technical Reports Server (NTRS)

Rosemeier, R. G.

1984-01-01

With the high speed growth of materials it becomes necessary to develop measuring systems which also have the capabilities of characterizing these materials at high speeds. One of the conventional techniques of characterizing materials was X-ray diffraction. Film, which is the oldest method of recording the X-ray diffraction phenomenon, is not quite adequate in most circumstances to record fast changing events. Even though conventional proportional counters and scintillation counters can provide the speed necessary to record these changing events, they lack the ability to provide image information which may be important in some types of experiment or production arrangements. A selected number of novel applications of using X-ray diffraction to characterize materials in real-time are discussed. Also, device characteristics of some X-ray intensifiers useful in instantaneous X-ray diffraction applications briefly presented. Real-time X-ray diffraction experiments with the incorporation of image X-ray intensification add a new dimension in the characterization of materials. The uses of real-time image intensification in laboratory and production arrangements are quite unlimited and their application depends more upon the ingenuity of the scientist or engineer.

Improving the oxidation resistance and stability of Ag nanoparticles by coating with multilayered reduced graphene oxide

NASA Astrophysics Data System (ADS)

Li, Yahui; Zhang, Huayu; Wu, Bowen; Guo, Zhuo

2017-12-01

A kind of coating nanostructure, Ag nanoparticles coated with multilayered reduced graphene oxide (RGO), is fabricated by employing a three-step reduction method in an orderly manner, which is significantly different from the conventional structures that are simply depositing or doping with Ag nanoparticles on RGO via chemical reduction. The as-prepared nanostructure is investigated by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected-area electronic diffraction (SEAD), scanning electron microscopy (SEM), and Fourier transform infrared spectroscopy (FTIR). The results show that the obtained Ag/RGO nanostructure is observed to be a perfect coating structure with well dispersed Ag particles, which is responsible for the remarkable oxidation resistance. The results of XPS spectra indicate the content of metallic Ag is far greater than that of Ag oxides despite of prolonged exposure to the air, which fully demonstrate the excellent stability of thus coating nanostructure.

Ultrasonic irradiation-assisted synthesis of Bi2S3 nanoparticles in aqueous ionic liquid at ambient condition.

PubMed

de la Parra-Arciniega, Salomé M; Garcia-Gomez, Nora A; Garza-Tovar, Lorena L; García-Gutiérrez, Domingo I; Sánchez, Eduardo M

2017-05-01

In this work, an easy, fast and environmentally friendly method to obtain Bi 2 S 3 nanostructures with sphere-like morphology is introduced. The promising material was successfully synthesized by a sonochemical route in 20% 1-ethyl-3-methylimidazolium ethyl sulfate [EMIM][EtSO 4 ] ionic liquid solution (IL). Morphological studies by electron microscopy (SEM and TEM) show that the use of IL in the synthesis of Bi 2 S 3 favors the formation of nanocrystals non-agglomerated. Micro Raman and energy dispersive X-ray spectroscopy (EDXS) were used to determine the composition and purity of the synthesized material. X-ray powder diffraction (XRD) and selective area electron diffraction (SAED) revealed that ultrasonic radiation accelerated the crystallization of Bi 2 S 3 into orthorhombic bismuthinite structure. The band gap calculated from the diffuse reflectance spectra (DRS) was found to be 1.5eV. Copyright © 2016 Elsevier B.V. All rights reserved.

A simple and low temperature process for super-hydrophilic rutile TiO 2 thin films growth

NASA Astrophysics Data System (ADS)

Mane, R. S.; Joo, Oh-Shim; Min, Sun-Ki; Lokhande, C. D.; Han, Sung-Hwan

2006-11-01

We investigate an environmentally friendly aqueous solution system for rutile TiO2 violet color nanocrystalline thin films growth on ITO substrate at room temperature. Film shows considerable absorption in visible region with excitonic maxima at 434 nm. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), UV-vis, water surface contact angle and energy dispersive X-ray analysis (EDX) techniques in addition to actual photo-image that shows purely rutile phase of TiO2 with violet color, super-hydrophilic and densely packed nanometer-sized spherical grains of approximate diameter 3.15 ± 0.4 nm, characterize the films. Band gap energy of 4.61 eV for direct transition was obtained for the rutile TiO2 films. Film surface shows super-hydrophilic behavior, as exhibited water contact angle was 7°. Strong visible absorption (not due to chlorine) leaves future challenge to use these films in extremely thin absorber (ETA) solar cells.

Preparation, Physical-Chemical Characterization, and Cytocompatibility of Polymeric Calcium Phosphate Cements

PubMed Central

Khashaba, Rania M.; Moussa, Mervet; Koch, Christopher; Jurgensen, Arthur R.; Missimer, David M.; Rutherford, Ronny L.; Chutkan, Norman B.; Borke, James L.

2011-01-01

Aim. Physicochemical mechanical and in vitro biological properties of novel formulations of polymeric calcium phosphate cements (CPCs) were investigated. Methods. Monocalcium phosphate, calcium oxide, and synthetic hydroxyapatite were combined with either modified polyacrylic acid, light activated polyalkenoic acid, or polymethyl vinyl ether maleic acid to obtain Types I, II, and III CPCs. Setting time, compressive and diametral strength of CPCs was compared with zinc polycarboxylate cement (control). Specimens were characterized using X-ray diffraction, scanning electron microscopy, and infrared spectroscopy. In vitro cytotoxicity of CPCs and control was assessed. Results. X-ray diffraction analysis showed hydroxyapatite, monetite, and brushite. Acid-base reaction was confirmed by the appearance of stretching peaks in IR spectra of set cements. SEM revealed rod-like crystals and platy crystals. Setting time of cements was 5–12 min. Type III showed significantly higher strength values compared to control. Type III yielded high biocompatibility. Conclusions. Type III CPCs show promise for dental applications. PMID:21941551

Physicochemical behavior of several kinds of paper under gamma irradiation

NASA Astrophysics Data System (ADS)

Jiménez-Reyes, Melania; Tenorio, Dolores; Rojas-Robles, Mariela; García-Rosales, Genoveva

2018-07-01

Several kinds of paper (Bond, Amate, Rice, Press, and Whatman#1) were studied in their original condition and were then exposed to gamma radiation between 3 and 15 kGy (0.9 kGy/h) with intervals of 3 kGy. The length and width of fibers (SEM) as well as pH were measured, and the chemical composition was determined by EDS. Pyrolysis characteristics (TGA and DTC), transmittance spectra by IR and X-ray diffraction patterns were studied as well. Whatman#1 contains only cellulose; whereas Bond, Press and Rice papers also contain calcite and Amate whewellite. All X-ray diffraction patterns showed Type I semicrystalline cellulose, but a slight presence of Type II was noted in the artisan papers (Amate and Rice). These results were confirmed by IR spectra and thermogravimetric analyses. Due to gamma irradiation no acidification nor change of fiber sizes or alteration of other studied parameters were observed. Therefore, these conditions may be recommended for the treatment of some deteriorated documents.

Development of Cu Reinforced SiC Particulate Composites

NASA Astrophysics Data System (ADS)

Singh, Harshpreet; Kumar, Lailesh; Nasimul Alam, Syed

2015-02-01

This paper presents the results of Cu-SiCp composites developed by powder metallurgy route and an attempt has been made to make a comparison between the composites developed by using unmilled Cu powder and milled Cu powder. SiC particles as reinforcement was blended with unmilled and as-milled Cu powderwith reinforcement contents of 10, 20, 30, 40 vol. % by powder metallurgy route. The mechanical properties of pure Cu and the composites developed were studied after sintering at 900°C for 1 h. Density of the sintered composites were found out based on the Archimedes' principle. X-ray diffraction of all the composites was done in order to determine the various phases in the composites. Scanning electron microscopy (SEM) and EDS (electron diffraction x-ray spectroscopy) was carried out for the microstructural analysis of the composites. Vickers microhardness tester was used to find out the hardness of the samples. Wear properties of the developed composites were also studied.

CdO-NPs; synthesis from 1D new nano Cd coordination polymer, characterization and application as anti-cancer drug for reducing the viability of cancer cells

NASA Astrophysics Data System (ADS)

Afzalian Mend, Behnaz; Delavar, Mahmoud; Darroudi, Majid

2017-04-01

The hexagonal CdO nano-particles (CdO-NPs) was prepared using new nano Cd coordination polymer, [Cd(NO3)(bipy)(pzca)]n (1) as a precursor, through direct calcination process at 500 °C. The precursor (1) was synthesized by sonochemical method. The new nano compound (1) was characterized by IR spectroscopy, elemental analyses, X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and thermal gravimetric analyses. The structure of nano coordination polymer was determined by comparing the XRD pattern of nano and single-crystal of compound (1). The nano CdO was characterized by scanning electron microscopy (SEM) and X-ray powder diffraction (XRD). In addition, the activity and efficiency of nano CdO as an anti-cancer drug was studied on cancer cells with different concentration. The results shows that the viability of cancer cells reduced above 2 μg/mL of CdO-NPs concentration.

Fluorescence and physical properties of the organic salt 2-chloro-4-nitrobenzoate-3-ammonium-phenol

NASA Astrophysics Data System (ADS)

Mani, Rajaboopathi; Rietveld, Ivo B.; Nicolaï, Béatrice; Varadharajan, Krishnakumar; Louhi-Kultanen, Marjatta; Narasimhan, Surumbarkuzhali

2015-09-01

Organic salt 2-chloro-4-nitrobenzoate (CNBA-) 3-ammonium-phenol (AP+) exhibits fluorescence at 338 nm in solution and frontier molecular orbitals generated from TDDFT calculations indicate that the ground state and the excited state are physically separated on AP+ and CNBA-. The crystal structure and physical-chemical properties of the CNBA- · AP+ were investigated using X-ray single crystal and powder diffraction, SEM, FTIR, UV-Vis-NIR, and fluorescence spectrometry. X-ray diffraction demonstrates that the two molecules are linked via N+-H⋯O- ammonium-carboxylate interactions, as expected considering their interaction propensities. Proton transfer has been confirmed by FTIR analysis. The melting point of CNBA- · AP+ was observed at 186 °C, which is higher than pure CNBA (140 °C) or AP (120 °C). The observation of a spatially separated HOMO and LUMO possessing a narrow ΔEST = 73.3 meV and an emission in the blue region is promising as an alternative method for the production of OLED materials.

Formation of Porous Germanium Layers by Silver-Ion Implantation

NASA Astrophysics Data System (ADS)

Stepanov, A. L.; Vorob'ev, V. V.; Nuzhdin, V. I.; Valeev, V. F.; Osin, Yu. N.

2018-04-01

We propose a method for the formation of porous germanium ( P-Ge) layers containing silver nanoparticles by means of high-dose implantation of low-energy Ag+ ions into single-crystalline germanium ( c-Ge). This is demonstrated by implantation of 30-keV Ag+ ions into a polished c-Ge plate to a dose of 1.5 × 1017 ion/cm2 at an ion beam-current density of 5 μA/cm2. Examination by high-resolution scanning electron microscopy (SEM), atomic-force microscopy (AFM), X-ray diffraction (XRD), energy-dispersive X-ray (EDX) microanalysis, and reflection high-energy electron diffraction (RHEED) showed that the implantation of silver ions into c-Ge surface led to the formation of a P-Ge layer with spongy structure comprising a network of interwoven nanofibers with an average diameter of ˜10-20 nm Ag nanoparticles on the ends of fibers. It is also established that the formation of pores during Ag+ ion implantation is accompanied by effective sputtering of the Ge surface.

Functional properties of poly(tetrafluoroethylene) (PTFE) gasket working in nuclear reactor conditions

NASA Astrophysics Data System (ADS)

Wyszkowska, Edyta; Leśniak, Magdalena; Kurpaska, Lukasz; Prokopowicz, Rafal; Jozwik, Iwona; Sitarz, Maciej; Jagielski, Jacek

2018-04-01

In this study structural and nanomechanical properties of polytetrafluoroethylene (PTFE) used as a gasket in the nuclear reactor have been deeply investigated. In order to reveal structural changes caused by long-term pressure, temperature and irradiation (possibly neutron and gamma), methods such as SEM, X-ray diffraction and Raman Spectroscopy have been used. Nanomechanical properties such as Young Modulus and hardness were investigated by means of the nanoindentation technique. Presented study confirmed the influence of working (radiative) environment on the functional properties of PTFE. The results of Raman spectroscopy and X-ray diffraction techniques revealed shift of the major band positions and band intensities increase. Moreover, changes of hardness and Young Modulus values of the irradiated material with respect to the virgin specimen have been recorded. This phenomenon can be attributed to the modifications in crystallinity of the material. Presented work suggest that morphology of the irradiated material altered from well-ordered parallel fibers to more dense and thicker ones.

Synthesis of boron nitride nanostructures from catalyst of iron compounds via thermal chemical vapor deposition technique

NASA Astrophysics Data System (ADS)

da Silva, Wellington M.; Ribeiro, Hélio; Ferreira, Tiago H.; Ladeira, Luiz O.; Sousa, Edésia M. B.

2017-05-01

For the first time, patterned growth of boron nitride nanostructures (BNNs) is achieved by thermal chemical vapor deposition (TCVD) technique at 1150 °C using a mixture of FeS/Fe2O3 catalyst supported in alumina nanostructured, boron amorphous and ammonia (NH3) as reagent gas. This innovative catalyst was synthesized in our laboratory and systematically characterized. The materials were characterized by X-ray diffraction (XRD), Raman spectroscopy, Fourier-transform infrared spectroscopy (FTIR), Thermogravimetric analysis (TGA), Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). The X-ray diffraction profile of the synthesized catalyst indicates the coexistence of three different crystal structures showing the presence of a cubic structure of iron oxide and iron sulfide besides the gamma alumina (γ) phase. The results show that boron nitride bamboo-like nanotubes (BNNTs) and hexagonal boron nitride (h-BN) nanosheets were successfully synthesized. Furthermore, the important contribution of this work is the manufacture of BNNs from FeS/Fe2O3 mixture.

Synthesis and spectral studies on Cd(II) dithiocarbamate complexes and their use as precursors for CdS nanoparticles

NASA Astrophysics Data System (ADS)

Sathiyaraj, Ethiraj; Padmavathy, Krishnaraj; Kumar, Chandran Udhaya; Krishnan, Kannan Gokula; Ramalingan, Chennan

2017-11-01

Bis(N-cyclopropyl-N-4-chlorobenzyldithiocarbamato-S,S‧)cadmium(II) (1) and (2,2‧-bipyridine) bis(N-cyclopropyl-N-4-chlorobenzyldithiocarbamato-S,S‧)cadmium(II) (2) have been synthesized and characterized by FT-IR, 1HNMR and 13C NMR analyses. For the complex 2, single crystal X-ray diffraction analysis and computational studies (optimized geometry, HOMO-LUMO and MEP) have been executed employing DFT/B3LYP method with LANL 2DZ basic set. The optimized bond lengths and bond angles agree well with the experimental results. The complexes 1 and 2 have been used as single source precursors for the synthesis of ethyleneglycol capped CdS1 and CdS2 nanoparticles, respectively. CdS1 and CdS2 nanoparticles have been synthesized by solvothermal method. PXRD, SEM, Elemental colour mapping, EDAX, TEM and UV-Vis spectroscopy have been used to characterize the as-prepared CdS nanoparticles. The X-ray diffraction pattern confirms both their hexagonal structures.

CMC-coated Fe3O4 nanoparticles as new MRI probes for hepatocellular carcinoma

NASA Astrophysics Data System (ADS)

Sitthichai, Sudarat; Pilapong, Chalermchai; Thongtem, Titipun; Thongtem, Somchai

2015-11-01

Pure Fe3O4 nanoparticles and Fe3O4 magnetic nanoparticles (MNPs) coated with carboxymethyl cellulose (CMC) were successfully prepared by co-precipitating of FeCl2·4H2O and FeCl3·6H2O in the solutions containing ammonia at 80 °C for 3 h. Phase, morphology, particle-sized distribution, surface chemistry, and weight loss were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM) including high-resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED), thermogravimetric analysis (TGA), and Fourier transform infrared (FTIR) spectroscopy. In this research, CMC-coated Fe3O4 MNPs consisting of Fe2+ and Fe3+ ions with 543.3-mM-1 s-1 high relaxivity were detected and were able to be used for magnetic resonance imaging (MRI) application with very good contrast for targeting hepatocellular carcinoma (HCC) without any further vectorization.

Attenuation of encrustation by self-assembled inorganic fullerene-like nanoparticles

NASA Astrophysics Data System (ADS)

Ron, Racheli; Zbaida, David; Kafka, Ilan Z.; Rosentsveig, Rita; Leibovitch, Ilan; Tenne, Reshef

2014-04-01

Ureteral stents and urethral catheters are commonly used medical devices for maintaining urinary flow. However, long-term placement (>30 days) of these devices in the urinary tracts is limited by the development of encrustation, a phenomenon that holds a prevalence of 50% within this patient population, resulting in a great deal of morbidity to the patients. Here we report the influence of surface coating of an all-silicone catheter with rhenium-doped fullerene-like molybdenum disulfide (Re:IF-MoS2) nanoparticles on the growth and attachment of in vitro encrustation stones. Scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS) and X-ray powder diffraction (XRD) analyses indicated a remarkable attenuation in encrustation occupation on the Re:IF-MoS2-coated catheter surfaces compared to neat catheters. The doped nanoparticles displayed a unique tendency to self-assemble into mosaic-like arrangements, modifying the surface to be encrustation-repellent. The mechanism of encrustation retardation on the surface coated catheters is discussed in some detail. The ramification of these results for the clogging of other body indwelling devices is briefly discussed.Ureteral stents and urethral catheters are commonly used medical devices for maintaining urinary flow. However, long-term placement (>30 days) of these devices in the urinary tracts is limited by the development of encrustation, a phenomenon that holds a prevalence of 50% within this patient population, resulting in a great deal of morbidity to the patients. Here we report the influence of surface coating of an all-silicone catheter with rhenium-doped fullerene-like molybdenum disulfide (Re:IF-MoS2) nanoparticles on the growth and attachment of in vitro encrustation stones. Scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS) and X-ray powder diffraction (XRD) analyses indicated a remarkable attenuation in encrustation occupation on the Re:IF-MoS2-coated catheter surfaces compared to neat catheters. The doped nanoparticles displayed a unique tendency to self-assemble into mosaic-like arrangements, modifying the surface to be encrustation-repellent. The mechanism of encrustation retardation on the surface coated catheters is discussed in some detail. The ramification of these results for the clogging of other body indwelling devices is briefly discussed. Electronic supplementary information (ESI) available. See DOI: 10.1039/c3nr06231g

Radiation damage free ghost diffraction with atomic resolution

DOE PAGES

Li, Zheng; Medvedev, Nikita; Chapman, Henry N.; ...

2017-12-21

The x-ray free electron lasers can enable diffractive structural determination of protein nanocrystals and single molecules that are too small and radiation-sensitive for conventional x-ray diffraction. However the electronic form factor may be modified during the ultrashort x-ray pulse due to photoionization and electron cascade caused by the intense x-ray pulse. For general x-ray imaging techniques, the minimization of the effects of radiation damage is of major concern to ensure reliable reconstruction of molecular structure. Here in this paper, we show that radiation damage free diffraction can be achieved with atomic spatial resolution by using x-ray parametric down-conversion and ghostmore » diffraction with entangled photons of x-ray and optical frequencies. We show that the formation of the diffraction patterns satisfies a condition analogous to the Bragg equation, with a resolution that can be as fine as the crystal lattice length scale of several Ångstrom. Since the samples are illuminated by low energy optical photons, they can be free of radiation damage.« less

Radiation damage free ghost diffraction with atomic resolution

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

Li, Zheng; Medvedev, Nikita; Chapman, Henry N.

The x-ray free electron lasers can enable diffractive structural determination of protein nanocrystals and single molecules that are too small and radiation-sensitive for conventional x-ray diffraction. However the electronic form factor may be modified during the ultrashort x-ray pulse due to photoionization and electron cascade caused by the intense x-ray pulse. For general x-ray imaging techniques, the minimization of the effects of radiation damage is of major concern to ensure reliable reconstruction of molecular structure. Here in this paper, we show that radiation damage free diffraction can be achieved with atomic spatial resolution by using x-ray parametric down-conversion and ghostmore » diffraction with entangled photons of x-ray and optical frequencies. We show that the formation of the diffraction patterns satisfies a condition analogous to the Bragg equation, with a resolution that can be as fine as the crystal lattice length scale of several Ångstrom. Since the samples are illuminated by low energy optical photons, they can be free of radiation damage.« less

Synchrotron Radiation X-ray Diffraction Techniques Applied to Insect Flight Muscle.

PubMed

Iwamoto, Hiroyuki

2018-06-13

X-ray fiber diffraction is a powerful tool used for investigating the molecular structure of muscle and its dynamics during contraction. This technique has been successfully applied not only to skeletal and cardiac muscles of vertebrates but also to insect flight muscle. Generally, insect flight muscle has a highly ordered structure and is often capable of high-frequency oscillations. The X-ray diffraction studies on muscle have been accelerated by the advent of 3rd-generation synchrotron radiation facilities, which can generate brilliant and highly oriented X-ray beams. This review focuses on some of the novel experiments done on insect flight muscle by using synchrotron radiation X-rays. These include diffraction recordings from single myofibrils within a flight muscle fiber by using X-ray microbeams and high-speed diffraction recordings from the flight muscle during the wing-beat of live insects. These experiments have provided information about the molecular structure and dynamic function of flight muscle in unprecedented detail. Future directions of X-ray diffraction studies on muscle are also discussed.

Microstructural, Optical and Dielectric Properties of Al-Incorporated SnO2 Nanoparticles

NASA Astrophysics Data System (ADS)

Ahmed, Ateeq; Tripathi, P.; Naseem Siddique, M.; Ali, Tinku

2017-08-01

In this work, Pure SnO2 and Al doped SnO2 nanoparticles with the composition Sn1-xAlxO2 (x = 0, and 0.05) have been successfully prepared using sol-gel technique. The effect of Al dopant on microstructural, optical and dielectric properties has been investigated by X-ray diffraction (XRD), Scanning electron microscopy (SEM), Ultraviolet (UV-Visible) absorption spectroscopy andImpedance spectroscopy (LCR meter)respectively. The XRD patterns indicated tetragonal rutile structure with single phase without any detectable impurity for all samples and incorporation of Al ions into the SnO2 lattice. Crystalline size decreased with aluminum content. The results of SEM confirm nanoparticles size decreases with Al dopant. UV-Visible results showed that optical band also decreases when Al is doped into pure SnO2 lattice. Frequency dependent dielectric properties of pure and doped SnO2 nanoparticles have been also studied.

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.

Characterisation of the rare cadmium chromate pigment in a 19th century tube colour by Raman, FTIR, X-ray and EPR

NASA Astrophysics Data System (ADS)

Christiansen, Marie Bitsch; Sørensen, Mikkel Agerbæk; Sanyova, Jana; Bendix, Jesper; Simonsen, Kim Pilkjær

2017-03-01

In an investigation of the artists' materials used by P. S. Krøyer the contents of the tube colours found in Krøyer's painting cabinet were examined. In most cases, the results of the pigment analyses were as expected based on our knowledge of artists' colours used in the late 1800s and early 1900s. However, in one of the tube colours labelled "Jaune de Cadmium Citron" (cadmium lemon yellow) an extremely rare cadmium chromate pigment was found. The pigment was analysed and characterised by Raman microscopy (MRS), scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS), attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR), powder X-ray diffraction (PXRD), single-crystal X-ray crystallography, and electron paramagnetic resonance (EPR) spectroscopy. Cadmium chromate was synthesised by precipitation from an aqueous solution of cadmium nitrate and potassium chromate, and the resulting yellow crystals proved identical to the pigment found in the tube colour "Jaune de Cadmium Citron". The structure determined by single-crystal X-ray diffraction identified the pigment as 2CdCrO4·KOH·H2O or more accurately as KCd2(CrO4)2(H3O2) illustrating the μ-H3O2- species. The yellow colour of the paint sample taken from the tube had a greenish hue, which became even more prominent upon storage and drying. EPR analysis of the sample showed the presence of paramagnetic degradation products containing Cr(III) and Cr(V).

Characterisation of the rare cadmium chromate pigment in a 19th century tube colour by Raman, FTIR, X-ray and EPR.

PubMed

Christiansen, Marie Bitsch; Sørensen, Mikkel Agerbæk; Sanyova, Jana; Bendix, Jesper; Simonsen, Kim Pilkjær

2017-03-15

In an investigation of the artists' materials used by P. S. Krøyer the contents of the tube colours found in Krøyer's painting cabinet were examined. In most cases, the results of the pigment analyses were as expected based on our knowledge of artists' colours used in the late 1800s and early 1900s. However, in one of the tube colours labelled "Jaune de Cadmium Citron" (cadmium lemon yellow) an extremely rare cadmium chromate pigment was found. The pigment was analysed and characterised by Raman microscopy (MRS), scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS), attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR), powder X-ray diffraction (PXRD), single-crystal X-ray crystallography, and electron paramagnetic resonance (EPR) spectroscopy. Cadmium chromate was synthesised by precipitation from an aqueous solution of cadmium nitrate and potassium chromate, and the resulting yellow crystals proved identical to the pigment found in the tube colour "Jaune de Cadmium Citron". The structure determined by single-crystal X-ray diffraction identified the pigment as 2CdCrO 4 ·KOH·H 2 O or more accurately as KCd 2 (CrO 4 ) 2 (H 3 O 2 ) illustrating the μ-H 3 O 2 - species. The yellow colour of the paint sample taken from the tube had a greenish hue, which became even more prominent upon storage and drying. EPR analysis of the sample showed the presence of paramagnetic degradation products containing Cr(III) and Cr(V). Copyright © 2016 Elsevier B.V. All rights reserved.

Synthesis, crystal structure, vibrational spectroscopy and photoluminescence of new hybrid compound containing chlorate anions of stanate (II)

NASA Astrophysics Data System (ADS)

Lassoued, Mohamed Saber; Abdelbaky, Mohammed S. M.; Lassoued, Abdelmajid; Meroño, Rafael Mendoza; Gadri, Abdellatif; Ammar, Salah; Ben Salah, Abdelhamid; García-Granda, Santiago

2017-08-01

The present work aimed at studying a new organic-inorganic bis (4-amino quinolinium) hexachloro stanate (II) dihydrate compound. It was prepared and characterized by single crystal X-ray diffraction, X-ray powder, Hirshfeld surface, Spectroscopy measurement, thermal study and photoluminescence properties. It was found to crystallize in the monoclinic system (P21/c space group) with the following lattice parameters: a = 7.2558(6) Å, b = 13.4876(5) Å, c = 17.2107(13) Å, β = 102.028 (12)°. Its crystal structure was determined and refined down to an R value of 0.06 and a wR value of 0.087. The structure consisted of two different alternating organic-inorganic layers. The crystal packing was stabilized by Nsbnd H⋯Cl and Osbnd H⋯Cl hydrogen bonds and π-π interactions. Hirshfeld surface analysis was used to investigate intermolecular interactions, as well 2D finger plots were conducted to reveal the contribution of these interactions in the crystal structure quantitatively. The X-ray powder is in agreement with the X-ray structure. Scanning electronic microscopy (SEM) was carried out. Furthermore, the room temperature Infra Red (IR) spectrum of the title compound was analyzed on the basis of data found in the literature. Solid state 13C NMR spectrum shows ten signals, confirming the solid state structure determined by X-ray diffraction. Thermal analysis shows two anomalies at 380 and 610 °C. The optical properties of the crystal were studied using optical absorption UV-visible and photoluminescence (PL) spectroscopy, which were investigated at room temperature.

Synthesis of Zeolite-X from Bottom Ash for H2 Adsorption

NASA Astrophysics Data System (ADS)

Kurniawan, R. Y.; Romadiansyah, T. Q.; Tsamarah, A. D.; Widiastuti, N.

2018-01-01

Zeolite-X was synthesized from bottom ash power plant waste using fusion method on air atmosphere. The fused product dissolved in demineralized water and aluminate solution was added to adjust the SiO2/Al2O3 molar ratio gel prior hydrothermal process. The synthesis results were characterized using X-Ray Diffraction (XRD), Scanning Electron Microscope (SEM), and Fourier Transform Infrared (FTIR). The results showed that the zeolite-X has a high crystallinity with octahedral particle. The pure-form zeolite-X then was characterized and tested for H2 gas adsorption by gravimetric method to determine the H2 gas adsorption capacity of zeolite-X from bottom ash and it was compared to synthetic zeolite-X.

Combining experiment and optical simulation in coherent X-ray nanobeam characterization of Si/SiGe semiconductor heterostructures

DOE PAGES

Tilka, J. A.; Park, J.; Ahn, Y.; ...

2016-07-06

Here, the highly coherent and tightly focused x-ray beams produced by hard x-ray light sources enable the nanoscale characterization of the structure of electronic materials but are accompanied by significant challenges in the interpretation of diffraction and scattering patterns. X-ray nanobeams exhibit optical coherence combined with a large angular divergence introduced by the x-ray focusing optics. The scattering of nanofocused x-ray beams from intricate semiconductor heterostructures produces a complex distribution of scattered intensity. We report here an extension of coherent xray optical simulations of convergent x-ray beam diffraction patterns to arbitrary x-ray incident angles to allow the nanobeam diffraction patternsmore » of complex heterostructures to be simulated faithfully. These methods are used to extract the misorientation of lattice planes and the strain of individual layers from synchrotron x-ray nanobeam diffraction patterns of Si/SiGe heterostructures relevant to applications in quantum electronic devices. The systematic interpretation of nanobeam diffraction patterns from semiconductor heterostructures presents a new opportunity in characterizing and ultimately designing electronic materials.« less

Perovskite-Type Oxides. I. Structural, Magnetic, and Morphological Properties of LaMn 1- xCu xO 3 and LaCo 1- xCu xO 3 Solid Solutions with Large Surface Area

NASA Astrophysics Data System (ADS)

Porta, Piero; De Rossi, Sergio; Faticanti, Marco; Minelli, Giuliano; Pettiti, Ida; Lisi, Luciana; Turco, Maria

1999-09-01

Perovskite-type compounds of general formula LaMn1-xCuxO3 and LaCo1-xCuxO3 (x=0.0, 0.2, 0.4, 0.6, 0.8, 1.0) were prepared by calcining the citrate gel precursors at 823, 923, and 1073 K. The decomposition of the precursors was followed by thermal analysis and the oxides were investigated by means of elemental analysis (atomic absorption and redox titration), X-ray powder diffraction, BET surface area, X-ray absorption (EXAFS and XANES), electron microscopy (SEM and TEM), and magnetic susceptibility. LaMn1-xCuxO3 samples are perovskite-like single phases up to x=0.6. At x=0.8 CuO and La2CuO4 phases are present in addition to perovskite. For x=1.0 the material is formed by CuO and La2CuO4. Mn(IV) was found by redox titration in all Mn-based perovskite samples, its fraction increasing with the increase in copper content. EXAFS and XANES analyses confirmed the presence of Mn(IV). Cation vacancies in equal amounts in the 12-coordinated A and octahedral B sites are suggested in the samples with x=0.0 and x=0.2, while for x=0.6 anionic vacancies are present. Materials with sufficiently high surface area (22-36 m2 g-1 for samples fired at 923 K and 14-22 m2 g-1 for those fired at 1073 K) were obtained. Crystallite sizes in the ranges 390-500 and 590-940 Å for samples calcined at 923 and 1073 K, respectively, were determined from the FWHM of the (102) X-ray diffraction peak. TEM patterns of LaMnO3 showed almost regular hexagonal prismatic crystals with sizes of the same order of magnitude (800 Å) of those drawn from X-ray diffraction, while no evidence of defect clustering was drawn out from TEM and electron diffraction images. For the sample with x=0.6, TEM and electron diffraction patterns revealed perturbation of the structure. Magnetic susceptibility studies show a ferromagnetic behavior that decreases with increase in x. LaCo1-xCuxO3 samples are perovskite-like single phases up to x=0.2. For x=0.4 a small amount of La2CuO4, in addition to perovskite, is detected. For x≥0.6 massive formation of La2CuO4 and CuO is observed. Only trivalent cobalt is found by redox titration. Magnetic susceptibility studies have shown that trivalent cobalt is present in all samples as a mixture of paramagnetic Co3+ and diamagnetic CoIII ions, the Co3+ fraction being, at least up to x=0.4, equal to ≈0.34. Antiferromagnetic behavior, which increases with increase in x, is observed in all LaCo1-xCuxO3 samples. LaCoO3 is a stoichiometric perovskite. The substitution of cobalt by Cu2+ leads to a positive charge defectivity which is compensated by oxygen vacancies. EXAFS and XANES analyses confirmed the presence of trivalent cobalt. Materials with fairly high surface area (in the ranges 19-27 and 13-21 m2 g-1 for samples calcined at 923 and 1073 K, respectively) were obtained. Crystallite sizes of ≈400 and ≈1000 Å for samples calcined at 923 and 1073 K, respectively, were determined from the FWHM of the (102) X-ray diffraction peak. Materials with not very clear morphology and crystals with definite structure are distinguishable by SEM for samples calcined at 1073 and at 1273 K, respectively. TEM patterns, for samples calcined at 1073 K, evidence almost regular hexagonal prismatic crystals connected to form "linked structures" and some "spotty crystals," suggesting short-range ordered local defects. For copper-containing samples, calcined at 1273 K, a higher degree of defectivity (probably associated with the interaction of anion vacancies) and the occurrence of "planar faults" are shown by TEM.

Synthesis and synchrotron characterisation of novel dual-template of hydroxyapatite scaffolds with controlled size porous distribution

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

Lima, Thiago A. R. M.; Ilavsky, Jan; Hammons, Joshua

Hydroxyapatite (HAP) scaffolds with a hierarchical porous architecture were prepared by a new dual-template (corn starch and cetyltrimethylammonium bromide (CTAB) surfactant) used to cast HAP nanoparticles and development scaffolds with size hierarchical porous distribution. The Powder X-Ray diffraction (XRD) results showed that only the HAP crystalline phase is present in the samples after calcination; the Scanning Electron Microscopy (SEM) combined with Small Angle (SAXS) and Ultra-Small Angle X-ray Scattering (USAXS) techniques showed that the porous arrangement is promoted by needle-like HAP nanoparticles, and that the pore size distributions depend on the drip-order of the calcium and the phosphate solutions duringmore » the template preparation stage.« less

Graphene nanoplate-MnO2 composites for supercapacitors: a controllable oxidation approach.

PubMed

Huang, Huajie; Wang, Xin

2011-08-01

Graphene nanoplate-MnO(2) composites have been synthesized by oxidising part of the carbon atoms in the framework of graphene nanoplates at ambient temperature. The composites were characterized by means of X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV). It was found that the oxidation extent of the carbon atoms in the graphene framework in these composites was dependent on the reaction time, which also influenced their microstructure, morphology and electrochemical properties. Compared with MnO(2) nanolamellas, the nanocomposite prepared with a reaction time of 3 h reveals better electrochemical properties as a supercapacitor electrode material. This journal is © The Royal Society of Chemistry 2011

Deuterium permeation of amorphous alumina coating on 316L prepared by MOCVD

NASA Astrophysics Data System (ADS)

Li, Shuai; He, Di; Liu, Xiaopeng; Wang, Shumao; Jiang, Lijun

2012-01-01

The deuterium permeation behavior of the alumina coating on 316L stainless steel prepared by metal organic chemical vapor deposition (MOCVD) was investigated. The alumina coating was also characterized by X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and scanning electron microscope (SEM). It was found that the as-prepared coating consisted of amorphous alumina. This alumina coating had a dense, crack-free and homogeneous morphology. Although the alumina coating was amorphous, effective suppression of deuterium permeation was demonstrated. The deuterium permeability of the alumina coating was 51-60 times less than that of the 316L stainless steel and 153-335 times less than that of the referred low activation martensitic steels at 860-960 K.

Effect of annealing temperature on titania nanoparticles

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

Manikandan, K., E-mail: sanjaymani367@gmail.com; Arumugam, S., E-mail: sanjaymani367@gmail.com; Chandrasekaran, G.

2014-04-24

Titania polycrystalline samples are prepared by using sol-gel route hydrolyzing a alkoxide titanium precursor under acidic conditions. The as prepared samples are treated with different calcination temperatures. The anatase phase of titania forms when treated below 600°C, above that temperature the anatase phase tends to transform into the rutile phase of titania. The experimental determination of average grain size, phase formation, lattice parameters and the crystal structures of titania samples at different calcinations is done using X-ray diffraction (XRD). Fourier Transform Infra-red Spectroscopy (FTIR), UV-vis-NIR spectroscopy and Scanning Electron Microscopy (SEM) and Energy Dispersive Analysis X-ray are used to characterizemore » the samples to bring impact on the respective properties.« less

Impact of physical and chemical parameters on the hydroxyapatite nanopowder synthesized by chemical precipitation method

NASA Astrophysics Data System (ADS)

Thu Trang Pham, Thi; Phuong Nguyen, Thu; Pham, Thi Nam; Phuong Vu, Thi; Tran, Dai Lam; Thai, Hoang; Thanh Dinh, Thi Mai

2013-09-01

In this paper, the synthesis of hydroxyapatite (HAp) nanopowder was studied by chemical precipitation method at different values of reaction temperature, settling time, Ca/P ratio, calcination temperature, (NH4)2HPO4 addition rate, initial concentration of Ca(NO3)2 and (NH4)2HPO4. Analysis results of properties, morphology, structure of HAp powder from infrared (IR) spectra, x-ray diffraction (XRD), energy dispersive x-ray (EDX) spectra and scanning electron microscopy (SEM) indicated that the synthesized HAp powder had cylinder crystal shape with size less than 100 nm, single-phase structure. The variation of the synthesis conditions did not affect the morphology but affected the size of HAp crystals.

Biosynthesis and characterization of silver nanoparticles prepared from two novel natural precursors by facile thermal decomposition methods

NASA Astrophysics Data System (ADS)

Goudarzi, Mojgan; Mir, Noshin; Mousavi-Kamazani, Mehdi; Bagheri, Samira; Salavati-Niasari, Masoud

2016-09-01

In this work, two natural sources, including pomegranate peel extract and cochineal dye were employed for the synthesis of silver nanoparticles. The natural silver complex from pomegranate peel extract resulted in nano-sized structures through solution-phase method, but this method was not efficient for cochineal dye-silver precursor and the as-formed products were highly agglomerated. Therefore, an alternative facile solid-state approach was investigated as for both natural precursors and the results showed successful production of well-dispersed nanoparticles with narrow size distribution for cochineal dye-silver precursor. The products were characterized by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), Energy dispersive X-ray microanalysis (EDX), and Transmission Electron Microscopy (TEM).

Fabrication and testing of a newly designed slit system for depth-resolved X-ray diffraction measurements

DOE PAGES

Sinsheimer, John; Bouet, Nathalie; Ghose, Sanjit; ...

2016-10-06

A new system of slits called `spiderweb slits' have been developed for depth-resolved powder or polycrystalline X-ray diffraction measurements. The slits act on diffracted X-rays to select a particular gauge volume of sample, while absorbing diffracted X-rays from outside of this volume. Although the slit geometry is to some extent similar to that of previously developed conical slits or spiral slits, this new design has advantages over the previous ones in use for complex heterogeneous materials and in situ and operando diffraction measurements. For example, the slits can measure a majority of any diffraction cone for any polycrystalline material, overmore » a continuous range of diffraction angles, and work for X-ray energies of tens to hundreds of kiloelectronvolts. In addition, the design is generated and optimized using ray-tracing simulations, and fabricated through laser micromachining. The first prototype was successfully tested at the X17A beamline at the National Synchrotron Light Source, and shows similar performance to simulations, demonstrating gauge volume selection for standard powders, for all diffraction peaks over angles of 2–10°. A similar, but improved, design will be implemented at the X-ray Powder Diffraction beamline at the National Synchrotron Light Source II.« less

Micro-emulsion-assisted synthesis of ZnS nanospheres and their photocatalytic activity

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

Li Yao; He Xiaoyan; Cao Minhua

2008-11-03

ZnS nanospheres with rough surface were synthesized by using a micro-emulsion-assisted solvothemal process. The molar ratio of [water]/[surfactant] played an important role in controlling the size of the ZnS nanospheres. X-ray powder diffraction (XRD), transmission electron microscopy (TEM), field emission-scanning electron microscope (FE-SEM), and selected area electron diffraction (SAED) were used for the characterization of the resulting ZnS nanospheres. A possible formation mechanism was proposed. These ZnS nanospheres exhibited a good photocatalytic activity for degradation of an aqueous p-nitrophenol solution and the total organic carbon (TOC) of the degradation product has also been investigated.

Sol-gel synthesis and characterization of hybrid inorganic-organic Tb(III)-terephthalate containing layered double hydroxides

NASA Astrophysics Data System (ADS)

Smalenskaite, A.; Salak, A. N.; Ferreira, M. G. S.; Skaudzius, R.; Kareiva, A.

2018-06-01

Mg3/Al1 and Mg3Al1-xTbx layered double hydroxides (LDHs) intercalated with terephthalate anion were synthesized using sol-gel method. The obtained materials were characterized by X-ray diffraction (XRD) analysis, infrared (FTIR) spectroscopy, fluorescence spectroscopy (FLS) and scanning electron microscopy (SEM). The Tb3+ substitution effects in the Mg3Al1-xTbx LDHs were investigated by changing the Tb3+ concentration in the cation layers. The study indicates that the organic guest-terephthalate in the interlayer spacing of the LDH host influences the luminescence of the hybrid inorganic-organic materials.

Bimetal-organic frameworks for functionality optimization: MnFe-MOF-74 as a stable and efficient catalyst for the epoxidation of alkenes with H2O2.

PubMed

Yuan, Kuo; Song, Tianqun; Wang, Dawei; Zou, Ye; Li, Jinfeng; Zhang, Xiaotao; Tang, Zhiyong; Hu, Wenping

2018-01-25

In this work, we synthesized a series of microcrystalline Mn x N 100-x -MOF-74 (N = Fe, Co and Ni) materials by a one-pot reaction. Powder X-ray diffraction (PXRD) patterns of Mn x N 100-x -MOF-74 matched well with those of single-metal MOF-74, and the scanning electron microscopy (SEM) images exhibited homogeneous nanocrystallites aggregated together. The amounts and dispersion of metals were analyzed by using inductively coupled plasma (ICP) and energy-dispersive X-ray spectroscopy (EDS), separately. Mn x N 100-x -MOF-74 could remain crystalline and efficiently catalyze the epoxidation of alkenes in DMF with NaHCO 3 and 30% H 2 O 2 . In particular, Mn 29.39 Fe 70.61 -MOF-74 can achieve almost 100% conversion for styrene with 95.0% selectivity towards styrene oxide and be reused at least five times without loss of activity.

Nd: YAG laser irradiation effects on structural and magnetic properties of Ni1+xZrxFe2-2xO4 nanoparticles

NASA Astrophysics Data System (ADS)

Saraf, Tukaram S.; Kounsalye, Jitendra S.; Birajdar, Shankar D.; Shamkuwar, N. R.

2018-05-01

The effect of 112 mJ Nd: YAG laser irradiation on structural, morphological, infrared and magnetic properties of Ni1+xZrxFe2-2xO4 spinel ferrite nanoparticles has been systematically investigated in the present work. The sol-gel auto combustion synthesis method was successfully executed for the synthesis of the present system. All the samples were characterized by X-ray diffraction technique (XRD), scanning electron microscopy (SEM) and infrared spectroscopy (IR) technique. The magnetic properties of the present samples were measured by pulse field hysteresis loop technique. All the properties were measured for laser irradiated samples as well, to understand the effect of irradiation on the properties. The single-phase cubic spinel structure was confirmed by X-ray diffraction patterns of all samples and the disordered structure was observed for irradiated samples. The two principle absorption bands in IR spectra also confirm the formation of the spinel structure. Spherical and agglomerated morphology was observed for Zr4+ substituted nickel ferrite, whereas scratched morphology was observed for the irradiated samples. The grain size confirms the nanocrystalline nature, the crystallite size also evident the same. The magnetic parameters decreased after Zr4+ ion doping and strongly influenced by the irradiation.

Dynamical scattering in coherent hard x-ray nanobeam Bragg diffraction

NASA Astrophysics Data System (ADS)

Pateras, A.; Park, J.; Ahn, Y.; Tilka, J. A.; Holt, M. V.; Kim, H.; Mawst, L. J.; Evans, P. G.

2018-06-01

Unique intensity features arising from dynamical diffraction arise in coherent x-ray nanobeam diffraction patterns of crystals having thicknesses larger than the x-ray extinction depth or exhibiting combinations of nanoscale and mesoscale features. We demonstrate that dynamical scattering effects can be accurately predicted using an optical model combined with the Darwin theory of dynamical x-ray diffraction. The model includes the highly divergent coherent x-ray nanobeams produced by Fresnel zone plate focusing optics and accounts for primary extinction, multiple scattering, and absorption. The simulation accurately reproduces the dynamical scattering features of experimental diffraction patterns acquired from a GaAs/AlGaAs epitaxial heterostructure on a GaAs (001) substrate.

Coherent x-ray diffraction imaging with nanofocused illumination.

PubMed

Schroer, C G; Boye, P; Feldkamp, J M; Patommel, J; Schropp, A; Schwab, A; Stephan, S; Burghammer, M; Schöder, S; Riekel, C

2008-08-29

Coherent x-ray diffraction imaging is an x-ray microscopy technique with the potential of reaching spatial resolutions well beyond the diffraction limits of x-ray microscopes based on optics. However, the available coherent dose at modern x-ray sources is limited, setting practical bounds on the spatial resolution of the technique. By focusing the available coherent flux onto the sample, the spatial resolution can be improved for radiation-hard specimens. A small gold particle (size <100 nm) was illuminated with a hard x-ray nanobeam (E=15.25 keV, beam dimensions approximately 100 x 100 nm2) and is reconstructed from its coherent diffraction pattern. A resolution of about 5 nm is achieved in 600 s exposure time.

DynAMITe: a prototype large area CMOS APS for breast cancer diagnosis using x-ray diffraction measurements

NASA Astrophysics Data System (ADS)

Konstantinidis, A.; Anaxagoras, T.; Esposito, M.; Allinson, N.; Speller, R.

2012-03-01

X-ray diffraction studies are used to identify specific materials. Several laboratory-based x-ray diffraction studies were made for breast cancer diagnosis. Ideally a large area, low noise, linear and wide dynamic range digital x-ray detector is required to perform x-ray diffraction measurements. Recently, digital detectors based on Complementary Metal-Oxide- Semiconductor (CMOS) Active Pixel Sensor (APS) technology have been used in x-ray diffraction studies. Two APS detectors, namely Vanilla and Large Area Sensor (LAS), were developed by the Multidimensional Integrated Intelligent Imaging (MI-3) consortium to cover a range of scientific applications including x-ray diffraction. The MI-3 Plus consortium developed a novel large area APS, named as Dynamically Adjustable Medical Imaging Technology (DynAMITe), to combine the key characteristics of Vanilla and LAS with a number of extra features. The active area (12.8 × 13.1 cm2) of DynaMITe offers the ability of angle dispersive x-ray diffraction (ADXRD). The current study demonstrates the feasibility of using DynaMITe for breast cancer diagnosis by identifying six breast-equivalent plastics. Further work will be done to optimize the system in order to perform ADXRD for identification of suspicious areas of breast tissue following a conventional mammogram taken with the same sensor.

Preparation and Characterization of Niobium Doped Lead-Telluride Glass Ceramics

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

Sathish, M.; Eraiah, B.; Anavekar, R. V.

2011-07-15

Niobium-lead-telluride glass ceramics of composition xNb{sub 2}O{sub 5}-(20-x) pbO-80TeO{sub 2}(where x = 0.1 mol% to 0.5 mol%) were prepared by using conventional melt quenching method. The prepared glass samples were initially amorphous in nature after annealed at 400 deg. c all samples were crystallized. This was confined by X-ray diffraction and scanning electron microscopy. The particle size of these glass ceramics have been calculated by using Debye-Scherer formula and the particle size is in the order of 15 nm to 60 nm. The scanning electron microscopy (SEM) photograph shows the presence of needle-like crystals in these samples.

Resolution enhancement in coherent x-ray diffraction imaging by overcoming instrumental noise.

PubMed

Kim, Chan; Kim, Yoonhee; Song, Changyong; Kim, Sang Soo; Kim, Sunam; Kang, Hyon Chol; Hwu, Yeukuang; Tsuei, Ku-Ding; Liang, Keng San; Noh, Do Young

2014-11-17

We report that reference objects, strong scatterers neighboring weak phase objects, enhance the phase retrieval and spatial resolution in coherent x-ray diffraction imaging (CDI). A CDI experiment with Au nano-particles exhibited that the reference objects amplified the signal-to-noise ratio in the diffraction intensity at large diffraction angles, which significantly enhanced the image resolution. The interference between the diffracted x-ray from reference objects and a specimen also improved the retrieval of the phase of the diffraction signal. The enhancement was applied to image NiO nano-particles and a mitochondrion and confirmed in a simulation with a bacteria phantom. We expect that the proposed method will be of great help in imaging weakly scattering soft matters using coherent x-ray sources including x-ray free electron lasers.

Synthesis of Mn doped ZnS nanocrystals: Crystallographic and morphological study

NASA Astrophysics Data System (ADS)

Shaikh, Azharuddin Z.; Shirsath, Narendra B.; Sonawane, Prabhakar S.

2018-05-01

The influence of doping concentration on the physical properties of ZnS nanocrystals synthesized using coprecipitation method at room temperature is reported in this paper. In particular, we have studied the structural properties of Zn1-xMnxS where (x=0.01, 0.03, 0.05) by X-ray diffraction. X-ray peak broadening analysis used to calculate the crystalline sizes, lattice parameters, number of unit cell per particle and volume of unit cell. Crystalline ZnS with a cubic structure is confirmed by XRD results. The grain size of pure and Mn doped samples were found in the range of 7nm to 9nm. All the physical parameters of cubic ZnS nanocrystals were calculated are similar with standard values. The scanning electron microscope (SEM) which revealed that the synthesized nanocrystals are well-crystalline and possessing cubic phase.

Laser ablation of Au-CuO core-shell nanocomposite in water for optoelectronic devices

NASA Astrophysics Data System (ADS)

Ismail, Raid A.; Abdul-Hamed, Ryam S.

2017-12-01

Core-shell gold-copper oxide Au-CuO nanocomposites were synthesized using laser ablation of CuO target in colloidal solution of Au nanoparticles (NPs). The effect of laser fluence on the structural, morphological, electrical, and optical properties of Au-CuO nanocomposites was investigated using x-ray diffraction (XRD), atomic force microscope (AFM), scanning electron microscope (SEM), transmission electron microscope (TEM), photoluminescence (PL), Fourier transformed infrared spectroscopy (FTIR), Hall measurement, and UV-vis spectroscopy. X-ray diffraction results confirm the formation of polycrystalline Au-CuO NPs with monoclinic structure. The optical energy gap for CuO was 4 eV and for the Au-CuO core-shell nanocomposites was found to be in the range of 3.4-3.7 eV. SEM and TEM investigations revealed that the structure and morphology of Au-CuO core-shell nanocomposites were strongly depending on the laser fluence. A formation of Au-CuO nanospheres and platelets structures was observed. The photoluminescence data showed an emission of broad visible peaks between 407 and 420 nm. The effect of laser fluence on the dark and illuminated I-V characteristics of Au-CuO/n-Si heterojunction photodetectors was investigated and analyzed. The experimental data demonstrated that the photodetector prepared at optimum laser fluence exhibited photosensitivity of 0.6 AW-1 at 800 nm.

Some studies on TiO2 films deposited by sol-gel technique

NASA Astrophysics Data System (ADS)

Narasimha Rao, K.; Vishwas, M.; Kumar Sharma, Sudhir; Arjuna Gowda, K. V.

2008-08-01

TiO2 films are extensively used in various applications including optical multi-layers, sensors, photo catalysis, environmental purification, and solar cells etc. These are prepared by both vacuum and non-vacuum methods. In this paper, we present the results on TiO2 thin films prepared by a sol-gel spin coating process in non-aqueous solvent. Titanium isopropoxide is used as TiO2 precursor. The films were annealed at different temperatures up to 3000 C for 5 hours in air. The influence of the various deposition parameters like spinning speed, spinning time and annealing temperature on the thickness of the TiO2 films has been studied. The variation of film thickness with time in ambient atmosphere was also studied. The optical, structural and morphological characteristics were investigated by optical transmittance-reflectance measurements, X-ray diffraction (XRD) and scanning electron microscopy (SEM) respectively. The refractive index and extinction coefficient of the films were determined by envelope technique and spectroscopic ellipsometry. TiO2 films exhibited high transparency (92%) in the visible region with a refractive index of 2.04 at 650 nm. The extinction coefficient was found to be negligibly small. The X-ray diffraction analysis showed that the TiO2 film deposited on glass substrate changes from amorphous to crystalline (anatase) phase with annealing temperature above 2500 C. SEM results show that the deposited films are uniform and crack free.

Effect of fluorine doping on highly transparent conductive spray deposited nanocrystalline tin oxide thin films

NASA Astrophysics Data System (ADS)

Moholkar, A. V.; Pawar, S. M.; Rajpure, K. Y.; Bhosale, C. H.; Kim, J. H.

2009-09-01

The undoped and fluorine doped thin films are synthesized by using cost-effective spray pyrolysis technique. The dependence of optical, structural and electrical properties of SnO 2 films, on the concentration of fluorine is reported. Optical absorption, X-ray diffraction, scanning electron microscope (SEM) and Hall effect studies have been performed on SnO 2:F (FTO) films coated on glass substrates. The film thickness varies from 800 to 1572 nm. X-ray diffraction pattern reveals the presence of cassiterite structure with (2 0 0) preferential orientation for FTO films. The crystallite size varies from 35 to 66 nm. SEM and AFM study reveals the surface of FTO to be made of nanocrystalline particles. The electrical study reveals that the films are degenerate and exhibit n-type electrical conductivity. The 20 wt% F doped film has a minimum resistivity of 3.8 × 10 -4 Ω cm, carrier density of 24.9 × 10 20 cm -3 and mobility of 6.59 cm 2 V -1 s -1. The sprayed FTO film having minimum resistance of 3.42 Ω/cm 2, highest figure of merit of 6.18 × 10 -2 Ω -1 at 550 nm and 96% IR reflectivity suggest, these films are useful as conducting layers in electrochromic and photovoltaic devices and also as the passive counter electrode.

Fabrication and testing of a newly designed slit system for depth-resolved X-ray diffraction measurements

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

Sinsheimer, John; Bouet, Nathalie; Ghose, Sanjit

2016-10-06

A new system of slits called `spiderweb slits' have been developed for depth-resolved powder or polycrystalline X-ray diffraction measurements. The slits act on diffracted X-rays to select a particular gauge volume of sample, while absorbing diffracted X-rays from outside of this volume. Although the slit geometry is to some extent similar to that of previously developed conical slits or spiral slits, this new design has advantages over the previous ones in use for complex heterogeneous materials andin situandoperandodiffraction measurements. For example, the slits can measure a majority of any diffraction cone for any polycrystalline material, over a continuous range ofmore » diffraction angles, and work for X-ray energies of tens to hundreds of kiloelectronvolts. The design is generated and optimized using ray-tracing simulations, and fabricated through laser micromachining. The first prototype was successfully tested at the X17A beamline at the National Synchrotron Light Source, and shows similar performance to simulations, demonstrating gauge volume selection for standard powders, for all diffraction peaks over angles of 2–10°. A similar, but improved, design will be implemented at the X-ray Powder Diffraction beamline at the National Synchrotron Light Source II.« less

Local terahertz field enhancement for time-resolved x-ray diffraction

DOE PAGES

Kozina, M.; Pancaldi, M.; Bernhard, C.; ...

2017-02-20

We report local field strength enhancement of single-cycle terahertz (THz) pulses in an ultrafast time-resolved x-ray diffraction experiment. We show that patterning the sample with gold microstructures increases the THz field without changing the THz pulse shape or drastically affecting the quality of the x-ray diffraction pattern. Lastly, we find a five-fold increase in THz-induced x-ray diffraction intensity change in the presence of microstructures on a SrTiO 3 thin-film sample.

Local terahertz field enhancement for time-resolved x-ray diffraction

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

Kozina, M.; Pancaldi, M.; Bernhard, C.

We report local field strength enhancement of single-cycle terahertz (THz) pulses in an ultrafast time-resolved x-ray diffraction experiment. We show that patterning the sample with gold microstructures increases the THz field without changing the THz pulse shape or drastically affecting the quality of the x-ray diffraction pattern. Lastly, we find a five-fold increase in THz-induced x-ray diffraction intensity change in the presence of microstructures on a SrTiO 3 thin-film sample.

The nucleation and growth mechanism of Ni-Sn eutectic in a single crystal superalloy

NASA Astrophysics Data System (ADS)

Jiang, Weiguo; Wang, Li; Li, Xiangwei; Lou, Langhong

2017-12-01

The microstructure of single crystal superalloy with and without tin layer on the surface of as-cast and heat-treatment state was investigated by optical microscope (OM) and scanning electron microscopy (SEM). The composition of different regions on the surface was tested by energy dispersive X-ray (EDS). The reaction intermetallic compound (IMC) formed in the heat treatment process was confirmed by X-ray diffraction (XRD). The orientations of different microstructure in samples as heat treatment state were determined by electron back-scattering diffraction (EBSD) method. The porosity location in the interdendritic region was observed by X-ray computed tomography (XCT). The experiment results showed that the remained Sn on the surface of the superalloy reacted with Ni, and then formed Ni3Sn4 in the as-cast state. Sn enriched by diffusion along the porosity located in the interdendritic region and γ + γ‧ (contain a little of Sn) eutectic and Ni3Sn2 formed in single crystal superalloy during heat treatment, and the recalescence behaviors were found. Ni3Sn2 nucleated independently in the cooled liquid at the front of (γ + γ‧) (Sn) eutectic. The nucleation and growth mechanism of the eutectic and Ni3Sn2 IMC during heat treatment was discussed in the present paper.

Rational design of Ag/TiO2 nanosystems by a combined RF-sputtering/sol-gel approach.

PubMed

Armelao, Lidia; Barreca, Davide; Bottaro, Gregorio; Gasparotto, Alberto; Maccato, Chiara; Tondello, Eugenio; Lebedev, Oleg I; Turner, Stuart; Van Tendeloo, Gustaaf; Sada, Cinzia; Stangar, Urska Lavrencic

2009-12-21

The present work is devoted to the preparation of Ag/TiO(2) nanosystems by an original synthetic strategy, based on the radio-frequency (RF) sputtering of silver particles on titania-based xerogels prepared by the sol-gel (SG) route. This approach takes advantage of the synergy between the microporous xerogel structure and the infiltration power characterizing RF-sputtering, whose combination enables the obtainment of a tailored dispersion of Ag-containing particles into the titania matrix. In addition, the system's chemico-physical features can be tuned further through proper ex situ thermal treatments in air at 400 and 600 degrees C. The synthesized composites are extensively characterized by the joint use of complementary techniques, that is, X-ray photoelectron and X-ray excited Auger electron spectroscopies (XPS, XE-AES), secondary ion mass spectrometry (SIMS), glancing incidence X-ray diffraction (GIXRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), electron diffraction (ED), high-angle annular dark field scanning TEM (HAADF-STEM), energy-filtered TEM (EF-TEM) and optical absorption spectroscopy. Finally, the photocatalytic performances of selected samples in the decomposition of the azo-dye Plasmocorinth B are preliminarily investigated. The obtained results highlight the possibility of tailoring the system characteristics over a broad range, directly influencing their eventual functional properties.

Hydrothermal synthesis of flower-like MoS2 nanospheres for electrochemical supercapacitors.

PubMed

Zhou, Xiaoping; Xu, Bin; Lin, Zhengfeng; Shu, Dong; Ma, Lin

2014-09-01

Flower-like MoS2 nanospheres were synthesized by a hydrothermal route. The structure and surface morphology of the as-prepared MoS2 was characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The supercapacitive behavior of MoS2 in 1 M KCl electrolyte was studied by means of cyclic voltammetry (CV), constant current charge-discharge cycling (CD) and electrochemical impedance spectroscopy (EIS). The XRD results indicate that the as-prepared MoS2 has good crystallinity. SEM images show that the MoS2 nanospheres have uniform sizes with mean diameter about 300 nm. Many nanosheets growing on the surface make the MoS2 nanospheres to be a flower-like structure. The specific capacitance of MoS2 is 122 F x g(-1) at 1 A x g(-1) or 114 F x g(-1) at 2 mv s(-1). All the experimental results indicate that MoS2 is a promising electrode material for electrochemical supercapacitors.

Thermal x-ray diffraction and near-field phase contrast imaging

NASA Astrophysics Data System (ADS)

Li, Zheng; Classen, Anton; Peng, Tao; Medvedev, Nikita; Wang, Fenglin; Chapman, Henry N.; Shih, Yanhua

2017-10-01

Using higher-order coherence of thermal light sources, the resolution power of standard x-ray imaging techniques can be enhanced. In this work, we applied the higher-order measurement to far-field x-ray diffraction and near-field phase contrast imaging (PCI), in order to achieve superresolution in x-ray diffraction and obtain enhanced intensity contrast in PCI. The cost of implementing such schemes is minimal compared to the methods that achieve similar effects by using entangled x-ray photon pairs.

Thermal x-ray diffraction and near-field phase contrast imaging

DOE PAGES

Li, Zheng; Classen, Anton; Peng, Tao; ...

2017-12-27

Using higher-order coherence of thermal light sources, the resolution power of standard x-ray imaging techniques can be enhanced. Here in this work, we applied the higher-order measurement to far-field x-ray diffraction and near-field phase contrast imaging (PCI), in order to achieve superresolution in x-ray diffraction and obtain enhanced intensity contrast in PCI. The cost of implementing such schemes is minimal compared to the methods that achieve similar effects by using entangled x-ray photon pairs.

Sol-gel synthesis, phase composition, morphological and structural characterization of Ca10(PO4)6(OH)2: XRD, FTIR, SEM, 3D SEM and solid-state NMR studies

NASA Astrophysics Data System (ADS)

Kareiva, Simonas; Klimavicius, Vytautas; Momot, Aleksandr; Kausteklis, Jonas; Prichodko, Aleksandra; Dagys, Laurynas; Ivanauskas, Feliksas; Sakirzanovas, Simas; Balevicius, Vytautas; Kareiva, Aivaras

2016-09-01

Aqueous sol-gel chemistry route based on ammonium-hydrogen phosphate as the phosphorus precursor, calcium acetate monohydrate as source of calcium ions, and 1,2-ethylendiaminetetraacetic acid (EDTA), or 1,2-diaminocyclohexanetetracetic acid (DCTA), or tartaric acid (TA), or ethylene glycol (EG), or glycerol (GL) as complexing agents have been used to prepare calcium hydroxyapatite (Ca10(PO4)6(OH)2, CHAp). The phase transformations, composition, and structural changes in the polycrystalline samples were studied by infrared spectroscopy (FTIR), X-ray powder diffraction analysis (XRD), and scanning electron microscopy (SEM). The local short-range (nano- and mezo-) scale effects in CHAp were studied using solid-state NMR spectroscopy. The spatial 3D data from the SEM images of CHAp samples obtained by TA, EG and GL sol-gel routes were recovered for the first time to our knowledge.

An image focusing means by using an opaque object to diffract x-rays

DOEpatents

Sommargren, Gary E.; Weaver, H. Joseph

1991-01-01

The invention provides a method and apparatus for focusing and imaging x-rays. An opaque sphere is used as a diffractive imaging element to diffract x-rays from an object so that the divergent x-ray wavefronts are transformed into convergent wavefronts and are brought to focus to form an image of the object with a large depth of field.

Soft X-Ray Diffraction Microscopy of a Frozen Hydrated Yeast Cell

DOE PAGES

Huang, Xiaojing; Nelson, Johanna; Kirz, Janos; ...

2009-11-01

We report the first image of an intact, frozen hydrated eukaryotic cell using x-ray diffraction microscopy, or coherent x-ray diffraction imaging. By plunge freezing the specimen in liquid ethane and maintaining it below -170 °C, artifacts due to dehydration, ice crystallization, and radiation damage are greatly reduced. In this example, coherent diffraction data using 520 eV x rays were recorded and reconstructed to reveal a budding yeast cell at a resolution better than 25 nm. This demonstration represents an important step towards high resolution imaging of cells in their natural, hydrated state, without limitations imposed by x-ray optics.

Application of focused-beam flat-sample method to synchrotron powder X-ray diffraction with anomalous scattering effect

NASA Astrophysics Data System (ADS)

Tanaka, M.; Katsuya, Y.; Matsushita, Y.

2013-03-01

The focused-beam flat-sample method (FFM), which is a method for high-resolution and rapid synchrotron X-ray powder diffraction measurements by combination of beam focusing optics, a flat shape sample and an area detector, was applied for diffraction experiments with anomalous scattering effect. The advantages of FFM for anomalous diffraction were absorption correction without approximation, rapid data collection by an area detector and good signal-to-noise ratio data by focusing optics. In the X-ray diffraction experiments of CoFe2O4 and Fe3O4 (By FFM) using X-rays near the Fe K absorption edge, the anomalous scattering effect between Fe/Co or Fe2+/Fe3+ can be clearly detected, due to the change of diffraction intensity. The change of observed diffraction intensity as the incident X-ray energy was consistent with the calculation. The FFM is expected to be a method for anomalous powder diffraction.

Rietveld analysis using powder diffraction data with anomalous scattering effect obtained by focused beam flat sample method

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

Tanaka, Masahiko, E-mail: masahiko@spring8.or.jp; Katsuya, Yoshio, E-mail: katsuya@spring8.or.jp; Sakata, Osami, E-mail: SAKATA.Osami@nims.go.jp

2016-07-27

Focused-beam flat-sample method (FFM) is a new trial for synchrotron powder diffraction method, which is a combination of beam focusing optics, flat shape powder sample and area detectors. The method has advantages for X-ray diffraction experiments applying anomalous scattering effect (anomalous diffraction), because of 1. Absorption correction without approximation, 2. High intensity X-rays of focused incident beams and high signal noise ratio of diffracted X-rays 3. Rapid data collection with area detectors. We applied the FFM to anomalous diffraction experiments and collected synchrotron X-ray powder diffraction data of CoFe{sub 2}O{sub 4} (inverse spinel structure) using X-rays near Fe K absorptionmore » edge, which can distinguish Co and Fe by anomalous scattering effect. We conducted Rietveld analyses with the obtained powder diffraction data and successfully determined the distribution of Co and Fe ions in CoFe{sub 2}O{sub 4} crystal structure.« less

A study on magneto-optic properties of CoxMg1-xFe2O4 nanoferrofluids

NASA Astrophysics Data System (ADS)

Karthick, R.; Ramachandran, K.; Srinivasan, R.

2018-04-01

Nanoparticles of CoxMg1-xFe2O4 (x = 0.1, 0.5, 0.9) were synthesized using chemical co-precipitation method. Characterization by X-ray diffraction technique confirmed the formation of cubic crystalline structure and the crystallite size of the samples obtained using Debye-Scherrer approximation were found to increase with increasing cobalt substitution. Surface morphology and the Chemical composition of the samples were visualized using scanning electron microscope (SEM) with energy dispersive analysis of X-rays (EDAX). Room temperature magnetic parameters of the nanoparticles by vibrating sample magnetometer (VSM) revealed the magnetic properties such as Saturation magnetization (Ms), Remanent magnetization (Mr) and Coercive field (Hc) found to increase with increasing cobalt substitution. Faraday rotation measurements on CoxMg1-xFe2O4 ferrofluids exhibited increase in rotation with cobalt substitution. Further, there is an increase in Faraday rotation with increasing magnetic field for all the samples.

Infiltration of CdTe nano crystals into a ZnO wire vertical matrix by using the isothermal closed space technique

NASA Astrophysics Data System (ADS)

Larramendi, S.; Vaillant Roca, Lidice; Saint-Gregoire, Pierre; Ferraz Dias, Johnny; Behar, Moni

2017-10-01

A ZnO nanorod structure was grown by the hydrothermal method and interpenetrated with CdTe using the isothermal closed space sublimation technique. The obtained structure was studied by using the Rutherford backscattering spectrometry (RBS), Scanning Electron Microscopy (SEM), High Resolution Transmission Electron Microscopy (HRTEM). The X-ray Diffraction (XRD) technique confirmed the presence of CdTe nanocrystals (NCs) of very small size formed on the surface and in the interspaces between the ZnO nanorods. The RBS observations together with the SEM observations give information on the obtained structure. Finally the photoluminescence studies show a strong energy confinement effect on the grown CdTe NCs.

Electrodeposition of Zn-doped α-nickel hydroxide with flower-like nanostructure for supercapacitors

NASA Astrophysics Data System (ADS)

You, Zheng; Shen, Kui; Wu, Zhicheng; Wang, Xiaofeng; Kong, Xianghua

2012-08-01

Zn-doped α-nickel hydroxide materials with flower-like nanostructures are synthesized by electrochemical deposition method. The samples are characterized by X-ray diffraction (XRD), field emission scanning electron microscope (SEM) and electrochemical measurements. XRD spectra indicate nickel hydroxide doped with Zn is α-Ni(OH)2 with excellent crystallization. The SEM observation shows that the formation of Zn-doped Ni(OH)2 includes two steps: a honeycomb-like film forms on the substrate first, then flower-like particles forms on the films. The nickel hydroxide doped with 5% Zn can maintain a maximum specific capacitance of 860 F g-1, suggesting its potential application in electrochemical capacitors.

Single step synthesis of nanostructured boron nitride for boron neutron capture therapy

NASA Astrophysics Data System (ADS)

Singh, Bikramjeet; Singh, Paviter; Kumar, Manjeet; Thakur, Anup; Kumar, Akshay

2015-05-01

Nanostructured Boron Nitride (BN) has been successfully synthesized by carbo-thermic reduction of Boric Acid (H3BO3). This method is a relatively low temperature synthesis route and it can be used for large scale production of nanostructured BN. The synthesized nanoparticles have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and differential thermal analyzer (DTA). XRD analysis confirmed the formation of single phase nanostructured Boron Nitride. SEM analysis showed that the particles are spherical in shape. DTA analysis showed that the phase is stable upto 900 °C and the material can be used for high temperature applications as well boron neutron capture therapy (BNCT).

Fabrication of high-k dielectric Calcium Copper Titanate (CCTO) target by solid state route

NASA Astrophysics Data System (ADS)

Tripathy, N.; Das, K. C.; Ghosh, S. P.; Bose, G.; Kar, J. P.

2016-02-01

CaCu3Ti4O12 (CCTO) ceramic pellet of 10mm diameter has been synthesized by adopting solid state route. The structural and morphological characterization of the ceramics sample was carried out by X-ray diffraction (XRD) and scanning electron microscope (SEM), respectively. XRD pattern revealed the CCTO phase formation, where as SEM micrograph shows the sample consisting of well defined grain and grain boundaries. The room temperature dielectric constant of the sample was found to be ∼ 5000 at 1kHz. After successful preparation of CCTO pellet, a 2 inch diameter CCTO sputtering target is also fabricated in order to deposit CCTO thin films for microelectronic applications.

Influence of Zeolite Coating on the Corrosion Resistance of AZ91D Magnesium Alloy

PubMed Central

Banerjee, P. Chakraborty; Woo, Ren Ping; Grayson, Sam Matthew; Majumder, Amrita; Raman, R. K. Singh

2014-01-01

The protective performance of zeolite coating on AZ91D magnesium alloy was evaluated using potentiodynamic polarisation and electrochemical impedance spectroscopy (EIS) in 0.1 M sodium chloride solution (NaCl). Electrical equivalent circuit (EEC) was developed based upon hypothetical corrosion mechanisms and simulated to correspond to the experimental data. The morphology and the chemical nature of the coating were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD) analysis. Post corrosion morphologies of the zeolite coated and the uncoated AZ91D alloy were investigated using SEM. The corrosion resistance of the zeolite coated specimen was at least one order of magnitude higher than the uncoated specimen. PMID:28788178

Influence of Zeolite Coating on the Corrosion Resistance of AZ91D Magnesium Alloy.

PubMed

Banerjee, P Chakraborty; Woo, Ren Ping; Grayson, Sam Matthew; Majumder, Amrita; Raman, R K Singh

2014-08-22

The protective performance of zeolite coating on AZ91D magnesium alloy was evaluated using potentiodynamic polarisation and electrochemical impedance spectroscopy (EIS) in 0.1 M sodium chloride solution (NaCl). Electrical equivalent circuit (EEC) was developed based upon hypothetical corrosion mechanisms and simulated to correspond to the experimental data. The morphology and the chemical nature of the coating were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD) analysis. Post corrosion morphologies of the zeolite coated and the uncoated AZ91D alloy were investigated using SEM. The corrosion resistance of the zeolite coated specimen was at least one order of magnitude higher than the uncoated specimen.

Magnetic properties of Zn1-xNixO

NASA Astrophysics Data System (ADS)

Mondal, A.; Giri, N.; Sarkar, S.; Ray, Ruma

2018-05-01

Ni doped ZnO (Zn1-xNixO for 0.01 ≤ x ≤ 0.11) have been prepared by chemical precipitation method. X-ray diffraction corroborates a hexagonal wurzite structure without any impurity phases upto 11% Ni doping. Morphology of the particles is investigated by FE-SEM which exhibits either rod or tube like structure depending on the dopant concentration. Magnetization of Zn1-xNixO for 0.03 ≤ x ≤ 0.11 measured at room temperature infers the paramagnetic behavior. Zero field cooled and field cooled magnetization for x = 0.11 follows Curie-Weiss behavior above 122 K with effective paramagnetic moment 3.9μB. The non-linear magnetic hysteresis loop at 2 K with a small coercivity (300 Oe) indicates signature of ferromagnetic ordering.

In Situ Neutron Diffraction of Rare-Earth Phosphate Proton Conductors Sr/Ca-doped LaPO4 at Elevated Temperatures

NASA Astrophysics Data System (ADS)

Al-Wahish, Amal; Al-Binni, Usama; Bridges, C. A.; Huq, A.; Bi, Z.; Paranthaman, M. P.; Tang, S.; Kaiser, H.; Mandrus, D.

Acceptor-doped lanthanum orthophosphates are potential candidate electrolytes for proton ceramic fuel cells. We combined neutron powder diffraction (NPD) at elevated temperatures up to 800° C , X-ray powder diffraction (XRD) and scanning electron microscopy (SEM) to investigate the crystal structure, defect structure, thermal stability and surface topography. NPD shows an average bond length distortion in the hydrated samples. We employed Quasi-Elastic Neutron Scattering (QENS) and electrochemical impedance spectroscopy (EIS) to study the proton dynamics of the rare-earth phosphate proton conductors 4.2% Sr/Ca-doped LaPO4. We determined the bulk diffusion and the self-diffusion coefficients. Our results show that QENS and EIS are probing fundamentally different proton diffusion processes. Supported by the U.S. Department of Energy.

Growth and characterization of single phase Cu{sub 2}O by thermal oxidation of thin copper films

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

Choudhary, Sumita; Sarma, J. V. N.; Gangopadhyay, Subhashis, E-mail: subhagan@yahoo.com

2016-04-13

We report a simple and efficient technique to form high quality single phase cuprous oxide films on glass substrate using thermal evaporation of thin copper films followed by controlled thermal oxidation in air ambient. Crystallographic analysis and oxide phase determination, as well as grain size distribution have been studied using X-ray diffraction (XRD) method, while scanning electron microscopy (SEM) has been utilized to investigate the surface morphology of the as grown oxide films. The formation of various copper oxide phases is found to be highly sensitive to the oxidation temperature and a crystalline, single phase cuprous oxide film can bemore » achieved for oxidation temperatures between 250°C to 320°C. Cu{sub 2}O film surface appeared in a faceted morphology in SEM imaging and a direct band gap of about 2.1 eV has been observed in UV-visible spectroscopy. X-ray photoelectron spectroscopy (XPS) confirmed a single oxide phase formation. Finally, a growth mechanism of the oxide film has also been discussed.« less

SAPO-34/AlMCM-41, as a novel hierarchical nanocomposite: preparation, characterization and investigation of synthesis factors using response surface methodology

NASA Astrophysics Data System (ADS)

Roohollahi, Hossein; Halladj, Rouein; Askari, Sima; Yaripour, Fereydoon

2018-06-01

SAPO-34/AlMCM-41, as a new hierarchical nanocomposite was successfully synthesized via hydrothermal and dry-gel conversion. In an experimental and statistical study, effect of five input parameters including synthesis period, drying temperature, NaOH/Si, water/dried-gel and SAPO% were investigated on range-order degree of mesochannels and the relative crystallinity. X-ray diffraction (XRD) patterns were recorded to characterize the ordered AlMCM-41 and crystalline SAPO-34 structures. Nitrogen adsorption-desorption technique, scanning electron microscopy (SEM), field-emission SEM (FESEM) equipped with an energy-dispersive X-ray spectroscopy (EDS-Map) and transmission electron microscopy (TEM) were used to study the textural properties, morphology and surface elemental composition. Two reduced polynomials were fitted to the responses with good precision. Further, based on analysis of variances, SAPO% and time duration of dry-gel conversion were observed as the most effective parameters on the composite structure. The hierarchical porosity, narrow pore size distribution, high external surface area and large specific pore volume were of interesting characteristics for this novel nanocomposite.

Thermal, structural, functional, optical and magnetic studies of pure and Ba doped CdO nanoparticles.

PubMed

Sivakumar, S; Venkatesan, A; Soundhirarajan, P; Khatiwada, Chandra Prasad

2015-12-05

In this research, a chemical precipitation method was used to synthesize undoped and doped cadmium oxide nanoparticles and studied by TG-DTA, XRD, FT-IR, SEM, with EDX and antibacterial activities, respectively. The melting points, thermal stability and the kinetic parameters like entropy (ΔS), enthalpy (ΔH), Gibb's energy (ΔG), activation energy (E), frequency factor (A) were evaluated from TG-DTA measurements. X-ray diffraction analysis (XRD) brought out the information about the synthesized products exist in spherical in shape with cubic structure. The functional groups and band area of the samples were established by Fourier transform infrared (FT-IR) spectroscopy. The direct and indirect band gap energy of pure and doped samples were determined by UV-Vis-DRS. The surface morphological, elemental compositions and particles sizes were evaluated by scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS). Finally, antibacterial activities indicated the Gram-positive and Gram-negative bacteria are more active in transporter, dehydrogenize and periplasmic enzymatic activities of pure and doped samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Structure and colossal dielectric permittivity of Ca2TiCrO6 ceramics

NASA Astrophysics Data System (ADS)

Yan-Qing, Tan; Meng, Yan; Yong-Mei, Hao

2013-01-01

A colossal permittivity ceramic material, Ca2TiCrO6, was successfully synthesized by the conventional solid-state reaction, and was characterized by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), x-ray photoemission spectroscopy (XPS) and x-ray diffraction (XRD). Rietveld refinement of XRD data indicated that the material crystallized in orthorhombic structure with space group pbnm. SEM displayed Ca2TiCrO6 ceramic grains packed uniformly with the size range 5-20 µm. XPS analyses indicated that elemental chromium and titanium of the material were in mixed valence. The corresponding dielectric property was tested in the frequency range 1 kHz-1 MHz and the temperature range 213-453 K, and the ceramics exhibited a relaxation-like dielectric behaviour. Importantly, the permittivity of Ca2TiCrO6 could reach 80 000 at 298 K (100 Hz) and was maintained at 40 000 up to 398 K at 1 MHz, which could be attributed to the ion disorder and mixed valence of Cr3+/Cr6+ and Ti3+/Ti4+.

Rapid extra-/intracellular biosynthesis of gold nanoparticles by the fungus Penicillium sp.

NASA Astrophysics Data System (ADS)

Du, Liangwei; Xian, Liang; Feng, Jia-Xun

2011-03-01

In this work, the fungus Penicillium was used for rapid extra-/intracellular biosynthesis of gold nanoparticles. AuCl4 - ions reacted with the cell filtrate of Penicillium sp. resulting in extracellular biosynthesis of gold nanoparticles within 1 min. Intracellular biosynthesis of gold nanoparticles was obtained by incubating AuCl4 - solution with fungal biomass for 8 h. The gold nanoparticles were characterized by means of visual observation, UV-Vis absorption spectroscopy, X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy (EDX). The extracellular nanoparticles exhibited maximum absorbance at 545 nm in UV-Vis spectroscopy. The XRD spectrum showed Bragg reflections corresponding to the gold nanocrystals. TEM exhibited the formed spherical gold nanoparticles in the size range from 30 to 50 nm with an average size of 45 nm. SEM and TEM revealed that the intracellular gold nanoparticles were well dispersed on the cell wall and within the cell, and they are mostly spherical in shape with an average diameter of 50 nm. The presence of gold was confirmed by EDX analysis.

Acetone sensors based on microsheet-assembled hierarchical Fe2O3 with different Fe3+ concentrations

NASA Astrophysics Data System (ADS)

Wang, Han; Yan, Lei; Li, Shuo; Li, Yu; Liu, Li; Du, Liting; Duan, Haojie; Cheng, Yali

2018-02-01

Several different morphologies of microsheet-assembled Fe2O3 have been fabricated by hydrothermal method using diverse concentrations of Fe3+ precursor solutions (0.025, 0.020, 0.015, 0.010 mol/L Fe3+). The as-synthesized materials have been characterized by scanning electron microscope (SEM), X-ray powder diffraction (XRD), and energy-dispersive X-ray spectrometry (EDS). The SEM images reflect that the morphologies of as-synthesized materials are affected by the concentrations of Fe3+ in precursor solutions. The less concentration of Fe3+, the more porous of Fe2O3 microflowers, and thinner of slices distributed on the surface. Furthermore, gas sensors based on these Fe2O3 microflowers manufactured and tested to various common gases. The optimum response value to 100 ppm acetone is 52 at the working temperature of 220 °C. Meanwhile, the Fe2O3 microflower sensors possess ultrafast response-recovery speed, which are 8 and 19 s, respectively. The possible sensing mechanism was mainly attributed to the high surface area, three-dimensional porous structure.

Mobility of rare earth elements in mine drainage: Influence of iron oxides, carbonates, and phosphates.

PubMed

Edahbi, Mohamed; Plante, Benoît; Benzaazoua, Mostafa; Ward, Matthew; Pelletier, Mia

2018-05-01

The geochemical behavior of rare earth elements (REE) was investigated using weathering cells. The influence of sorption and precipitation on dissolved REE mobility and fractionation is evaluated using synthetic iron-oxides, carbonates, and phosphates. Sorption cell tests are conducted on the main lithologies of the expected waste rocks from the Montviel deposit. The sorbed materials are characterized using a scanning electron microscope (SEM) equipped with a microanalysis system (energy dispersive spectroscopy EDS) (SEM-EDS), X-ray diffraction (XRD), and X-ray absorption near edge structure (XANES) in order to understand the effect of the synthetic minerals on REE mobility. The results confirm that sorption and precipitation control the mobility and fractionation of REE. The main sorbent phases are the carbonates, phosphates (present as accessory minerals in the Montviel waste rocks), and iron oxides (main secondary minerals generated upon weathering of the Montviel lithologies). The XANES results show that REE are present as trivalent species after weathering. Thermodynamic equilibrium calculations results using Visual Minteq suggest that REE could precipitate as secondary phosphates (REEPO 4 ). Copyright © 2018 Elsevier Ltd. All rights reserved.

Structure, Morphology, and Optical Properties of Amorphous and Nanocrystalline Gallium Oxide Thin Films

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

Kumar, S. Sampath; Rubio, E. J.; Noor-A-Alam, M.

Ga2O3 thin films were produced by sputter deposition by varying the substrate temperature (Ts) in a wide range (Ts=25-800 oC). The structural characteristics and optical properties of Ga2O3 films were evaluated using X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectrometry (EDS), Rutherford backscattering spectrometry (RBS) and spectrophotometric measurements. The effect of growth temperature is significant on the chemistry, crystal structure and morphology of Ga2O3 films. XRD and SEM analyses indicate that the Ga2O3 films grown at lower temperatures were amorphous while those grown at Ts≥500 oC were nanocrystalline. RBS measurements indicate the well-maintained stoichiometry of Ga2O3 films atmore » Ts=300-700 oC. The spectral transmission of the films increased with increasing temperature. The band gap of the films varied from 4.96 eV to 5.17 eV for a variation in Ts in the range 25-800 oC. A relationship between microstructure and optical property is discussed.« less

Photoelectrochemical Performance of TiO2/Ti Electrode for Organic Compounds

NASA Astrophysics Data System (ADS)

Maulidiyah, M.; Wijawan, I. B. P.; Wibowo, D.; Aladin, A.; Hamzah, B.; Nurdin, M.

2018-05-01

Photoelectrochemical performance of TiO2/Ti electrode was investigated by using organic compounds. The TiO2/Ti electrode was prepared by anodic oxidation at a potential bias of 25 V for 4 h then calcined for 450 °C to obtain the anatase polymorph. Subsequently, it was characterized by X-Ray Diffraction (XRD) and Scanning Electron Microscope-Energy Dispersive X-ray (SEM-EDX). The XRD pattern showed that TiO2 has anatase phase as confirmed by 2θ peaks at 37.93° 63.00°, and 83.00°. Using SEM-EDX data the TiO2 layer was formed on Ti plate with the composition of Ti (4.5 keV) and O (0.5 keV) elements. Furthermore, the photoelectrochemical sensing on the three organic compounds (ascorbic acid, glucose, and titan yellow) with the electrolyte addition showed that the linearity of TiO2/Ti electrode were 0.937, 0.968, and 0.938, meanwhile without the electrolyte were 0.998, 0.989, and 0.923, respectively.

Nano-sized ZnO powders prepared by co-precipitation method with various pH

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

Purwaningsih, S. Y., E-mail: sriyanisaputri@gmail.com; Pratapa, S.; Triwikantoro,

2016-04-19

In this work, nano-sized ZnO powders have been synthesized by the co-precipitation method with Zn(CH3COOH)2.2H2O, HCl, and NH3.H2O as raw materials in various pH ranging from 8 to 10. The purity, microstructure, chemical group analysis, morphology of the prepared ZnO powders were studied by X-ray diffraction (XRD), Fourier transform infrared spectrometer (FTIR), energy dispersive X-ray spectrometry (EDX), and scanning electron microscope (SEM), respectively. Rietveld refinement of XRD data showed that ZnO crystallizes in the wurtzite structure with high purity. The obtained powders were nano-sized particles with the average crystallite size about 17.9 ± 2.1 nm synthesized with pH of 9.5, atmore » 85°C, and stirring time of 6 h. The SEM results have visualied the morphology of ZnO nanoparticles with spherical-like shape. The effect of processing conditions on morphology of ZnO was also discussed.« less

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

Chandraboss, V.L.; Natanapatham, L.; Karthikeyan, B.

Graphical abstract: The hetero-junctions that are formed between the ZnO and the Bi provide an internal electric field that facilitates separation of the electron-hole pairs and induces faster carrier migration. Thus they often enhanced photocatalytic reaction. - Highlights: • Bi-doped ZnO nanocomposite material was prepared by precipitation method. • Characterized by XRD, HR-SEM with EDX, UV–visible DRS and FT-RAMAN analysis. • Bi-doped ZnO nanocomposite material was used to photodegradation of Congo red. • Mechanism and photocatalytic effect of nanocomposite material have been discussed. - Abstract: Bismuth (Bi)-doped ZnO nanocomposite material was prepared by precipitation method with doping precursors of bismuthmore » nitrate pentahydrate and oxalic acid, characterized by X-ray diffraction (XRD), High Resolution-Scanning Electron Microscopy (HR-SEM) with Energy Dispersive X-ray (EDX) analysis, UV–visible Diffuse Reflectance Spectroscopy (UV–visible DRS) and Fourier Transform-Raman (FT-RAMAN) analysis. The enhanced photocatalytic activity of the Bi-doped ZnO is demonstrated through photodegradation of Congo red under UV-light irradiation. The mechanism of photocatalytic effect of Bi-doped ZnO nanocomposite material has been discussed.« less

Electrochemical synthesis and photoelectrochemical properties of grass-like nanostructured α-Fe2O3 photoanodes for use in solar water oxidation

NASA Astrophysics Data System (ADS)

Hanedar, Yesim; Demir, Umit; Oznuluer, Tuba

2016-10-01

Grass-like nanostructured α-Fe2O3 photoelectrodes were prepared for the first time through a simple cathodic electrodeposition method from an oxygenated aqueous solution of Fe3+ at room temperature without using surfactant, capping agents or any other additives. The α-Fe2O3 electrodeposits were characterized by X-ray photoelectron spectroscopy (XPS), energy dispersive spectroscopy (EDS), scanning electron microscopy (SEM), X-ray diffraction (XRD), UV-vis absorption and photoelectrochemical (PEC) techniques. The SEM and XRD results indicated that the as-deposited α-Fe2O3 are composed of single crystalline nanoleaves. The formation mechanisms of α-Fe2O3 have also been proposed based on a series of cyclic voltammetric and XPS studies. This new electrochemical method is expected to be a useful technique for the fabrication of single crystalline and photoactive α-Fe2O3 nanostructures directly onto the electrode surface, which is required in most applications, such as energy conversion and storage and sensors.

Dynamical effects in Bragg coherent x-ray diffraction imaging of finite crystals

NASA Astrophysics Data System (ADS)

Shabalin, A. G.; Yefanov, O. M.; Nosik, V. L.; Bushuev, V. A.; Vartanyants, I. A.

2017-08-01

We present simulations of Bragg coherent x-ray diffractive imaging (CXDI) data from finite crystals in the frame of the dynamical theory of x-ray diffraction. The developed approach is based on a numerical solution of modified Takagi-Taupin equations and can be applied for modeling of a broad range of x-ray diffraction experiments with finite three-dimensional crystals of arbitrary shape also in the presence of strain. We performed simulations for nanocrystals of a cubic and hemispherical shape of different sizes and provided a detailed analysis of artifacts in the Bragg CXDI reconstructions introduced by the dynamical diffraction. Based on our theoretical analysis we developed an analytical procedure to treat effects of refraction and absorption in the reconstruction. Our results elucidate limitations for the kinematical approach in the Bragg CXDI and suggest a natural criterion to distinguish between kinematical and dynamical cases in coherent x-ray diffraction on a finite crystal.

X-ray analyses of thermally grown and reactively sputtered tantalum oxide films on NiTi alloy

NASA Astrophysics Data System (ADS)

McNamara, Karrina; Tofail, Syed A. M.; Conroy, Derek; Butler, James; Gandhi, Abbasi A.; Redington, Wynette

2012-08-01

Sputter deposition of tantalum (Ta) on the surface of NiTi alloy is expected to improve the alloy's corrosion resistance and biocompatibility. Tantalum is a well-known biomaterial which is not affected by body fluids and is not irritating to human tissue. Here we compare the oxidation chemistry crystal structure evolution of tantalum oxide films grown on NiTi by reactive O2 sputtering and by thermal oxidation of sputter deposited Ta films. The effect of sputtering parameters and post-sputtering treatments on the morphology, oxidation state and crystal structure of the tantalum oxide layer have been investigated by field-emission scanning electron microscopy (FE-SEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). The study has found that it may be better to avoid oxidation at and above 600 °C. The study establishes that reactive sputtering in presence of low oxygen mixture yields thicker film with better control of the film quality except that the surface oxidation state of Ta is slightly lower.

Structure, crystallization and dielectric resonances in 2-13 GHz of waste-derived glass-ceramic

NASA Astrophysics Data System (ADS)

Yao, Rui; Liao, SongYi; Chen, XiaoYu; Wang, GuangRong; Zheng, Feng

2016-12-01

Structure, kinetics of crystallization, and dielectric resonances of waste-derived glass-ceramic prepared via quench-heating route were studied as a function of dosage of iron ore tailing (IOT) within 20-40 wt% using X-ray diffraction (XRD), fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), scanning electron microscopy (SEM) with energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), and vector network analyzer (VNA) measurements. The glass-ceramic mainly consisted of ferrite crystals embedded in borosilicate glass matrix. Crystallization kinetics and morphologies of ferrite crystals as well as coordination transformation of boron between [BO4] and [BO3] in glass network were adjustable by changing the amount of IOT. Dielectric resonances in 6-13 GHz were found to be dominated by oscillations of Ca2+ cations in glass network with [SiO4] units on their neighboring sites. Ni2+ ions made a small contribution to those resonances. Diopside formed when IOT exceeded 35 wt%, which led to weakening of the resonances.

Characterization and Evaluation of Ti-Zr-V Non-evaporable Getter Films Used in Vacuum Systems

NASA Astrophysics Data System (ADS)

Ferreira, M. J.; Seraphim, R. M.; Ramirez, A. J.; Tabacniks, M. H.; Nascente, P. A. P.

Among several methods used to obtain ultra-high vacuum (UHV) for particles accelerators chambers, it stands out the internal coating with metallic films capable of absorbing gases, called NEG (non-evaporable getter). Usually these materials are constituted by elements of great chemical reactivity and solubility (such as Ti, Zr, and V), at room temperature for oxygen and other gases typically found in UHV, such as H2, CO, and CO2. Gold and ternary Ti-Zr-V films were produced by magnetron sputtering, and their composition, structure, morphology, and aging characteristics were characterized by energy-dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), field emission gun sc anning electronmicroscopy (FEG-SEM), atomic force microscopy (AFM), high resolution transmission electron microscopy (HRTEM). The comparison between the produced films and commercial samples indicated that the desirable characteristics depend on the nanometric structure of the films and that this structure is sensitive to the heat treatments.

Jingle-bell-shaped ferrite hollow sphere with a noble metal core: Simple synthesis and their magnetic and antibacterial properties

NASA Astrophysics Data System (ADS)

Li, Siheng; Wang, Enbo; Tian, Chungui; Mao, Baodong; Kang, Zhenhui; Li, Qiuyu; Sun, Guoying

2008-07-01

In this paper, a simple strategy is developed for rational fabrication of a class of jingle-bell-shaped hollow structured nanomaterials marked as Ag@ MFe 2O 4 ( M=Ni, Co, Mg, Zn), consisting of ferrite hollow shells and metal nanoparticle cores, using highly uniform colloidal Ag@C microspheres as template. The final composites were obtained by direct adsorption of metal cations Fe 3+ and M 2+ on the surface of the Ag@C spheres followed by calcination process to remove the middle carbon shell and transform the metal ions into pure phase ferrites. The as-prepared composites were characterized by X-ray photoelectron spectroscopy (XPS), energy-dispersive X-ray analysis (EDX), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-vis spectroscopy and SQUID magnetometer. The results showed that the composites possess the magnetic property of the ferrite shell and the optical together with antibacterial property of the Ag core.

Preliminary study on the mode of occurrence of arsenic in high arsenic coals from southwest Guizhou Province

USGS Publications Warehouse

Ding, Z.; Zheng, B.; Zhang, Jiahua; Belkin, H.E.; Finkelman, R.B.; Zhao, F.; Zhou, D.; Zhou, Y.; Chen, C.

1999-01-01

Coal samples from high arsenic coal areas have been analyzed by electron microprobe analyzer (EMPA), scanning electron microscopy with an energy dispersive X-ray analyzer (SEM-EDX), X-ray diffraction analysis (XRD), low temperature ashing (LTA), transmission electron microscopy (TEM), X-ray absorption fine structure (XAFS), instrument neutron activation analysis (INAA) and wet chemical analysis. Although some As-bearing minerals such as pyrite, arsenopyrite, realgar (?), As-bearing sulfate, and As-bearing clays are found in the high arsenic coals, their contents do not account for the abundance of arsenic in the some coals. Analysis of the coal indicates that arsenic exists mainly in the form of As5+ and As3+, combined with compounds in the organic matrix. The occurrence of such exceptionally high arsenic contents in coal and the fact that the arsenic is dominantly organically associated are unique observations. The modes of occurrence of arsenic in high As-coals are discussed.

The preparation and cathodoluminescence of ZnS nanowires grown by chemical vapor deposition

NASA Astrophysics Data System (ADS)

Huang, Meng-Wen; Cheng, Yin-Wei; Pan, Ko-Ying; Chang, Chen-Chuan; Shieu, F. S.; Shih, Han C.

2012-11-01

Single crystal ZnS nanowires were successfully synthesized in large quantities on Si (1 0 0) substrates by simple thermal chemical vapor deposition without using any catalyst. The morphology, composition, and crystal structure were characterized by field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), energy-dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS), and cathodoluminescence (CL) spectroscopy. SEM observations show that the nanowires have diameters about 20-50 nm and lengths up to several tens of micrometers. XRD and TEM results confirmed that the nanowires exhibited both wurtzite and zinc blende structures with growth directions aligned along [0 0 0 2] and [1 1 1], respectively. The CL spectrum revealed emission bands in the UV and blue regions. The blue emissions at 449 and ˜581 nm were attributed to surface states and impurity-related defects of the nanowires, respectively. The perfect crystal structure of the nanowires indicates their potential applications in nanotechnology and in the fabrication of nanodevices.

Evaluation of White Bentonite Modified by Acid Attack

NASA Astrophysics Data System (ADS)

Andrade, C. G. Bastos; Fermino, D. M.; Fernandes, M. G.; Valenzuela-Diaz, F. R.

For industrial use, the smectite clays must be cleared of impurities, usually obtained by acid modification, using a high concentration solution of inorganic acid at temperatures under boiling point. In the present paper, a sample of white bentonite from Paraiba, Brazil, was modified by hydrochloric acid under moderate conditions (90°C, reaction times of 1, 6, 12, 18 and 24hours in close reactor, concentration of the aqueous solution of hydrochloric acid 1.5 M, acid solution/clay ratio of 1g/10mL). The purpose of these attacks is to reduce the concentration of impurities with minimal change in the clay minerals structure. The modified samples were characterized by X-ray diffraction (XRD), X-ray fluorescence (XRF), Cation Exchange Capacity (CEC), Stereomicroscopy, Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Detector (EDS). Thus, this modified bentonite tends to be a good economic and environmental alternative in manufacturing of products with high added value such as cosmetics and polymer/clay nanocomposites.

Influences of Co doping on the structural and optical properties of ZnO nanostructured

NASA Astrophysics Data System (ADS)

Majeed Khan, M. A.; Wasi Khan, M.; Alhoshan, Mansour; Alsalhi, M. S.; Aldwayyan, A. S.

2010-07-01

Pure and Co-doped ZnO nanostructured samples have been synthesized by a chemical route. We have studied the structural and optical properties of the samples by using X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), field-emission transmission electron microscope (FETEM), energy-dispersive X-ray (EDX) analysis and UV-VIS spectroscopy. The XRD patterns show that all the samples are hexagonal wurtzite structures. Changes in crystallite size due to mechanical activation were also determined from X-ray measurements. These results were correlated with changes in particle size followed by SEM and TEM. The average crystallite sizes obtained from XRD were between 20 to 25 nm. The TEM images showed the average particle size of undoped ZnO nanostructure was about 20 nm whereas the smallest average grain size at 3% Co was about 15 nm. Optical parameters such as absorption coefficient ( α), energy band gap ( E g ), the refractive index ( n), and dielectric constants ( σ) have been determined using different methods.

Direct-write maskless lithography using patterned oxidation of Si-substrate Induced by femtosecond laser pulses

NASA Astrophysics Data System (ADS)

Kiani, Amirkianoosh; Venkatakrishnan, Krishnan; Tan, Bo

2013-03-01

In this study we report a new method for direct-write maskless lithography using oxidized silicon layer induced by high repetition (MHz) ultrafast (femtosecond) laser pulses under ambient condition. The induced thin layer of predetermined pattern can act as an etch stop during etching process in alkaline etchants such as KOH. The proposed method can be leading to promising solutions for direct-write maskless lithography technique since the proposed method offers a higher degree of flexibility and reduced time and cost of fabrication which makes it particularly appropriate for rapid prototyping and custom scale manufacturing. A Scanning Electron Microscope (SEM), Micro-Raman, Energy Dispersive X-ray (EDX), optical microscope and X-ray diffraction spectroscopy (XRD) were used to evaluate the quality of oxidized layer induced by laser pulses.

Flake like V{sub 2}O{sub 5} nanoparticles for ethanol sensing at room temperature

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

Chitra, M.; Uthayarani, K.; Rajasekaran, N.

2016-05-23

The versatile redox property of vanadium oxide explores it in various applications like catalysis, electrochromism, electrochemistry, energy storage, sensors, microelectronics, batteries etc., In this present work, vanadium oxide was prepared via hydrothermal route followed by calcination. The structural and lattice parameters were analysed from the powder X-ray diffraction (XRD) pattern. The morphology and the composition of the sample were obtained from Field emission Scanning electron microscopic (FeSEM) and Energy Dispersive X-ray (EDAX) Spectrometric analysis respectively. The sensitivity, response – recovery time of the sample towards ethanol (0 ppm – 300 ppm) sensing at room temperature was measured and the present investigation onmore » vanadium oxide nanoparticles over the flakes shows better sensitivity (30%) at room temperature.« less

Preparation of Ag-loaded octahedral Bi2WO6 photocatalyst and its photocatalytic activity

NASA Astrophysics Data System (ADS)

An, Liang; Wang, Guanghui; Zhou, Xuan; Wang, Yi; Gao, Fang; Cheng, Yang

2014-12-01

In this work, an Ag-loaded octahedral Bi2WO6 photocatalyst has been successfully prepared by the hydrothermal method and photo deposition method. X-ray diffraction (XRD), energy dispersive analysis of X-ray (EDX), field-emission scanning electron microscopy (FE-SEM) and ultra-violet adsorption spectrum (UV-Vis) were employed for characterization of the composite photocatalyst. Furthermore, two different photocatalysts including the obtained Ag-loaded octahedral Bi2WO6 were employed here for photodegradation of model contaminated water of Orange II (OII). Results show that Ag-loaded Bi2WO6 photocatalyst exhibits superior photocatalytic properties compared to the undoped Bi2WO6. The reasons for improvement in photocatalytic activity of the Ag-loaded octahedral Bi2WO6 were also discussed.

Archaeometric study of black-coated pottery from Pompeii by different analytical techniques.

PubMed

Scarpelli, Roberta; Clark, Robin J H; De Francesco, Anna Maria

2014-01-01

Complementary spectroscopic methods were used to characterize ceramic body and black coating of fine pottery found at Pompeii (Italy). This has enabled us to investigate local productions and to clarify the technological changes over the 4th-1st centuries BC. Two different groups of ceramics were originally distinguished on the basis of macroscopic observations. Optical microscopy (OM), X-ray diffraction (XRD) and X-ray fluorescence (XRF) seem to indicate the usage of the same raw materials for the production of black-coated ceramics at Pompeii for about three centuries. Raman microscopy (RM) and micro-analysis (SEM/EDS) suggest different production treatments for both raw material processing and firing practice (duration of the reducing step and the cooling rate). Copyright © 2013 Elsevier B.V. All rights reserved.

In situ formation deposited ZnO nanoparticles on silk fabrics under ultrasound irradiation.

PubMed

Khanjani, Somayeh; Morsali, Ali; Joo, Sang W

2013-03-01

Deposition of zinc(II) oxide (ZnO) nanoparticles on the surface of silk fabrics was prepared by sequential dipping steps in alternating bath of potassium hydroxide and zinc nitrate under ultrasound irradiation. This coating involves in situ generation and deposition of ZnO in a one step. The effects of ultrasound irradiation, concentration and sequential dipping steps on growth of the ZnO nanoparticles have been studied. Results show a decrease in the particles size as increasing power of ultrasound irradiation. Also, increasing of the concentration and sequential dipping steps increase particle size. The physicochemical properties of the nanoparticles were determined by powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and wavelength dispersive X-ray (WDX). Copyright © 2012 Elsevier B.V. All rights reserved.

Structural and optical properties of Ni-doped CdS thin films prepared by chemical bath deposition method

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

Premarani, R.; Saravanakumar, S., E-mail: sarophy84@gmail.com; Chandramohan, R.

2015-06-24

The structural and optical behavior of undoped Cadmiun Sulphide (CdS) and Ni-doped CdS thinfilms prepared by Chemical Bath Deposition (CBD) technique is reported. The crystallite sizes of the thinfilms have been characterized by X-ray diffraction pattern (XRD). The particle sizes increase with the increase of Ni content in the CdS thinfilms. Scanning Electron Microscope (SEM) results indicated that CdS thinfilms is made up of aggregate of spherical-like particles. The composition was estimated by Energy Dispersive Analysis of X-ray (EDX) and reported. Spectroscopic studies revealed considerable improvement in transmission and the band gap of the films changes with addition of Nimore » dopant that is associated with variation in crystallite sizes in the nano regime.« less

Preparation and characterization of copper telluride thin films by modified chemical bath deposition (M-CBD) method

NASA Astrophysics Data System (ADS)

Pathan, H. M.; Lokhande, C. D.; Amalnerkar, D. P.; Seth, T.

2003-09-01

Copper telluride thin films were deposited using modified chemical method using copper(II) sulphate; pentahydrate [CuSO 4·5H 2O] and sodium tellurite [Na 2TeO 3] as cationic and anionic sources, respectively. Modified chemical method is based on the immersion of the substrate into separately placed cationic and anionic precursors. The preparative conditions such as concentration, pH, immersion time, immersion cycles, etc. were optimized to get good quality copper telluride thin films at room temperature. The films have been characterized for structural, compositional, optical and electrical transport properties by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDAX), Rutherford back scattering (RBS), optical absorption/transmission, electrical resistivity and thermoemf measurement techniques.

Crystallographic and magnetic properties of nanocrystalline perovskite structure SmFeO3 orthoferrite

NASA Astrophysics Data System (ADS)

Kumar, Ashwini; Shen, Jingdong; Zhao, Huihui; Zhengjian, Qi; Li, Qi

2018-05-01

In this article, we present the structural and magnetic studies of pristine SmFeO3 nanocrystalline ceramic samples as sintered at temperature 850 °C and 1000 °C. X-ray powder diffraction data confirm the existence of single-phase nature with orthorhombic (Pbnm) structure of the samples. The SEM image reveals spherical particles with a size range of 60-130 nm for SFO-850 and SFO-1000 samples. X-ray absorption spectroscopy studies on Fe L3,2 and O K-edges of SmFeO3 sample revealed the homo-valence state of Fe in these materials. From magnetization studies it has been observed the materials exhibit ferromagnetic and antiferromagnetic (canted spin structure) sub-lattices, which results strong magnetic anisotropy in the system.

Chrome-free Samarium-based Protective Coatings for Magnesium Alloys

NASA Astrophysics Data System (ADS)

Hou, Legan; Cui, Xiufang; Yang, Yuyun; Lin, Lili; Xiao, Qiang; Jin, Guo

The microstructure of chrome-free samarium-based conversion coating on magnesium alloy was investigated and the corrosion resistance was evaluated as well. The micro-morphology, transverse section, crystal structure and composition of the coating were observed by scanning electron microscopy (SEM), X-ray diffraction (XRD), energy dispersive spectroscopy (EDS) and X- ray photoelectron spectroscopy (XPS), respectively. The corrosion resistance was evaluated by potentiodynamic polarization curve and electrochemical impedance spectroscopy (EIS). The results reveal that the morphology of samarium conversion coating is of crack-mud structure. Tiny cracks distribute in the compact coating deposited by samarium oxides. XRD, EDS and XPS results characterize that the coating is made of amorphous and trivalent-samarium oxides. The potentiodynamic polarization curve, EIS and OCP indicate that the samarium conversion coating can improve the corrosion resistance of magnesium alloys.

Controlled synthesis of carbon-encapsulated copper nanostructures by using smectite clays as nanotemplates.

PubMed

Tsoufis, Theodoros; Colomer, Jean-François; Maccallini, Enrico; Jankovič, Lubos; Rudolf, Petra; Gournis, Dimitrios

2012-07-23

Rhomboidal and spherical metallic-copper nanostructures were encapsulated within well-formed graphitic shells by using a simple chemical method that involved the catalytic decomposition of acetylene over a copper catalyst that was supported on different smectite clays surfaces by ion-exchange. These metallic-copper nanostructures could be separated from the inorganic support and remained stable for months. The choice of the clay support influenced both the shape and the size of the synthesized Cu nanostructures. The synthesized materials and the supported catalysts from which they were produced were studied in detail by TEM and SEM, powder X-ray diffraction, thermal analysis, as well as by Raman and X-ray photoelectron spectroscopy. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Micro-Raman and FT-IR spectroscopic studies of ceramic shards excavated from ancient Stratonikeia city at Eskihisar village in West-South Turkey

NASA Astrophysics Data System (ADS)

Bahçeli, Semiha; Güleç, Gamze; Erdoğan, Hasan; Söğüt, Bilal

2016-02-01

In this study, micro-Raman and Fourier transformed infrared (FT-IR) spectroscopies, X-ray diffraction (XRD) and scanning electron microscope with energy dispersive X-ray (SEM-EDX) were used to characterize the mineralogical structures of pigments of four ceramic fragments in which one of them belongs to Hellenistic period (1st - IVth century BC) and other three ceramic shards belong to Early Rome (IVth century BC- 1st century AD) excavated from Stratonikeia ancient city. In the results of investigations on these four ceramic fragments, the various phases were identified: quartz, kaolinite, albit (or Na-feldspar), calcite, anastase, hematite and magnetite. Furthermore, the obtained findings indicate that firing temperature is about 800-850 °C for all the shards.

Structural, optical and photoelectric properties of sprayed CdS thin films

NASA Astrophysics Data System (ADS)

Chandel, Tarun; Dwivedi, Shailendra Kumar; Zaman, M. Burhanuz; Rajaram, P.

2018-05-01

In this study, CdS thin films were grown via a facile spray pyrolysis technique. The crystalline phase, morphological, compositional and optical properties of the CdS thin films have been studied using X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy, and UV-vis absorption spectroscopy, respectively. XRD patterns show that the grown CdS films crystallized in the hexagonal structure. Scanning electron microscopy (SEM) study shows that the surfaces of the films are smooth and are uniformly covered with nanoparticles. EDAX results reveal that the grown films have good stochiometry. UV-vis spectroscopy shows that the grown films have transparency above 80% over the entire visible region. The photo-electric response of the CdS films grown on glass substrates has been observed.

A facile and green preparation of reduced graphene oxide using Eucalyptus leaf extract

NASA Astrophysics Data System (ADS)

Li, Chengyang; Zhuang, Zechao; Jin, Xiaoying; Chen, Zuliang

2017-11-01

In this paper, a green and facile synthesis of reduced graphene oxide (GO) by Eucalyptus leaf extract (EL-RGO) was investigated, which was characterized with ultraviolet-visible spectroscopy (UV), Raman spectroscopy, X-ray diffraction (XRD), scanning electron microscope (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and Thermal gravimetric analysis (TG). Eucalyptus leaf extract also play both reducing and capping stabilizing agents prepared EL-RGO as shown a good stability and electrochemical properties. This approach could provide an alternative method to prepare EL-RGO in large-scale production. Moreover, the good electrochemical property and biocompatibility can be used in various applications. In addition, the merit of this study is that both the oxidized products and the reducing agents are environmental friendly by green reduction.

PVP capped CdS nanoparticles for UV-LED applications

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

Sivaram, H.; Selvakumar, D.; Jayavel, R., E-mail: rjvel@annauniv.edu

Polyvinlypyrrolidone (PVP) capped cadmium sulphide (CdS) nanoparticles are synthesized by wet chemical method. The powder X-ray diffraction (XRD) result indicates that the nanoparticles are crystallized in cubic phase. The optical properties are characterized by UV-Vis absorption. The morphology of CdS nanoparticles are studied using Scanning electron microscope (SEM). The thermal behavior of the as prepared nanoparticles has been examined by Thermo gravimetric analysis (TGA). The optical absorption study of pvp capped CdS reveal a red shift confirms the UV-LED applications.

Preparation and characterization of bismuth oxichloride (BiOCl) nanoparticles and nano zerovalent iron (nZVI)

NASA Astrophysics Data System (ADS)

Sarwan, Bhawna; Pare, Brijesh; Deep Acharya, Aman

2017-05-01

In this work, we have synthesized nano scale zerovalent iron (nZVI) particles by borohydride reduction method and bismuth oxichloride (BiOCl) by a hydrolysis method. X-ray powder diffraction (XRD) was used for the structural and chemical characterization, while scanning/transmission electron microscopy (SEM/TEM) were employed to determine the physical properties of the nanoparticles. The reactivity of synthesized nanoparticles was compared by decolorization of nile blue (NB) dye under visible irradiation.

Ion dynamics in nanocrystalline LiMnPO{sub 4} synthesised by novel template free hydrothermal approach

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

Vijayan, Lakshmi, E-mail: lakshmivijayan@gmail.com; Cheruku, Rajesh; Govindaraj, G.

A dense core rectangular shaped nanocrystalline LiMnPO{sub 4} material was synthesized by template free sucrose assisted hydrothermal synthesis. The material possess orthorhombic crystal structure with Pnma, space group having four formula units. The structural characterization was accomplished through X-ray diffraction, thermo gravimetry/differential thermal analysis. Morphology was identified by the SEM, VSM was used to verify the magnetic behavior of the material and electrical characterization was done through impedance spectroscopy and the results were reported.

Template synthesis of indium nanowires using anodic aluminum oxide membranes.

PubMed

Chen, Feng; Kitai, Adrian H

2008-09-01

Indium nanowires with diameters approximately 300 nm have been synthesized by a hydraulic pressure technique using anodic aluminum oxide (AAO) templates. The indium melt is injected into the AAO template and solidified to form nanostructures. The nanowires are dense, continuous and uniformly run through the entire approximately 60 microm thickness of the AAO template. X-ray diffraction (XRD) reveals that the nanowires are polycrystalline with a preferred orientation. SEM is performed to characterize the morphology of the nanowires.

Interaction of hydrogen chloride with alumina. [influence of outgas and temperature conditions on adsorption

NASA Technical Reports Server (NTRS)

Bailey, R. R.; Wightman, J. P.

1975-01-01

The influence of outgas conditions and temperature on the adsorptive properties of two aluminas Alon-c and Al6sG were studied using adsorption isotherm measurements. Alon-C and Al6SG were characterized using X-ray powder diffraction, thermogravimetric analysis (TGA), scanning electron microscopy (SEM) and BET nitrogen surface areas. Some of these techniques were applied to two other aluminas but no isotherm data was obtained. Isotherm data and techniques applied to each alumina are summarized in tabular form.

Nonvolatile RRAM cells from polymeric composites embedding recycled SiC powders.

PubMed

De Girolamo Del Mauro, Anna; Nenna, Giuseppe; Miscioscia, Riccardo; Freda, Cesare; Portofino, Sabrina; Galvagno, Sergio; Minarini, Carla

2014-10-21

Silicon carbide powders have been synthesized from tires utilizing a patented recycling process. Dynamic light scattering, Raman spectroscopy, SEM microscopy, and X-ray diffraction have been carried out to gather knowledge about powders and the final composite structure. The obtained powder has been proven to induce resistive switching in a PMMA polymer-based composite device. Memory effect has been detected in two-terminal devices having coplanar contacts and quantified by read-write-erase measurements in terms of level separation and persistence.

Characterization of the Microstructure of the Compositionally Complex Alloy Al1Mo0.5Nb1Ta0.5Ti1Zr1 (Postprint)

DTIC Science & Technology

2016-05-01

limited to X-ray diffraction ( XRD ) and scanning electron microscopy (SEM). The alloy was reported to contain two bcc phases with similar lattice...it appears that the interface between the two phases is fairly coherent. Interestingly, the XRD study described in [8] suggested that there were two...line-scan shown in (h). 3 Distribution A. Approved for public reledifference in lattice parameter measurements realized in bulk samples ( XRD ) vs

Laser sintered thin layer graphene and cubic boron nitride reinforced nickel matrix nanocomposites

NASA Astrophysics Data System (ADS)

Hu, Zengrong; Tong, Guoquan

2015-10-01

Laser sintered thin layer graphene (Gr)-cubic boron nitride (CBN)-Ni nanocomposites were fabricated on AISI 4140 plate substrate. The composites fabricating process, composites microstructure and mechanical properties were studied. Scanning electron microscopy (SEM), X-ray diffraction (XRD) and Raman spectroscopy were employed to study the micro structures and composition of the composites. XRD and Raman tests proved that graphene and CBN were dispersed in the nanocomposites. Nanoindentation test results indicate the significant improvements were achieved in the composites mechanical properties.

Electrocrystallization and Properties of Supersaturated Solid Solutions of Copper

NASA Astrophysics Data System (ADS)

Povetkin, V. V.; Ivanova, T. E.; Ismagilova, A. V.

2018-03-01

The role of the alloying element in the formation of the structure and properties of electrolytic copper alloys has been determined. The X-ray diffraction analysis (XRD) and scanning electron microscopy (SEM) have shown that electrochemical alloying of copper with low-melting metals leads to the formation of supersaturated solid solutions (SSS) on the cathode, crushing of the crystal structure, smoothing of the surface relief, hardening of the deposits obtained, increasing their solderability and corrosive resistance to acidic media.

DEVELOPMENT OF LiCo0.90Mg0.05Al0.05O2 THIN FILMS BY PULSED LASER DEPOSITION TECHNIQUE

NASA Astrophysics Data System (ADS)

Vasanthi, R.; Ruthmangani, I.; Manoravi, P.; Joseph, M.; Kesavamoorthy, R.; Sundar, C.; Selladurai, S.

LiCo0.90Mg0.05Al0.05O2 bulk powders are synthesized using combustion process and made into a thin film by depositing on silicon wafer using a pulsed laser ablation technique. A comparative study by SEM (Scanning Electron Microscope) XRD (X-ray diffraction), Infrared spectroscopy and Raman Spectroscopy is performed on both bulk and PLD thin films.

Advantages of barium peroxide in the powder synthesis of perovskite superconductors

NASA Technical Reports Server (NTRS)

Hepp, A. F.; Gaier, J. R.; Philipp, W. H.; Warner, J. D.; Garlick, R. G.; Pouch, J. J.

1988-01-01

This paper compares reaction chemistry, material processing, and material characteristics for the solid state reaction using BaCO3 or BaO2 in the synthesis of perovskite superconductors. Results are presented for weight loss and X-ray diffraction, sample morphology and homogeneity as monitored by SEM and EDS, and the superconductivity critical temperature and ac susceptibility. Greater mass density, increased sample homogeneity, lower resistance, and improved reproducibility for material are found when BaO32 is used.

Characterization of graphene oxide produced by Hummers method and its supercapacitor applications

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

Akgül, Ö., E-mail: omeraakgul@gmail.com; Tanrıverdi, A., E-mail: aa.kudret@hotmail.com; Alver, Ü., E-mail: ualver@ktu.edu.tr

2016-03-25

In this study, Graphene Oxide (GO) is produced using Hummers method. The produced GO were investigated by x-ray diffraction (XRD), fourier transform infrared spectroscopy (FTIR), UV-Vis spectrum, Raman spectroscopy and scanning electron microscopy (SEM). GO films on Ni foam were prepared by doctor-blading technique. The electrochemical performances of the as-synthesized GO electrode was evaluated using cyclic voltammetry (CV) in 6 M KOH aqueous solution. Capacitances of GO electrode was measured as 0.76 F/g.

Influence of the Martensitic Transformation on the Microscale Plastic Strain Heterogeneities in a Duplex Stainless Steel

NASA Astrophysics Data System (ADS)

Lechartier, Audrey; Martin, Guilhem; Comby, Solène; Roussel-Dherbey, Francine; Deschamps, Alexis; Mantel, Marc; Meyer, Nicolas; Verdier, Marc; Veron, Muriel

2017-01-01

The influence of the martensitic transformation on microscale plastic strain heterogeneity of a duplex stainless steel has been investigated. Microscale strain heterogeneities were measured by digital image correlation during an in situ tensile test within the SEM. The martensitic transformation was monitored in situ during tensile testing by high-energy synchrotron X-ray diffraction. A clear correlation is shown between the plasticity-induced transformation of austenite to martensite and the development of plastic strain heterogeneities at the phase level.

Instrument and method for X-ray diffraction, fluorescence, and crystal texture analysis without sample preparation

NASA Technical Reports Server (NTRS)

Gendreau, Keith (Inventor); Martins, Jose Vanderlei (Inventor); Arzoumanian, Zaven (Inventor)

2010-01-01

An X-ray diffraction and X-ray fluorescence instrument for analyzing samples having no sample preparation includes a X-ray source configured to output a collimated X-ray beam comprising a continuum spectrum of X-rays to a predetermined coordinate and a photon-counting X-ray imaging spectrometer disposed to receive X-rays output from an unprepared sample disposed at the predetermined coordinate upon exposure of the unprepared sample to the collimated X-ray beam. The X-ray source and the photon-counting X-ray imaging spectrometer are arranged in a reflection geometry relative to the predetermined coordinate.

Comparative studies of mononuclear Ni(II) and UO2(II) complexes having bifunctional coordinated groups: Synthesis, thermal analysis, X-ray diffraction, surface morphology studies and biological evaluation

NASA Astrophysics Data System (ADS)

Fahem, Abeer A.

2012-03-01

Two Schiff base ligands derived from condensation of phthalaldehyde and o-phenylenediamine in 1:2 (L1) and 2:1 (L2) having bifunctional coordinated groups (NH2 and CHO groups, respectively) and their metal complexes with Ni(II) and UO2(II) have been synthesized and characterized by elemental analysis, molar conductance, magnetic susceptibilities and spectral data (IR, 1H NMR, mass and solid reflectance) as well as thermal, XRPD and SEM analysis. The formula [Ni(L1)Cl2]·2.5H2O, [UO2(L1)(NO3)2]·2H2O, [Ni(L2)Cl2]·1.5H2O and [UO2(L2)(NO3)2] have been suggested for the complexes. The vibrational spectral data show that the ligands behave as neutral ligands and coordinated to the metal ions in a tetradentate manner. The Ni(II) complexes are six coordinate with octahedral geometry and the ligand field parameters: Dq, B, β and LFSE were calculated while, UO2(II) complexes are eight coordinate with dodecahedral geometry and the force constant, FUsbnd O and bond length, RUsbnd O were calculated. The thermal decomposition of complexes ended with metal chloride/nitrate as a final product and the highest thermal stability is displayed by [UO2(L2)(NO3)2] complex. The X-ray powder diffraction data revealed the formation of nano sized crystalline complexes. The SEM analysis provides the morphology of the synthesized compounds and SEM image of [UO2(L2)(NO3)2] complex exhibits nano rod structure. The growth-inhibiting potential of the ligands and their complexes has been assessed against a variety of bacterial and fungal strains.

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

PubMed

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

2015-02-05

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

Rare earth substitution on structural and optical behaviour of CdSe thin films

NASA Astrophysics Data System (ADS)

Singh, Sarika; Shrivastava, A. K.; Tapdiya, Swati

2018-05-01

A series of Sm2+,Gd2+ doped with Cadmium selenide CdSe (x =0.01) has been prepared by using Chemical bath deposition technique. Structural, Optical and Morphological studies were performed using X-ray diffraction (XRD), UV-Visible spectrometer, Raman Studies and Scanning Electron Microscopy (SEM). XRD patterns confirm the samples with Sm,Gd ions, some diffraction peaks appeared which belongs to the cubic phase structure. The values of lattice parameter (a) decreased and particle size decrease on doping. Morphology of the grown films reveals that surface are homogeneous and uniformly spread on the substrates. The elemental analysis of CdSe doped Sm and Gd (1%) different composition was analyzed by Energy Dispersive X-Rays (EDX). The optical values of some important parameters of the studied films were calculated by UVstudy are determined from transmission spectra at wavelength 200 to 900nm. Optical band gap Eg was calculated by tauc relation. Energy band gap of CdSe doped with Sm and Gd varies at 1.8eV and 1.9eV respectively. Bandgap In Raman analysis, a prominent peak shows that confirmation of nano crystalline phase. And intensity of peaks was decreasing after doping.

One step synthesis of porous graphene by laser ablation: A new and facile approach

NASA Astrophysics Data System (ADS)

Kazemizadeh, Fatemeh; Malekfar, Rasoul

2018-02-01

Porous graphene (PG) was obtained using one step laser process. Synthesis was carried out by laser ablation of nickel-graphite target under ultra-high flow of argon gas. The field emission scanning electron microscopy (FE-SEM) results showed the formation of a porous structure and the transmission electron microscopy (TEM) revealed that the porosity of PGs increase under intense laser irradiation. Structural characterization study using Raman spectroscopy, X-ray powder diffraction (XRD) and selected area electron diffraction (SAED) technique showed that the obtained PGs display high crystalline structure in the form of few layer rhombohedral graphitic arrangement that can be interpreted as the phase prior to the formation of other carbon nanostructures.

Philip A. Parilla | NREL

Science.gov Websites

atomic layer deposition for applications. He also manages the majority of X-ray characterization equipment at NREL, specifically X-ray diffraction and X-ray fluorescence instrumentation. Additionally, he for EERE's Hydrogen Storage program. He is also an expert in X-ray diffraction and X-ray fluorescence

Simulations of X-ray diffraction of shock-compressed single-crystal tantalum with synchrotron undulator sources.

PubMed

Tang, M X; Zhang, Y Y; E, J C; Luo, S N

2018-05-01

Polychromatic synchrotron undulator X-ray sources are useful for ultrafast single-crystal diffraction under shock compression. Here, simulations of X-ray diffraction of shock-compressed single-crystal tantalum with realistic undulator sources are reported, based on large-scale molecular dynamics simulations. Purely elastic deformation, elastic-plastic two-wave structure, and severe plastic deformation under different impact velocities are explored, as well as an edge release case. Transmission-mode diffraction simulations consider crystallographic orientation, loading direction, incident beam direction, X-ray spectrum bandwidth and realistic detector size. Diffraction patterns and reciprocal space nodes are obtained from atomic configurations for different loading (elastic and plastic) and detection conditions, and interpretation of the diffraction patterns is discussed.

Simulations of X-ray diffraction of shock-compressed single-crystal tantalum with synchrotron undulator sources

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

Tang, M. X.; Zhang, Y. Y.; E, J. C.

Polychromatic synchrotron undulator X-ray sources are useful for ultrafast single-crystal diffraction under shock compression. Here, simulations of X-ray diffraction of shock-compressed single-crystal tantalum with realistic undulator sources are reported, based on large-scale molecular dynamics simulations. Purely elastic deformation, elastic–plastic two-wave structure, and severe plastic deformation under different impact velocities are explored, as well as an edge release case. Transmission-mode diffraction simulations consider crystallographic orientation, loading direction, incident beam direction, X-ray spectrum bandwidth and realistic detector size. Diffraction patterns and reciprocal space nodes are obtained from atomic configurations for different loading (elastic and plastic) and detection conditions, and interpretation of themore » diffraction patterns is discussed.« less

Coherent X-ray diffraction imaging of nanoengineered polymeric capsules

NASA Astrophysics Data System (ADS)

Erokhina, S.; Pastorino, L.; Di Lisa, D.; Kiiamov, A. G.; Faizullina, A. R.; Tayurskii, D. A.; Iannotta, S.; Erokhin, V.

2017-10-01

For the first time, nanoengineered polymeric capsules and their architecture have been studied with coherent X-ray diffraction imaging technique. The use of coherent X-ray diffraction imaging technique allowed us to analyze the samples immersed in a liquid. We report about the significant difference between polymeric capsule architectures under dry and liquid conditions.

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

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

Murray, Thomas D.; Johns Hopkins University School of Medicine, Baltimore, MD 21205; Lyubimov, Artem Y.

A highly X-ray-transparent, silicon nitride-based device has been designed and fabricated to harvest protein microcrystals for high-resolution X-ray diffraction data collection using microfocus beamlines and XFELs. Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming themore » challenges intrinsic to microcrystal analysis is to pair so-called ‘fixed-target’ sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« 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

Photocatalytic properties of h-WO3 nanoparticles obtained by annealing and h-WO3 nanorods prepared by hydrothermal method

NASA Astrophysics Data System (ADS)

Boyadjiev, Stefan I.; Nagy-Kovács, Teodóra; Lukács, István; Szilágyi, Imre M.

2016-03-01

In the present study, two different methods for preparing hexagonal WO3 (h-WO3) photocatalysts were used - controlled thermal decomposition and hydrothermal synthesis. WO3 nanoparticles with hexagonal structure were obtained by annealing (NH4)xWO3-y at 500 °C in air. WO3 nanorods were prepared by a hydrothermal method using sodium tungstate Na2WO4, HCl, (COOH)2 and NaSO4 precursors at 200 °C. The formation, morphology, structure and composition of the as-prepared nanoparticles and nanorods were studied by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), and scanning electron microscopy combined with energy-dispersive X-ray spectroscopy (SEM-EDX). The photocatalytic activity of the h-WO3 nanoparticles and nanorods was studied by decomposing methyl orange in aqueous solution under UV light irradiation.

Influence of Fe ions on structural, optical and thermal properties of SnO{sub 2} nanoparticles

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

Ahmed, Ateeq, E-mail: ateeqamu124@gmail.com; Tripathi, P.; Khan, Wasi

2016-05-23

In the present work, Fe doped SnO{sub 2} nanoparticles with the composition Sn{sub 1-x}Fe{sub x}O{sub 2} (x = 0, 0.02, 0.04 and 0.06) have been successfully synthesized using sol-gel auto combustion technique. The samples are characterized by X-ray diffraction (XRD), Scanning electron microscopy (SEM), Energy dispersive X-ray analysis (EDAX), Ultraviolet (UV-Visible) absorption spectroscopy and thermal gravimetric analysis (TGA). The XRD study shows that all the samples have been found in tetragonal rutile structure without any extra phase and average crystallite size which lies in the range of 6-17 nm. The EDAX spectrum confirmed the doping of Fe ion into tin oxidemore » nanomaterial. The optical band gap of doped SnO{sub 2} is found to decrease with increasing Fe ion concentration, which is due to the formation of donor energy levels in the actual band gap of SnO{sub 2}.« less

Synthesis and characterization of FeSe1-xTex (x=0, 0.5, 1) superconductors

NASA Astrophysics Data System (ADS)

Zargar, Rayees A.; Hafiz, A. K.; Awana, V. P. S.

2015-08-01

In this study, FeTe1-xSex (x=0,0.5,1) samples were prepared by conventional solid state reaction method and investigated by powder XRD, SEM, Raman and resistivity measurement techniques to reveal the effect of tellurium (Te) substitution in FeSe matrix. Rietveld analysis was performed on room temperature recorded, X-ray diffraction (XRD) patterns of pure FeSe, FeTe and FeSe0.5Te0.5 which shows that all the compounds are crystallized in a tetragonal structure. SEM images show the dense surface morphology. Raman spectra recorded in the range from 100 to 700 cm-1 at ambient temperature has been interpreted by P4/nmm space group of the lattice. The variation in intensity and shift in peak positions of some phonon modes has been discussed on the basis of variation in crystalline field effect by substituting Te in FeSe lattice. The resistivity versus temperature curves reveals that FeSe becomes superconductor at 7 K and FeSe0.5Te0.5 shows superconductivity below 14 K while FeTe is non-superconducting compound.

X-Ray Structure determination of the Glycine Cleavage System Protein H of Mycobacterium tuberculosis Using An Inverse Compton Synchrotron X-Ray Source

PubMed Central

Abendroth, Jan; McCormick, Michael S.; Edwards, Thomas E.; Staker, Bart; Loewen, Roderick; Gifford, Martin; Rifkin, Jeff; Mayer, Chad; Guo, Wenjin; Zhang, Yang; Myler, Peter; Kelley, Angela; Analau, Erwin; Hewitt, Stephen Nakazawa; Napuli, Alberto J.; Kuhn, Peter; Ruth, Ronald D.; Stewart, Lance J.

2010-01-01

Structural genomics discovery projects require ready access to both X-ray and NMR instrumentation which support the collection of experimental data needed to solve large numbers of novel protein structures. The most productive X-ray crystal structure determination laboratories make extensive frequent use of tunable synchrotron X-ray light to solve novel structures by anomalous diffraction methods. This requires that frozen cryo-protected crystals be shipped to large government-run synchrotron facilities for data collection. In an effort to eliminate the need to ship crystals for data collection, we have developed the first laboratory-scale synchrotron light source capable of performing many of the state-of-the-art synchrotron applications in X-ray science. This Compact Light Source is a first-in-class device that uses inverse Compton scattering to generate X-rays of sufficient flux, tunable wavelength and beam size to allow high-resolution X-ray diffraction data collection from protein crystals. We report on benchmarking tests of X-ray diffraction data collection with hen egg white lysozyme, and the successful high-resolution X-ray structure determination of the Glycine cleavage system protein H from Mycobacterium tuberculosis using diffraction data collected with the Compact Light Source X-ray beam. PMID:20364333

Preparation of N-doped ZnO-loaded halloysite nanotubes catalysts with high solar-light photocatalytic activity.

PubMed

Cheng, Zhi-Lin; Sun, Wei

2015-01-01

N-doped ZnO nanoparticles were successfully assembled into hollow halloysite nanotubes (HNTs) by using the impregnation method. The catalysts based on N-doped ZnO-loaded HNTs nanocomposites (N-doped ZnO/HNTs) were characterized by X-ray diffraction (XRD), transmission electron microscopy-energy dispersive X-ray (TEM-EDX), scanning electron microscopy-energy dispersive X-ray (SEM-EDX), UV-vis and Fourier transform infrared spectroscopy (FT-IR) techniques. The XRD pattern showed ZnO nanoparticles with hexagonal structure loaded on HNTs. The TEM-EDX analysis indicated ZnO particles with the crystal size of ca.10 nm scattered in hollow structure of HNTs, and furthermore the concentration of N atom in nanocomposites was up to 2.31%. The SEM-EDX verified most of N-ZnO nanoparticles existing in hollow nanotubes of HNTs. Besides containing an obvious ultraviolet absorbance band, the UV-vis spectra of the N-doped ZnO/HNTs catalysts showed an available visible absorbance band by comparing to HNTs and non-doped ZnO/HNTs. The photocatalytic activity of the N-doped ZnO/HNTs catalysts was evaluated by the degradation of methyl orange (MO) solution with the concentration of 20 mg/L under the simulated solar-light irradiation. The result showed that the N-doped ZnO/HNTs catalyst exhibited a desirable solar-light photocatalytic activity.

Characterization of the Roman curse tablet

NASA Astrophysics Data System (ADS)

Liu, Wen; Zhang, Boyang; Fu, Lin

2017-08-01

The Roman curse tablet, produced in ancient Rome period, is a metal plate that inscribed with curses. In this research, several techniques were used to find out the physical structure and chemical composition of the Roman curse tablet, and testified the hypothesis that whether the tablet is made of pure lead or lead alloy. A sample of Roman Curse Tablet from the Johns Hopkins Archaeological Museum was analyzed using several different characterization techniques to determine the physical structure and chemical composition. The characterization techniques used were including optical microscopy, scanning electron microscopy (SEM), atomic force microscopy (AFM), and differential scanning calorimetry (DSC). Because of the small sample size, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and X-ray fluorescence (XRF) cannot test the sample. Results from optical microscopy and SEM, enlarged images of the sample surface were studied. The result revealed that the sample surface has a rough, non-uniform, and grainy surface. AFM provides three-dimensional topography of the sample surface, studying the sample surface in atomic level. DSC studies the thermal property, which is most likely a lead-alloy, not a pure lead. However, none of these tests indicated anything about the chemical composition. Future work will be required due to the lack of measures finding out its chemical composition. Therefore, from these characterization techniques above, the Roman curse tablet sample is consisted of lead alloy, not pure lead.

Mineralogy and geochemistry of atmospheric particulates in western Iran

NASA Astrophysics Data System (ADS)

Ahmady-Birgani, Hesam; Mirnejad, Hassan; Feiznia, Sadat; McQueen, Ken G.

2015-10-01

This study investigates the mineralogy and physico-chemical properties of atmospheric particulates collected at Abadan (southwestern Iran) near the Persian Gulf coast and Urmia (northwestern Iran) during ambient and dust events over 6 months (winter 2011; spring 2012). Particle sizes collected were: TSP (total suspended particulates); PM10 (particulates <10 μm); and PM2.5 (particulates <2.5 μm). Minerals were identified using X-ray diffraction (XRD); particle morphology and composition were examined by scanning electron microscopy and energy dispersive X-ray spectroscopy (SEM-EDX). Major minerals detected are calcite, quartz, clay minerals and gypsum, with relative abundance related to sampling site, collection period, wind direction, sampling head, and total sample amount. The anomalously high calcite content appears a characteristic feature originated from calcareous soils of the region. SEM observations indicated a wide range of particle morphologies over the 1-50 μm size range, with spherical, platy, cubic, elongate and prismatic shapes and rounding from angular to rounded. Energy dispersive X-ray analysis of TSP samples from both sites for non-dusty periods indicated that the sampled mineral suite contained Al, Mg, Na, Cl, P, S, Ca, K, Fe, Ti, and Si, mostly reflecting calcite, quartz, aluminosilicates, clays, gypsum and halite. Additionally, As, Pb, Zn, Mn, Sc, Nd, W, Ce, La, Ba and Ni were detected in TSP, PM10 and PM2.5 samples collected during dust events.

Laboratory plant study on the melting process of asbestos waste

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

Sakai, Shinichi; Terazono, Atsushi; Takatsuki, Hiroshi

The melting process was studied as a method of changing asbestos into non-hazardous waste and recovering it as a reusable resource. In an initial effort, the thermal behaviors of asbestos waste in terms of physical and chemical structure have been studied. Then, 10 kg/h-scale laboratory plant experiments were carried out. By X-ray diffraction analysis, the thermal behaviors of sprayed-on asbestos waste revealed that chrysotile asbestos waste change in crystal structure at around 800 C, and becomes melted slag, mainly composed of magnesium silicate, at around 1,500 C. Laboratory plant experiments on the melting process of sprayed-on asbestos have shown thatmore » melted slag can be obtained. X-ray diffraction analysis of the melted slag revealed crystal structure change, and SEM analysis showed the slag to have a non-fibrous form. And more, TEM analysis proved the very high treatment efficiency of the process, that is, reduction of the asbestos content to 1/10{sup 6} as a weight basis. These analytical results indicate the effectiveness of the melting process for asbestos waste treatment.« less

Green synthesis of soya bean sprouts-mediated superparamagnetic Fe 3O 4 nanoparticles

NASA Astrophysics Data System (ADS)

Cai, Yan; Shen, Yuhua; Xie, Anjian; Li, Shikuo; Wang, Xiufang

2010-10-01

Superparamagnetic Fe 3O 4 nanoparticles were first synthesized via soya bean sprouts (SBS) templates under ambient temperature and normal atmosphere. The reaction process was simple, eco-friendly, and convenient to handle. The morphology and crystalline phase of the nanoparticles were determined from scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and X-ray diffraction (XRD) spectra. The effect of SBS template on the formation of Fe 3O 4 nanoparticles was investigated using X-ray photoemission spectroscopy (XPS) and Fourier-transform infrared spectroscopy (FT-IR). The results indicate that spherical Fe 3O 4 nanoparticles with an average diameter of 8 nm simultaneously formed on the epidermal surface and the interior stem wall of SBS. The SBS are responsible for size and morphology control during the whole formation of Fe 3O 4 nanoparticles. In addition, the superconducting quantum interference device (SQUID) results indicate the products are superparamagnetic at room temperature, with blocking temperature ( TB) of 150 K and saturation magnetization of 37.1 emu/g.

Structural and magnetic properties of Ni0.8M0.2Fe2O4 (M = Cu, Co) nano-crystalline ferrites

NASA Astrophysics Data System (ADS)

Vijaya Babu, K.; Satyanarayana, G.; Sailaja, B.; Santosh Kumar, G. V.; Jalaiah, K.; Ravi, M.

2018-06-01

Nano-crystalline nickel ferrites are interesting materials due to their large physical and magnetic properties. In the present work, two kinds of spinel ferrites Ni0.8M0.2Fe2O4 (M = Cu, Co) are synthesized by using sol-gel auto-combustion method and the results are compared with NiFe2O4. The structural properties of synthesized ferrites are determined by using X-ray powder diffraction; scanning electron microscope and Fourier transform infrared spectroscopy. The cation distribution obtained from X-ray diffraction show that cobalt/copper occupies only tetrahedral site in spinel lattice. The lattice constant increases with the substitution of cobalt/copper. The structural parameters like bond lengths, tetrahedral and octahedral edges have been varied with the substitution. The microstructural study is carried out by using SEM technique and the average grain size is increased with nickel ferrite. The initial permeability (μi) is improving with the substitution. The observed g-value from ESR is approximately equal to standard value.

Hydrothermal synthesis and characterization of hydroxyapatite and fluorhydroxyapatite nano-size powders.

PubMed

Montazeri, Leila; Javadpour, Jafar; Shokrgozar, Mohammad Ali; Bonakdar, Shahin; Javadian, Sayfoddin

2010-08-01

Pure hydroxyapatite (HAp) and fluoride-containing apatite powders (FHAp) were synthesized using a hydrothermal method. The powders were assessed by x-ray diffraction (XRD), Fourier transform infrared (FTIR), scanning electron microscope (SEM) and F-selective electrode. X-ray diffraction results revealed the formation of single phase apatite structure for all the compositions synthesized in this work. However, the addition of a fluoride ion led to a systematic shift in the (3 0 0) peak of the XRD pattern as well as modifications in the FTIR spectra. It was found that the efficiency of fluoride ion incorporation decreased with the increase in the fluoride ion content. Fluorine incorporation efficiency was around 60% for most of the FHAp samples prepared in the current study. Smaller and less agglomerated particles were obtained by fluorine substitution. The bioactivity of the powder samples with different fluoride contents was compared by performing cell proliferation, alkaline phosphatase (ALP) and Alizarin red staining assays. Human osteoblast cells were used to assess the cellular responses to the powder samples in this study. Results demonstrated a strong dependence of different cell activities on the level of fluoridation.

Anti-contamination device for cryogenic soft X-ray diffraction microscopy

DOE PAGES

Huang, Xiaojing; Miao, Huijie; Nelson, Johanna; ...

2011-05-01

Cryogenic microscopy allows one to view frozen hydrated biological and soft matter specimens with good structural preservation and a high degree of stability against radiation damage. We describe a liquid nitrogen-cooled anti-contamination device for cryogenic X-ray diffraction microscopy. The anti-contaminator greatly reduces the buildup of ice layers on the specimen due to condensation of residual water vapor in the experimental vacuum chamber. We show by coherent X-ray diffraction measurements that this leads to fivefold reduction of background scattering, which is important for far-field X-ray diffraction microscopy of biological specimens.

Observation of electromigration in a Cu thin line by in situ coherent x-ray diffraction microscopy

NASA Astrophysics Data System (ADS)

Takahashi, Yukio; Nishino, Yoshinori; Furukawa, Hayato; Kubo, Hideto; Yamauchi, Kazuto; Ishikawa, Tetsuya; Matsubara, Eiichiro

2009-06-01

Electromigration (EM) in a 1-μm-thick Cu thin line was investigated by in situ coherent x-ray diffraction microscopy (CXDM). Characteristic x-ray speckle patterns due to both EM-induced voids and thermal deformation in the thin line were observed in the coherent x-ray diffraction patterns. Both parts of the voids and the deformation were successfully visualized in the images reconstructed from the diffraction patterns. This result not only represents the first demonstration of the visualization of structural changes in metallic materials by in situ CXDM but is also an important step toward studying the structural dynamics of nanomaterials using x-ray free-electron lasers in the near future.

Nanostructured zirconium phosphate as ion exchanger: Synthesis, size dependent property and analytical application in radiochemical separation.

PubMed

Chakraborty, Rajesh; Bhattacharaya, Koustava; Chattopadhyay, Pabitra

2014-02-01

Nanostructured zirconium phosphates (ZPs) of different sizes were synthesized using Tritron X-100 (polyethylene glycol-p-isooctylphenyl ether) surfactant. The materials were characterized by FTIR and powdered X-ray diffraction (XRD). The structural and morphological details of the material were established by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The SEM study was followed by energy dispersive spectroscopic analysis (EDS) for elemental analysis of the sample. The particle sizes were determined by dynamic light scattering (DLS) method. Ion exchange capacity of these nanomaterials towards different metal ions was measured and size-dependent ion exchange property of the materials was investigated thoroughly. The nanomaterial of the smallest size (ca. 21.04nm) was employed to separate carrier-free (137m)Ba from (137)Cs in column chromatographic technique using 1.0M HNO3 as eluting agent at pH=5. © 2013 Elsevier Ltd. All rights reserved.

Synthesis and microstructural studies of annealed Cu(2)O/Cu(x)S bilayer as transparent electrode material for photovoltaic and energy storage devices.

PubMed

Taleatu, B A; Arbab, E A A; Omotoso, E; Mola, G T

2014-10-01

Cu2 O thin film and a transparent bilayer have been fabricated by electrodeposition method. The growths were obtained in potentiostatic mode with gradual degradation of anodic current. X-ray diffraction (XRD) study showed that the bilayer is polycrystalline and it possesses mixture of different crystallite phases of copper oxides. Surface morphology of the films was investigated by scanning electron microscopy (SEM). The SEM images revealed that the films were uniformly distributed and the starting material (Cu2 O) had cubical structure. Grains agglomeration and crystallinity were enhanced by annealing. Optical studies indicated that all the samples have direct allowed transition. Energy band gap of the bilayer film was reduced by annealing treatment thus corroborating quantum confinement upshot. © 2014 The Authors Journal of Microscopy © 2014 Royal Microscopical Society.

Structural and magnetic characterization of Ti doped cobalt ferrite (CoFe2O4)

NASA Astrophysics Data System (ADS)

Pal, Jaswinder; Kumar, Sunil; Kaur, Randeep; Agrawal, P.; Singh, Mandeep; Singh, Anupinder

2018-05-01

Synthesis of Co1-xTixFe2O4 solid solutions for 0.1≤x≤0.4 using the solid-state-reaction rate has been done. The prepared samples were characterized by using XRD (X-ray diffraction) and SEM (Scanning Electron Microscopy). Magnetic studies have been done using Vibrating Sample Magnetometer (VSM). XRD confirmed that Cobalt Ferrite spinel cubic structure in all prepared samples. The lattice parameter `a' increases with increase in the concentration of Ti. SEM micrograph shows good grain growth in all samples. Magnetic Study reveals that the M-H curves of all the prepared samples taken at room temperature are very well saturated. The maximum value of remnant magnetization (Mr ˜13.9 emu/g) and saturation magnetization (Ms ˜74.4 emu/g) has been observed for x =0.2 sample. Coercivity does not show any regular variation with increase in the molar concentration of Ti in CoFe2O4 at A-site.

Improved magnetic and electrical properties of Cu doped Fe-Ni invar alloys synthesized by chemical reduction technique

NASA Astrophysics Data System (ADS)

Ahmad, Sajjad; Ziya, Amer Bashir; Ashiq, Muhammad Naeem; Ibrahim, Ather; Atiq, Shabbar; Ahmad, Naseeb; Shakeel, Muhammad; Khan, Muhammad Azhar

2016-12-01

Fe-Ni-Cu invar alloys of various compositions (Fe65Ni35-xCux, x=0, 0.2, 0.6, 1, 1.4 and 1.8) were synthesized via chemical reduction route. These alloys were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometry (VSM) techniques. The XRD analysis revealed the formation of face centered cubic (fcc) structure. The lattice parameter and the crystallite size of the investigated alloys were calculated and the line broadening indicated the nano-crystallites size of alloy powder. The particle size was estimated from SEM and it decreases by the incorporation of Cu and found to be in the range of 24-40 nm. The addition of Cu in these alloys appreciably enhances the saturation magnetization and it increases from 99 to 123 emu/g. Electrical conductivity has been improved with Cu addition. The thermal conductivity was calculated using the Wiedemann-Franz law.

Note: application of a pixel-array area detector to simultaneous single crystal X-ray diffraction and X-ray absorption spectroscopy measurements.

PubMed

Sun, Cheng-Jun; Zhang, Bangmin; Brewe, Dale L; Chen, Jing-Sheng; Chow, G M; Venkatesan, T; Heald, Steve M

2014-04-01

X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS) are two main x-ray techniques in synchrotron radiation facilities. In this Note, we present an experimental setup capable of performing simultaneous XRD and XAS measurements by the application of a pixel-array area detector. For XRD, the momentum transfer in specular diffraction was measured by scanning the X-ray energy with fixed incoming and outgoing x-ray angles. By selecting a small fixed region of the detector to collect the XRD signal, the rest of the area was available for collecting the x-ray fluorescence for XAS measurements. The simultaneous measurement of XRD and X-ray absorption near edge structure for Pr0.67Sr0.33MnO3 film was demonstrated as a proof of principle for future time-resolved pump-probe measurements. A static sample makes it easy to maintain an accurate overlap of the X-ray spot and laser pump beam.

X-Ray Diffraction Wafer Mapping Method for Rhombohedral Super-Hetero-Epitaxy

NASA Technical Reports Server (NTRS)

Park, Yoonjoon; Choi, Sang Hyouk; King, Glen C.; Elliott, James R.; Dimarcantonio, Albert L.

2010-01-01

A new X-ray diffraction (XRD) method is provided to acquire XY mapping of the distribution of single crystals, poly-crystals, and twin defects across an entire wafer of rhombohedral super-hetero-epitaxial semiconductor material. In one embodiment, the method is performed with a point or line X-ray source with an X-ray incidence angle approximating a normal angle close to 90 deg, and in which the beam mask is preferably replaced with a crossed slit. While the wafer moves in the X and Y direction, a narrowly defined X-ray source illuminates the sample and the diffracted X-ray beam is monitored by the detector at a predefined angle. Preferably, the untilted, asymmetric scans are of {440} peaks, for twin defect characterization.

Diffraction based method to reconstruct the spectrum of the Thomson scattering x-ray source

NASA Astrophysics Data System (ADS)

Chi, Zhijun; Yan, Lixin; Zhang, Zhen; Zhou, Zheng; Zheng, Lianmin; Wang, Dong; Tian, Qili; Wang, Wei; Nie, Zan; Zhang, Jie; Du, Yingchao; Hua, Jianfei; Shi, Jiaru; Pai, Chihao; Lu, Wei; Huang, Wenhui; Chen, Huaibi; Tang, Chuanxiang

2017-04-01

As Thomson scattering x-ray sources based on the collision of intense laser and relativistic electrons have drawn much attention in various scientific fields, there is an increasing demand for the effective methods to reconstruct the spectrum information of the ultra-short and high-intensity x-ray pulses. In this paper, a precise spectrum measurement method for the Thomson scattering x-ray sources was proposed with the diffraction of a Highly Oriented Pyrolytic Graphite (HOPG) crystal and was demonstrated at the Tsinghua Thomson scattering X-ray source. The x-ray pulse is diffracted by a 15 mm (L) ×15 mm (H)× 1 mm (D) HOPG crystal with 1° mosaic spread. By analyzing the diffraction pattern, both x-ray peak energies and energy spectral bandwidths at different polar angles can be reconstructed, which agree well with the theoretical value and simulation. The higher integral reflectivity of the HOPG crystal makes this method possible for single-shot measurement.

Diffraction based method to reconstruct the spectrum of the Thomson scattering x-ray source.

PubMed

Chi, Zhijun; Yan, Lixin; Zhang, Zhen; Zhou, Zheng; Zheng, Lianmin; Wang, Dong; Tian, Qili; Wang, Wei; Nie, Zan; Zhang, Jie; Du, Yingchao; Hua, Jianfei; Shi, Jiaru; Pai, Chihao; Lu, Wei; Huang, Wenhui; Chen, Huaibi; Tang, Chuanxiang

2017-04-01

As Thomson scattering x-ray sources based on the collision of intense laser and relativistic electrons have drawn much attention in various scientific fields, there is an increasing demand for the effective methods to reconstruct the spectrum information of the ultra-short and high-intensity x-ray pulses. In this paper, a precise spectrum measurement method for the Thomson scattering x-ray sources was proposed with the diffraction of a Highly Oriented Pyrolytic Graphite (HOPG) crystal and was demonstrated at the Tsinghua Thomson scattering X-ray source. The x-ray pulse is diffracted by a 15 mm (L) ×15 mm (H)× 1 mm (D) HOPG crystal with 1° mosaic spread. By analyzing the diffraction pattern, both x-ray peak energies and energy spectral bandwidths at different polar angles can be reconstructed, which agree well with the theoretical value and simulation. The higher integral reflectivity of the HOPG crystal makes this method possible for single-shot measurement.

Gas gun shock experiments with single-pulse x-ray phase contrast imaging and diffraction at the Advanced Photon Source

NASA Astrophysics Data System (ADS)

Luo, S. N.; Jensen, B. J.; Hooks, D. E.; Fezzaa, K.; Ramos, K. J.; Yeager, J. D.; Kwiatkowski, K.; Shimada, T.

2012-07-01

The highly transient nature of shock loading and pronounced microstructure effects on dynamic materials response call for in situ, temporally and spatially resolved, x-ray-based diagnostics. Third-generation synchrotron x-ray sources are advantageous for x-ray phase contrast imaging (PCI) and diffraction under dynamic loading, due to their high photon fluxes, high coherency, and high pulse repetition rates. The feasibility of bulk-scale gas gun shock experiments with dynamic x-ray PCI and diffraction measurements was investigated at the beamline 32ID-B of the Advanced Photon Source. The x-ray beam characteristics, experimental setup, x-ray diagnostics, and static and dynamic test results are described. We demonstrate ultrafast, multiframe, single-pulse PCI measurements with unprecedented temporal (<100 ps) and spatial (˜2 μm) resolutions for bulk-scale shock experiments, as well as single-pulse dynamic Laue diffraction. The results not only substantiate the potential of synchrotron-based experiments for addressing a variety of shock physics problems, but also allow us to identify the technical challenges related to image detection, x-ray source, and dynamic loading.

Potentiodynamic Polarization Studies and Surface Chemical Composition of Bismuth Titanate (Bi x Ti y O z ) Films Produced through Radiofrequency Magnetron Sputtering.

PubMed

Alfonso, José E; Olaya, Jhon J; Pinzón, Manuel J; Marco, José F

2013-10-08

The applications of Bismuth Titanate (Bi x Ti y O z ) materials have been focused on their electronic and optical properties, but with respect to the use of these compounds in applications like corrosion resistance, have been very few or nonexistent. For this reason, in the present investigation Bi x Ti y O z thin films were deposited using RF magnetron sputtering onto silicon wafers, stainless steel 316L, and titanium alloy (Ti₆Al₄V) substrates, in order to carry out a study of the corrosion behavior of this compound. The structural properties of the coatings were studied through X-ray diffraction (XRD), the morphology was determined using Scanning Electron Microscopy (SEM), the corrosion resistance behavior of the coated and uncoated substrates was evaluated via the Potentiodynamic Polarization technique, and surface chemical composition was evaluated through X-ray photoelectron spectroscopy (XPS). The XRD results indicated that the films were amorphous. The SEM micrographs showed that the deposited films were homogeneous, but in some cases there were cracks. The potentiodynamic polarization technique showed that the corrosion current in the coated substrates decreased by an order of two magnitudes with respect to the uncoated substrates, but in both cases the corrosion mechanism was pitting due to the pores in the film. The XPS analysis shows that the deposited films contain both Bi 3+ and Ti 4+ .

Microstructure, crystallography and diagenetic alteration in fossil ostrich eggshells from Upper Palaeolithic sites of Indian peninsular region.

PubMed

Jain, Sonal; Bajpai, Sunil; Kumar, Giriraj; Pruthi, Vikas

2016-05-01

Biominerals studies are of importance as they provide an understanding of natural evolutionary processes. In this study we have investigated the fossil ostrich eggshells using Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD) and Electron Backscatter Diffraction (EBSD). SEM studies demonstrated the ultrastructure of fossil eggshells and formation of calcified cuticular layer. The presence of calcified cuticle layer in eggshell is the basis for ancient DNA studies as it contains preserved biomolecules. EBSD accentuates the crystallographic structure of the ostrich eggshells with sub-micrometer resolution. It is a non-destructive tool for evaluating the extent of diagenesis in a biomineral. EBSD analysis revealed the presence of dolomite in the eggshells. This research resulted in the complete recognition of the structure of ostrich eggshells as well as the nature and extent of diagenesis in these eggshells which is vital for genetic and paleoenvironmental studies. Copyright © 2016 Elsevier Ltd. All rights reserved.

Facile synthesis of Co3O4 hexagonal plates by flux method

NASA Astrophysics Data System (ADS)

Han, Ji-Long; Meng, Qing-Fen; Gao, Sheng-Li

2018-01-01

Using a novel flux method, a hexagonal plate of Co3O4 was directly synthesized. In this method, CoCl2·6H2O, NaOH, and the cosolvent H3BO3 were heated to 750 °C for 2 h in a corundum crucible. The products were characterized with X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and high-resolution transmission electron microscope (HRTEM). Furthermore, XRD studies indicated that the product consisted of a cubic phase of Co3O4, and the phase existed in a completely crystalline form. Then, SEM results indicated that these hexagonal plates tiered up and they had diameters in the range of 2-10 μm. According to the results of SAED and HRTEM analyses, the interlayer spacing was about 0.24 nm, which corresponds to the interlayer distance of (3 1 1) crystal plane of cubic Co3O4.

X-ray and neutron diffraction studies of crystallinity in hydroxyapatite coatings.

PubMed

Girardin, E; Millet, P; Lodini, A

2000-02-01

To standardize industrial implant production and make comparisons between different experimental results, we have to be able to quantify the crystallinity of hydroxyapatite. Methods of measuring crystallinity ratio were developed for various HA samples before and after plasma spraying. The first series of methods uses X-ray diffraction. The advantage of these methods is that X-ray diffraction equipment is used widely in science and industry. In the second series, a neutron diffraction method is developed and the results recorded are similar to those obtained by the modified X-ray diffraction methods. The advantage of neutron diffraction is the ability to obtain measurements deep inside a component. It is a nondestructive method, owing to the very low absorption of neutrons in most materials. Copyright 2000 John Wiley & Sons, Inc.

X-ray Diffraction Gratings for Astrophysics

NASA Astrophysics Data System (ADS)

Paerels, Frits

2010-12-01

Over the past year, we have celebrated the tenth anniversary of the Chandra and XMM-Newton X-ray observatories. Both carry powerful, novel diffraction grating spectrometers, which have opened true X-ray spectroscopy for astrophysics. I will describe the design and operation of these instruments, as the background to some of the beautiful results they have produced. But these designs do not exhaust the versatility and essential simplicity of diffraction grating spectrometers, and I will discuss applications for the International X-ray Observatory IXO.

Amorphous boron gasket in diamond anvil cell research

NASA Astrophysics Data System (ADS)

Lin, Jung-Fu; Shu, Jinfu; Mao, Ho-kwang; Hemley, Russell J.; Shen, Guoyin

2003-11-01

Recent advances in high-pressure diamond anvil cell experiments include high-energy synchrotron x-ray techniques as well as new cell designs and gasketing procedures. The success of high-pressure experiments usually depends on a well-prepared sample, in which the gasket plays an important role. Various gasket materials such as diamond, beryllium, rhenium, and stainless steel have been used. Here we introduce amorphous boron as another gasket material in high-pressure diamond anvil cell experiments. We have applied the boron gasket for laser-heating x-ray diffraction, radial x-ray diffraction, nuclear resonant inelastic x-ray scattering, and inelastic x-ray scattering. The high shear strength of the amorphous boron maximizes the thickness of the sample chamber and increases the pressure homogeneity, improving the quality of high-pressure data. Use of amorphous boron avoids unwanted x-ray diffraction peaks and reduces the absorption of incident and x rays exiting the gasket material. The high quality of the diffraction patterns makes it possible to refine the cell parameters with powder x-ray diffraction data under high pressure and high temperature. The reactivity of boron prevents its use at high temperatures, however. When heated, boron may also react with the specimen to produce unwanted phases. The relatively porous boron starting material at ambient conditions also poses some challenges for sample preparation.

X-Ray Sum Frequency Diffraction for Direct Imaging of Ultrafast Electron Dynamics

NASA Astrophysics Data System (ADS)

Rouxel, Jérémy R.; Kowalewski, Markus; Bennett, Kochise; Mukamel, Shaul

2018-06-01

X-ray diffraction from molecules in the ground state produces an image of their charge density, and time-resolved x-ray diffraction can thus monitor the motion of the nuclei. However, the density change of excited valence electrons upon optical excitation can barely be monitored with regular diffraction techniques due to the overwhelming background contribution of the core electrons. We present a nonlinear x-ray technique made possible by novel free electron laser sources, which provides a spatial electron density image of valence electron excitations. The technique, sum frequency generation carried out with a visible pump and a broadband x-ray diffraction pulse, yields snapshots of the transition charge densities, which represent the electron density variations upon optical excitation. The technique is illustrated by ab initio simulations of transition charge density imaging for the optically induced electronic dynamics in a donor or acceptor substituted stilbene.

Fine Structure in Multi-Phase Zr8Ni21-Zr7Ni10-Zr2Ni7 Alloy Revealed by Transmission Electron Microscope

PubMed Central

Shen, Haoting; Bendersky, Leonid A.; Young, Kwo; Nei, Jean

2015-01-01

The microstructure of an annealed alloy with a Zr8Ni21 composition was studied by both scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The presence of three phases, Zr8Ni21, Zr2Ni7, and Zr7Ni10, was confirmed by SEM/X-ray energy dispersive spectroscopy compositional mapping and TEM electron diffraction. Distribution of the phases and their morphology can be linked to a multi-phase structure formed by a sequence of reactions: (1) L → Zr2Ni7 + L’; (2) peritectic Zr2Ni7 + L’ → Zr2Ni7 + Zr8Ni21 + L”; (3) eutectic L” → Zr8Ni21 + Zr7Ni10. The effect of annealing at 960 °C, which was intended to convert a cast structure into a single-phase Zr8Ni21 structure, was only moderate and the resulting alloy was still multi-phased. TEM and crystallographic analysis of the Zr2Ni7 phase show a high density of planar (001) defects that were explained as low-energy boundaries between rotational variants and stacking faults. The crystallographic features arise from the pseudo-hexagonal structure of Zr2Ni7. This highly defective Zr2Ni7 phase was identified as the source of the broad X-ray diffraction peaks at around 38.4° and 44.6° when a Cu-K was used as the radiation source. PMID:28793460

Characterization of ZnAl cast alloys with Na addition

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

Gancarz, Tomasz, E-mail: t.gancarz@imim.pl; Cempura, Grzegorz; Skuza, Wojciech

2016-01-15

This study was aimed at evaluating the microstructural change and thermal, electrical and mechanical properties with the addition of Na to eutectic ZnAl alloys. Solders based on eutectic ZnAl containing 0.2 to 3.0 (wt.%) of Na were developed for high temperature solder. Differential scanning calorimetry (DSC) measurements were performed to determine the melting temperatures of the alloys. Thermal linear expansion and electrical resistivity measurements were performed over − 50 °C to 300 °C and 30 °C to 300 °C temperature ranges, respectively. The microstructure of the specimens was analyzed using scanning (SEM) and transmission electron microscopy (TEM) techniques. Chemical microanalysismore » was performed by energy-dispersive X-ray spectroscopy (EDS) on SEM and TEM. The precipitates of NaZn{sub 13} were confirmed by X-ray diffraction (XRD) measurements and selected area electron diffraction (SAED) techniques. The addition of Na to eutectic ZnAl alloy increased the electrical resistivity and reduced the coefficient of thermal expansion; however, the melting point did not change. The mechanical properties, strain and microhardness increased with Na content in alloys. - Highlights: • High temperature soldering materials of ZnAl with Na were designed and characterized. • Precipitates of NaZn{sub 13}were observed and confirmed using TEM and XRD. • Addition of Na to eutectic ZnAl cussed increased mechanical properties. • NaZn{sub 13} caused increased electrical resistivity and microhardness, and reduced the CTE.« less

Spectroscopic investigations on Pr³+ and Nd³+ doped strontium-lithium-bismuth borate glasses.

PubMed

Rajesh, D; Balakrishna, A; Seshadri, M; Ratnakaram, Y C

2012-11-01

Spectroscopic investigations on different concentrations (0.1, 0.5, 1.0, 1.5 and 2.0mol%) of Pr(3+) and Nd(3+) doped strontium lithium bismuth borate glasses have been done. X-ray diffraction, SEM with EDS, absorption and luminescence spectra were recorded for all the glass matrices and analyzed. X-ray diffraction profiles and SEM images conformed amorphous nature of investigated glass samples. EDS spectra of host glass and Pr(3+)doped glass matrices gave information about the chemical composition of glass samples. From the absorption spectra of Pr(3+) and Nd(3+) ions, Judd-Ofelt (J-O) intensity parameters (Ω(λ),λ=2, 4 and 6) have been calculated and compared with other glass matrices. The emission characteristics such as radiative lifetimes (τ(R)), measured and calculated branching ratios (β) and stimulated emission cross-sections (σ(P)) have been obtained for the observed emission transitions of Pr(3+) and Nd(3+) ions in the above glass matrix for all the concentrations. From the emission spectra of Pr(3+) and Nd(3+) doped glass matrices, the effect of concentration on the quenching of intensity of (1)D(2)→(3)H(4) transition of Pr(3+) ion and (4)F(3/2)→(4)I(9/2), (4)I(11/2) and (4)I(13/2) transitions of Nd(3+) have been studied and discussed. Copyright © 2012 Elsevier B.V. All rights reserved.

Single crystal X-ray structure of the artists' pigment zinc yellow

NASA Astrophysics Data System (ADS)

Simonsen, Kim Pilkjær; Christiansen, Marie Bitsch; Vinum, Morten Gotthold; Sanyova, Jana; Bendix, Jesper

2017-08-01

The artists' pigment zinc yellow is in general described as a complex potassium zinc chromate with the empirical formula 4ZnCrO4·K2O·3H2O. Even though the pigment has been in use since the second half of the 19th century also in large-scale industrial applications, the exact structure had hitherto been unknown. In this work, zinc yellow was synthesised by precipitation from an aqueous solution of zinc nitrate and potassium chromate under both neutral and basic conditions, and the products were compared with the pigment used in industrial paints. Analyses by Raman microscopy (MRS), scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS), attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR), and powder X-ray diffraction (PXRD), showed that the synthesised products and the industrial pigment were identical. Single-crystal X-ray crystallography determined the structure of zinc yellow as KZn2(CrO4)2(H2O)(OH) or as KZn2(CrO4)2(H3O2) emphasizing the μ-H3O2- moiety. Notably, the zinc yellow is isostructural to the recently structurally characterized cadmium analog and both belong to the natrochalcite structure type.

Synthesis and surface characterization of alumina-silica-zirconia nanocomposite ceramic fibres on aluminium at room temperature

NASA Astrophysics Data System (ADS)

Mubarak Ali, M.; Raj, V.

2010-04-01

Alumina-silica-zirconia nanocomposite (ASZNC) ceramic fibres were synthesized by conventional anodization route. Scanning Electron Microscopy (SEM), Atomic Force microscopy (AFM), X-Ray Diffraction (XRD) and Energy Dispersive X-Ray spectroscopy (EDAX) were used to characterize the morphology and crystalloid structure of ASZNC fibres. Current density (DC) is one of the important parameters to get the alumina-silica-zirconia nanocomposite (ASZNC) ceramic fibres by this route. Annealing of the films exhibited a drastic change in the properties due to improved crystallinity. The root mean square roughness of the sample observed from atomic force microscopic analysis is about 71.5 nm which is comparable to the average grain size of the coatings which is about 72 nm obtained from X-Ray diffraction. The results indicate that, the ASZNC fibres are arranged well in the nanostructure. The thickness of the coating increased with the anodizing time, but the coatings turned rougher and more porous. At the initial stage the growth of ceramic coating increases inwards to the metal substrate and outwards to the coating surface simultaneously. Subsequently, it mainly grows towards the metal substrate and the density of the ceramic coating increases gradually, which results in the decrease of the total thickness as anodizing time increases. This new approach of preparing ASZNC ceramic fibres may be important in applications ranging from gas sensors to various engineering materials.

Synthesis of novel CeO2-BiVO4/FAC composites with enhanced visible-light photocatalytic properties.

PubMed

Zhang, Jin; Wang, Bing; Li, Chuang; Cui, Hao; Zhai, Jianping; Li, Qin

2014-09-01

To utilize visible light more effectively in photocatalytic reactions, a fly ash cenosphere (FAC)-supported CeO2-BiVO4 (CeO2-BiVO4/FAC) composite photocatalyst was prepared by modified metalorganic decomposition and impregnation methods. The physical and photophysical properties of the composite have been characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and energy dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS), and UV-Visible diffuse reflectance spectra. The XRD patterns exhibited characteristic diffraction peaks of both BiVO4 and CeO2 crystalline phases. The XPS results showed that Ce was present as both Ce(4+) and Ce(3+) oxidation states in CeO2 and dispersed on the surface of BiVO4 to constitute a p-n heterojunction composite. The absorption threshold of the CeO2-BiVO4/FAC composite shifted to a longer wavelength in the UV-Vis absorption spectrum compared to the pure CeO2 and pure BiVO4. The composites exhibited enhanced photocatalytic activity for Methylene Blue (MB) degradation under visible light irradiation. It was found that the 7.5wt.% CeO2-BiVO4/FAC composite showed the highest photocatalytic activity for MB dye wastewater treatment. Copyright © 2014. Published by Elsevier B.V.

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

Mishra, Ashutosh; Dwivedi, Jagrati, E-mail: hemu.dwi@gmail.com; Shukla, Kritika

Five Chromium (III) complexes have been prepared using Schiff base ligands which derived from benzoin and five different amino acids (H{sub 2}N-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{sup −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 designedmore » for studying of the solid objects, using JEOL JSM 5600 instrument.« less

Influence of Te and Se doping on ZnO films growth by SILAR method

NASA Astrophysics Data System (ADS)

Güney, Harun; Duman, Ćaǧlar

2016-04-01

The AIP Successive ionic layer adsorption and reaction (SILAR) is an economic and simple method to growth thin films. In this study, SILAR method is used to growth Selenium (Se) and Tellurium (Te) doped zinc oxide (ZnO) thin films with different doping rates. For characterization of the films X-ray diffraction (XRD), absorbance and scanning electron microscopy (SEM) are used. XRD results are showed well-defined strongly (002) oriented crystal structure for all samples. Also, absorbance measurements show, Te and Se concentration are proportional and inversely proportional with band gap energy, respectively. SEM measurements show that the surface morphology and thickness of the material varied with Se and/or Te and varying concentrations.

Morphology-controllable of Sn doped ZnO nanorods prepared by spray pyrolysis for transparent electrode application

NASA Astrophysics Data System (ADS)

Hameed, M. Shahul; Princice, J. Joseph; Babu, N. Ramesh; Zahirullah, S. Syed; Deshmukh, Sampat G.; Arunachalam, A.

2018-05-01

Transparent conductive Sn doped ZnO nanorods have been deposited at various doping level by spray pyrolysis technique on glass substrate. The structural, surface morphological and optical properties of these films have been investigated with the help of X-ray diffraction (XRD), scanning electron microscope (SEM), atomic force microscope (AFM) and UV-Vis spectrophotometer respectively. XRD patterns revealed a successful high quality growth of single crystal ZnO nanorods with hexagonal wurtzite structure having (002) preferred orientation. The scanning electron microscope (SEM) image of the prepared films exposed the uniform distribution of Sn doped ZnO nanorod shaped grains. All these films were highly transparent in the visible region with average transmittance of 90%.

Influence of Te and Se doping on ZnO films growth by SILAR method

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

Güney, Harun, E-mail: harunguney25@hotmail.com; Duman, Çağlar, E-mail: caglarduman@erzurum.edu.tr

2016-04-18

The AIP Successive ionic layer adsorption and reaction (SILAR) is an economic and simple method to growth thin films. In this study, SILAR method is used to growth Selenium (Se) and Tellurium (Te) doped zinc oxide (ZnO) thin films with different doping rates. For characterization of the films X-ray diffraction (XRD), absorbance and scanning electron microscopy (SEM) are used. XRD results are showed well-defined strongly (002) oriented crystal structure for all samples. Also, absorbance measurements show, Te and Se concentration are proportional and inversely proportional with band gap energy, respectively. SEM measurements show that the surface morphology and thickness ofmore » the material varied with Se and/or Te and varying concentrations.« less

A facile synthesis of metal nanoparticle - graphene composites for better absorption of solar radiation

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

Sharma, Bindu; Mulla, Rafiq; Rabinal, M. K., E-mail: mkrabinal@yahoo.com

2015-06-24

Herein, a facile chemical approach has been adopted to prepare silver nanoparticles (AgNPs)- graphene (G) composite to study photothermal effect. Sodium borohydride (SBH), a strong reducing agent has been selected for this work. Effect of SBH concentrations on optical behavior of AgNPs-G composite was also investigated. Resultant materials were characterized by various techniques including X-ray diffraction (XRD), fourier transform infrared spectroscopy (FTIR), optical absorption, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). SEM micrographs confirm wrapping of AgNPs into graphene whereas XRD analysis reveals their particle size variation between 47 nm to 69 nm. Optical studies throw a light on theirmore » strong absorption behavior towards solar radiation.« less

The PM2.5 capture of poly (lactic acid)/nano MOFs eletrospinning membrane with hydrophilic surface

NASA Astrophysics Data System (ADS)

Wang, Yating; Dai, Xiu; Li, Xu; Wang, Xinlong

2018-03-01

In this article, metal organic frameworks (MOFs) material is introduced in the poly (lactic acid) (PLA) by electrospinning to fabricate the nanocomposite membrane. The acrylic acid (AA) is grafted onto the membrane under UV light. The prepared membrane is studied by scanning electron microscopy (SEM), x-ray diffraction (XRD), thermogravimetry (TG), contact angle test and tensile strength test. The SEM image and XRD indicate that nano MOFs particles adhere to the membrane. Contact angle test shows that grafting AA on the composite fiber membrane improves its hydrophilicity effectively. TG analyses show that the particulate matter (PM) capture capacity of PLA membrane with 2 wt% ZIF-8 content is 22%, which rises to 37% after grafting.

Single step synthesis of nanostructured boron nitride for boron neutron capture therapy

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

Singh, Bikramjeet; Singh, Paviter; Kumar, Akshay, E-mail: akshaykumar.tiet@gmail.com

2015-05-15

Nanostructured Boron Nitride (BN) has been successfully synthesized by carbo-thermic reduction of Boric Acid (H{sub 3}BO{sub 3}). This method is a relatively low temperature synthesis route and it can be used for large scale production of nanostructured BN. The synthesized nanoparticles have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and differential thermal analyzer (DTA). XRD analysis confirmed the formation of single phase nanostructured Boron Nitride. SEM analysis showed that the particles are spherical in shape. DTA analysis showed that the phase is stable upto 900 °C and the material can be used for high temperature applications asmore » well boron neutron capture therapy (BNCT)« less

Preparation of a novel breviscapine-loaded halloysite nanotubes complex for controlled release of breviscapine

NASA Astrophysics Data System (ADS)

Gao, Min; Lu, Liqian; Wang, Xiaoyue; Lin, Houke; Zhou, Qingsong

2017-11-01

For sustain the release rate and prolong half-life of breviscapine in vivo, the breviscapine-loaded halloysite nanotubes complex was prepared. The breviscapine was encapsulated into halloysite nanotubes (HNTs) using a vacuum process. The complex were investigated by scanning electron microscopy (SEM), differential scanning calorimetry (DSC), transmission electron microscope (TEM), X-ray diffraction (XRD) and fourier transform infrared spectroscopy(FT-IR). The formation of breviscapine-loaded HNTs complex was proved by the test results of SEM, DSC, TEM and IR analysise. The results confirmed that breviscapine was successfully loaded in the halloysite nanotubes. Additionally, the in vitro drug release of breviscapine from breviscapine-loaded HNTs complex was investigated, the result indicated this complex has apparent sustained-release effect.

Development of an adaptable coherent x-ray diffraction microscope with the emphasis on imaging hydrated specimens.

PubMed

Nam, Daewoong; Park, Jaehyun; Gallagher-Jones, Marcus; Shimada, Hiroki; Kim, Sangsoo; Kim, Sunam; Kohmura, Yoshiki; Ishikawa, Tetsuya; Song, Changyong

2013-11-01

This paper describes the development of a versatile coherent x-ray diffraction microscope capable of imaging biological specimens in solution. The microscope is a flexible platform accommodating various conditions, from low vacuum (10(-2) Pa) to helium gas filled ambient pressure. This flexibility greatly expands the application area, from in situ materials science to biology systems in their native state, by significantly relaxing restrictions to the sample environment. The coherent diffraction microscope has been used successfully to image a yeast cell immersed in buffer solution. We believe that the design of this coherent diffraction microscope can be directly adapted to various platforms such as table top soft x-ray laser, synchrotron x-ray sources, and x-ray free electron laser with minor relevant adjustments.

Development of an adaptable coherent x-ray diffraction microscope with the emphasis on imaging hydrated specimens

NASA Astrophysics Data System (ADS)

Nam, Daewoong; Park, Jaehyun; Gallagher-Jones, Marcus; Shimada, Hiroki; Kim, Sangsoo; Kim, Sunam; Kohmura, Yoshiki; Ishikawa, Tetsuya; Song, Changyong

2013-11-01

This paper describes the development of a versatile coherent x-ray diffraction microscope capable of imaging biological specimens in solution. The microscope is a flexible platform accommodating various conditions, from low vacuum (10-2 Pa) to helium gas filled ambient pressure. This flexibility greatly expands the application area, from in situ materials science to biology systems in their native state, by significantly relaxing restrictions to the sample environment. The coherent diffraction microscope has been used successfully to image a yeast cell immersed in buffer solution. We believe that the design of this coherent diffraction microscope can be directly adapted to various platforms such as table top soft x-ray laser, synchrotron x-ray sources, and x-ray free electron laser with minor relevant adjustments.

Thin Film Research. Volume 1

DTIC Science & Technology

1985-05-30

Order (FECO) ......... 23 3. X -Ray Diffraction ............................... 26 4. Transmission Electron Microscopy (TEM) ............... 26 5...remained amorphous after bombardment, as evidenced by X - ray diffraction, and showed no other changes. 0 (2) For Sb203, the crystallite size was reduced...main effect on MgF2 was the reduction in crystallite size. The films were too thir. for meaningful x - ray diffraction analysis. Durability and

X-Ray Diffraction and the Discovery of the Structure of DNA

ERIC Educational Resources Information Center

Crouse, David T.

2007-01-01

A method is described for teaching the analysis of X-ray diffraction of DNA through a series of steps utilizing the original methods used by James Watson, Francis Crick, Maurice Wilkins and Rosalind Franklin. The X-ray diffraction pattern led to the conclusion of the basic helical structure of DNA and its dimensions while basic chemical principles…

High Resolution X-Ray Diffraction of Macromolecules with Synchrotron Radiation

NASA Technical Reports Server (NTRS)

Stojanoff, Vivian; Boggon, Titus; Helliwell, John R.; Judge, Russell; Olczak, Alex; Snell, Edward H.; Siddons, D. Peter; Rose, M. Franklin (Technical Monitor)

2000-01-01

We recently combined synchrotron-based monochromatic X-ray diffraction topography methods with triple axis diffractometry and rocking curve measurements: high resolution X-ray diffraction imaging techniques, to better understand the quality of protein crystals. We discuss these methods in the light of results obtained on crystals grown under different conditions. These non destructive techniques are powerful tools in the characterization of the protein crystals and ultimately will allow to improve, develop, and understand protein crystal growth. High resolution X-ray diffraction imaging methods will be discussed in detail in light of recent results obtained on Hen Egg White Lysozyme crystals and other proteins.

Hard X-ray polarizer to enable simultaneous three-dimensional nanoscale imaging of magnetic structure and lattice strain

DOE PAGES

Logan, Jonathan; Harder, Ross; Li, Luxi; ...

2016-01-01

Recent progress in the development of dichroic Bragg coherent diffractive imaging, a new technique for simultaneous three-dimensional imaging of strain and magnetization at the nanoscale, is reported. This progress includes the installation of a diamond X-ray phase retarder at beamline 34-ID-C of the Advanced Photon Source. Here, the performance of the phase retarder for tuning X-ray polarization is demonstrated with temperature-dependent X-ray magnetic circular dichroism measurements on a gadolinium foil in transmission and on a Gd 5Si 2Ge 2crystal in diffraction geometry with a partially coherent, focused X-ray beam. Feasibility tests for dichroic Bragg coherent diffractive imaging are presented. Thesemore » tests include (1) using conventional Bragg coherent diffractive imaging to determine whether the phase retarder introduces aberrations using a nonmagnetic gold nanocrystal as a control sample, and (2) collecting coherent diffraction patterns of a magnetic Gd 5Si 2Ge 2nanocrystal with left- and right-circularly polarized X-rays. Future applications of dichroic Bragg coherent diffractive imaging for the correlation of strain and lattice defects with magnetic ordering and inhomogeneities are considered.« less

Three Dimensional Variable-Wavelength X-Ray Bragg Coherent Diffraction Imaging

DOE PAGES

Cha, W.; Ulvestad, A.; Allain, M.; ...

2016-11-23

Here, we present and demonstrate a formalism by which three-dimensional (3D) Bragg x-ray coherent diffraction imaging (BCDI) can be implemented without moving the sample by scanning the energy of the incident x-ray beam. This capability is made possible by introducing a 3D Fourier transform that accounts for x-ray wavelength variability. We also demonstrate the approach by inverting coherent Bragg diffraction patterns from a gold nanocrystal measured with an x-ray energy scan. Furthermore, variable-wavelength BCDI will expand the breadth of feasible in situ 3D strain imaging experiments towards more diverse materials environments, especially where sample manipulation is difficult.

Synchrotron X-Ray Diffraction Analysis of Meteorites in Thin Section: Preliminary Results

NASA Technical Reports Server (NTRS)

Treiman, A. H.; Lanzirotti, A.; Xirouchakis, D.

2004-01-01

X-ray diffraction is the pre-eminent technique for mineral identification and structure determination, but is difficult to apply to grains in thin section, the standard meteorite preparation. Bright focused X-ray beams from synchrotrons have been used extensively in mineralogy and have been applied to extraterrestrial particles. The intensity and small spot size achievable in synchrotron X-ray beams makes them useful for study of materials in thin sections. Here, we describe Synchrotron X-ray Diffraction (SXRD) in thin section as done at the National Synchrotron Light Source, and cite examples of its value for studies of meteorites in thin section.

Three Dimensional Variable-Wavelength X-Ray Bragg Coherent Diffraction Imaging

NASA Astrophysics Data System (ADS)

Cha, W.; Ulvestad, A.; Allain, M.; Chamard, V.; Harder, R.; Leake, S. J.; Maser, J.; Fuoss, P. H.; Hruszkewycz, S. O.

2016-11-01

We present and demonstrate a formalism by which three-dimensional (3D) Bragg x-ray coherent diffraction imaging (BCDI) can be implemented without moving the sample by scanning the energy of the incident x-ray beam. This capability is made possible by introducing a 3D Fourier transform that accounts for x-ray wavelength variability. We demonstrate the approach by inverting coherent Bragg diffraction patterns from a gold nanocrystal measured with an x-ray energy scan. Variable-wavelength BCDI will expand the breadth of feasible in situ 3D strain imaging experiments towards more diverse materials environments, especially where sample manipulation is difficult.

Three Dimensional Variable-Wavelength X-Ray Bragg Coherent Diffraction Imaging.

PubMed

Cha, W; Ulvestad, A; Allain, M; Chamard, V; Harder, R; Leake, S J; Maser, J; Fuoss, P H; Hruszkewycz, S O

2016-11-25

We present and demonstrate a formalism by which three-dimensional (3D) Bragg x-ray coherent diffraction imaging (BCDI) can be implemented without moving the sample by scanning the energy of the incident x-ray beam. This capability is made possible by introducing a 3D Fourier transform that accounts for x-ray wavelength variability. We demonstrate the approach by inverting coherent Bragg diffraction patterns from a gold nanocrystal measured with an x-ray energy scan. Variable-wavelength BCDI will expand the breadth of feasible in situ 3D strain imaging experiments towards more diverse materials environments, especially where sample manipulation is difficult.

In-situ X-ray diffraction system using sources and detectors at fixed angular positions

DOEpatents

Gibson, David M [Voorheesville, NY; Gibson, Walter M [Voorheesville, NY; Huang, Huapeng [Latham, NY

2007-06-26

An x-ray diffraction technique for measuring a known characteristic of a sample of a material in an in-situ state. The technique includes using an x-ray source for emitting substantially divergent x-ray radiation--with a collimating optic disposed with respect to the fixed source for producing a substantially parallel beam of x-ray radiation by receiving and redirecting the divergent paths of the divergent x-ray radiation. A first x-ray detector collects radiation diffracted from the sample; wherein the source and detector are fixed, during operation thereof, in position relative to each other and in at least one dimension relative to the sample according to a-priori knowledge about the known characteristic of the sample. A second x-ray detector may be fixed relative to the first x-ray detector according to the a-priori knowledge about the known characteristic of the sample, especially in a phase monitoring embodiment of the present invention.

Structural and morphological study of Fe-doped Bi-based superconductor

NASA Astrophysics Data System (ADS)

Singh, Yadunath; Kumar, Rohitash

2018-05-01

In the present work, we report the study of iron-doped Bi-based superconductor sample with stoichiometric composition of Bi2Sr2Can-1(Cu1-x Fex)3O2n+4 where n=3 and x = 0.7. This sample was prepared by grinding the precursor oxides in the Ball mill for 6 hours continuous at the rate of 400 rpm for a proper mixing and to obtain the required grain size. Then the solid-state reaction method was used to prepare the sample. X-ray diffraction (XRD) and scanning electron microscopy (SEM) in combination with energy dispersive X-ray fluorescence analysis (EDX) were performed for determination of the crystal structure, surface morphology and trace the material elements of samples, respectively. The surface microscopy data were collected over a selected area of the surface of the material and a two-dimensional image generated that displays spatial variations in properties including chemical characterization and orientation of materials.

Eco-friendly preparation of large-sized graphene via short-circuit discharge of lithium primary battery.

PubMed

Kang, Shaohong; Yu, Tao; Liu, Tingting; Guan, Shiyou

2018-02-15

We proposed a large-sized graphene preparation method by short-circuit discharge of the lithium-graphite primary battery for the first time. LiC x is obtained through lithium ions intercalation into graphite cathode in the above primary battery. Graphene was acquired by chemical reaction between LiC x and stripper agents with dispersion under sonication conditions. The gained graphene is characterized by Raman spectrum, X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), Atomic force microscope (AFM) and Scanning electron microscopy (SEM). The results indicate that the as-prepared graphene has a large size and few defects, and it is monolayer or less than three layers. The quality of graphene is significant improved compared to the reported electrochemical methods. The yield of graphene can reach 8.76% when the ratio of the H 2 O and NMP is 3:7. This method provides a potential solution for the recycling of waste lithium ion batteries. Copyright © 2017 Elsevier Inc. All rights reserved.

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.

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.

Magnetic cellulose/Ag as a novel eco-friendly nanobiocomposite to catalyze synthesis of chromene-linked nicotinonitriles.

PubMed

Maleki, Ali; Movahed, Hamed; Ravaghi, Parisa

2017-01-20

In this work, design, preparation and performance of magnetic cellulose/Ag nanobiocomposite as a recyclable and highly efficient heterogeneous nanocatalyst is described. Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD) pattern, vibrating sample magnetometer (VSM) curve, field-emission scanning electron microscopy (FE-SEM) image, energy dispersive X-ray (EDX) analysis and thermogravimetric analysis/differential thermal analysis (TGA/DTA) were used for the characterization. Then, its activity was investigated in the synthesis of 2-amino-6-(2-oxo-2H-chromen-3-yl)-4-phenylnicotinonitrile derivatives. The main advantages of the reaction are high yields and short reaction times. The remarkable magnetic property of the nanobiocomposite catalyst provides easy separation from the reaction mixture by an external magnet without considerable loss of its catalytic activity. Copyright © 2016 Elsevier Ltd. All rights reserved.

Electrospinning β-SiC fibers from SiC nanoparticles dispersed in various polymer solutions as the electrospinning agents

NASA Astrophysics Data System (ADS)

Fuad, A.; Fatriani, N.; Yogihati, C. I.; Taufiq, A.; Latifah, E.

2018-04-01

Silicon carbide (SiC) fibers were synthesized by electrospinning method from SiC nanoparticles dispersed in polymer solutions, i.e., polyethylene glycol (PEG) and polyvinyl alcohol (PVA). The SiC nanoparticle used in this research was synthesized from sucrose and natural silica via a sonochemical method. The natural silica was extracted from local pyrophyllite by a sol-gel method. The characterization was performed via x-ray fluorescence (XRF), X-ray diffraction (XRD), scanning electron microscopy (SEM). The XRD characterization results showed that the sample possessed a β-SiC phase and formed a cubic-structured crystal with a lattice parameter of a = b = c = 4.3448 Å. The use of PEG and PVA in the electrospinning process resulted in fractal and fiber structured SiC, respectively.

Green synthesis and spectral characterization of silver nanoparticles from Lakshmi tulasi (Ocimum sanctum) leaf extract

NASA Astrophysics Data System (ADS)

Subba Rao, Y.; Kotakadi, Venkata S.; Prasad, T. N. V. K. V.; Reddy, A. V.; Sai Gopal, D. V. R.

2013-02-01

A simple method for the green synthesis of silver nanoparticles (AgNPs) using aqueous extract of Lakshmi tulasi (Ocimum sanctum) leaf as a reducing and stabilizing agent. AgNPs were rapidly synthesized using aqueous extract of tulasi leaf with AgNO3 solution within 15 min. The green synthesized AgNPs were characterized using physic-chemical techniques viz., UV-Vis, X-ray diffraction (XRD), scanning electron microscope (SEM) coupled with X-ray energy dispersive spectroscopy (EDX) and Fourier transform-infrared spectroscopy (FT-IR). Characterization data reveals that the particles were crystalline in nature and triangle shaped with an average size of 42 nm. The zeta potential of AgNPs were found to be -55.0 mV. This large negative zeta potential value indicates repulsion among AgNPs and their dispersion stability.

Low-temperature synthesis and structural properties of ferroelectric K 3WO 3F 3 elpasolite

NASA Astrophysics Data System (ADS)

Atuchin, V. V.; Gavrilova, T. A.; Kesler, V. G.; Molokeev, M. S.; Aleksandrov, K. S.

2010-06-01

Low-temperature ferroelectric G2 polymorph of K 3WO 3F 3 has been prepared by chemical synthesis. Structural and chemical properties of the final product have been evaluated with X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). Structure parameters of G2-K 3WO 3F 3 are refined by the Rietveld method from XRD data measured at room temperature (space group Cm, Z = 2, a = 8.7350(3) Å, b = 8.6808(5) Å, c = 6.1581(3) Å, β = 135.124(3) Å, V = 329.46(3) Å 3; RB = 2.47%). Partial ordering of oxygen and fluorine atoms has been found over anion positions. Mechanism of ferroelectric phase transition in A 2BMO 3F 3 oxyfluorides is discussed.

Microscale Interface Synthesis of Ni-B Amorphous Nanoparticles from NiSO4 by Sodium Borohydride Reduction in Microreactor

NASA Astrophysics Data System (ADS)

Xu, Lei; Peng, Jinhui; Meng, Binfang; Li, Wei; Liu, Bingguo; Luo, Huilong

2016-09-01

Amorphous nanoparticles have attracted a large amount of interest due to their superior catalytic activity and unique selectivity. The Ni-B amorphous nanoparticles were synthesized from aqueous reduction of NiSO4 by sodium borohydride in microscale interface at room temperature. The size, morphology, elemental compositions, and the chemical composition on the surface of Ni-B amorphous nanoparticles were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). All the results showed that the synthesized particles are Ni-B amorphous nanoparticles with uniform in size distribution and having good dispersion. The mean particle diameter of Ni-B amorphous nanoparticles was around 9 nm. The present work provides an alternative synthesis route for the Ni-B amorphous nanoparticles.

Microfluidic reactor synthesis and photocatalytic behavior of Cu@Cu2O nanocomposite

NASA Astrophysics Data System (ADS)

Xu, Lei; Srinivasakannan, C.; Peng, Jinhui; Yan, Mi; Zhang, Di; Zhang, Libo

2015-03-01

The Cu@Cu2O nanocomposites were synthesized by solution-phase synthesis of Cu nanoparticles in microfluidic reactor at room temperature, followed by controlling the oxidation process. The size, morphology, elemental compositions, and the chemical composition on the surface of Cu@Cu2O nanocomposite were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). Experimental results demonstrated that the surface of the Cu nanoparticles was oxidized to Cu2O which serves as the shell of nanoparticle. The amount of Cu2O can be controlled by varying the drying temperature. Additionally the binary Cu@Cu2O nanocomposite along with H2O2 exhibited its potential as an excellent photocatalyst for degradation of methylene blue (MB) under UV irradiation.

Nanostructure CdS/ZnO heterojunction configuration for photocatalytic degradation of Methylene blue

NASA Astrophysics Data System (ADS)

Velanganni, S.; Pravinraj, S.; Immanuel, P.; Thiruneelakandan, R.

2018-04-01

In the present manuscript, thin films of Zinc Oxide (ZnO) have been deposited on a FTO substrate using a simple successive ionic layer adsorption and reaction (SILAR) and chemical bath deposition (CBD) method. Cadmium Sulphide (CdS) nanoparticles are sensitized over ZnO thin films using SILAR method. The synthesized nanostructured CdS/ZnO heterojunction thin films was characterized by X-ray diffraction (XRD), Scanning electron microscopy (SEM), High resolution transmission electron microscopy (HR-TEM), X-ray photoelectron spectroscopy (XPS), UV-Vis spectroscopy and Raman spectroscopy techniques. The band gap of CdS nanoparticles over ZnO nanostructure was found to be about 3.20 eV. The photocatalytic activities of the deposited CdS/ZnO thin films were evaluated by the degradation of methylene blue (MB) in an aqueous solution under sun light irradiation.

Photocatalytic Degradation Effect of μ-Dielectric Barrier Discharge Plasma Treated Titanium Dioxide Nanoparticles on Environmental Contaminant.

PubMed

Seo, Hyeon Jin; Hwang, Ki-Hwan; Na, Young Hoon; Boo, Jin-Hyo

2018-09-01

This study focused on the photocatalytic degradation effect of the μ-dielectric barrier discharge (μ-DBD) plasma treated titanium dioxide (TiO2) nanoparticles on environmental contaminant such as formaldehyde. TiO2 nanoparticles were treated by a μ-DBD plasma source with nitrogen gas. We analyzed the degradation of formaldehyde with the plasma treated TiO2 nanoparticles by UV-visible spectrophotometer (UV-VIS), and demonstrated that the photocatalytic activity of the μ-DBD plasma-treated TiO2 nanoparticles showed significantly high catalytic efficiency rather than without plasma treated TiO2 nanoparticles. Field emission scanning electron microscopes (FE-SEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and water contact angle analyzer were used to measure the effects of photocatalytic degradation for the plasma treated TiO2 nanoparticles.

Direct laser sintered WC-10Co/Cu nanocomposites

NASA Astrophysics Data System (ADS)

Gu, Dongdong; Shen, Yifu

2008-04-01

In the present work, the direct metal laser sintering (DMLS) process was used to prepare the WC-Co/Cu nanocomposites in bulk form. The WC reinforcing nanoparticles were added in the form of WC-10 wt.% Co composite powder. The microstructural features and mechanical properties of the laser-sintered sample were characterized by X-ray diffraction (XRD), atomic force microscope (AFM), scanning electron microscope (SEM), energy dispersive X-ray spectroscope (EDX), and nanoindentation tester. It showed that the original nanometric nature of the WC reinforcing particulates was well retained without appreciable grain growth after laser processing. A homogeneous distribution of the WC reinforcing nanoparticles with a coherent particulate/matrix interfacial bonding was obtained in the laser-sintered structure. The 94.3% dense nanocomposites have a dynamic nanohardness of 3.47 GPa and a reduced elastic modulus of 613.42 GPa.

Hydroxyapatite coatings produced on commercially pure titanium by micro-arc oxidation.

PubMed

Huang, Yong; Wang, Yingjun; Ning, Chengyun; Nan, Kaihui; Han, Yong

2007-09-01

A porous hydroxyapatite (HA) coating on commercially pure titanium was prepared by micro-arc oxidation (MAO) in electrolytic solution containing calcium acetate and beta-glycerol phosphate disodium salt pentahydrate (beta-GP). The thickness, phase, composition morphology and biocompatibility of the oxide coating were characterized by x-ray diffraction (XRD), electron probe microanalysis (EPMA), scanning electron microscopy (SEM) with an energy dispersive x-ray spectrometer (EDS) and cell culture. The thickness of the MAO film was about 20 microm, and the coating was porous and uneven without any apparent interface to the titanium substrates. The result of XRD showed that the porous coating was made up of HA film. The favorable osteoblast cell affinity gives HA film good biocompatibility. HA coatings are expected to have significant uses for medical applications such as dental implants and artificial bone joints.

Immobilization of Chlorosulfonyl-Calix[4]arene onto the surface of silica gel through the directly estrification

NASA Astrophysics Data System (ADS)

Taghvaei-Ganjali, Saeed; Zadmard, Reza; Saber-Tehrani, Mandana

2012-06-01

For the first time Chlorosulfonyl-Calix[4]arene has been chemically bonded to silica gel through the directly estrification without silane coupling agent to prepare Chlorosulfonyl-Calix[4]arene-bonded silica gel. Sample characterization was performed by various techniques such as elemental analysis, Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDAX), powder X-ray diffraction (XRD), N2 adsorption-desorption, thermal gravimetric analysis (TGA), 29Si CP/MAS spectroscopy and acid-base titration. All data approve the successful incorporation of organic group via covalent bond. From the comparison between sulfur content determined by elemental analysis and the number of H+ determined by acid-base titration, it was shown that two ester units took place onto the new synthesized sample and two acidic sites exist on the surface.

Nanostructured ZnO Films for Room Temperature Ammonia Sensing

NASA Astrophysics Data System (ADS)

Dhivya Ponnusamy; Sridharan Madanagurusamy

2014-09-01

Zinc oxide (ZnO) thin films have been deposited by a reactive dc magnetron sputtering technique onto a thoroughly cleaned glass substrate at room temperature. X-ray diffraction revealed that the deposited film was polycrystalline in nature. The field emission scanning electron micrograph (FE-SEM) showed the uniform formation of a rugby ball-shaped ZnO nanostructure. Energy dispersive x-ray analysis (EDX) confirmed that the film was stoichiometric and the direct band gap of the film, determined using UV-Vis spectroscopy, was 3.29 eV. The ZnO nanostructured film exhibited better sensing towards ammonia (NH3) at room temperature (˜30°C). The fabricated ZnO film based sensor was capable of detecting NH3 at as low as 5 ppm, and its parameters, such as response, selectivity, stability, and response/recovery time, were also investigated.

Size and morphology controlled NiSe nanoparticles as efficient catalyst for the reduction reactions

NASA Astrophysics Data System (ADS)

Subbarao, Udumula; Marakatti, Vijaykumar S.; Amshumali, Mungalimane K.; Loukya, B.; Singh, Dheeraj Kumar; Datta, Ranjan; Peter, Sebastian C.

2016-12-01

Facile and efficient ball milling and polyol methods were employed for the synthesis of nickel selenide (NiSe) nanoparticle. The particle size of the NiSe nanoparticle has been controlled mechanically by varying the ball size in the milling process. The role of the surfactants in the formation of various morphologies was studied. The compounds were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray energy dispersive spectroscopy (EDS). The efficiency of the NiSe nanoparticle as a catalyst was tested for the reduction of para-nitroaniline (PNA) to para-phenyldiamine (PPD) and para-nitrophenol (PNP) to para-aminophenol (PAP) using NaBH4 as the reducing agent. Particle size, morphology and the presence of surfactant played a crucial role in the reduction process.

The effect of exit beam phase aberrations on parallel beam coherent x-ray reconstructions

NASA Astrophysics Data System (ADS)

Hruszkewycz, S. O.; Harder, R.; Xiao, X.; Fuoss, P. H.

2010-12-01

Diffraction artifacts from imperfect x-ray windows near the sample are an important consideration in the design of coherent x-ray diffraction measurements. In this study, we used simulated and experimental diffraction patterns in two and three dimensions to explore the effect of phase imperfections in a beryllium window (such as a void or inclusion) on the convergence behavior of phasing algorithms and on the ultimate reconstruction. A predictive relationship between beam wavelength, sample size, and window position was derived to explain the dependence of reconstruction quality on beryllium defect size. Defects corresponding to this prediction cause the most damage to the sample exit wave and induce signature error oscillations during phasing that can be used as a fingerprint of experimental x-ray window artifacts. The relationship between x-ray window imperfection size and coherent x-ray diffractive imaging reconstruction quality explored in this work can play an important role in designing high-resolution in situ coherent imaging instrumentation and will help interpret the phasing behavior of coherent diffraction measured in these in situ environments.

The effect of exit beam phase aberrations on parallel beam coherent x-ray reconstructions.

PubMed

Hruszkewycz, S O; Harder, R; Xiao, X; Fuoss, P H

2010-12-01

Diffraction artifacts from imperfect x-ray windows near the sample are an important consideration in the design of coherent x-ray diffraction measurements. In this study, we used simulated and experimental diffraction patterns in two and three dimensions to explore the effect of phase imperfections in a beryllium window (such as a void or inclusion) on the convergence behavior of phasing algorithms and on the ultimate reconstruction. A predictive relationship between beam wavelength, sample size, and window position was derived to explain the dependence of reconstruction quality on beryllium defect size. Defects corresponding to this prediction cause the most damage to the sample exit wave and induce signature error oscillations during phasing that can be used as a fingerprint of experimental x-ray window artifacts. The relationship between x-ray window imperfection size and coherent x-ray diffractive imaging reconstruction quality explored in this work can play an important role in designing high-resolution in situ coherent imaging instrumentation and will help interpret the phasing behavior of coherent diffraction measured in these in situ environments.

Femtosecond X-ray Diffraction From Two-Dimensional Protein Crystals

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

Frank, Matthias; Carlson, David B.; Hunter, Mark

2014-02-28

Here we present femtosecond x-ray diffraction patterns from two-dimensional (2-D) protein crystals using an x-ray free electron laser (XFEL). To date it has not been possible to acquire x-ray diffraction from individual 2-D protein crystals due to radiation damage. However, the intense and ultrafast pulses generated by an XFEL permits a new method of collecting diffraction data before the sample is destroyed. Utilizing a diffract-before-destroy methodology at the Linac Coherent Light Source, we observed Bragg diffraction to better than 8.5 Å resolution for two different 2-D protein crystal samples that were maintained at room temperature. These proof-of-principle results show promisemore » for structural analysis of both soluble and membrane proteins arranged as 2-D crystals without requiring cryogenic conditions or the formation of three-dimensional crystals.« less

Influence of gamma ray irradiation on stoichiometry of hydrothermally synthesized bismuth telluride nanoparticles

NASA Astrophysics Data System (ADS)

Abishek, N. S.; Naik, K. Gopalakrishna

2018-05-01

Bismuth telluride (Bi2Te3) nanoparticles were synthesized by the hydrothermal method at 200 °C for 24 h. The synthesized Bi2Te3 nanoparticles were irradiated with gamma rays at doses of 50 kGy and 100 kGy. The structural characterization of the pre-irradiated and post-irradiated samples was carried out by X-ray diffraction technique and was found to have rhombohedral phase having R3 ¯m (166) space group. The X-ray diffraction peaks were found to shift towards lower diffraction angle with gamma ray irradiation. The morphologies and compositions of the grown Bi2Te3 nanoparticles were studied using Field Emission Scanning Electron Microscope and X-ray energy dispersive analysis, respectively. The possible cause for the shift in the X-ray diffraction peaks with gamma ray irradiation has been discussed in the present work.

High Power Optical Coatings by Atomic Layer Deposition and Signatures of Laser-Induced Damage

DTIC Science & Technology

2012-08-28

diffraction angle 0 into crystal lattice spacing d by the Bragg condition, mX = 2d sin 0. Here X is the x - ray wavelength... angle x - ray diffraction (GAXRD) measurements, which were made at a fixed shallow incidence angle of 0.5°. Detector scans were done to measure the...was finished with 200 hafnia cycles m the fmal half period rather than 400. Crystallinity was measured by x - ray diffraction (XRD) with

Materials identification using a small-scale pixellated x-ray diffraction system

NASA Astrophysics Data System (ADS)

O'Flynn, D.; Crews, C.; Drakos, I.; Christodoulou, C.; Wilson, M. D.; Veale, M. C.; Seller, P.; Speller, R. D.

2016-05-01

A transmission x-ray diffraction system has been developed using a pixellated, energy-resolving detector (HEXITEC) and a small-scale, mains operated x-ray source (Amptek Mini-X). HEXITEC enables diffraction to be measured without the requirement of incident spectrum filtration, or collimation of the scatter from the sample, preserving a large proportion of the useful signal compared with other diffraction techniques. Due to this efficiency, sufficient molecular information for material identification can be obtained within 5 s despite the relatively low x-ray source power. Diffraction data are presented from caffeine, hexamine, paracetamol, plastic explosives and narcotics. The capability to determine molecular information from aspirin tablets inside their packaging is demonstrated. Material selectivity and the potential for a sample classification model is shown with principal component analysis, through which each different material can be clearly resolved.

Structure, microstructure and infrared studies of Ba{sub 0.06}(Na{sub 1/2}Bi{sub 1/2}){sub 0.94}TiO{sub 3}-NaNbO{sub 3} ceramics

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

Roy, Sumit K., E-mail: sumit.sxc13@gmail.com; Singh, S. N., E-mail: snsphyru@gmail.com; Prasad, K., E-mail: k.prasad65@gmail.com

2016-05-06

Lead-free solid solutions (1-x)Ba{sub 0.06}(Na{sub 1/2}Bi{sub 1/2}){sub 0.94}TiO{sub 3}-xNaNbO{sub 3} (0 ≤ x ≤ 1.0) were prepared by conventional ceramic fabrication technique. X-ray diffraction and Rietveld refinement analyses of these ceramics were carried out using X’Pert HighScore Plus software to determine the crystal symmetry, space group and unit cell dimensions. Rietveld refinement revealed that NaNbO{sub 3} with orthorhombic structure was completely diffused into Ba{sub 0.06}(Na{sub 1/2}Bi{sub 1/2}){sub 0.94}TiO{sub 3} lattice having the rhombohedral-tetragonal symmetry. EDS and SEM studies were carried out in order to evaluate the quality and purity of the compounds. SEM images showed a change in grain shapemore » with the increase of NaNbO{sub 3} content. FTIR spectra confirmed the formation of solid solution.« less

Dynamic X-ray diffraction sampling for protein crystal positioning

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

Scarborough, Nicole M.; Godaliyadda, G. M. Dilshan P.; Ye, Dong Hye

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction,more » significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Furthermore, by usingin situtwo-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations.« less

Dynamic X-ray diffraction sampling for protein crystal positioning

DOE PAGES

Scarborough, Nicole M.; Godaliyadda, G. M. Dilshan P.; Ye, Dong Hye; ...

2017-01-01

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction,more » significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Furthermore, by usingin situtwo-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations.« less

Dynamic X-ray diffraction sampling for protein crystal positioning

PubMed Central

Scarborough, Nicole M.; Godaliyadda, G. M. Dilshan P.; Ye, Dong Hye; Kissick, David J.; Zhang, Shijie; Newman, Justin A.; Sheedlo, Michael J.; Chowdhury, Azhad U.; Fischetti, Robert F.; Das, Chittaranjan; Buzzard, Gregery T.; Bouman, Charles A.; Simpson, Garth J.

2017-01-01

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction, significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Using in situ two-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations. PMID:28009558

Dynamic X-ray diffraction sampling for protein crystal positioning.

PubMed

Scarborough, Nicole M; Godaliyadda, G M Dilshan P; Ye, Dong Hye; Kissick, David J; Zhang, Shijie; Newman, Justin A; Sheedlo, Michael J; Chowdhury, Azhad U; Fischetti, Robert F; Das, Chittaranjan; Buzzard, Gregery T; Bouman, Charles A; Simpson, Garth J

2017-01-01

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction, significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Using in situ two-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations.

Novel perovskite coating of strontium zirconate in Inconel substrate

NASA Astrophysics Data System (ADS)

Venkatesh, G.; Blessto, B.; Rao, C. Santhosh Kumar; Subramanian, R.; Berchmans, L. John

2018-02-01

Thermal Barrier Coatings (TBC) provides a low thermal conductivity barrier to heat transfer from the hot gas in the engine to the surface of the coated alloy component. SrZrO3 powder are prepared by Sol Gel synthesis method. The synthesized powder sample is characterized by X Ray Diffraction Technique (XRD), Scanning Electron Microscope (SEM) and Transmission Electron Microscope (TEM) and the results are interpreted. The Polycrystalline nature of SrZrO3 is confirmed and lattice spacing are determined in XRD. SEM shows sub-micron sized particles and a fringed pattern is observed in TEM. The IN718 specimen is Wire Cut and Sand Blasted. A SrZrO3 double layer is coated over the Inconel specimen through a Bond Coat made of NiCoCrAlY by Plasma spraying Process and also characterized. SEM analysis of the Coating shows diffusion of Fe, Sr into the substrate.

Fixture for supporting and aligning a sample to be analyzed in an x-ray diffraction apparatus

DOEpatents

Green, L.A.; Heck, J.L. Jr.

1985-04-23

A fixture is provided for supporting and aligning small samples of material on a goniometer for x-ray diffraction analysis. A sample-containing capillary is accurately positioned for rotation in the x-ray beam by selectively adjusting the fixture to position the capillary relative to the x and y axes thereof to prevent wobble and position the sample along the z axis or the axis of rotation. By employing the subject fixture relatively small samples of materials can be analyzed in an x-ray diffraction apparatus previously limited to the analysis of much larger samples.

Fixture for supporting and aligning a sample to be analyzed in an X-ray diffraction apparatus

DOEpatents

Green, Lanny A.; Heck, Jr., Joaquim L.

1987-01-01

A fixture is provided for supporting and aligning small samples of material on a goniometer for X-ray diffraction analysis. A sample-containing capillary is accurately positioned for rotation in the X-ray beam by selectively adjusting the fixture to position the capillary relative to the x and y axes thereof to prevent wobble and position the sample along the z axis or the axis of rotation. By employing the subject fixture relatively small samples of materials can be analyzed in an X-ray diffraction apparatus previously limited to the analysis of much larger samples.

[Preparation of nano zero-valent iron/Sargassum horneri based activated carbon for removal of Cr (VI) from aqueous solution].

PubMed

Zeng, Gan-Ning; Wu, Xiao; Zheng, Lin; Wu, Xi; Tu, Mei-Ling; Wang, Tie-Gan; Ai, Ning

2015-02-01

Nanoscale zero-valent iron supported on Sargassum horneri activated carbon (NZVI/SAC) was synthesized by zinc chloride activation and incipient wetness method, and characterized with X-ray diffraction (XRD), Scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). XRD confirmed the existence of nano zero-valent iron, and SEM revealed that the material consisted of mainly 30-150 nm spherical particles aggregated into chains of individual units. The valence state of iron conformed with the nuclear-shell model. The effects of NZVI loading on AC, pH and the initial concentration of Cr(VI) on the removal of Cr(VI) were investigated. The final Cr(VI) removal percentage was up to 100% under the following conditions: 30 degrees C, pH = 2, NZVI/SAC dosage of 2 g x L(-1) and the amounts of NZVI loaded on SAC of 30%. And the equilibrium time was 10 minutes. These results showed that NZVI/SAC could be potentially applied for removal of high concentration Cr(VI). By analyzing the chemical change of NZVI/ SAC, we demonstrated that Cr(VI) was mainly reduced to insoluble Cr (III) compound in the reaction when pH was less than 4, and adsorbed by NZVI and SAC when pH was over 4.

Morphological Comparison of U3O8 Ore Concentrates from Canada Key Lake and Namibia Sources

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

Schwartz, Daniel S.; Tandon, Lav; Martinez, Patrick Thomas

Uranium ore concentrates from two different sources were examined using scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). The ore powders are referred to as Namibia (id. no. 90036, LIMS id. no. 18775) and Canada Key Lake (id. no. 90019, LIMS id. no. 18774). Earlier work identified the ores as the U₃O₈ phase of uranium oxide using x-ray diffraction. Both sets of powders were in the form of dark brown to black powder fines. However, the Canada Key Lake concentrates contained larger chunks of material on the millimeter scale that were easily visible to the unaided eye. The powdersmore » were mounted for SEM examination by hand dispersing a small amount onto conductive sticky tape. Two types of applicators were used and compared: a fine-tipped spatula and a foam-tipped applicator. The sticky tape was on a standard SEM “tee” mount, which was tapped to remove loose contamination before being inserted into the SEM.« less

JMFA2—a graphically interactive Java program that fits microfibril angle X-ray diffraction data

Treesearch

Steve P. Verrill; David E. Kretschmann; Victoria L. Herian

2006-01-01

X-ray diffraction techniques have the potential to decrease the time required to determine microfibril angles dramatically. In this paper, we discuss the latest version of a curve-fitting toll that permits us to reduce the time required to evaluate MFA X-ray diffraction patterns. Further, because this tool reflects the underlying physics more accurately than existing...

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

DOE PAGES

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.; ...

2015-08-11

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called `fixed-target' sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessarymore » to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. In addition, the features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

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

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called `fixed-target' sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessarymore » to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. In addition, the features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

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

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called `fixed-target' sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary tomore » fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15µm) loaded into the chips yielded a complete, high-resolution (<1.6Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

PubMed Central

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.; Vo, Huy; Uervirojnangkoorn, Monarin; Brunger, Axel T.; Berger, James M.

2015-01-01

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called ‘fixed-target’ sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs. PMID:26457423

Characterization of Limestone as Raw Material to Hydrated Lime

NASA Astrophysics Data System (ADS)

Salem Hwidi, Rajeb; Nuraiti Tengku Izhar, Tengku; Saad, Farah Naemah Mohd

2018-03-01

In Malaysia, limestone is essentially important for the economic growth as raw materials in the industry sector. Nevertheless, a little attention was paid to the physical, chemical, mineralogical, and morphological properties of the limestone using X-ray fluorescence (X-RF), X-ray diffraction (X-RD), Fourier transform infrared spectroscopy (FTIR), and Scanning electron microscopy / energy dispersive x-ray spectroscopy (SEM-EDS) respectively. Raw materials (limestone rocks) were collected from Bukit Keteri area, Chuping, Kangar, Perlis, Malaysia. Lab crusher and lab sieved were utilized to prepare five different size of ground limestone at (75 µm, 150 µm, 225 µm, 300, and 425 µm) respectively. It is found that the main chemical composition of bulk limestone was Calcium oxide (CaO) at 97.58 wt.% and trace amount of MnO, Al2O3, and Fe2O3 at 0.02%, 0.35%, and 0.396% respectively. XRD diffractograms showed characteristic peaks of calcite and quartz. Furthermore, main FTIR absorption bands at 1,419, 874.08 and 712.20 cm-1 indicated the presence of calcite. The micrographs showed clearly the difference of samples particle size. Furthermore, EDS peaks of Ca, O, and C elements confirmed the presence of CaCO3 in the samples.

A facile thermal decomposition route to synthesise CoFe2O4 nanostructures

NASA Astrophysics Data System (ADS)

Kalpanadevi, K.; Sinduja, C. R.; Manimekalai, R.

2014-01-01

The synthesis of CoFe2O4 nanoparticles has been achieved by a simple thermal decomposition method from an inorganic precursor, cobalt ferrous cinnamate hydrazinate (CoFe2(cin)3(N2H4)3) which was obtained by a novel precipitation method from the corresponding metal salts, cinnamic acid and hydrazine hydrate. The precursor was characterized by hydrazine and metal analyses, infrared spectral analysis and thermo gravimetric analysis. Under appropriate annealing, CoFe2(cin)3(N2H4)3 yielded CoFe2O4 nanoparticles, which were characterized for their size and structure using X-Ray diffraction (XRD), high resolution transmission electron microscopic (HRTEM), selected area electron diffraction (SAED) and scanning electron microscopic (SEM) techniques.

Influence of the divalent and trivalent ions substitution on the structural and magnetic properties of Mg0.5-xCdxCo0.5Cr0.04TbyFe1.96-yO4 ferrites prepared by sol-gel method

NASA Astrophysics Data System (ADS)

Mustafa, Ghulam; Islam, M. U.; Zhang, Wenli; Anwar, Abdul Waheed; Jamil, Yasir; Murtaza, Ghulam; Ali, Ihsan; Hussain, Mudassar; Ali, Akbar; Ahmad, Mukhtar

2015-08-01

A series of the divalent and trivalent co-substituted Mg0.5-xCdxCo0.5Cr0.04TbyFe1.96-yO4 spinel ferrite systems (where x=0-0.5 in steps of 0.1 and y=0.00-0.10 in steps 0.02) are synthesized by sol-gel auto combustion method. The product materials were characterized by the thermo gravimetric analysis and differential scanning calorimetry (TGA/DSC), Fourier transform infrared spectra (FTIR), nitrogen adsorption (BET), X-ray diffraction (XRD), scanning electron microscope (SEM), atomic force microscopy (AFM) and vibrating sample magnetometer (VSM). The X-ray diffraction patterns and Fourier transform infrared spectroscopy confirm spinel nanocrystalline phase. The crystallite size is determined by Scherer's formula from 36.6 to 69.4 nm. The X-ray density is found in the range of 5.09-6.43 (g/cm3). The morphological features are studied using scanning electron microscope and AFM. Saturation magnetization (Ms) and remanence (Mr) magnetization extracted from M-H loops exhibit the decreasing trends 21.4-16 emu/g and 9.1-6.3 emu/g, respectively. A significant decrease in the intrinsic parameters is observed in the prepared samples due to the weakening of the A-B interaction as iron enters into the tetrahedral A-site. The coercivity lies in the range of 300-869 Oe as a function of co-substitution contents. The coercivity of the sample with x=0.1, y=0.02 was found maximum i.e. 869 Oe. The obtained results suggest that the investigated materials may be potential candidates for high density recording media applications.

Improvement of critical current density in thallium-based (Tl,Bi)Sr(1.6)Ba(0.4)Ca2Cu3O(x) superconductors

NASA Technical Reports Server (NTRS)

Ren, Z. F.; Wang, C. A.; Wang, J. H.; Miller, D. J.; Goretta, K. C.

1995-01-01

Epitaxial (Tl,Bi)Sr(1.6)Ba(0.4)Ca2Cu3O(x) ((Tl,Bi)-1223) thin films on (100) single crystal LaAlO3 substrates were synthesized by a two-step procedure. Phase development, microstructure, and relationships between film and substrate were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Resistance versus temperature, zero-field-cooled and field cooled magnetization, and transport critical current density (J(sub c)) were measured. The zero-resistance temperature was 105-111 K. J(sub c) at 77 K and zero field was greater than 2 x 10(exp 6) A/sq cm. The films exhibited good flux pinning properties.

Impedance spectroscopy studies in cobalt ferrite-reduced graphene oxide nanocomposite

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

Supriya, Sweety, E-mail: sweety@iitp.ac.in; Kumar, Sunil, E-mail: sunil.pph13@iitp.ac.in; Kar, Manoranjan, E-mail: mano@iitp.ac.in

2016-05-06

(1-x)Cobalt ferrite-(x)reduced graphene oxidenanocomposites with x=0, 0.1, 0.2 and 0.3 were prepared by the ultrasonic method. The crystal symmetry modification due to reduced graphene oxide and cobalt ferrite interaction has been studied by employing the X-ray diffraction technique. Morphology of the samples was studied by the Field emission scanning electron microscopy (FE-SEM). Study on electrical properties of the cobalt ferrite-reduced graphene oxide nanocomposites explores the possible application of these composites as anode material. Impedance decreases with an increase in frequency as well as temperature, which supports an increase in ac electrical conductivity. The modified Debye relaxation model can explain themore » behavior of impedance in cobalt ferrite-reduced graphene oxide nanocomposites.« less

Uranium Redox Transformations after U(VI) Coprecipitation with Magnetite Nanoparticles.

PubMed

Pidchenko, Ivan; Kvashnina, Kristina O; Yokosawa, Tadahiro; Finck, Nicolas; Bahl, Sebastian; Schild, Dieter; Polly, Robert; Bohnert, Elke; Rossberg, André; Göttlicher, Jörg; Dardenne, Kathy; Rothe, Jörg; Schäfer, Thorsten; Geckeis, Horst; Vitova, Tonya

2017-02-21

Uranium redox states and speciation in magnetite nanoparticles coprecipitated with U(VI) for uranium loadings varying from 1000 to 10 000 ppm are investigated by X-ray absorption spectroscopy (XAS). It is demonstrated that the U M 4 high energy resolution X-ray absorption near edge structure (HR-XANES) method is capable to clearly characterize U(IV), U(V), and U(VI) existing simultaneously in the same sample. The contributions of the three different uranium redox states are quantified with the iterative transformation factor analysis (ITFA) method. U L 3 XAS and transmission electron microscopy (TEM) reveal that initially sorbed U(VI) species recrystallize to nonstoichiometric UO 2+x nanoparticles within 147 days when stored under anoxic conditions. These U(IV) species oxidize again when exposed to air. U M 4 HR-XANES data demonstrate strong contribution of U(V) at day 10 and that U(V) remains stable over 142 days under ambient conditions as shown for magnetite nanoparticles containing 1000 ppm U. U L 3 XAS indicates that this U(V) species is protected from oxidation likely incorporated into octahedral magnetite sites. XAS results are supported by density functional theory (DFT) calculations. Further characterization of the samples include powder X-ray diffraction (pXRD), scanning electron microscopy (SEM) and Fe 2p X-ray photoelectron spectroscopy (XPS).

Mechanism of Action of TiF4 on Dental Enamel Surface: SEM/EDX, KOH-Soluble F, and X-Ray Diffraction Analysis.

PubMed

Comar, Lívia P; Souza, Beatriz M; Al-Ahj, Luana P; Martins, Jessica; Grizzo, Larissa T; Piasentim, Isabelle S; Rios, Daniela; Buzalaf, Marília Afonso Rabelo; Magalhães, Ana Carolina

2017-10-12

This in vitro study aimed to evaluate the action of TiF4 on sound and carious bovine and human enamel. Sound (S) and pre-demineralised (DE) bovine and human (primary and permanent) enamel samples were treated with TiF4 (pH 1.0) or NaF varnishes (pH 5.0), containing 0.95, 1.95, or 2.45% F for 12 h. The enamel surfaces were analysed using SEM-EDX (scanning electron microscopy/energy-dispersive X-ray spectroscopy) (n = 10, 5 S and 5 DE) and KOH-soluble fluoride was quantified (n = 20, 10 S and 10 DE). Hydroxyapatite powder produced by precipitation method was treated with the corresponding fluoride solutions for 1 min (n = 2). The formed compounds were detected using X-ray diffraction (XRD). All TiF4 varnishes produced a coating layer rich in Ti and F on all types of enamel surface, with micro-cracks in its extension. TiF4 (1.95 and 2.45% F) provided higher fluoride deposition than NaF, especially for bovine enamel (p < 0.0001). It also induced a higher fluoride deposition on DE samples compared to S samples (p < 0.0001), except for primary enamel. The Ti content was higher for bovine and human primary enamel than human permanent enamel, with some differences between S and DE. The XRD analysis showed that TiF4 induced the formation of new compounds such as CaF2, TiO2, and Ti(HPO4)2·H2O. In conclusion, TiF4 (>0.95% F) interacts better, when compared to NaF, with bovine and human primary enamel than with human permanent enamel. TiF4 provoked higher F deposition compared to NaF. Carious enamel showed higher F uptake than sound enamel by TiF4 application, while Ti uptake was dependent on the enamel condition and origin. © 2017 S. Karger AG, Basel.

Synthesis and characterization of high quantum yield and oscillator strength 6-chloro-2-(4-cynophenyl)-4-phenyl quinoline (cl-CN-DPQ) organic phosphor for solid-state lighting.

PubMed

Ghate, Minakshi; Dahule, H K; Thejo Kalyani, N; Dhoble, S J

2018-03-01

A novel blue luminescent 6-chloro-2-(4-cynophenyl) substituted diphenyl quinoline (Cl-CN DPQ) organic phosphor has been synthesized by the acid-catalyzed Friedlander reaction and then characterized to confirm structural, optical and thermal properties. Structural properties of Cl-CN-DPQ were analyzed by Fourier transform infrared (FTIR), nuclear magnetic resonance (NMR) spectroscopy, X-ray diffraction technique (XRD) and scanning electron microscopy (SEM) and energy dispersive analysis of X-ray (EDAX) spectroscopy. FTIR spectra confirmed the presence of different functional groups and bond stretching. 1 H-NMR and 13 C-NMR confirmed the formation of an organic Cl-CN-DPQ compound. X-ray diffraction study provided its crystalline nature. The surface morphology of Cl-CN-DPQ was analyzed by SEM, while EDAX spectroscopy revealed the elemental analysis. Differential thermal analysis (TGA/DTA) disclosed its thermal stability up to 250°C. The optical properties of Cl-CN-DPQ were investigated by UV-vis absorption and photoluminescence (PL) measurements. Cl-CN-DPQ exhibits intense blue emission at 434 nm in a solid-state crystalline powder with CIE co-ordinates (0.157, 0.027), when excited at 373 nm. Cl-CN-DPQ shows remarkable Stokes shift in the range 14800-5100 cm -1 , which is the characteristic feature of intense light emission. A narrow full width at half-maximum (FWHM) value of PL spectra in the range 42-48 nm was observed. Oscillator strength, energy band gap, quantum yield, and fluorescence energy yield were also examined using UV-vis absorption and photoluminescence spectra. These results prove its applications towards developing organic luminescence devices and displays, organic phosphor-based solar cells and displays, organic lasers, chemical sensors and many more. Copyright © 2017 John Wiley & Sons, Ltd.

A single-phase white light emitting Pr3+ doped Ba2CaWO6 phosphor: synthesis, photoluminescence and optical properties

NASA Astrophysics Data System (ADS)

Sreeja, E.; Vidyadharan, Viji; Jose, Saritha K.; George, Anns; Joseph, Cyriac; Unnikrishnan, N. V.; Biju, P. R.

2018-04-01

Pr3+ doped Ba2CaWO6 phosphor were prepared by traditional high-temperature solid-state reaction technique. The structure evolution was systematically investigated by X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDS), Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) analysis. The X-ray powder diffraction patterns indicate that the prepared phosphors crystallized in the cubic double-perovskite structure. The functional groups were identified using FTIR spectra and the elements present in the composition were confirmed by the EDS profile. The morphology of the phosphor was identified using SEM and TEM analysis. The PL spectra illustrated that these phosphors could be efficiently excited by charge transfer band of host and the maximum luminescence intensity was observed at 0.06 wt% of Pr3+ ion. Upon the charge transfer band excitation, emission spectra showed peaks at 489, 532, 647, 685 and 737 nm corresponding to 3P0→3H4, 3P1→3H5, 3P0→3F2, 3P0→3F3 and 3P0→3F4 transitions respectively. The concentration quenching of Ba2CaWO6:Pr3+ phosphor can be mainly attributed to dipole-dipole interaction. The CIE coordinates were estimated to be close to the white region. The decay curves are well fitted with double exponential decay models. The standard and modified Judd-Ofelt (JO) theories were used to determine the Judd-Ofelt intensity parameters, radiative transition probabilities and branching ratios. The optical properties indicate that Ba2CaWO6:Pr3+ phosphors can produce white light emission from a single phase host and its potential application for solid-state lighting and display devices.

Synthesis, physical properties and self-assembly behavior of azole-fused pyrene derivatives

NASA Astrophysics Data System (ADS)

Xiao, Jinchong; Xiao, Xuyu; Zhao, Yanlei; Wu, Bo; Liu, Zhenying; Zhang, Xuemin; Wang, Sujuan; Zhao, Xiaohui; Liu, Lei; Jiang, Li

2013-05-01

A novel selenadiazole-fused pyrene derivative PySe was successfully synthesized and characterized. Its single structure is almost planar and adopts a sandwich-herringbone packing model. The self-assembly behaviors based on compound PySe and its analogue thiadiazole-fused pyrene derivative PyS were studied in detail and the as-formed nanostructures were fully characterized by means of UV-vis absorption, emission spectra, X-ray diffraction, field emission SEM and TEM. We attribute the bathochromic shift absorption and emission spectra of PyS and PySe in aqueous solution to the formation of J-type aggregation. In addition, our investigation demonstrated that the shape and size of the as-prepared nanostructures could be tuned by different chalcogen analogues and the volume ratio of water to organic solvent.A novel selenadiazole-fused pyrene derivative PySe was successfully synthesized and characterized. Its single structure is almost planar and adopts a sandwich-herringbone packing model. The self-assembly behaviors based on compound PySe and its analogue thiadiazole-fused pyrene derivative PyS were studied in detail and the as-formed nanostructures were fully characterized by means of UV-vis absorption, emission spectra, X-ray diffraction, field emission SEM and TEM. We attribute the bathochromic shift absorption and emission spectra of PyS and PySe in aqueous solution to the formation of J-type aggregation. In addition, our investigation demonstrated that the shape and size of the as-prepared nanostructures could be tuned by different chalcogen analogues and the volume ratio of water to organic solvent. Electronic supplementary information (ESI) available: TGA analysis, spectra characterization data for compound 1, 2, 3 and X-ray crystallographic data for compound PySe (2, CIF). CCDC 917821. For ESI and crystallographic data in CIF or other electronic format see DOI: 10.1039/c3nr00523b

High-resolution x-ray diffraction microscopy of specifically labeled yeast cells

PubMed Central

Nelson, Johanna; Huang, Xiaojing; Steinbrener, Jan; Shapiro, David; Kirz, Janos; Marchesini, Stefano; Neiman, Aaron M.; Turner, Joshua J.; Jacobsen, Chris

2010-01-01

X-ray diffraction microscopy complements other x-ray microscopy methods by being free of lens-imposed radiation dose and resolution limits, and it allows for high-resolution imaging of biological specimens too thick to be viewed by electron microscopy. We report here the highest resolution (11–13 nm) x-ray diffraction micrograph of biological specimens, and a demonstration of molecular-specific gold labeling at different depths within cells via through-focus propagation of the reconstructed wavefield. The lectin concanavalin A conjugated to colloidal gold particles was used to label the α-mannan sugar in the cell wall of the yeast Saccharomyces cerevisiae. Cells were plunge-frozen in liquid ethane and freeze-dried, after which they were imaged whole using x-ray diffraction microscopy at 750 eV photon energy. PMID:20368463

High-resolution x-ray diffraction microscopy of specifically labeled yeast cells

DOE PAGES

Nelson, Johanna; Huang, Xiaojing; Steinbrener, Jan; ...

2010-04-20

X-ray diffraction microscopy complements other x-ray microscopy methods by being free of lens-imposed radiation dose and resolution limits, and it allows for high-resolution imaging of biological specimens too thick to be viewed by electron microscopy. We report here the highest resolution (11-13 nm) x-ray diffraction micrograph of biological specimens, and a demonstration of molecular-specific gold labeling at different depths within cells via through-focus propagation of the reconstructed wavefield. The lectin concanavalin A conjugated to colloidal gold particles was used to label the α-mannan sugar in the cell wall of the yeast Saccharomyces cerevisiae. Cells were plunge-frozen in liquid ethane andmore » freeze-dried, after which they were imaged whole using x-ray diffraction microscopy at 750 eV photon energy.« less

The thermal stability of the carbon-palladium films for hydrogen sensor applications

NASA Astrophysics Data System (ADS)

Rymarczyk, Joanna; Czerwosz, ElŻbieta; Diduszko, Ryszard; Kozłowski, Mirosław

2017-08-01

The thermal stability of two types of C-Pd films prepared in PVD process were studied. These films are composed of Pd nanograins embedded in a multiphase carbonaceous matrix. These films were distinguished by Pd content. These films were annealed in a range of temperatures 50÷1000°C. The structural, topographical and molecular changes were studied by scanning electron microscopy (SEM), infrared spectroscopy (FTIR) and X-ray diffraction (XRD) methods. The results show that investigated films are thermally stable up to 200°C.

Effect of alkali treatment on the physical and surface properties of Indian hemp fibers

NASA Astrophysics Data System (ADS)

Sangappa, Rao, B. Lakshmeesha; Asha, S.; Somashekar, R.

2013-02-01

The Plant fibers are rich in cellulose and they are a cheap, easily renewable source of fibers with the potential for polymer reinforcement. The presence of surface impurities and the large amount of hydroxyl groups make plant fibers less attractive for reinforcement of polymeric materials. Hemp (Cannabis Sativa L.) fibers were subjected to alkalization using 1N sodium hydroxide (NaOH). The structural properties and surface morphology of untreated and chemically modified fibers have been studied using X-ray diffraction (WAXS) and Scanning electron microscopy (SEM) respectively.

Improving the reactivity of phenylacetylene macrocycles toward topochemical polymerization by side chains modification

PubMed Central

Daigle, Maxime; Cantin, Katy

2014-01-01

Summary The synthesis and self-assembly of two new phenylacetylene macrocycle (PAM) organogelators were performed. Polar 2-hydroxyethoxy side chains were incorporated in the inner part of the macrocycles to modify the assembly mode in the gel state. With this modification, it was possible to increase the reactivity of the macrocycles in the xerogel state to form polydiacetylenes (PDAs), leading to a significant enhancement of the polymerization yields. The organogels and the PDAs were characterized using Raman spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM). PMID:25161718

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

Marimuthu, T.; Anandhan, N., E-mail: anandhan-kn@rediffmail.com; Mummoorthi, M.

Zinc oxide (ZnO) and zinc oxide/eosin yellow (ZnO/EY) thin films were potentiostatically deposited onto fluorine doped tin oxide (FTO) glass substrate. Effect of eosin yellow dye on structural, morphological and optical properties was studied. X-ray diffraction patterns, micro Raman spectra and photoluminescence (PL) spectra reveal hexagonal wurtzite structure with less atomic defects in 101 plane orientation of the ZnO/EY film. Scanning electron microscopy (SEM) images show flower for ZnO and porous like structure for ZnO/EY thin film, respectively. DSSC was constructed and evaluated by measuring the current density verses voltage curve.

In Situ Investigation of a Self-Accelerated Cocrystal Formation by Grinding Pyrazinamide with Oxalic Acid.

PubMed

Kulla, Hannes; Greiser, Sebastian; Benemann, Sigrid; Rademann, Klaus; Emmerling, Franziska

2016-07-14

A new cocrystal of pyrazinamide with oxalic acid was prepared mechanochemically and characterized by PXRD, Raman spectroscopy, solid-state NMR spectroscopy, DTA-TG, and SEM. Based on powder X-ray diffraction data the structure was solved. The formation pathway of the reaction was studied in situ using combined synchrotron PXRD and Raman spectroscopy. Using oxalic acid dihydrate the initially neat grinding turned into a rapid self-accelerated liquid-assisted grinding process by the release of crystallization water. Under these conditions, the cocrystal was formed directly within two minutes.

Effect of processing parameters on the characteristics of high-Tc superconductor YBa2Cu3Oy

NASA Technical Reports Server (NTRS)

Bansal, Narottam P.

1988-01-01

SEM, thermogravimetric analysis, powder X-ray diffraction,and measurements of electrical resistivity and magnetic susceptibility, are presently used to characterize the influence of sintering temperature, sintering and annealing atmospheres, and quench-rate on the properties of the YBa2Cu3Oy superconducting oxide. It is established that annealing in oxygen, together with slow cooling rates, are required for preparation of high-Tc superconductors with sharp transitions; rapid quenching from high temperature does not yield good superconductors, due to low oxygen content.

The peculiarity of the formation of zinc films on a glass substrate

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

Tomaev, V. V., E-mail: tvaza@mail.ru; Saint Petersburg Mining University, Russia, 199106, St. Petersburg, V.O., 21-st line, 2; Polishchuk, V. A., E-mail: vpvova2010@yandex.ru

2016-06-17

Thin Nanocrystalline films of the zinc have been fabricated by thermal spraying on the glass substrate. Morphologies and structure of the films had been investigated by the methods X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). It is found that the surface of the films has a different types of the nanocrystals zinc. Were detected intergrowths of two or more the nanocrystals, hexagonal shape. Using the theory of homogeneous and heterogeneous nucleation of a new phase, had been evaluated the geometrical and thermodynamic parameters nanocrystals zinc.

Crystallography of Magnetite Plaquettes and their Significance as Asymmetric Catalysts for the Synthesis of Chiral Organics in Carbonaceous Chondrites

NASA Technical Reports Server (NTRS)

Chan, Q. H. S.; Zolensky, M. E.

2015-01-01

We have previously observed the magnetite plaquettes in carbonaceous chondrites using scanning electron microscope (SEM) imaging, examined the crystal orientation of the polished surfaces of magnetite plaquettes in CI Orgueil using electron backscattered diffraction (EBSD) analysis, and concluded that these magnetite plaquettes are likely naturally asymmetric materials. In this study, we expanded our EBSD observation to other magnetite plaquettes in Orgueil, and further examined the internal structure of these remarkable crystals with the use of X-ray computed microtomography.

A Novel Method for Depositing Precious Metal Films on Difficult Surfaces

NASA Technical Reports Server (NTRS)

Veitch, L. C.; Phillip, W. H.

1994-01-01

A guanidine-based vehicle was developed to deposit precious metal coatings on surfaces known to be difficult to coat. To demonstrate this method, a platinum coating was deposited on alumina fibers using a guanidine-platinum solution. X-ray diffraction confirmed that the only species present in the coating was platinum and that all of the carbon species had been removed upon heat treatment. SEM results showed that some porosity was present but that the coatings uniformly covered the fiber surface and adhered well to the finer.

Effect of preparation conditions on the nanostructure of hydroxyapatite and brushite phases

NASA Astrophysics Data System (ADS)

Mansour, S. F.; El-dek, S. I.; Ahmed, M. A.; Abd-Elwahab, S. M.; Ahmed, M. K.

2016-10-01

Hydroxyapatite (HAP) and dicalcium phosphate dihydrate (brushite) nanoparticles were prepared by co-precipitation method. The obtained products were characterized by X-ray powder diffraction (XRD), Fourier transformation infra-red spectroscopy (FTIR) and thermo-gravimetric analysis (TGA). Scanning electron microscopy (SEM) and transmission electron microscope (TEM) were used to investigate the morphology of the powdered samples as well as their microstructure, respectively. Brushite samples were obtained in a spherical shape, while hydroxyapatite was formed in a needle and rice shape depending on the pH value.

Solvothermal synthesis of fusiform hexagonal prism SrCO{sub 3} microrods via ethylene glycol solution

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

Shi Liange; Du Fanglin

2007-08-07

Fusiform hexagonal prism SrCO{sub 3} microrods were prepared by a simple solvothermal route at 120 deg. C, and characterized by X-ray powder diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and Fourier transform infrared (FT-IR) spectroscopy. By controlling the content of ethylene glycol (EG), it was found that ethylene glycol (EG) played an important role in the formation of such SrCO{sub 3} microrods. Finally, effects of other solvents on the products, including 1,2-propanediol and glycerin, were also investigated.

Coherent x-ray zoom condenser lens for diffractive and scanning microscopy.

PubMed

Kimura, Takashi; Matsuyama, Satoshi; Yamauchi, Kazuto; Nishino, Yoshinori

2013-04-22

We propose a coherent x-ray zoom condenser lens composed of two-stage deformable Kirkpatrick-Baez mirrors. The lens delivers coherent x-rays with a controllable beam size, from one micrometer to a few tens of nanometers, at a fixed focal position. The lens is suitable for diffractive and scanning microscopy. We also propose non-scanning coherent diffraction microscopy for extended objects by using an apodized focused beam produced by the lens with a spatial filter. The proposed apodized-illumination method will be useful in highly efficient imaging with ultimate storage ring sources, and will also open the way to single-shot coherent diffraction microscopy of extended objects with x-ray free-electron lasers.

Scanning force microscope for in situ nanofocused X-ray diffraction studies

PubMed Central

Ren, Zhe; Mastropietro, Francesca; Davydok, Anton; Langlais, Simon; Richard, Marie-Ingrid; Furter, Jean-Jacques; Thomas, Olivier; Dupraz, Maxime; Verdier, Marc; Beutier, Guillaume; Boesecke, Peter; Cornelius, Thomas W.

2014-01-01

A compact scanning force microscope has been developed for in situ combination with nanofocused X-ray diffraction techniques at third-generation synchrotron beamlines. Its capabilities are demonstrated on Au nano-islands grown on a sapphire substrate. The new in situ device allows for in situ imaging the sample topography and the crystallinity by recording simultaneously an atomic force microscope (AFM) image and a scanning X-ray diffraction map of the same area. Moreover, a selected Au island can be mechanically deformed using the AFM tip while monitoring the deformation of the atomic lattice by nanofocused X-ray diffraction. This in situ approach gives access to the mechanical behavior of nanomaterials. PMID:25178002

Synthesis of SiO(x) powder using DC arc plasma.

PubMed

Jung, Chan-Ok; Park, Dong-Wha

2013-02-01

SiO(x) was prepared by DC arc plasma and applied to the anode material of lithium ion batteries. A pellet of a mixture of Si and SiO2 was used as the raw material. The ratios of the silicon and silicon dioxide (SiO2) mixtures were varied by controlling the Si-SiO2 molar ratio (Si-SiO2 = 1-4). Hydrogen gas was used as the reduction atmosphere in the chamber. The prepared SiO(x) was collected on the chamber wall. The obtained SiO(x) was characterized by X-ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM), energy dispersive spectroscopy (EDS), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). XRD and TEM showed that the phase composition of the prepared particles was composed of amorphous SiO(x) and crystalline Si. The prepared SiO(x) showed wire and spherical morphology. XPS indicated the bonding state and 'x' value of the prepared SiO(x), which was close to one. The result of prepared SiO(x) is discussed from thermodynamic equilibrium calculations. The electrochemical behavior of the silicon monoxide anode was investigated.

X-ray topography using the forward transmitted beam under multiple-beam diffraction conditions

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

Tsusaka, Y., E-mail: tsusaka@sci.u-hyogo.ac.jp; Takano, H.; Takeda, S.

2016-02-15

X-ray topographs are taken for a sapphire wafer with the [0001] surface normal, as an example, by forward transmitted synchrotron x-ray beams combined with two-dimensional electronic arrays in the x-ray detector having a spatial resolution of 1 μm. They exhibit no shape deformation and no position shift of the dislocation lines on the topographs. Since the topography is performed under multiple-beam diffraction conditions, the topographic images of a single diffraction (two-wave approximation condition) or plural diffractions (six-wave approximation condition) can be recorded without large specimen position changes. As usual Lang topographs, it is possible to determine the Burgers vector ofmore » each dislocation line. Because of high parallelism of the incoming x-rays and linear sensitivity of the electronic arrays to the incident x-rays, the present technique can be used to visualize individual dislocations in single crystals of the dislocation density as high as 1 × 10{sup 5} cm{sup −2}.« less

Multiple defocused coherent diffraction imaging: method for simultaneously reconstructing objects and probe using X-ray free-electron lasers.

PubMed

Hirose, Makoto; Shimomura, Kei; Suzuki, Akihiro; Burdet, Nicolas; Takahashi, Yukio

2016-05-30

The sample size must be less than the diffraction-limited focal spot size of the incident beam in single-shot coherent X-ray diffraction imaging (CXDI) based on a diffract-before-destruction scheme using X-ray free electron lasers (XFELs). This is currently a major limitation preventing its wider applications. We here propose multiple defocused CXDI, in which isolated objects are sequentially illuminated with a divergent beam larger than the objects and the coherent diffraction pattern of each object is recorded. This method can simultaneously reconstruct both objects and a probe from the coherent X-ray diffraction patterns without any a priori knowledge. We performed a computer simulation of the prposed method and then successfully demonstrated it in a proof-of-principle experiment at SPring-8. The prposed method allows us to not only observe broad samples but also characterize focused XFEL beams.

Eu2+,Dy3+ codoped SrAl2O4 nanocrystalline phosphor for latent fingerprint detection in forensic applications

NASA Astrophysics Data System (ADS)

Sharma, Vishal; Das, Amrita; Kumar, Vinay

2016-01-01

In this work, europium and dysprosium doped strontium aluminate (SrAl2O4:Eu2+,Dy3+) nanophosphor is synthesized and its novel application for the detection of latent fingerprints on various contact surfaces is reported. The SrAl2O4:Eu2+,Dy3+ is synthesized using a combustion method and shows long-lasting afterglow luminescence. The powder particles are characterized using field emission scanning electron microscopy (FE-SEM), SEM-energy dispersive x-ray analysis, x-ray diffraction and photoluminescence spectrophotometry. The FE-SEM image analysis reveals that the nanoparticles are mostly 8-15 nm in size with an irregular spherical shape. This nano-structured powder was applied to fresh and aged fingerprints deposited on porous, semi-porous and non-porous contact surfaces, such as ordinary colored paper, glossy paper, glass, aluminum foil, a yellow foil chocolate wrapper, a soft drink can, a PET bottle, a compact disc and a computer mouse. The results are reproducible and show great sensitivity and high contrast in the developed fingermark regions on these surfaces. These nanophosphor particles also show a strong and long-lasting afterglow property, making them a suitable candidate for use as a fingerprint developing agent on luminescent and highly patterned surfaces. These kinds of powders have shown that they can remove the interference from background luminescence, which is not possible using ordinary luminescent fingerprinting powders.

Angular rheology study of colloidal nanocrystals using Coherent X-ray Diffraction

NASA Astrophysics Data System (ADS)

Liang, Mengning; Harder, Ross; Robinson, Ian

2007-03-01

A new method using coherent x-ray diffraction provides a way to investigate the rotational motion of a colloidal suspension of crystals in real time. Coherent x-ray diffraction uses the long coherence lengths of synchrotron sources to illuminate a nanoscale particle coherently over its spatial dimensions. The penetration of high energy x-rays into various media allows for in-situ measurements making it ideal for suspensions. This technique has been used to image the structure of nanocrystals for some time but also has the capability of providing information about the orientation and dynamics of crystals. The particles are imaged in a specific diffraction condition allowing us to determine their orientation and observe how they rotate in real time with exceptional resolution. Such sensitivity allows for the study of rotational Brownian motion of nanocrystals in various suspensions and conditions. We present a study of the angular rheology of alumina and TiO2 colloidal nanocrystals in media using coherent x-ray diffraction.

Characterization of polycrystalline materials using synchrotron X-ray imaging and diffraction techniques

NASA Astrophysics Data System (ADS)

Ludwig, W.; King, A.; Herbig, M.; Reischig, P.; Marrow, J.; Babout, L.; Lauridsen, E. M.; Proudhon, H.; Buffière, J. Y.

2010-12-01

The combination of synchrotron radiation x-ray imaging and diffraction techniques offers new possibilities for in-situ observation of deformation and damage mechanisms in the bulk of polycrystalline materials. Minute changes in electron density (i.e., cracks, porosities) can be detected using propagation based phase contrast imaging, a 3-D imaging mode exploiting the coherence properties of third generation synchrotron beams. Furthermore, for some classes of polycrystalline materials, one may use a 3-D variant of x-ray diffraction imaging, termed x-ray diffraction contrast tomography. X-ray diffraction contrast tomography provides access to the 3-D shape, orientation, and elastic strain state of the individual grains from polycrystalline sample volumes containing up to thousand grains. Combining both imaging modalities, one obtains a comprehensive description of the materials microstructure at the micrometer length scale. Repeated observation during (interrupted) mechanical tests provide unprecedented insight into crystallographic and grain microstructure related aspects of polycrystalline deformation and degradation mechanisms.

Quantitative analysis of thoria phase in Th-U alloys using diffraction studies

NASA Astrophysics Data System (ADS)

Thakur, Shital; Krishna, P. S. R.; Shinde, A. B.; Kumar, Raj; Roy, S. B.

2017-05-01

In the present study the quantitative phase analysis of Th-U alloys in bulk form namely Th-52 wt% U and Th-3wt%U has been performed over the data obtained from both X ray diffraction and neutron diffraction technique using Rietveld method of FULLPROF software. Quantifying thoria (ThO2) phase present in bulk of the sample is limited due to surface oxidation and low penetration of x rays in high Z material. Neutron diffraction study probing bulk of the samples has been presented in comparison with x-ray diffraction study.

Selenium single-wavelength anomalous diffraction de novo phasing using an X-ray-free electron laser

DOE PAGES

Hunter, Mark S.; Yoon, Chun Hong; DeMirci, Hasan; ...

2016-11-04

Structural information about biological macromolecules near the atomic scale provides important insight into the functions of these molecules. To date, X-ray crystallography has been the predominant method used for macromolecular structure determination. However, challenges exist when solving structures with X-rays, including the phase problem and radiation damage. X-ray-free electron lasers (X-ray FELs) have enabled collection of diffraction information before the onset of radiation damage, yet the majority of structures solved at X-ray FELs have been phased using external information via molecular replacement. De novo phasing at X-ray FELs has proven challenging due in part to per-pulse variations in intensity andmore » wavelength. Here we report the solution of a selenobiotinyl-streptavidin structure using phases obtained by the anomalous diffraction of selenium measured at a single wavelength (Se-SAD) at the Linac Coherent Light Source. Finally, our results demonstrate Se-SAD, routinely employed at synchrotrons for novel structure determination, is now possible at X-ray FELs.« less

Macromolecular structures probed by combining single-shot free-electron laser diffraction with synchrotron coherent X-ray imaging.

PubMed

Gallagher-Jones, Marcus; Bessho, Yoshitaka; Kim, Sunam; Park, Jaehyun; Kim, Sangsoo; Nam, Daewoong; Kim, Chan; Kim, Yoonhee; Noh, Do Young; Miyashita, Osamu; Tama, Florence; Joti, Yasumasa; Kameshima, Takashi; Hatsui, Takaki; Tono, Kensuke; Kohmura, Yoshiki; Yabashi, Makina; Hasnain, S Samar; Ishikawa, Tetsuya; Song, Changyong

2014-05-02

Nanostructures formed from biological macromolecular complexes utilizing the self-assembly properties of smaller building blocks such as DNA and RNA hold promise for many applications, including sensing and drug delivery. New tools are required for their structural characterization. Intense, femtosecond X-ray pulses from X-ray free-electron lasers enable single-shot imaging allowing for instantaneous views of nanostructures at ambient temperatures. When combined judiciously with synchrotron X-rays of a complimentary nature, suitable for observing steady-state features, it is possible to perform ab initio structural investigation. Here we demonstrate a successful combination of femtosecond X-ray single-shot diffraction with an X-ray free-electron laser and coherent diffraction imaging with synchrotron X-rays to provide an insight into the nanostructure formation of a biological macromolecular complex: RNA interference microsponges. This newly introduced multimodal analysis with coherent X-rays can be applied to unveil nano-scale structural motifs from functional nanomaterials or biological nanocomplexes, without requiring a priori knowledge.

Exploration of New Principles in Spintronics Based on Topological Insulators (Option 1)

DTIC Science & Technology

2012-05-14

on the surface and found that our crystals are exceedingly homogeneous (Supplementary Information). The persistently narrow X - ray diffraction peaks...modified Bridgman method (see Supplementary Information for details). X - ray diffraction measurements indicated the monotonic shrinkage of a and c axis...and annealing at that temperature for 4 days. X - ray diffraction analyses confirmed that all the samples have the same crystal structure (R 3m

Efficient modeling of Bragg coherent x-ray nanobeam diffraction

DOE PAGES

Hruszkewycz, S. O.; Holt, M. V.; Allain, M.; ...

2015-07-02

X-ray Bragg diffraction experiments that utilize tightly focused coherent beams produce complicated Bragg diffraction patterns that depend on scattering geometry, characteristics of the sample, and properties of the x-ray focusing optic. In this paper, we use a Fourier-transform-based method of modeling the 2D intensity distribution of a Bragg peak and apply it to the case of thin films illuminated with a Fresnel zone plate in three different Bragg scattering geometries. Finally, the calculations agree well with experimental coherent diffraction patterns, demonstrating that nanodiffraction patterns can be modeled at nonsymmetric Bragg conditions with this approach—a capability critical for advancing nanofocused x-raymore » diffraction microscopy.« less

Biosensing applications of titanium dioxide coated graphene modified disposable electrodes.

PubMed

Kuralay, Filiz; Tunç, Selma; Bozduman, Ferhat; Oksuz, Lutfi; Oksuz, Aysegul Uygun

2016-11-01

In the present work, preparation of titanium dioxide coated graphene (TiO2/graphene) and the use of this nanocomposite modified electrode for electrochemical biosensing applications were detailed. The nanocomposite was prepared with radio frequency (rf) rotating plasma method which serves homogeneous distribution of TiO2 onto graphene. TiO2/graphene was characterized with scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) and X-ray diffraction (XRD) analysis. Then, this nanocomposite was dissolved in phosphate buffer solution (pH 7.4) and modified onto disposable pencil graphite electrode (PGE) by dip coating for the investigation of the biosensing properties of the prepared electrode. TiO2/graphene modified PGE was characterized with SEM, EDS and cyclic voltammetry (CV). The sensor properties of the obtained surface were examined for DNA and DNA-drug interaction. The detection limit was calculated as 1.25mgL(-1) (n=3) for double-stranded DNA (dsDNA). RSD% was calculated as 2.4% for three successive determinations at 5mgL(-1) dsDNA concentration. Enhanced results were obtained compared to the ones obtained with graphene and unmodified (bare) electrodes. Copyright © 2016 Elsevier B.V. All rights reserved.

Multifunctional AgNPs@Wool: colored, UV-protective and antioxidant functional textiles

NASA Astrophysics Data System (ADS)

Shabbir, Mohd; Mohammad, Faqeer

2018-02-01

Nanomaterials have great impact on textile industry for multifunctional and smart clothing as per the need of present, and further, green nanotechnology is the current hotspot of research and industrial developments. Silver nanoparticles (AgNPs) are synthesized (in situ) by using natural compounds of plant extracts (naphthoquinones, phenolics/flavonoids, polyphenols) as reducing or stabilizing agents, and simultaneously deposited on wool fabric for coloration, UV protection and antioxidant properties. UV-visible spectroscopy is used to monitor the route of biosynthesis of nanoparticles and transmission electron microscopy for morphological characteristics of synthesized AgNPs. Spherical and almost oval-shaped AgNPs were synthesized by naphthoquinones, polyphenols and flavonoids, respectively. Scanning electron microscopy (SEM) coupled with energy dispersive X-ray (EDX) spectroscopy, X-ray diffraction pattern (XRD) and Fourier transform infrared spectroscopy were used for the AgNPs@Wool fabrics characterization. SEM-EDX analysis and XRD patterns confirmed the successful deposition of silver nanoparticles on wool. Coloration characteristics in terms of color strength (K/S) and CIEL*a*b*c*h° values, UV protection abilities in terms of UV transmittance and UV protection factor, and % antioxidant activity of AgNPs@Wool are suggestive of good-to-excellent results.

Radiation-induced changes in electrical conductivity and structure of BaPbO3 after γ-irradiation

NASA Astrophysics Data System (ADS)

Shan, Qing; Cai, Pingkun; Zhang, Xinlei; Li, Jiatong; Chu, Shengnan; Jia, Wenbao

2015-11-01

Several barium plumbate (BaPbO3) solid samples, made from PbO and BaCO3 powder by chemistry liquid-phase coprecipitation, were investigated before and after γ-irradiation. The solid samples were irradiated by a 60Co γ-irradiation source whose dose rate is about 0.7 kGy per hour. The irradiation times were 0, 72, 144, 216, 288 and 360 h. Then, the four-probe method, X-ray diffraction (XRD), scanning electron microscope (SEM) and X-ray photoelectron spectroscopy (XPS) were used to indicate the changes in electrical conductivity and microstructure of BaPbO3 after γ-irradiation. The XRD results indicated that the content of PbO was reduced as the irradiation dose was increased and eventually vanished from the surface of samples. However, there was no new obvious substance phase found from the XRD atlas. It seems that the PbO transformed into nearly amorphous Pb5O8. The conjecture could be proved by the results of annealing experiment and SEM. The XPS results seem to show that the microstructure of BaPbO3 was slightly changed.

Structural properties and optical characterization of flower-like Mg doped NiO

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

Allaedini, Ghazaleh, E-mail: jiny-ghazaleh@yahoo.com; Tasirin, Siti Masrinda; Aminayi, Payam

In this study, un-doped and Mg doped NiO nanoparticles have been synthesized through a simple sol-gel method. To investigate the effect of Mg-doping on the structure of NiO, the obtained nanoparticles were characterized using scanning electron microscopy (SEM). Flower/star like morphology was clearly observed in the SEM micrographs. The BET (Brunauer-Emmett-Teller) nitrogen absorption isotherm exhibits high specific surface area (∼37 m{sup 2} /g) for the Mg doped NiO nanoparticles. X-Ray diffraction (XRD) of the prepared Mg-NiO nanoparticles showed a face-centered cubic (f.c.c) structure, and the average particle size was estimated to be 32 nm using Scherrer’s formula. Energy Dispersive X-Ray (EDX)more » confirms that the NiO particles are successfully doped with Mg. Photoluminescence (PL) and UV-Vis optical absorption characteristics of the prepared nanoparticles have also been investigated in this study. The PL emission response showed a blue shift when NiO was doped with Mg, which is indicative of interstitial oxygen. The UV-Vis results demonstrate a band gap increase as NiO nanoparticles are doped with Mg.« less

Combined effect of pulse electron beam treatment and thin hydroxyapatite film on mechanical features of biodegradable AZ31 magnesium alloy

NASA Astrophysics Data System (ADS)

Surmeneva, M. A.; Tyurin, A. I.; Teresov, A. D.; Koval, N. N.; Pirozhkova, T. S.; Shuvarin, I. A.; Surmenev, R. A.

2015-11-01

The morphology, elemental, phase composition, nanohardness, and Young's modulus of the hydroxyapatite (HA) coating deposited via radio frequency (RF) magnetron sputtering onto the AZ31 surface were investigated by atomic force microscopy (AFM), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), and nanoindentationtechniques. The calcium phosphate (Ca/P) molar ratio of the HA coating deposited via RF-magnetron sputtering onto AZ31 substrates according to EDX was 1.57+0.03. The SEM experiments revealed significant differences in the morphology of the HA film deposited on untreated and treated with the pulsed electron beam (PEB) AZ31 substrate. Nanoindentation studies demonstrated significant differences in the mechanical responses of the HA film deposited on the initial and PEB-modified AZ31 substrates. The nanoindentation hardness and the Young's modulus of the HA film on the magnesium alloy modified using the PEB treatment were higher than that of the HA layer on the untreated substrate. Moreover, the HA film fabricated onto the PEB-treated surface was more resistant to plastic deformation than the same film on the untreated AZ31 surface.

Structural and electrical properties of CZTS thin films by electrodeposition

NASA Astrophysics Data System (ADS)

Rao, M. C.; Basha, Sk. Shahenoor

2018-06-01

CZTS (Cu2ZnSnS4) thin films were coated on ITO glass substrates by single bath electrodeposition technique. The prepared films were subsequently characterized by XRD, SEM, FTIR, UV-visible spectroscopy and Raman studies. The thickness of the thin films was measured by wedge method. X-ray diffraction studies revealed the formation of polycrystalline phase. The morphological surface of the prepared thin films was examined by SEM and AFM and showed the presence of microcrystals on the surface of the samples. The elemental analysis and their compositional ratios present in the samples were confirmed by the energy dispersive X-ray analysis. Functional groups and the position of band structure involved in the materials were confirmed by FTIR. Optical absorption studies were performed on the prepared thin films in the wavelength ranging from 300 to 1000 nm and the energy bandgap values were found to be in the range from 1.39 to 1.60 eV. Raman spectral peak which was observed at 360 cm-1 correspond to kesterite phase, was formed due to the vibration of the molecules. Electrical measurements confirmed the nature of the thin film depending on the charge concentration present in the samples.

Polyamidoamine dendrimers-assisted electrodeposition of gold-platinum bimetallic nanoflowers.

PubMed

Qian, Lei; Yang, Xiurong

2006-08-24

Novel Au-Pt bimetallic flower nanostructures fabricated on a polyamidoamine dendrimers-modified surface by electrodeposition are reported. These polyamidoamine dendrimers were stable, and they assisted the formation of Au-Pt bimetallic nanoflowers during the electrodeposition process. These nanoflowers were characterized by field-emitted scanning electron microscopy (FE-SEM), energy-dispersive spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), X-ray diffraction, and electrochemical methods. FE-SEM images showed that the bimetallic nanoflower included two parts: the "light" and the "pale" part. The two parts consisted of many small bimetallic nanoparticles, which was attributed to the progressive nucleation process. Moreover, the "light" part contained more bimetallic nanoparticles. The morphologies of bimetallic nanoflowers depended on the electrodeposition time and potential and the layer number of assembled dendrimers. The average size of nanoflowers increased with the increase in electrodeposition time. The layer number of assembled dendrimers obviously affected the size and morphologies of the "pale" parts of deposited nanoflowers. EDS and XPS indicated that the content of Au element was higher than that of Pt element in the nanoflowers. The bimetallic nanoflowers-modified electrode had electrochemical properties similar to those of bare gold and platinum electrodes. It also exhibited significant electrocatalytic activities toward oxygen reduction.

Synthesis, Optical and Structural Properties of Copper Sulfide Nanocrystals from Single Molecule Precursors

PubMed Central

Ajibade, Peter A.; Botha, Nandipha L.

2017-01-01

We report the synthesis and structural studies of copper sulfide nanocrystals from copper (II) dithiocarbamate single molecule precursors. The precursors were thermolysed in hexadecylamine (HDA) to prepare HDA-capped CuS nanocrystals. The optical properties of the nanocrystals studied using UV–visible and photoluminescence spectroscopy showed absorption band edges at 287 nm that are blue shifted, and the photoluminescence spectra show emission curves that are red-shifted with respect to the absorption band edges. These shifts are as a result of the small crystallite sizes of the nanoparticles leading to quantum size effects. The structural studies were carried out using powder X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), and atomic force microscopy. The XRD patterns indicates that the CuS nanocrystals are in hexagonal covellite crystalline phases with estimated particles sizes of 17.3–18.6 nm. The TEM images showed particles with almost spherical or rod shapes, with average crystallite sizes of 3–9.8 nm. SEM images showed morphology with ball-like microspheres on the surfaces, and EDS spectra confirmed the presence of CuS nanoparticles. PMID:28336865

Wear Properties of ECAP-Processed AM80 Magnesium Alloy

NASA Astrophysics Data System (ADS)

Gopi, K. R.; Shivananda Nayaka, H.; Sahu, Sandeep

2017-07-01

AM80 magnesium alloy was subjected to equal-channel angular pressing (ECAP), and microstructural evolution was studied using scanning electron microscope (SEM). Grain size was found to decrease up to 3 µm after four passes. An increase in number of ECAP passes led to a corresponding increase in hardness of the processed samples. Unprocessed and ECAP-processed samples were subjected to wear test using pin-on-disk wear test machine to study the wear behavior. Effects of varying loads (30 and 40 N) with sliding distances (2500 and 5000 m) were studied. The results showed reduction in wear mass loss for the ECAP-processed samples in comparison with unprocessed condition. Coefficient of friction (COF) was studied for different loads, and improvement in COF values was observed for ECAP-processed samples compared to unprocessed condition. Worn surfaces were studied using SEM and energy-dispersive x-ray spectrometer, and they exhibited plastic deformation, delamination, plowing, wear debris and oxidation in the sliding direction. X-ray diffraction analysis was conducted on the worn surfaces to identify the phases. It revealed the presence of magnesium oxide and magnesium aluminum oxide which led to oxidation wear in the sliding direction. Wear mechanism was found to be abrasive and oxidation wear.

Structural studies on the substitution of Ag, Na doped LCSMO CMR manganites

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

Subhashini, P., E-mail: subhashinisvu@gmail.com; Krishnaiah, M.; Munirathinam, B.

2016-05-06

Synthesis and characterization of colossal magnetoresistance (CMR) materials has been a subject of scientific research due to the unique transport, magnetotransport, and magnetic properties. The single phase polycrystalline La{sub 0.7}Ca{sub 0.1}Sr{sub 0.1}M{sub 0.1}MnO{sub 3} (LCSMO) (M=Ag and Na) samples prepared using nitrate route method. The structural properties are studied at different dopants by X-ray diffraction. The surface morphology and elemental analysis of both samples were carried out by scanning electron microscopy (SEM) and energy dispersive X-ray technique (EDAX) respectively. The structural analysis shows that the LCSMO is crystallized in an orthorhombic perovskite structure belonging to Pnma space group. The crystalmore » size of the sample is calculated using Scherrer formula. The SEM images show that the polycrystalline grains are observed to be near spherical shape and uniform in size. EDAX spectra taken from the surface of the synthesized powders show a nominal composition near the desired one for M=Na sample where as some vacancies are present in the A-site in the case of Ag substitution as will be discussed in this paper.« less

Preparation and Properties of Surface-Coated HMX with Viton and Graphene Oxide

NASA Astrophysics Data System (ADS)

Wang, Jingyu; Ye, Baoyun; An, Chongwei; Wu, Bidong; Li, Hequn; Wei, Yanju

2016-07-01

To improve the safety performance of HMX (octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine) particles, the new carbon material graphene oxide (GO) and Viton were used to coat HMX via a solvent-slurry process. For comparison, the HMX/Viton/graphite (HMX/Viton/G) and HMX/Viton composites were also prepared by the same process. Atomic force microscopy (AFM), scanning electron microscopy (SEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and differential scanning calorimetry (DSC) were employed to characterize the morphology, composition, and thermal decomposition of samples. The impact sensitivity and shock wave sensitivity of HMX-based composites were also measured and analyzed. The results of SEM, XRD, and XPS indicate that the cladding layer of HMX-based composites is successfully constructed. HMX/Viton/GO composites exhibit better thermal stability compared to HMX and HMX/Viton. The results show that both impact and shock wave sensitivities of HMX/Viton/GO composites are much lower than that of HMX/Viton. In addition, GO sheets exhibit a better desensitizing effect than G sheets. These combined properties suggest that nano-GO has good compatibility with explosives and can be utilized as a desensitizer in HMX particles.

Effects of (Ce, Cu) Co-doping on the Structural and Optical Properties of ZnO Aerogels Synthesized in Supercritical Ethanol

NASA Astrophysics Data System (ADS)

Djouadi, D.; Slimi, O.; Hammiche, L.; Chelouche, A.; Touam, T.

2018-03-01

Undoped, Ce-doped, Cu-doped and (Ce,Cu ) co-doped ZnO aerogels were synthesized by sol-gel process in supercritical conditions of ethanol. [Cu]/[Zn] and [Ce]/[Zn] atomic ratios were fixed at 0.02 (2%). The aerogels were investigated without any additional treatments by using X-ray diffraction (XRD), UV–visible spectrophotometry, scanning electron microscopy (SEM), Energy-dispersive X-ray spectroscopy (EDS), Fourier transforms infrared spectroscopy (FTIR) and photoluminescence spectroscopy (PL). XRD results revealed that all the samples are well crystallized in hexagonal wurtzite structure. EDS measurements showed that highly pure aerogels are prepared. SEM analysis indicated that the morphology of the samples is dependent on Cu and Ce dopants. From UV-visible spectroscopy analyses, it was shown that the absorption and the band gap of the aerogels are strongly affected by Ce and Cu dopants. FTIR spectra demonstrated that co-doping induces a shift of Zn-O bond vibration band toward low wavenumbers. The room temperature photoluminescence spectra put into evidence that the visible emission intensity is influenced by Ce and Cu doping. In particular, the co-doping leads to the appearance of a blue emission band at 443 nm.

Ultrasonic-assisted synthesis of ZrO2 nanoparticles and their application to improve the chemical stability of Nafion membrane in proton exchange membrane (PEM) fuel cells.

PubMed

Taghizadeh, Mohammad Taghi; Vatanparast, Morteza

2016-12-01

Zirconium dioxide (ZrO2) nanoparticles were fabricated successfully via ultrasonic-assisted method using ZrO(NO3)2·H2O, ethylenediamine and hydrazine as precursors in aqueous solution. Morphology, structure and composition of the obtained products were characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), dynamic light scattering (DLS), Fourier transform infrared spectroscopy (FT-IR) and diffuse reflectance spectroscopy (DRS). Then, the synthesized nanoparticles were used to prepare Nafion/ZrO2 nanocomposite membranes. The properties of the membranes were studied by ion exchange capacity (IEC) proton conductivity (σ), thermal stability and water uptake measurements. The ex-situ Fenton's test was used to investigate the chemical stability of the membranes. From our results, compared with Nafion membrane, the nanocomposite membrane exhibited lower fluoride release and weight loss. Therefore, it can concluded that Nafion/ZrO2 nanocomposite exhibit more chemical stability than the pure Nafion membrane. ATR-FTIR spectra and SEM surface images of membranes also confirm these results. Copyright © 2016 Elsevier Inc. All rights reserved.

Influence of a novel co-doping (Zn + F) on the physical properties of nano structured (1 1 1) oriented CdO thin films applicable for window layer of solar cell

NASA Astrophysics Data System (ADS)

Anitha, M.; Saravanakumar, K.; Anitha, N.; Amalraj, L.

2018-06-01

Un-doped and co-doped (Zn + F) cadmium oxide (CdO) thin films were prepared by modified spray pyrolysis technique using a nebulizer on glass substrates kept at 200 °C. They were characterized by X-ray diffraction (XRD), X-ray photoelectron spectra (XPS), scanning electron microscopy (SEM), UV-vis spectroscopy, Hall Effect and photoluminescence (PL) respectively. The thin films were having thickness in the range of 520-560 nm. They were well crystalline and displayed high transparency of about >70% in the visible region. It was clearly seen from the SEM photographs that co-doping causes notable changes in the surface morphology. Electrical study exhibited the resistivity of co-doped CdO thin films drastically fell to 1.43 × 10-4 Ω-cm compared with the un-doped CdO thin film. The obtained PL spectra were well corroborated with the structural and optical studies. The high transparency, wide band gap energy and enhanced electrical properties obtained infer that Zn + F co-doped CdO thin films find application in optoelectronic devices, especially in window layer of solar cells.

Additive assisted hydrothermal synthesis, characterization and optical properties of one dimensional DyPO4:Ce3+ nanostructures

NASA Astrophysics Data System (ADS)

Khajuria, H.; Kumar, M.; Singh, R.; Ladol, J.; Nawaz Sheikh, H.

2018-05-01

One dimensional nanostructures of cerium doped dysprosium phosphate (DyPO4:Ce3+) were synthesized via hydrothermal route in the presence of different surfactants [sodium dodecyl sulfate (SDS), dodecyl sulfosuccinate (DSS), polyvinyl pyrollidone (PVP)] and solvent [ethylene glycol and water]. The prepared nanostructures were characterized by Powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FTIR), Field emission scanning electron microscopy (FE-SEM), Transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), UV-VIS-NIR absorption spectrophotometer and photoluminescence (PL) studies. The PXRD and FTIR results indicate purity, good crystallinity and effective doping of Ce3+ in nanostructures. SEM and TEM micrographs display nanorods, nanowires and nanobundles like morphology of DyPO4:Ce3+. Energy-dispersive X-ray spectra (EDS) of DyPO4:Ce3+nanostructures confirm the presence of dopant. UV-VIS-NIR absorption spectra of prepared compounds are used to calculate band gap and explore their optical properties. Luminescent properties of DyPO4:Ce3+ was studied by using PL emission spectra. The effect of additives and solvents on the uniformity, morphology and optical properties of the nanostructures were studied in detail.

Synthesis, characterization and antimicrobial activity of dextran sulphate stabilized silver nanoparticles

NASA Astrophysics Data System (ADS)

Cakić, Milorad; Glišić, Slobodan; Nikolić, Goran; Nikolić, Goran M.; Cakić, Katarina; Cvetinov, Miroslav

2016-04-01

Dextran sulphate stabilized silver nanoparticles (AgNPs - DS) were synthesized from aqueous solution of silver nitrate (AgNO3) and dextran sulphate sodium salt (DS). The characterization of AgNPs - DS was performed by ultraviolet-visible spectroscopy (UV-VIS), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and antimicrobial activity. The formation of AgNPs - DS was monitored by colour changes of the reaction mixture from yellowish to brown and by measuring the surface plasmon resonance absorption peak in UV-VIS spectra at 420 nm. The SEM analysis was used for size and shape determination of AgNPs - DS. The presence of elemental silver and its crystalline structure in AgNPs - DS were confirmed by EDX and XRD analyses. The possible functional groups of DS responsible for the reduction and stabilization of AgNPs were determinated by FTIR spectroscopy. The AgNPs - DS showed strong antibacterial activity against Staphylococcus aureus ATCC 25923, Bacillus cereus ATCC 11778, Bacillus luteus in haus strain, Bacillus subtilis ATTC 6633, Listeria monocytogenes ATCC 15313, Escherichia coli ATTC 25922, Pseudomonas aeruginosa ATTC 27853, Klebsiella pneumoniae ATTC 700603, Proteus vulgaris ATTC 8427, and antifungal activity against Candida albicans ATTC 2091.

Chemical synthesis of hierarchical NiCo2S4 nanosheets like nanostructure on flexible foil for a high performance supercapacitor.

PubMed

Kim, D -Y; Ghodake, G S; Maile, N C; Kadam, A A; Sung Lee, Dae; Fulari, V J; Shinde, S K

2017-08-29

In this study, hierarchical interconnected nickel cobalt sulfide (NiCo 2 S 4 ) nanosheets were effectively deposited on a flexible stainless steel foil by the chemical bath deposition method (CBD) for high-performance supercapacitor applications. The resulting NiCo 2 S 4 sample was characterized by X-ray powder diffraction (XRD), field emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HR-TEM), and electrochemical measurements. XRD and X-ray photoelectron spectroscopy (XPS) results confirmed the formation of the ternary NiCo 2 S 4 sample with a pure cubic phase. FE-SEM and HR-TEM revealed that the entire foil surface was fully covered with the interconnected nanosheets like surface morphology. The NiCo 2 S 4 nanosheets demonstrated impressive electrochemical characteristics with a specific capacitance of 1155 F g -1 at 10 mV s -1 and superior cycling stability (95% capacity after 2000 cycles). These electrochemical characteristics could be attributed to the higher active area and higher conductivity of the sample. The results demonstrated that the interconnected NiCo 2 S 4 nanosheets are promising as electrodes for supercapacitor and energy storage applications.

Simple solution-combustion synthesis of Ni-NiO@C nanocomposites with highly electrocatalytic activity for methanol oxidation

NASA Astrophysics Data System (ADS)

Yu, Jie; Ni, Yonghong; Zhai, Muheng

2018-01-01

Transition metal and its oxide composite nanomaterials are attracting increasing research interest due to their superior properties and extensive applications in many fields. In this paper, Ni-NiO@C nanocomposites were successfully synthesized in one step via a simple solution-combustion route, employing NiCl2 as the Ni source, oxygen in the atmosphere as the oxygen source, and ethanol as the solvent. The final product was characterized by powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (EDS), (high resolution) transmission electron microscopy (TEM/HRTEM), and Raman spectra. N2 gas sorption-desorption experiments uncovered that the BET surface area of Ni-NiO@C nanocomposites reached 161.9 m2 g-1, far higher than 34.2 m2 g-1 of Ni-NiO. The electrochemical measurement showed that the as-produced Ni-NiO@C nanocomposites presented better catalytic activity for the electro-oxidation of methanol than Ni-NiO and NiO, which provides a new catalyst selection for the electro-oxidation of methanol.

Structural, photoconductivity, and dielectric studies of polythiophene-tin oxide nanocomposites

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

Murugavel, S., E-mail: starin85@gmail.com; Malathi, M., E-mail: mmalathi@vit.ac.in

2016-09-15

Highlights: • Synthesis of polythiophene-tin oxide nanocomposites confirmed by FTIR and EDAX. • SEM shows SnO{sub 2} nanoparticles embedded within polythiophene matrix. • Stability and isoelectric point suggest nanoparticle–matrix interaction. • High dielectric constant due to high Maxwell–Wagner interfacial polarization. - Abstract: Polythiophene-tinoxide (PT-SnO{sub 2}) nanocomposites were prepared by in situ chemical oxidative polymerization, in the presence of various concentrations of SnO{sub 2} nanoparticles. Samples were characterized by X-ray diffraction, Fourier-transform infrared spectroscopy, thermogravimetric analysis, X-ray photoelectron spectroscopy and Zeta potential measurements. Morphologies and elemental compositions were investigated by transmission electron microscopy, field-emission scanning electron microscopy and energy-dispersive X-ray spectroscopy.more » The photoconductivity of the nanocomposites was studied by field-dependent dark and photo conductivity measurements. Their dielectric properties were investigated using dielectric spectroscopy, in the frequency range of 1kHz–1 MHz. The results indicated that the SnO{sub 2} nanoparticles in the PT-SnO{sub 2} nanocomposite were responsible for its enhanced dielectric performance.« less

Electrospinning Hetero-Nanofibers In2O3/SnO2 of Homotype Heterojunction with High Gas Sensing Activity

PubMed Central

Du, Haiying; Yao, PengJun; Sun, Yanhui; Wang, Jing; Wang, Huisheng; Yu, Naisen

2017-01-01

In2O3/SnO2 composite hetero-nanofibers were synthesized by an electrospinning technique for detecting indoor volatile organic gases. The physical and chemical properties of In2O3/SnO2 hetero-nanofibers were characterized and analyzed by X-ray diffraction (XRD), field emission scanning electron microscope (FE-SEM), Energy Dispersive X-Ray Spectroscopy (EDX), specific surface Brunauer–Emmett–Teller (BET) and X-ray photoelectron spectroscopy (XPS). Gas sensing properties of In2O3/SnO2 composite hetero-nanofibers were measured with six kinds of indoor volatile organic gases in concentration range of 0.5~50 ppm at the operating temperature of 275 °C. The In2O3/SnO2 composite hetero-nanofibers sensor exhibited good formaldehyde sensing properties, which would be attributed to the formation of n-n homotype heterojunction in the In2O3/SnO2 composite hetero-nanofibers. Finally, the sensing mechanism of the In2O3/SnO2 composite hetero-nanofibers was analyzed based on the energy-band principle. PMID:28792433

Attenuation of encrustation by self-assembled inorganic fullerene-like nanoparticles.

PubMed

Ron, Racheli; Zbaida, David; Kafka, Ilan Z; Rosentsveig, Rita; Leibovitch, Ilan; Tenne, Reshef

2014-05-21

Ureteral stents and urethral catheters are commonly used medical devices for maintaining urinary flow. However, long-term placement (>30 days) of these devices in the urinary tracts is limited by the development of encrustation, a phenomenon that holds a prevalence of 50% within this patient population, resulting in a great deal of morbidity to the patients. Here we report the influence of surface coating of an all-silicone catheter with rhenium-doped fullerene-like molybdenum disulfide (Re:IF-MoS2) nanoparticles on the growth and attachment of in vitro encrustation stones. Scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS) and X-ray powder diffraction (XRD) analyses indicated a remarkable attenuation in encrustation occupation on the Re:IF-MoS2-coated catheter surfaces compared to neat catheters. The doped nanoparticles displayed a unique tendency to self-assemble into mosaic-like arrangements, modifying the surface to be encrustation-repellent. The mechanism of encrustation retardation on the surface coated catheters is discussed in some detail. The ramification of these results for the clogging of other body indwelling devices is briefly discussed.

Characterization of Detonation Soot Produced During Steady and Overdriven Conditions for Three High Explosive Formulations

NASA Astrophysics Data System (ADS)

Podlesak, David; Amato, Ronald; Dattelbaum, Dana; Firestone, Millicent; Gustavsen, Richard; Huber, Rachel; Ringstrand, Bryan

2015-06-01

The detonation of high explosives (HE) produces a dense fluid of molecular gases and solid carbon. The solid detonation carbon contains various carbon allotropes such as detonation nanodiamonds, ``onion-like'' carbon, graphite and amorphous carbon, with the formation of the different forms dependent upon pressure, temperature and the environmental conditions of the detonation. We have collected solid carbon residues from controlled detonations of three HE formulations (Composition B-3, PBX 9501, and PBX 9502). Soot was collected from experiments designed to produce both steady and overdriven conditions, and from detonations in both an ambient (air) atmosphere and in an inert Ar atmosphere. Structural studies to glean the features of the solid carbon products have been performed using scanning electron microscopy (SEM), transmission electron microscopy (TEM), powder X-ray diffraction (XRD), Raman spectroscopy, small-angle X-ray scattering (SAXS), and X-Ray Pair Distribution Function measurements (PDF). Bulk soot was also analyzed for elemental and isotopic compositions. We will discuss differences in the structure and composition of the detonation carbon as a function of formulation, detonation conditions, and the surrounding atmosphere.

Novel Bi/BiOBr/AgBr composite microspheres: Ion exchange synthesis and photocatalytic performance

NASA Astrophysics Data System (ADS)

Lyu, Jianchang; Li, Zhenlu; Ge, Ming

2018-06-01

Novel Bi/BiOBr/AgBr composite microspheres were prepared by a rational in situ ion exchange reaction between Bi/BiOBr microspheres and AgNO3. The characteristic of the as-obtained ternary microspheres was tested by X-ray diffraction (XRD), energy dispersive X-ray spectrometer (EDS), scanning electron microscope (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectroscopy (UV-vis DRS) and photoluminescence (PL). Under visible light irradiation, Bi/BiOBr/AgBr microspheres exhibited an excellent photocatalytic efficiency for rhodamine B (RhB) degradation, which was about 1.4 and 4.9 times as high as that of Bi/BiOBr and BiOBr/AgBr, demonstrating that the highest separation efficiency of charge carriers in the heterostructured Bi/BiOBr/AgBr. The photocatalytic activity of Bi/BiOBr/AgBr microspheres just exhibited a slight decrease after three consecutive cycles. The photocatalytic mechanism investigation confirmed that the superoxide radicals (O2•-) were the dominant reactive oxygen species for RhB degradation in Bi/BiOBr/AgBr suspension.

Preparation of Ag/AgCl/BiMg{sub 2}VO{sub 6} composite and its visible-light photocatalytic activity

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

Guo, Rui; Zhang, Gaoke, E-mail: gkzhang@whut.edu.cn; Liu, Jiu

2013-05-15

Graphical abstract: - Abstract: A novel composite photocatalyst Ag/AgCl/BiMg{sub 2}VO{sub 6} was synthesized by depositing Ag/AgCl nanoparticles on BiMg{sub 2}VO{sub 6} substrate via a precipitation–photoreduction method and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray analysis (EDXA), X-ray photoelectron spectroscopy (XPS) and UV–vis diffuse reflectance spectrophotometer (UV–vis DRS). The photocatalyst showed high and stable photocatalytic activity for photocatalytic degradation of acid red G under visible-light irradiation (λ > 420 nm). In addition, the active ·O{sub 2}{sup −} and h{sup +}, as main reactive species, played the major roles during the reaction process.more » The high photocatalytic activity of the composite may be related to the efficient electron–hole pairs separation at the photocatalyst interfaces, as well as the surface plasmon resonance of Ag nanoparticles formed on AgCl particles in the degradation reaction.« less

Effect of the microstructure on the thermoelectric properties of polycrystalline lanthanum chalcogenides

NASA Technical Reports Server (NTRS)

Lockwood, A.; Wood, C.; Vandersande, J.; Zoltan, A.; Parker, J.; Danielson, L.; Alexander, M.; Whittenberger, D.

1987-01-01

Small amounts of second phase materials can have important effects on the thermoelectric properties of polycrystalline gamma-La(3-x)X4 (X-S, Te; X in the range of 0 to 1/3). Microscopic examination by SEM of hot pressed La(3-x)Te4 samples has revealed from 1-5 vol. pct of La2O2Te, an amount which is not detected by X-ray powder diffraction measurements. This amount of La2O2Te resulting from oxygen contamination can reduce the concentration of electrons by as much as 10 to 75 percent below the electron concentration calculated for single phase La(3-x)Te4 in the composition range of greatest interest. Small amounts of second phase materials can also lower the lattice thermal conductivity by scattering low frequency phonons. These results indicate that microstructural effects should be considered when electrical and thermal properties of polycrystalline materials are analyzed.

Influence of La-Mn substitutions on magnetic properties of M-type strontium hexaferrites

NASA Astrophysics Data System (ADS)

Zi, Z. F.; Ma, X. H.; Wei, Y. Y.; Liu, Q. C.; Zhang, M.; Zhu, X. B.; Sun, Y. P.

2018-05-01

M-type strontium hexaferrites of Sr1-xLaxFe12-xMnxO19 (0.0≤x≤0.4) were synthesized by the chemical coprecipitation method. X-ray diffraction (XRD) studies indicate that the samples are single-phase with the space group of P63/mmc. The results of field-emission scanning electronic microscopy (FE-SEM) show that the grains are regular hexagonal platelets with sizes from 0.7 to 1.4 μm. It is observed that the value of Hc increases at low substitution (x ≤ 0.1), reaches a maximum at x = 0.1 and then decreases at x ≥ 0.1, while the value of Ms decreases monotonously with increasing x. The variations of magnetic properties can be tentatively attributed to the effects of La-Mn substitutions. The results above indicate that our samples might be promising candidates for permanent magnets in the future.

HiSPoD: a program for high-speed polychromatic X-ray diffraction experiments and data analysis on polycrystalline samples

DOE PAGES

Sun, Tao; Fezzaa, Kamel

2016-06-17

Here, a high-speed X-ray diffraction technique was recently developed at the 32-ID-B beamline of the Advanced Photon Source for studying highly dynamic, yet non-repeatable and irreversible, materials processes. In experiments, the microstructure evolution in a single material event is probed by recording a series of diffraction patterns with extremely short exposure time and high frame rate. Owing to the limited flux in a short pulse and the polychromatic nature of the incident X-rays, analysis of the diffraction data is challenging. Here, HiSPoD, a stand-alone Matlab-based software for analyzing the polychromatic X-ray diffraction data from polycrystalline samples, is described. With HiSPoD,more » researchers are able to perform diffraction peak indexing, extraction of one-dimensional intensity profiles by integrating a two-dimensional diffraction pattern, and, more importantly, quantitative numerical simulations to obtain precise sample structure information.« less

Synthesis of NiS-Graphene Nanocomposites and its Electrochemical Performance for Supercapacitors

NASA Astrophysics Data System (ADS)

Pandey, Chandan Abhishek; Ravuri, Syamsai; Ramachandran, R.; Santhosh, R.; Ghosh, Sourav; Sitaraman, S. R.; Grace, Andrews Nirmala

The aim of this work is to synthesize nickel sulfide-graphene (NiS/G) nanocomposites with different compositions and to analyze the structural and electrochemical capacity and compatibility for their application as supercapacitor material with enhanced charge storage capacity and reduced impedance. NiS nanoparticles (NPs) loaded on graphene were synthesized at various concentrations of graphene by a simple hydrothermal route from nickel sulphate and graphene oxide as precursors in the presence of PVP as surfactant and thioacetamide (TAA) as sulfur source. The composites structural, morphological and physical properties were analyzed by X-ray diffraction (XRD), Field Emission Scanning Electron Microscopy (FE-SEM), Energy-dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy (XPS) and Fourier Transform-infrared (FT-IR) analysis. SEM measurements showed the presence of surface attachment of the NiS NPs onto the graphene sheets. To assess the properties of the nanocomposites for their applicability in supercapacitors, electrochemical analysis was carried out in 6M KOH electrolyte. Three different samples with different graphene contents — GNiS-10 with 10 wt.%, GNiS-20 with 20 wt.% and GNiS-40 with 40 wt.% were prepared. The specific capacitances obtained for the nanocomposites were calculated to be 84.33F/g, 129.66F/g, 187.53F/g at 10mV/s scan rate, respectively. The EIS data showed that the loading of NiS NPs on graphene caused the reduction in impedance at high frequency and has a long cycle life (over 1000 cycles).

Hierarchical MnO2 nanosheets synthesized via electrodeposition-hydrothermal method for supercapacitor electrodes

NASA Astrophysics Data System (ADS)

Zheng, Dongdong; Qiang, Yujie; Xu, Shenying; Li, Wenpo; Yu, Shanshan; Zhang, Shengtao

2017-02-01

Metal oxides have emerged as one kind of important supercapacitor electrode materials. Herein, we report hierarchical MnO2 nanosheets prepared of indium tin oxide (ITO) coated glass substrates via a hybrid two-step protocol, including a cathodic electrodeposition technique and a hydrothermal process. The samples are characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscope (SEM) with energy dispersive X-ray spectroscopy (EDX), and transmission electron microscope (TEM). SEM and TEM images show that the as-synthesized MnO2 nanosheets are hierarchical and porous, which could increase the active surface and short paths for fast ion diffusion. The results of nitrogen adsorption-desorption analysis indicate that the BET surface area of the MnO2 nanosheets is 53.031 m2 g-1. Furthermore, the electrochemical properties of the MnO2 are elucidated by cyclic voltammograms (CV), galvanostatic charge-discharge (GCD) tests, and electrochemical impedance spectroscopy (EIS) in 0.1 M Na2SO4 electrolyte. The electrochemical results demonstrate that the as-grown MnO2 nanosheet exhibits an excellent specific capacitance of 335 F g-1 at 0.5 A g-1 when it is applied as a potential electrode material for an electrochemical supercapacitor. Additionally, the MnO2 nanosheet electrode also presents high rate capability and good cycling stability with 91.8% retention after 1000 cycles. These excellent properties indicate that the hierarchical MnO2 nanosheets are a potential electrode material for electrochemical supercapacitors.

X-ray diffraction and X-ray standing-wave study of the lead stearate film structure

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

Blagov, A. E.; Dyakova, Yu. A.; Kovalchuk, M. V.

2016-05-15

A new approach to the study of the structural quality of crystals is proposed. It is based on the use of X-ray standing-wave method without measuring secondary processes and considers the multiwave interaction of diffraction reflections corresponding to different harmonics of the same crystallographic reflection. A theory of multiwave X-ray diffraction is developed to calculate the rocking curves in the X-ray diffraction scheme under consideration for a long-period quasi-one-dimensional crystal. This phase-sensitive method is used to study the structure of a multilayer lead stearate film on a silicon substrate. Some specific structural features are revealed for the surface layer ofmore » the thin film, which are most likely due to the tilt of the upper layer molecules with respect to the external normal to the film surface.« less

Molybdenum cell for x-ray diffraction measurements of fluid alkali metals at high temperatures and high pressures

NASA Astrophysics Data System (ADS)

Matsuda, Kazuhiro; Tamura, Kozaburo; Katoh, Masahiro; Inui, Masanori

2004-03-01

We have developed a sample cell for x-ray diffraction measurements of fluid alkali metals at high temperatures and high pressures. All parts of the cell are made of molybdenum which is resistant to the chemical corrosion of alkali metals. Single crystalline molybdenum disks electrolytically thinned down to 40 μm were used as the walls of the cell through which x rays pass. The crystal orientation of the disks was controlled in order to reduce the background from the cell. All parts of the cell were assembled and brazed together using a high-temperature Ru-Mo alloy. Energy dispersive x-ray diffraction measurements have been successfully carried out for fluid rubidium up to 1973 K and 16.2 MPa. The obtained S(Q) demonstrates the applicability of the molybdenum cell to x-ray diffraction measurements of fluid alkali metals at high temperatures and high pressures.

High-resolution ab initio three-dimensional x-ray diffraction microscopy

DOE PAGES

Chapman, Henry N.; Barty, Anton; Marchesini, Stefano; ...

2006-01-01

Coherent x-ray diffraction microscopy is a method of imaging nonperiodic isolated objects at resolutions limited, in principle, by only the wavelength and largest scattering angles recorded. We demonstrate x-ray diffraction imaging with high resolution in all three dimensions, as determined by a quantitative analysis of the reconstructed volume images. These images are retrieved from the three-dimensional diffraction data using no a priori knowledge about the shape or composition of the object, which has never before been demonstrated on a nonperiodic object. We also construct two-dimensional images of thick objects with greatly increased depth of focus (without loss of transverse spatialmore » resolution). These methods can be used to image biological and materials science samples at high resolution with x-ray undulator radiation and establishes the techniques to be used in atomic-resolution ultrafast imaging at x-ray free-electron laser sources.« less

Enhancing resolution in coherent x-ray diffraction imaging.

PubMed

Noh, Do Young; Kim, Chan; Kim, Yoonhee; Song, Changyong

2016-12-14

Achieving a resolution near 1 nm is a critical issue in coherent x-ray diffraction imaging (CDI) for applications in materials and biology. Albeit with various advantages of CDI based on synchrotrons and newly developed x-ray free electron lasers, its applications would be limited without improving resolution well below 10 nm. Here, we review the issues and efforts in improving CDI resolution including various methods for resolution determination. Enhancing diffraction signal at large diffraction angles, with the aid of interference between neighboring strong scatterers or templates, is reviewed and discussed in terms of increasing signal-to-noise ratio. In addition, we discuss errors in image reconstruction algorithms-caused by the discreteness of the Fourier transformations involved-which degrade the spatial resolution, and suggest ways to correct them. We expect this review to be useful for applications of CDI in imaging weakly scattering soft matters using coherent x-ray sources including x-ray free electron lasers.

A portable X-ray diffraction apparatus for in situ analyses of masters' paintings

NASA Astrophysics Data System (ADS)

Eveno, Myriam; Duran, Adrian; Castaing, Jacques

2010-09-01

It is rare that the analyses of materials in paintings can be carried out by taking micro-samples. Valuable works of art are best studied in situ by non-invasive techniques. For that purpose, a portable X-ray diffraction and fluorescence apparatus has been designed and constructed at the C2RMF. This apparatus has been used for paintings of Rembrandt, Leonardo da Vinci, Van Gogh, Mantegna, etc. Results are given to illustrate the performance of X-ray diffraction, especially when X-ray fluorescence does not bring sufficient information to conclude.

X-ray fractography on fatigue fractured surface of austenitic stainless steel

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

Yajima, Zenjiro; Tokuyama, Hideki; Kibayashi, Yasuo

1995-12-31

X-ray diffraction observation of the material internal structure beneath fracture surfaces provide fracture analysis with useful information to investigate the conditions and mechanisms of fracture. X-ray fractography is a generic name given to this technique. In the present study, X-ray fractography was applied to fatigue fracture surfaces of austenitic stainless steel (AISI 304) which consisted of solution treatment. The fatigue tests were carried out on compact tension (CT) specimens. The plastic strain on the fracture surface was estimated from measuring the line broadening of X-ray diffraction profiles. The line broadening of X-ray diffraction profiles was measured on and beneath fatiguemore » fracture surfaces. The depth of the plastic zone left on fracture surfaces was evaluated from the line broadening. The results are discussed on the basis of fracture mechanics.« less

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.

Diffraction and Imaging Study of Imperfections of Protein Crystals with Coherent X-rays

NASA Technical Reports Server (NTRS)

Hu, Z. W.; Thomas, B. R.; Chernov, A. A.; Chu, Y. S.; Lai, B.

2004-01-01

High angular-resolution x-ray diffraction and phase contrast x-ray imaging were combined to study defects and perfection of protein crystals. Imperfections including line defects, inclusions and other microdefects were observed in the diffraction images of a uniformly grown lysozyme crystal. The observed line defects carry distinct dislocation features running approximately along the <110> growth front and have been found to originate mostly in a central growth area and occasionally in outer growth regions. Slow dehydration led to the broadening of a fairly symmetric 4 4 0 rocking curve by a factor of approximately 2.6, which was primarily attributed to the dehydration-induced microscopic effects that are clearly shown in diffraction images. X-ray imaging and diffraction characterization of the quality of apoferritin crystals will also be discussed in the presentation.

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.

THE EFFECT OF SATELLITE LINES FROM THE X-RAY SOURCE ON X-RAY DIFFRACTION PEAKS

EPA Science Inventory

The article discusses the development of a method for relating reactivity to crystallite size and strain parameters obtained by the Warren-Averbach technique. EPA has been using crystallite size and strain data obtained from x-ray diffraction (XRD) peak profile analysis to predic...

History and Solution of the Phase Problem in theTheory of Structure Determination of Crystals from X-ray Diffraction Experiments

ScienceCinema

Wolf, Emil [University of Rochester, Rochester, New York, United States

2017-12-09

Since the pioneering work of Max von Laue on interference and diffraction of x-rays, carried out almost 100 years ago, numerous attempts have been made to determine structures of crystalline media from x-ray diffraction experiments. The usefulness of all of them has been limited by the inability of measuring phases of the diffracted beams. In this talk, the most important research carried out in this field will be reviewed and a recently obtained solution of the phase problem will be presented.

XRayView: a teaching aid for X-ray crystallography.

PubMed

Phillips, G N

1995-10-01

A software package, XRayView, has been developed that uses interactive computer graphics to introduce basic concepts of x-ray diffraction by crystals, including the reciprocal lattice, the Ewald sphere construction, Laue cones, the wavelength dependence of the reciprocal lattice, primitive and centered lattices and systematic extinctions, rotation photography. Laue photography, space group determination and Laue group symmetry, and the alignment of crystals by examination of reciprocal space. XRayView is designed with "user-friendliness" in mind, using pull-down menus to control the program. Many of the experiences of using real x-ray diffraction equipment to examine crystalline diffraction can be simulated. Exercises are available on-line to guide the users through many typical x-ray diffraction experiments.

Application of MEMS-based x-ray optics as tuneable nanosecond choppers

NASA Astrophysics Data System (ADS)

Chen, Pice; Walko, Donald A.; Jung, Il Woong; Li, Zhilong; Gao, Ya; Shenoy, Gopal K.; Lopez, Daniel; Wang, Jin

2017-08-01

Time-resolved synchrotron x-ray measurements often rely on using a mechanical chopper to isolate a set of x-ray pulses. We have started the development of micro electromechanical systems (MEMS)-based x-ray optics, as an alternate method to manipulate x-ray beams. In the application of x-ray pulse isolation, we recently achieved a pulse-picking time window of half a nanosecond, which is more than 100 times faster than mechanical choppers can achieve. The MEMS device consists of a comb-drive silicon micromirror, designed for efficiently diffracting an x-ray beam during oscillation. The MEMS devices were operated in Bragg geometry and their oscillation was synchronized to x-ray pulses, with a frequency matching subharmonics of the cycling frequency of x-ray pulses. The microscale structure of the silicon mirror in terms of the curvature and the quality of crystallinity ensures a narrow angular spread of the Bragg reflection. With the discussion of factors determining the diffractive time window, this report showed our approaches to narrow down the time window to half a nanosecond. The short diffractive time window will allow us to select single x-ray pulse out of a train of pulses from synchrotron radiation facilities.

Fabrication of high-resolution x-ray diffractive optics at King's College London

NASA Astrophysics Data System (ADS)

Charalambous, Pambos S.; Anastasi, Peter A. F.; Burge, Ronald E.; Popova, Katia

1995-09-01

The fabrication of high resolution x-ray diffractive optics, and Fresnel zone plates (ZPs) in particular, is a very demanding multifaceted technological task. The commissioning of more (and brighter) synchrotron radiation sources, has increased the number of x-ray imaging beam lines world wide. The availability of cheaper and more effective laboratory x-ray sources, has further increased the number of laboratories involved in x-ray imaging. The result is an ever increasing demand for x-ray optics with a very wide range of specifications, reflecting the particular type of x-ray imaging performed at different laboratories. We have been involved in all aspects of high resolution nanofabrication for a number of years, and we have explored many different methods of lithography, which, although unorthodox, open up possibilities, and increase our flexibility for the fabrication of different diffractive optical elements, as well as other types of nanostructures. The availability of brighter x-ray sources, means that the diffraction efficiency of the ZPs is becoming of secondary importance, a trend which will continue in the future. Resolution, however, is important and will always remain so. Resolution is directly related to the accuracy af pattern generation, as well as the ability to draw fine lines. This is the area towards which we have directed most of our efforts so far.

Influences of PZT addition on phase formation and magnetic properties of perovskite Pb(Fe0.5Nb0.5)O3-based ceramics

NASA Astrophysics Data System (ADS)

Amonpattaratkit, P.; Jantaratana, P.; Ananta, S.

2015-09-01

In this work, the investigation of phase formation, crystal structure, microstructure, microchemical composition and magnetic properties of perovskite (1-x)PFN-xPZT (x=0.1-0.5) multiferroic ceramics derived from a combination of perovskite stabilizer PZT and a wolframite-type FeNbO4 B-site precursor was carried out by using a combination of X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX) analyzer and vibrating sample magnetometer (VSM) techniques. The addition of PZT phase and its concentration have been found to have pronounced effects on the perovskite phase formation, densification, grain growth and magnetic properties of the sintered ceramics. XRD spectra from these ceramics reveal transformation of the (pseudo) cubic into the tetragonal perovskite structure. When increasing PZT content, the degree of perovskite phase formation and the tetragonality value of the ceramics increase gradually accompanied with the variation of cell volume, the M-H hysteresis loops, however, become narrower accompanied by the decrease of maximum magnetization (Mmax), remanent polarization (Mr), and coercive field (HC).

Structure and magnetic/electrochemical properties of Cu-doped BiFeO3 nanoparticles prepared by a simple solution method

NASA Astrophysics Data System (ADS)

Khajonrit, Jessada; Phumying, Santi; Maensiri, Santi

2016-06-01

BiFe1- x Cu x O3 (x = 0, 0.05, 0.1, 0.2, and 0.3) nanoparticles were prepared by a simple solution method. The prepared nanoparticles were characterized by X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM), Brunauer-Emmett-Teller (BET) method analysis using the Barret-Joyner-Halenda (BJH) model, and X-ray absorption spectroscopy (XAS). Magnetization properties were obtained using a vibrating sample magnetometer (VSM) at room temperature. Magnetization was clearly enhanced by increasing Cu content and decreasing particle size. Zero-field-cooled (ZFC) and field-cooled (FC) temperature-dependent magnetization measurements showed that blocking temperature increased with increasing Cu content. Electrochemical properties were investigated by cyclic voltammetry (CV) and the galvanostatic charge-discharge (GCD) method. The performance of the fabricated supercapacitor was improved for the BiFe0.95Cu0.05O3 electrode. The highest specific capacitance was 568.13 F g-1 at 1 A g-1 and the capacity retention was 77.13% after 500 cycles.

Development and characterization of Mn2+-doped MgO nanoparticles by solution combustion synthesis

NASA Astrophysics Data System (ADS)

Basha, Md. Hussain; Gopal, N. O.; Rao, J. L.; Nagabhushana, H.; Nagabhushana, B. M.; Chakradhar, R. P. S.

2015-06-01

Mn doped MgO Nanoparticles have been prepared by Solution Combustion Synthesis. The synthesized sample is characterized by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Electron Paramagnetic Resonance (EPR). The prepared MgO:Mn (1 mol%) nano crystals appear to be of simple cubic crystalline phase with lattice parameters a = 4.218(2) Å and cell volume = 74.98 (7) Å3. SEM micrograph of powders show highly porous, many agglomerates with irregular morphology, large voids, cracks and pores. EPR spectrum of the sample at room temperature exhibit an isotropic sextet hyperfine pattern, centered at g=1.99, characteristic if Mn2+ ions with S=I=5/2.The observed g value and the hyperfine value reveal the ionic bonding between Mn2+ and its surroundings.

Structural analysis of zeolite NaA synthesized by a cost-effective hydrothermal method using kaolin and its use as water softener.

PubMed

Loiola, A R; Andrade, J C R A; Sasaki, J M; da Silva, L R D

2012-02-01

Zeolite 4A (LTA) has been successfully synthesized by a hydrothermal method, where kaolin was used as silica and alumina source. The synthesized zeolite was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), laser granulometry, and FTIR spectroscopy. XRD data from the Rietveld refinement method confirmed only one crystallographic phase. Zeolite A morphology was observed by SEM analysis, and it showed well-defined crystals with slightly different sizes but with the same cubic shape. Particle size distribution of the crystals was confirmed by laser granulometry, whereas FTIR spectroscopy revealed significant structural differences between the starting material and the final zeolite product used as water softener. Copyright © 2010 Elsevier Inc. All rights reserved.

Hydroxyapatite nanocrystals: simple preparation, characterization and formation mechanism.

PubMed

Mohandes, Fatemeh; Salavati-Niasari, Masoud; Fathi, Mohammadhossein; Fereshteh, Zeinab

2014-12-01

Crystalline hydroxyapatite (HAP) nanoparticles and nanorods have been successfully synthesized via a simple precipitation method. To control the shape and particle size of HAP nanocrystals, coordination ligands derived from 2-hydroxy-1-naphthaldehyde were first prepared, characterized by Fourier transform infrared (FT-IR) and proton nuclear magnetic resonance ((1)H-NMR) spectroscopies, and finally applied in the synthesis process of HAP. On the other hand, the HAP nanocrystals were also characterized by several techniques including powder X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). According to the FE-SEM and TEM micrographs, it was found that the morphology and crystallinity of the HAP powders depended on the coordination mode of the ligands. Copyright © 2014 Elsevier B.V. All rights reserved.

Phase study and surface morphology of beta-alumina

NASA Astrophysics Data System (ADS)

Tak, S. K.

2018-05-01

Beta alumina ceramic is well known as a polycrystalline ceramic material. The characteristic crystal structure of beta-alumina makes it useful as a separator in sodium sulphur batteries and other electrochemical devices requiring the passage of sodium ions. β"-alumina powders for this study were prepared by zeta process. The pellets were sintered at different microwave power levels and power schedule to optimize the sintering conditions to obtain preferred β" phase with improved microstructure. Phase identification was studied by X-ray diffraction (XRD). XRD analysis shows increase in β'' phase as the sintering temperature was increased from 1400°C to 1600°C. Surface morphology of the pellets was carried out by Scanning Electron microscopy (SEM). SEM studies revealed the formation and growth of platelet grains with interconnected porosity.

Development of regenerated cellulose/halloysites nanocomposites via ionic liquids.

PubMed

Hanid, Nurbaiti Abdul; Wahit, Mat Uzir; Guo, Qipeng; Mahmoodian, Shaya; Soheilmoghaddam, Mohammad

2014-01-01

In this study, regenerated cellulose/halloysites (RC/HNT) nanocomposites with different nanofillers loading were fabricated by dissolving the cellulose in 1-ethyl-3-methylimidazolium chloride (EMIMCl) ionic liquid. The films were prepared via solution casting method and were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The mechanical properties were investigated by tensile testing. It clearly displayed a good enhancement of both tensile strength and Young's modulus with HNT loading up to 5 wt%. As the HNT loadings increased to 5 wt%, the thermal behaviour and water resistance rate was also increased. The TEM and SEM images also depicted even dispersion of the HNT and a good intertubular interaction between the HNT and the cellulose matrix. Copyright © 2013 Elsevier Ltd. All rights reserved.

Synthesis and Thermal and Photo Behaviors of New Polyamide/Organocaly Nanocomposites Containing Para Phenylenediacrylic Moiety

NASA Astrophysics Data System (ADS)

Faghihi, Khalil; Soleimani, Masoumeh; Shabanian, Meisam; Abootalebi, Ashraf Sadat

2011-06-01

New type of aromatic polyamide/montmorillonite nanocomposites were produced using solution process in N-methyl-2-pyrolidone. Amide chains were synthesized from 4,4'-diaminodiphenyl sulfone and p-phenylenediacrylic acid in N-methyl-2-pyrolidone. The resulting nanocomposite films containing 5-15 mass % of organoclay were characterized for FT-IR, scanning electronmicroscopy (SEM), X-ray diffraction (XRD), thermogravimetric analysis (TGA), optical transparency and water absorption measurements. The distribution of organoclay and nanostructure of the composites were investigated by (XRD) and SEM analyses. Thermogravimetric analysis indicated an increase in thermal stability of nanocomposites as compared to pristine polyamide. The percentage optical transparency and water absorption of these hybrids was found to be much reduced upon the addition of modified layered silicate indicating decreased permeability.